#------------------------------------------------------------------------------
#$Date: 2020-07-31 04:13:22 +0300 (Fri, 31 Jul 2020) $
#$Revision: 254693 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/87/1558716.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1558716
loop_
_publ_author_name
'McMonagle, Charlie'
'Comar, Priyanka'
'Nichol, Gary Stephen'
'Allan, David Robert'
'Barreda-Argūeso, José A'
'Gonzalez, Jesus Antonio'
'Rodriguez, Fernando'
'Valiente, Rafael'
'Turner, Gemma'
'Brechin, Euan K.'
'Moggach, Stephen A.'
_publ_section_title
;
 Pressure-and Temperature Induced Phase Transitions, Piezochromism, NLC
 Behaviour and Pressure Controlled Jahn-Teller Switching in a Cu-based
 Framework
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03229H
_journal_year                    2020
_chemical_formula_moiety         'C54 H48 Cu3 N6 O12, C4 H10 O'
_chemical_formula_sum            'C58 H58 Cu3 N6 O13'
_chemical_formula_weight         1237.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-12-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                116.604(6)
_cell_angle_beta                 100.395(4)
_cell_angle_gamma                98.422(4)
_cell_formula_units_Z            1
_cell_length_a                   7.7799(3)
_cell_length_b                   15.1586(9)
_cell_length_c                   15.4901(9)
_cell_measurement_reflns_used    9584
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      76.4050
_cell_measurement_theta_min      5.7750
_cell_volume                     1551.99(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -37.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 121

#__ type_ start__ end____ width___ exp.time_
  2 omega  -95.00  -34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -30.0000 61

#__ type_ start__ end____ width___ exp.time_
  3 omega  -37.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 121

#__ type_ start__ end____ width___ exp.time_
  4 omega  -50.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000   38.0000  -30.0000 75

#__ type_ start__ end____ width___ exp.time_
  5 omega  -96.00   -2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  125.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
  6 omega -148.00  -79.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -99.0000   30.0000 69

#__ type_ start__ end____ width___ exp.time_
  7 omega  -50.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000   38.0000   90.0000 75

#__ type_ start__ end____ width___ exp.time_
  8 omega -143.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -38.0000  -60.0000 121

#__ type_ start__ end____ width___ exp.time_
  9 omega   94.00  143.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  125.0000 -120.0000 49

#__ type_ start__ end____ width___ exp.time_
 10 omega    1.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  -99.0000  -30.0000 105

#__ type_ start__ end____ width___ exp.time_
 11 omega   34.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -38.0000   60.0000 59

#__ type_ start__ end____ width___ exp.time_
 12 omega  100.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000 -180.0000 78

#__ type_ start__ end____ width___ exp.time_
 13 omega  100.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000   30.0000 78

#__ type_ start__ end____ width___ exp.time_
 14 omega   57.00  150.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000  -60.0000 93

#__ type_ start__ end____ width___ exp.time_
 15 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  -90.0000 84

#__ type_ start__ end____ width___ exp.time_
 16 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
 17 omega   57.00  150.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000 -180.0000 93

#__ type_ start__ end____ width___ exp.time_
 18 omega  100.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000  150.0000 78

#__ type_ start__ end____ width___ exp.time_
 19 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
 20 omega  100.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000   90.0000 78

#__ type_ start__ end____ width___ exp.time_
 21 omega   81.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   63.0000  150.0000 97

#__ type_ start__ end____ width___ exp.time_
 22 omega   33.00  155.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -63.0000   60.0000 122

#__ type_ start__ end____ width___ exp.time_
 23 omega   34.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -38.0000 -150.0000 59

#__ type_ start__ end____ width___ exp.time_
 24 omega   34.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -38.0000  150.0000 59

#__ type_ start__ end____ width___ exp.time_
 25 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
 26 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  120.0000 84

#__ type_ start__ end____ width___ exp.time_
 27 omega   63.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   25.0000  -90.0000 115

#__ type_ start__ end____ width___ exp.time_
 28 omega   34.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -38.0000  -60.0000 59

#__ type_ start__ end____ width___ exp.time_
 29 omega   32.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  150.0000 84

#__ type_ start__ end____ width___ exp.time_
 30 omega    1.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   60.0000 46

#__ type_ start__ end____ width___ exp.time_
 31 omega    1.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   30.0000 46

#__ type_ start__ end____ width___ exp.time_
 32 omega  -39.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000    0.0000 131

#__ type_ start__ end____ width___ exp.time_
 33 omega -151.00  -20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -77.0000  -90.0000 131

#__ type_ start__ end____ width___ exp.time_
 34 omega -143.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -57.0000 -180.0000 121

#__ type_ start__ end____ width___ exp.time_
 35 omega -143.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -57.0000  120.0000 121

#__ type_ start__ end____ width___ exp.time_
 36 omega -151.00  -20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -77.0000   60.0000 131

#__ type_ start__ end____ width___ exp.time_
 37 omega -151.00  -20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -77.0000    0.0000 131

#__ type_ start__ end____ width___ exp.time_
 38 omega -143.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -57.0000   60.0000 121

#__ type_ start__ end____ width___ exp.time_
 39 omega -151.00  -75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -77.0000 -150.0000 76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0305141000
_diffrn_orient_matrix_UB_12      0.0679958000
_diffrn_orient_matrix_UB_13      -0.0483282000
_diffrn_orient_matrix_UB_21      -0.0709540000
_diffrn_orient_matrix_UB_22      -0.0957698000
_diffrn_orient_matrix_UB_23      -0.1046274000
_diffrn_orient_matrix_UB_31      -0.1935574000
_diffrn_orient_matrix_UB_32      -0.0083973000
_diffrn_orient_matrix_UB_33      0.0112142000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20345
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         76.540
_diffrn_reflns_theta_min         3.322
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       rod
_exptl_crystal_F_000             639
_exptl_crystal_recrystallization_method
'The material was recrystallised from diethyl ether by slow evaporation'
_exptl_crystal_size_max          0.1991
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.0449
_refine_diff_density_max         1.505
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5968
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1433P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4475
_reflns_number_total             5968
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03229h2.cif
_cod_data_source_block           CuPyrIII
_cod_original_cell_volume        1551.99(15)
_cod_database_code               1558716
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cu Gd'
_chemical_oxdiff_usercomment     '@ 200 K PC1469'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O7, C28, C30, C29, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O7(0.5) C28(0.5) H28A(0.5) H28B(0.5) C30(0.5) H30A(0.5) H30B(0.5)
 C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C30(H30A,H30B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 15/12/14
_olex2_date_sample_submission    15/12/14
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id PC1469
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 1.0000 1.0000 0.0304(2) Uani 1 2 d S T P . .
Cu2 Cu -0.5000 0.5000 0.5000 0.0301(2) Uani 1 2 d S T P . .
Cu3 Cu -1.0000 0.5000 1.0000 0.0286(2) Uani 1 2 d S T P . .
O1 O 0.3909(4) 1.11057(19) 1.0055(2) 0.0339(5) Uani 1 1 d . . . . .
O2 O 0.6116(4) 0.9971(2) 0.8932(2) 0.0393(6) Uani 1 1 d . . . . .
O3 O -0.2896(3) 0.6004(2) 0.61108(18) 0.0345(6) Uani 1 1 d . . . . .
O4 O -0.6199(4) 0.6076(2) 0.5013(2) 0.0397(6) Uani 1 1 d . . . . .
O5 O -0.9043(4) 0.5058(2) 0.89402(19) 0.0346(6) Uani 1 1 d . . . . .
O6 O -1.2445(4) 0.3812(2) 0.8851(2) 0.0438(7) Uani 1 1 d . . . . .
N1 N 0.1410(4) 1.3913(3) 0.9970(3) 0.0358(7) Uani 1 1 d . . . . .
N2 N 0.2291(4) 0.8776(3) 0.8823(3) 0.0397(8) Uani 1 1 d . . . . .
N3 N -0.6552(4) 0.4953(3) 0.6172(3) 0.0403(8) Uani 1 1 d . . . . .
C1 C 0.0802(6) 1.3137(3) 1.0104(4) 0.0439(9) Uani 1 1 d . . . . .
H1 H -0.0321 1.3078 1.0260 0.053 Uiso 1 1 calc R . . . .
C2 C 0.1738(6) 1.2401(4) 1.0026(4) 0.0454(10) Uani 1 1 d . . . . .
H2 H 0.1252 1.1852 1.0126 0.054 Uiso 1 1 calc R . . . .
C3 C 0.3387(5) 1.2472(3) 0.9800(3) 0.0349(8) Uani 1 1 d . . . . .
C4 C 0.4039(5) 1.3304(3) 0.9685(3) 0.0386(8) Uani 1 1 d . . . . .
H4 H 0.5171 1.3392 0.9544 0.046 Uiso 1 1 calc R . . . .
C5 C 0.3029(5) 1.4003(3) 0.9778(3) 0.0381(8) Uani 1 1 d . . . . .
H5 H 0.3497 1.4572 0.9704 0.046 Uiso 1 1 calc R . . . .
C6 C 0.4345(5) 1.1651(3) 0.9658(3) 0.0352(8) Uani 1 1 d . . . . .
C7 C 0.5564(7) 1.1522(4) 0.9075(4) 0.0488(11) Uani 1 1 d . . . . .
H7 H 0.5919 1.2043 0.8912 0.059 Uiso 1 1 calc R . . . .
C8 C 0.6301(6) 1.0673(3) 0.8713(3) 0.0425(9) Uani 1 1 d . . . . .
C9 C 0.7389(9) 1.0602(5) 0.7984(5) 0.0667(16) Uani 1 1 d . . . . .
H9A H 0.8477 1.0392 0.8153 0.100 Uiso 1 1 calc GR . . . .
H9B H 0.7740 1.1270 0.8024 0.100 Uiso 1 1 calc GR . . . .
H9C H 0.6658 1.0098 0.7300 0.100 Uiso 1 1 calc GR . . . .
C10 C 0.0787(5) 0.9082(3) 0.8912(3) 0.0409(9) Uani 1 1 d . . . . .
H10 H 0.0887 0.9733 0.9458 0.049 Uiso 1 1 calc R . . . .
C11 C -0.0901(5) 0.8521(3) 0.8270(3) 0.0388(8) Uani 1 1 d . . . . .
H11 H -0.1928 0.8781 0.8378 0.047 Uiso 1 1 calc R . . . .
C12 C -0.1091(5) 0.7566(3) 0.7457(3) 0.0343(8) Uani 1 1 d . . . . .
C13 C 0.0488(6) 0.7239(3) 0.7374(3) 0.0496(11) Uani 1 1 d . . . . .
H13 H 0.0436 0.6588 0.6842 0.059 Uiso 1 1 calc R . . . .
C14 C 0.2119(6) 0.7859(4) 0.8061(4) 0.0518(12) Uani 1 1 d . . . . .
H14 H 0.3173 0.7619 0.7987 0.062 Uiso 1 1 calc R . . . .
C15 C -0.2840(5) 0.6934(3) 0.6661(3) 0.0352(8) Uani 1 1 d . . . . .
C16 C -0.4193(6) 0.7413(3) 0.6558(4) 0.0512(11) Uani 1 1 d . . . . .
H16 H -0.4069 0.8078 0.7088 0.061 Uiso 1 1 calc R . . . .
C17 C -0.5730(5) 0.6989(3) 0.5730(3) 0.0447(9) Uani 1 1 d . . . . .
C18 C -0.6931(8) 0.7660(4) 0.5660(5) 0.0697(16) Uani 1 1 d . . . . .
H18A H -0.6966 0.7708 0.5047 0.104 Uiso 1 1 calc GR . . . .
H18B H -0.6454 0.8344 0.6248 0.104 Uiso 1 1 calc GR . . . .
H18C H -0.8157 0.7367 0.5640 0.104 Uiso 1 1 calc GR . . . .
C19 C -0.5849(6) 0.5149(4) 0.7099(3) 0.0512(11) Uani 1 1 d . . . . .
H19 H -0.4570 0.5359 0.7358 0.061 Uiso 1 1 calc R . . . .
C20 C -0.6887(6) 0.5066(4) 0.7725(3) 0.0526(12) Uani 1 1 d . . . . .
H20 H -0.6321 0.5190 0.8380 0.063 Uiso 1 1 calc R . . . .
C21 C -0.8753(5) 0.4798(3) 0.7365(3) 0.0351(8) Uani 1 1 d . . . . .
C22 C -0.9505(5) 0.4610(3) 0.6400(3) 0.0386(8) Uani 1 1 d . . . . .
H22 H -1.0780 0.4420 0.6126 0.046 Uiso 1 1 calc R . . . .
C23 C -0.8362(5) 0.4704(4) 0.5840(3) 0.0414(9) Uani 1 1 d . . . . .
H23 H -0.8890 0.4586 0.5182 0.050 Uiso 1 1 calc R . . . .
C24 C -0.9879(5) 0.4641(3) 0.8006(3) 0.0352(8) Uani 1 1 d . . . . .
C25 C -1.1636(6) 0.4037(4) 0.7536(3) 0.0520(12) Uani 1 1 d . . . . .
H25 H -1.2119 0.3873 0.6857 0.062 Uiso 1 1 calc R . . . .
C26 C -1.2804(6) 0.3634(4) 0.7962(3) 0.0461(10) Uani 1 1 d . . . . .
C27 C -1.4572(8) 0.2904(5) 0.7269(4) 0.0754(18) Uani 1 1 d . . . . .
H27A H -1.4433 0.2206 0.6979 0.113 Uiso 1 1 calc GR . . . .
H27B H -1.4967 0.3063 0.6729 0.113 Uiso 1 1 calc GR . . . .
H27C H -1.5477 0.2966 0.7644 0.113 Uiso 1 1 calc GR . . . .
O7 O -0.0556(15) 1.0179(8) 0.6178(8) 0.088(3) Uani 0.5 1 d . U . . .
C28 C -0.002(2) 0.9310(12) 0.6114(13) 0.088(4) Uani 0.5 1 d . U . . .
H28A H 0.0167 0.9325 0.6770 0.105 Uiso 0.5 1 calc R . . . .
H28B H 0.1134 0.9291 0.5927 0.105 Uiso 0.5 1 calc R . . . .
C30 C 0.0930(19) 1.1054(11) 0.6847(11) 0.080(3) Uani 0.5 1 d . U . . .
H30A H 0.1317 1.1077 0.7503 0.096 Uiso 0.5 1 calc R . . . .
H30B H 0.1970 1.1027 0.6558 0.096 Uiso 0.5 1 calc R . . . .
C29 C -0.148(2) 0.8394(13) 0.5331(14) 0.100(4) Uani 0.5 1 d . U . . .
H29A H -0.1370 0.8248 0.4662 0.150 Uiso 0.5 1 calc GR . . . .
H29B H -0.2662 0.8527 0.5389 0.150 Uiso 0.5 1 calc GR . . . .
H29C H -0.1374 0.7806 0.5426 0.150 Uiso 0.5 1 calc GR . . . .
C31 C 0.034(2) 1.1881(12) 0.6963(14) 0.098(5) Uani 0.5 1 d . U . . .
H31A H -0.0001 1.1859 0.6312 0.148 Uiso 0.5 1 calc GR . . . .
H31B H 0.1308 1.2500 0.7434 0.148 Uiso 0.5 1 calc GR . . . .
H31C H -0.0711 1.1886 0.7228 0.148 Uiso 0.5 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -8 9 0.0100 0.0577 -7.9099 8.9297 -0.9712 -0.1809 0.1554
0 -5 1 0.0283 -0.0001 -4.9954 1.4978 -0.4121 0.3217 0.0588
0 -3 -7 0.0346 0.1708 -2.9172 -6.8875 0.1293 0.9879 -0.0858
5 0 -4 0.0869 4.9640 -0.2488 -3.5833 0.0048 0.0465 -0.9989
0 3 7 0.0098 0.3026 2.9172 6.6009 -0.1299 -0.9915 -0.0091
-5 -1 0 0.0917 -4.6631 -1.0727 0.3280 0.0535 0.3993 0.9153
-1 8 -9 0.0263 -0.5753 8.0070 -8.6850 0.9817 0.1827 -0.0533
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 . 2_677 ?
O1 Cu1 O2 87.18(11) 2_677 . ?
O1 Cu1 O2 92.82(11) . . ?
O1 Cu1 O2 92.82(11) 2_677 2_677 ?
O1 Cu1 O2 87.18(11) . 2_677 ?
O1 Cu1 N2 90.04(12) . 2_677 ?
O1 Cu1 N2 90.04(12) 2_677 . ?
O1 Cu1 N2 89.96(12) 2_677 2_677 ?
O1 Cu1 N2 89.96(12) . . ?
O2 Cu1 O2 180.0 2_677 . ?
O2 Cu1 N2 93.21(12) 2_677 2_677 ?
O2 Cu1 N2 86.79(12) 2_677 . ?
O2 Cu1 N2 93.21(12) . . ?
O2 Cu1 N2 86.79(12) . 2_677 ?
N2 Cu1 N2 180.0 2_677 . ?
O3 Cu2 O3 180.00(12) . 2_466 ?
O3 Cu2 O4 87.35(11) 2_466 . ?
O3 Cu2 O4 92.64(11) . . ?
O3 Cu2 O4 87.36(11) . 2_466 ?
O3 Cu2 O4 92.65(11) 2_466 2_466 ?
O3 Cu2 N3 89.78(11) 2_466 . ?
O3 Cu2 N3 90.22(11) . . ?
O3 Cu2 N3 89.78(11) . 2_466 ?
O3 Cu2 N3 90.22(11) 2_466 2_466 ?
O4 Cu2 O4 180.0 2_466 . ?
O4 Cu2 N3 86.23(12) . . ?
O4 Cu2 N3 93.77(12) 2_466 . ?
O4 Cu2 N3 93.76(12) . 2_466 ?
O4 Cu2 N3 86.23(12) 2_466 2_466 ?
N3 Cu2 N3 180.0 . 2_466 ?
O5 Cu3 O5 180.00(6) 2_367 . ?
O5 Cu3 O6 90.13(11) . . ?
O5 Cu3 O6 89.87(11) 2_367 . ?
O5 Cu3 O6 90.13(11) 2_367 2_367 ?
O5 Cu3 O6 89.87(11) . 2_367 ?
O5 Cu3 N1 89.53(12) . 1_445 ?
O5 Cu3 N1 89.53(12) 2_367 2_477 ?
O5 Cu3 N1 90.47(12) . 2_477 ?
O5 Cu3 N1 90.47(12) 2_367 1_445 ?
O6 Cu3 O6 180.0 2_367 . ?
N1 Cu3 O6 87.29(13) 1_445 2_367 ?
N1 Cu3 O6 92.71(13) 2_477 2_367 ?
N1 Cu3 O6 92.70(13) 1_445 . ?
N1 Cu3 O6 87.30(13) 2_477 . ?
N1 Cu3 N1 180.0(2) 2_477 1_445 ?
C6 O1 Cu1 123.9(2) . . ?
C8 O2 Cu1 123.8(2) . . ?
C15 O3 Cu2 124.3(3) . . ?
C17 O4 Cu2 123.8(3) . . ?
C24 O5 Cu3 127.1(2) . . ?
C26 O6 Cu3 121.1(3) . . ?
C1 N1 Cu3 124.5(3) . 1_665 ?
C1 N1 C5 117.9(3) . . ?
C5 N1 Cu3 117.6(3) . 1_665 ?
C10 N2 Cu1 115.1(3) . . ?
C14 N2 Cu1 127.9(3) . . ?
C14 N2 C10 116.8(4) . . ?
C19 N3 Cu2 127.9(3) . . ?
C19 N3 C23 117.0(3) . . ?
C23 N3 Cu2 115.1(3) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.7(4) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 C6 119.8(4) . . ?
C4 C3 C2 117.2(4) . . ?
C4 C3 C6 122.9(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 123.0(4) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
O1 C6 C3 116.0(3) . . ?
O1 C6 C7 126.1(4) . . ?
C7 C6 C3 117.9(4) . . ?
C6 C7 H7 117.8 . . ?
C6 C7 C8 124.5(4) . . ?
C8 C7 H7 117.8 . . ?
O2 C8 C7 126.0(4) . . ?
O2 C8 C9 117.3(4) . . ?
C7 C8 C9 116.6(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10 117.8 . . ?
N2 C10 C11 124.5(4) . . ?
C11 C10 H10 117.8 . . ?
C10 C11 H11 120.4 . . ?
C10 C11 C12 119.1(4) . . ?
C12 C11 H11 120.4 . . ?
C11 C12 C13 116.3(4) . . ?
C11 C12 C15 123.4(3) . . ?
C13 C12 C15 120.2(3) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13 120.0 . . ?
N2 C14 C13 123.2(4) . . ?
N2 C14 H14 118.4 . . ?
C13 C14 H14 118.4 . . ?
O3 C15 C12 115.3(3) . . ?
O3 C15 C16 126.2(4) . . ?
C16 C15 C12 118.4(4) . . ?
C15 C16 H16 117.5 . . ?
C15 C16 C17 125.0(4) . . ?
C17 C16 H16 117.5 . . ?
O4 C17 C16 125.5(4) . . ?
O4 C17 C18 116.0(4) . . ?
C16 C17 C18 118.5(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19 118.2 . . ?
N3 C19 C20 123.7(4) . . ?
C20 C19 H19 118.2 . . ?
C19 C20 H20 120.8 . . ?
C21 C20 C19 118.4(4) . . ?
C21 C20 H20 120.8 . . ?
C20 C21 C24 118.8(3) . . ?
C22 C21 C20 118.4(3) . . ?
C22 C21 C24 122.7(3) . . ?
C21 C22 H22 120.7 . . ?
C21 C22 C23 118.7(4) . . ?
C23 C22 H22 120.7 . . ?
N3 C23 C22 123.8(4) . . ?
N3 C23 H23 118.1 . . ?
C22 C23 H23 118.1 . . ?
O5 C24 C21 114.7(3) . . ?
O5 C24 C25 127.1(3) . . ?
C25 C24 C21 118.1(3) . . ?
C24 C25 H25 116.6 . . ?
C24 C25 C26 126.9(4) . . ?
C26 C25 H25 116.6 . . ?
O6 C26 C25 125.7(4) . . ?
O6 C26 C27 117.3(4) . . ?
C25 C26 C27 116.9(4) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C28 O7 C30 107.6(12) . . ?
O7 C28 H28A 110.2 . . ?
O7 C28 H28B 110.2 . . ?
O7 C28 C29 107.4(13) . . ?
H28A C28 H28B 108.5 . . ?
C29 C28 H28A 110.2 . . ?
C29 C28 H28B 110.2 . . ?
O7 C30 H30A 110.4 . . ?
O7 C30 H30B 110.4 . . ?
H30A C30 H30B 108.6 . . ?
C31 C30 O7 106.7(13) . . ?
C31 C30 H30A 110.4 . . ?
C31 C30 H30B 110.4 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.963(3) . ?
Cu1 O1 1.963(3) 2_677 ?
Cu1 O2 1.989(3) 2_677 ?
Cu1 O2 1.989(3) . ?
Cu1 N2 2.376(3) 2_677 ?
Cu1 N2 2.376(3) . ?
Cu2 O3 1.966(3) . ?
Cu2 O3 1.966(3) 2_466 ?
Cu2 O4 1.988(3) 2_466 ?
Cu2 O4 1.988(3) . ?
Cu2 N3 2.375(3) . ?
Cu2 N3 2.375(3) 2_466 ?
Cu3 O5 1.952(2) 2_367 ?
Cu3 O5 1.952(2) . ?
Cu3 O6 2.221(3) 2_367 ?
Cu3 O6 2.221(3) . ?
Cu3 N1 2.097(3) 1_445 ?
Cu3 N1 2.097(3) 2_477 ?
O1 C6 1.274(5) . ?
O2 C8 1.251(5) . ?
O3 C15 1.268(5) . ?
O4 C17 1.270(5) . ?
O5 C24 1.279(5) . ?
O6 C26 1.246(5) . ?
N1 Cu3 2.097(3) 1_665 ?
N1 C1 1.320(5) . ?
N1 C5 1.347(5) . ?
N2 C10 1.328(5) . ?
N2 C14 1.327(5) . ?
N3 C19 1.317(6) . ?
N3 C23 1.341(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.393(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.391(5) . ?
C3 C4 1.388(6) . ?
C3 C6 1.496(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.381(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.400(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.409(6) . ?
C8 C9 1.504(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 0.9500 . ?
C10 C11 1.372(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.393(5) . ?
C12 C13 1.396(5) . ?
C12 C15 1.498(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.376(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.404(6) . ?
C17 C18 1.504(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19 0.9500 . ?
C19 C20 1.404(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.384(6) . ?
C21 C22 1.383(5) . ?
C21 C24 1.509(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.384(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(6) . ?
C25 H25 0.9500 . ?
C25 C26 1.433(5) . ?
C26 C27 1.492(7) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
O7 C28 1.409(16) . ?
O7 C30 1.434(17) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.49(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.34(2) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C6 C3 -178.7(2) . . . . ?
Cu1 O1 C6 C7 4.1(6) . . . . ?
Cu1 O2 C8 C7 -8.7(7) . . . . ?
Cu1 O2 C8 C9 172.1(4) . . . . ?
Cu1 N2 C10 C11 175.5(4) . . . . ?
Cu1 N2 C14 C13 -174.7(4) . . . . ?
Cu2 O3 C15 C12 -179.3(2) . . . . ?
Cu2 O3 C15 C16 -2.8(6) . . . . ?
Cu2 O4 C17 C16 7.8(7) . . . . ?
Cu2 O4 C17 C18 -173.1(4) . . . . ?
Cu2 N3 C19 C20 -177.7(4) . . . . ?
Cu2 N3 C23 C22 178.2(4) . . . . ?
Cu3 O5 C24 C21 -178.2(2) . . . . ?
Cu3 O5 C24 C25 -1.4(6) . . . . ?
Cu3 O6 C26 C25 9.2(7) . . . . ?
Cu3 O6 C26 C27 -173.6(4) . . . . ?
Cu3 N1 C1 C2 176.5(4) 1_665 . . . ?
Cu3 N1 C5 C4 -176.4(3) 1_665 . . . ?
O1 C6 C7 C8 9.9(8) . . . . ?
O3 C15 C16 C17 -10.8(8) . . . . ?
O5 C24 C25 C26 -9.6(8) . . . . ?
N1 C1 C2 C3 0.2(8) . . . . ?
N2 C10 C11 C12 -0.5(7) . . . . ?
N3 C19 C20 C21 -2.4(9) . . . . ?
C1 N1 C5 C4 2.1(7) . . . . ?
C1 C2 C3 C4 1.4(7) . . . . ?
C1 C2 C3 C6 -176.6(4) . . . . ?
C2 C3 C4 C5 -1.2(6) . . . . ?
C2 C3 C6 O1 -21.5(6) . . . . ?
C2 C3 C6 C7 155.9(5) . . . . ?
C3 C4 C5 N1 -0.5(7) . . . . ?
C3 C6 C7 C8 -167.2(4) . . . . ?
C4 C3 C6 O1 160.6(4) . . . . ?
C4 C3 C6 C7 -22.0(6) . . . . ?
C5 N1 C1 C2 -1.9(7) . . . . ?
C6 C3 C4 C5 176.7(4) . . . . ?
C6 C7 C8 O2 -7.2(8) . . . . ?
C6 C7 C8 C9 172.0(5) . . . . ?
C10 N2 C14 C13 0.9(8) . . . . ?
C10 C11 C12 C13 1.4(7) . . . . ?
C10 C11 C12 C15 -174.4(4) . . . . ?
C11 C12 C13 C14 -1.3(8) . . . . ?
C11 C12 C15 O3 -164.6(4) . . . . ?
C11 C12 C15 C16 18.6(6) . . . . ?
C12 C13 C14 N2 0.1(9) . . . . ?
C12 C15 C16 C17 165.6(5) . . . . ?
C13 C12 C15 O3 19.7(6) . . . . ?
C13 C12 C15 C16 -157.1(5) . . . . ?
C14 N2 C10 C11 -0.7(7) . . . . ?
C15 C12 C13 C14 174.7(5) . . . . ?
C15 C16 C17 O4 7.9(9) . . . . ?
C15 C16 C17 C18 -171.2(5) . . . . ?
C19 N3 C23 C22 -2.4(7) . . . . ?
C19 C20 C21 C22 1.0(8) . . . . ?
C19 C20 C21 C24 176.1(4) . . . . ?
C20 C21 C22 C23 -0.5(7) . . . . ?
C20 C21 C24 O5 20.1(6) . . . . ?
C20 C21 C24 C25 -157.0(5) . . . . ?
C21 C22 C23 N3 1.2(7) . . . . ?
C21 C24 C25 C26 167.2(5) . . . . ?
C22 C21 C24 O5 -165.0(4) . . . . ?
C22 C21 C24 C25 17.9(6) . . . . ?
C23 N3 C19 C20 3.0(8) . . . . ?
C24 C21 C22 C23 -175.4(4) . . . . ?
C24 C25 C26 O6 4.1(9) . . . . ?
C24 C25 C26 C27 -173.2(5) . . . . ?
C28 O7 C30 C31 -175.1(12) . . . . ?
C30 O7 C28 C29 -173.7(11) . . . . ?
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.5790 12952 12013
2 0.4210 0 12013
