#------------------------------------------------------------------------------
#$Date: 2020-04-04 07:12:49 +0300 (Sat, 04 Apr 2020) $
#$Revision: 250066 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/45/4134521.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_4134521
loop_
_publ_author_name
'Zhan, Shun-Ze'
'Zhang, Guo-Hui'
'Li, Jing-Hong'
'Liu, Jia-Li'
'Zhu, Si-Hui'
'Lu, Weigang'
'Zheng, Ji'
'Ng, Seik Weng'
'Li, Dan'
_publ_section_title
;
 Exohedral Cuprofullerene: Sequentially Expanding Metal Olefin Up to a
 C₆₀@Cu₂₄ Rhombicuboctahedron.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5943
_journal_page_last               5947
_journal_paper_doi               10.1021/jacs.0c00090
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C150 H120 Cu24 O72, 3(C20 H14 Cl2)'
_chemical_formula_sum            'C210 H162 Cl6 Cu24 O72'
_chemical_formula_weight         5575.05
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   25.6664(6)
_cell_length_b                   25.6664(6)
_cell_length_c                   24.6267(9)
_cell_measurement_reflns_used    9249
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      73.7100
_cell_measurement_theta_min      3.4250
_cell_volume                     14049.7(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -48.00  15.00   0.50   10.00    --    0.00 -38.00  60.00  126
  2  ω    -84.00 -59.00   0.50   10.00    --    0.00 -38.00  60.00   50
  3  ω     33.00  58.00   0.50   10.00    --    0.00  27.00 -91.00   50
  4  ω     14.00 112.00   0.50   60.00    --   95.80 -30.00 -90.00  196
  5  ω    139.00 179.00   0.50   60.00    --   95.80  15.00 -30.00   80
  6  ω     72.00 102.00   0.50   60.00    --   95.80  15.00 -30.00   60
  7  ω      9.00 111.00   0.50   60.00    --   95.80 -27.00 106.00  204
  8  ω    150.00 176.00   0.50   60.00    --   95.80  15.00  90.00   52
  9  ω     85.00 130.00   0.50   60.00    --   95.80  15.00  90.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0672352000
_diffrn_orient_matrix_UB_12      -0.0247037000
_diffrn_orient_matrix_UB_13      -0.0119109000
_diffrn_orient_matrix_UB_21      0.0117125000
_diffrn_orient_matrix_UB_22      -0.0030851000
_diffrn_orient_matrix_UB_23      -0.0609534000
_diffrn_orient_matrix_UB_31      -0.0120483000
_diffrn_orient_matrix_UB_32      -0.0647104000
_diffrn_orient_matrix_UB_33      0.0075112000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15603
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.216
_diffrn_reflns_theta_min         3.444
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.475
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_description       block
_exptl_crystal_F_000             8388
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.032
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         6122
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0904P)²+135.6152P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5451
_reflns_number_total             6122
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c00090_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4134518--4134521.cif.'
_cod_original_cell_volume        14049.7(8)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4134521
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H O Cu'
_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.
;
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 O(H) groups
2. Restrained distances
 C19-C20
 1.3 with sigma of 0.02
 O8'-O7
 2.2 with sigma of 0.02
 O8'-C20
 1.2 with sigma of 0.02
 Cl1'-C29
 1.5 with sigma of 0.02
 C28-Cl1'
 2.6 with sigma of 0.02
 C30-Cl1'
 2.6 with sigma of 0.02
3. Rigid bond restraints
 C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C19') \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O8') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl1') \\sim Ueq, Uanis(Cl1') \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Others
 Fixed Sof: O6(0.6) H6(0.6) O6'(0.4) H6'(0.4) O8(0.6) H8(0.6) O8'(0.4)
 H8'(0.4) C16(0.6) C16'(0.4) C17(0.6) H17A(0.6) H17B(0.6) C17'(0.4) H17C(0.4)
 H17D(0.4) C18(0.6) H18A(0.6) H18B(0.6) C18'(0.4) H18C(0.4) H18D(0.4) C19(0.6)
 H19A(0.6) H19B(0.6) C19'(0.4) H19C(0.4) H19D(0.4) Cl1(0.5) Cl1'(0.5) H26(0.5)
 H29(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B), C17'(H17C,
 H17D), C18(H18A,H18B), C18'(H18C,H18D), C19(H19A,H19B), C19'(H19C,H19D),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C29(H29), C28(H28), C27(H27), C31(H31), C32(H32), C33(H33), C34(H34)
6.c Fitted hexagon refined as free rotating group:
 C26(C35,C30,C29,C28,C27)
6.d Idealised tetrahedral OH refined as rotating group:
 O6(H6), O6'(H6'), O8(H8), O8'(H8')
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.732
_oxdiff_exptl_absorpt_empirical_full_min 0.635
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.58663(3) 0.31407(3) 0.53990(2) 0.02003(17) Uani 1 1 d . . . . .
Cu2 Cu 0.46709(2) 0.20942(3) 0.45703(2) 0.02006(17) Uani 1 1 d . . . . .
Cu3 Cu 0.43234(2) 0.15718(2) 0.33509(2) 0.02052(17) Uani 1 1 d . . . . .
Cu4 Cu 0.44688(2) 0.27536(3) 0.25276(2) 0.02099(17) Uani 1 1 d . . . . .
O1 O 0.55708(14) 0.25088(14) 0.59455(13) 0.0285(7) Uani 1 1 d . . . . .
O2 O 0.61970(14) 0.21505(15) 0.58736(15) 0.0350(8) Uani 1 1 d . . . . .
O3 O 0.44761(14) 0.15363(13) 0.51749(13) 0.0290(7) Uani 1 1 d . . . . .
O4 O 0.48267(16) 0.09364(15) 0.49196(15) 0.0370(8) Uani 1 1 d . . . . .
O5 O 0.48750(15) 0.28765(15) 0.52117(14) 0.0335(7) Uani 1 1 d . . . . .
O6 O 0.4802(2) 0.3282(2) 0.6031(2) 0.0226(10) Uani 0.6 1 d . . P A 1
H6 H 0.516756 0.349780 0.600769 0.034 Uiso 0.6 1 calc GR . P A 1
O6' O 0.3830(5) 0.2422(7) 0.5318(5) 0.060(3) Uani 0.4 1 d . . P B 2
H6' H 0.378878 0.236732 0.498942 0.089 Uiso 0.4 1 calc GR . P B 2
O7 O 0.50533(13) 0.42693(14) 0.42399(13) 0.0269(6) Uani 1 1 d D . . . .
O8 O 0.5013(4) 0.4299(4) 0.5162(3) 0.0285(18) Uani 0.6 1 d . U P C 1
H8 H 0.533355 0.460866 0.510937 0.043 Uiso 0.6 1 calc GR . P C 1
O8' O 0.4184(4) 0.3489(4) 0.4545(5) 0.031(2) Uani 0.4 1 d D U P C 2
H8' H 0.399921 0.356742 0.431932 0.046 Uiso 0.4 1 calc GR . P C 2
O9 O 0.38720(14) 0.19778(15) 0.44293(12) 0.0302(7) Uani 1 1 d . . . . .
O10 O 0.35994(15) 0.1532(2) 0.36178(16) 0.0479(10) Uani 1 1 d . . . . .
O11 O 0.37424(16) 0.26335(18) 0.2878(2) 0.0589(13) Uani 1 1 d . . . . .
O12 O 0.40497(13) 0.33942(16) 0.34634(14) 0.0349(8) Uani 1 1 d . . . . .
C1 C 0.61968(16) 0.34919(17) 0.46677(16) 0.0185(7) Uani 1 1 d . . . . .
C2 C 0.60313(16) 0.28695(16) 0.46774(16) 0.0178(7) Uani 1 1 d . . . . .
C3 C 0.55340(17) 0.24350(17) 0.43324(16) 0.0189(8) Uani 1 1 d . . . . .
C4 C 0.52210(16) 0.26404(17) 0.39924(16) 0.0183(7) Uani 1 1 d . . . . .
C5 C 0.52137(16) 0.19886(16) 0.32249(16) 0.0177(7) Uani 1 1 d . . . . .
C6 C 0.50436(16) 0.24032(17) 0.34350(16) 0.0188(7) Uani 1 1 d . . . . .
C7 C 0.51104(16) 0.29008(17) 0.30930(16) 0.0183(7) Uani 1 1 d . . . . .
C8 C 0.53394(16) 0.29662(17) 0.25517(15) 0.0176(7) Uani 1 1 d . . . . .
C9 C 0.54149(16) 0.32795(17) 0.39809(16) 0.0178(7) Uani 1 1 d . . . . .
C10 C 0.58807(17) 0.36853(17) 0.43037(15) 0.0174(7) Uani 1 1 d . . . . .
C11 C 0.57236(19) 0.21279(19) 0.60478(18) 0.0258(9) Uani 1 1 d . . . . .
C12 C 0.5326(2) 0.1617(2) 0.6430(2) 0.0311(10) Uani 1 1 d . . . . .
H12A H 0.538293 0.177720 0.679590 0.037 Uiso 1 1 calc R . . . .
H12B H 0.546222 0.132555 0.642704 0.037 Uiso 1 1 calc R . . . .
C13 C 0.4652(2) 0.1288(2) 0.6300(2) 0.0322(10) Uani 1 1 d . . . . .
H13A H 0.443128 0.106624 0.661976 0.039 Uiso 1 1 calc R . . . .
H13B H 0.453329 0.158438 0.622148 0.039 Uiso 1 1 calc R . . . .
C14 C 0.4472(2) 0.0856(2) 0.5828(2) 0.0339(10) Uani 1 1 d . . . . .
H14A H 0.404239 0.057711 0.585198 0.041 Uiso 1 1 calc R . . . .
H14B H 0.467339 0.062424 0.586660 0.041 Uiso 1 1 calc R . . . .
C15 C 0.46068(19) 0.11343(19) 0.52654(19) 0.0273(9) Uani 1 1 d . . . . .
C16 C 0.4591(5) 0.2987(5) 0.5577(5) 0.023(2) Uani 0.6 1 d . . P A 1
C16' C 0.4411(10) 0.2812(10) 0.5432(10) 0.041(5) Uani 0.4 1 d . . P B 2
C17 C 0.3935(3) 0.2777(3) 0.5491(3) 0.0175(13) Uani 0.6 1 d . . P A 1
H17A H 0.372564 0.266182 0.583682 0.021 Uiso 0.6 1 calc R . P A 1
H17B H 0.375841 0.242739 0.525553 0.021 Uiso 0.6 1 calc R . P A 1
C17' C 0.4488(8) 0.3254(7) 0.5823(7) 0.047(3) Uani 0.4 1 d . . P B 2
H17C H 0.489073 0.343381 0.597305 0.057 Uiso 0.4 1 calc R . P B 2
H17D H 0.420515 0.305939 0.611797 0.057 Uiso 0.4 1 calc R . P B 2
C18 C 0.3864(3) 0.3279(3) 0.5236(3) 0.0200(13) Uani 0.6 1 d . . P A 1
H18A H 0.343911 0.313218 0.517617 0.024 Uiso 0.6 1 calc R . P A 1
H18B H 0.400826 0.361084 0.549115 0.024 Uiso 0.6 1 calc R . P A 1
C18' C 0.4394(8) 0.3749(8) 0.5588(6) 0.053(4) Uani 0.4 1 d . . P B 2
H18C H 0.440001 0.400710 0.587923 0.063 Uiso 0.4 1 calc R . P B 2
H18D H 0.400259 0.357083 0.541409 0.063 Uiso 0.4 1 calc R . P B 2
C19 C 0.4183(4) 0.3507(4) 0.4721(4) 0.030(2) Uani 0.6 1 d D U P A 1
H19A H 0.421079 0.317570 0.456198 0.036 Uiso 0.6 1 calc R . P A 1
H19B H 0.391342 0.356940 0.448943 0.036 Uiso 0.6 1 calc R . P A 1
C19' C 0.4908(10) 0.4145(9) 0.5153(9) 0.040(5) Uani 0.4 1 d . U P B 2
H19C H 0.503481 0.456590 0.521350 0.048 Uiso 0.4 1 calc R . P B 2
H19D H 0.525203 0.409500 0.522135 0.048 Uiso 0.4 1 calc R . P B 2
C20 C 0.4757(2) 0.4022(2) 0.4654(2) 0.0351(11) Uani 1 1 d D . . . .
C21 C 0.35097(19) 0.1750(2) 0.40388(19) 0.0287(9) Uani 1 1 d . . . . .
C22 C 0.2909(2) 0.1719(3) 0.4088(2) 0.0409(13) Uani 1 1 d . . . . .
H22A H 0.292165 0.195606 0.439998 0.049 Uiso 1 1 calc R . . . .
H22B H 0.260357 0.130480 0.415915 0.049 Uiso 1 1 calc R . . . .
C23 C 0.27193(19) 0.1937(2) 0.3597(2) 0.0310(10) Uani 1 1 d . . . . .
H23A H 0.229063 0.178963 0.362233 0.037 Uiso 1 1 calc R . . . .
H23B H 0.278530 0.175982 0.327515 0.037 Uiso 1 1 calc R . . . .
C24 C 0.3044(2) 0.2622(2) 0.3520(3) 0.0480(15) Uani 1 1 d . . . . .
H24A H 0.279708 0.271983 0.329065 0.058 Uiso 1 1 calc R . . . .
H24B H 0.307688 0.280794 0.387108 0.058 Uiso 1 1 calc R . . . .
C25 C 0.3668(2) 0.2898(2) 0.3271(2) 0.0336(10) Uani 1 1 d . . . . .
Cl1 Cl 0.21274(13) -0.01211(13) 0.44676(10) 0.0442(6) Uani 0.5 1 d . . P D 1
Cl1' Cl 0.29064(17) 0.13538(17) 0.63881(15) 0.0679(9) Uani 0.5 1 d D U P D 2
C26 C 0.2275(2) 0.0254(2) 0.50098(16) 0.081(2) Uani 1 1 d . U . . .
H26 H 0.216156 0.001737 0.469845 0.097 Uiso 0.5 1 calc R . P D 2
C35 C 0.18391(15) 0.02050(17) 0.53748(18) 0.0457(13) Uani 1 1 d G U . D .
C30 C 0.20080(19) 0.0559(2) 0.58402(16) 0.0616(17) Uani 1 1 d DG U . D .
C29 C 0.2612(2) 0.0961(2) 0.59407(17) 0.0715(19) Uani 1 1 d DG U . D .
H29 H 0.272532 0.119792 0.625208 0.086 Uiso 0.5 1 calc R . P E 1
C28 C 0.30478(15) 0.1010(2) 0.5576(2) 0.092(3) Uani 1 1 d DG U . D .
H28 H 0.345209 0.127970 0.564295 0.110 Uiso 1 1 calc R . . . .
C27 C 0.28789(18) 0.0657(2) 0.51103(19) 0.0663(18) Uani 1 1 d G U . D .
H27 H 0.317022 0.068943 0.486613 0.080 Uiso 1 1 calc R . . . .
C31 C 0.1587(3) 0.0519(3) 0.6211(3) 0.0476(13) Uani 1 1 d . . . . .
H31 H 0.170404 0.075715 0.652111 0.057 Uiso 1 1 calc R . . D .
C32 C 0.0975(4) 0.0109(3) 0.6109(3) 0.0661(19) Uani 1 1 d . . . . .
H32 H 0.069582 0.008200 0.636375 0.079 Uiso 1 1 calc R . . . .
C33 C 0.0770(2) -0.0242(2) 0.5675(2) 0.0405(12) Uani 1 1 d . . . . .
H33 H 0.036088 -0.049873 0.561592 0.049 Uiso 1 1 calc R . . . .
C34 C 0.1208(3) -0.0201(3) 0.5310(3) 0.0538(15) Uani 1 1 d . . . . .
H34 H 0.108125 -0.045270 0.500769 0.065 Uiso 1 1 calc R . . D .
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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 O2 97.87(14) . 3_665 ?
O1 Cu1 O5 88.88(12) . . ?
O1 Cu1 C1 153.90(14) . . ?
O1 Cu1 C2 112.40(14) . . ?
O2 Cu1 O5 90.28(13) 3_665 . ?
O2 Cu1 C1 107.66(15) 3_665 . ?
O2 Cu1 C2 149.05(15) 3_665 . ?
C1 Cu1 O5 96.20(13) . . ?
C1 Cu1 C2 41.65(15) . . ?
C2 Cu1 O5 96.42(14) . . ?
O3 Cu2 O5 88.87(12) . . ?
O3 Cu2 O9 99.19(14) . . ?
O3 Cu2 C3 111.26(15) . . ?
O3 Cu2 C4 152.82(15) . . ?
O9 Cu2 O5 91.05(13) . . ?
O9 Cu2 C3 148.92(15) . . ?
O9 Cu2 C4 107.47(14) . . ?
C3 Cu2 O5 95.47(13) . . ?
C4 Cu2 O5 95.72(13) . . ?
C4 Cu2 C3 41.70(15) . . ?
O10 Cu3 O7 92.78(15) . 18_545 ?
O10 Cu3 O12 97.73(17) . 18_545 ?
O10 Cu3 C5 153.34(16) . . ?
O10 Cu3 C6 111.74(16) . . ?
O12 Cu3 O7 89.64(12) 18_545 18_545 ?
O12 Cu3 C5 108.33(16) 18_545 . ?
O12 Cu3 C6 149.84(16) 18_545 . ?
C5 Cu3 O7 92.93(13) . 18_545 ?
C5 Cu3 C6 41.77(15) . . ?
C6 Cu3 O7 95.02(13) . 18_545 ?
O4 Cu4 O7 88.39(12) 17 18_545 ?
O4 Cu4 C7 147.68(15) 17 . ?
O4 Cu4 C8 106.57(15) 17 . ?
O11 Cu4 O4 101.1(2) . 17 ?
O11 Cu4 O7 94.12(14) . 18_545 ?
O11 Cu4 C7 110.46(19) . . ?
O11 Cu4 C8 151.49(19) . . ?
C7 Cu4 O7 95.73(13) . 18_545 ?
C8 Cu4 O7 93.24(13) . 18_545 ?
C8 Cu4 C7 41.30(15) . . ?
C11 O1 Cu1 130.4(3) . . ?
C11 O2 Cu1 133.0(3) . 2_655 ?
C15 O3 Cu2 131.6(3) . . ?
C15 O4 Cu4 132.5(3) . 18_545 ?
Cu1 O5 Cu2 97.11(11) . . ?
C16 O5 Cu1 117.3(5) . . ?
C16 O5 Cu2 137.8(5) . . ?
C16' O5 Cu1 142.0(12) . . ?
C16' O5 Cu2 112.5(11) . . ?
C16 O6 H6 109.5 . . ?
C16' O6' H6' 109.5 . . ?
Cu4 O7 Cu3 95.03(11) 17 17 ?
C20 O7 Cu3 130.0(3) . 17 ?
C20 O7 Cu4 130.0(3) . 17 ?
C20 O8 H8 109.5 . . ?
C20 O8' H8' 109.5 . . ?
C21 O9 Cu2 133.1(3) . . ?
C21 O10 Cu3 130.3(3) . . ?
C25 O11 Cu4 130.9(3) . . ?
C25 O12 Cu3 132.0(3) . 17 ?
C2 C1 Cu1 70.2(2) . . ?
C2 C1 Cu1 113.8(3) 3_665 . ?
C2 C1 C2 120.5(4) . 3_665 ?
C2 C1 C10 119.1(3) . . ?
C10 C1 Cu1 121.7(3) . . ?
C10 C1 C2 107.9(3) . 3_665 ?
C1 C2 Cu1 68.2(2) . . ?
C1 C2 Cu1 117.1(3) 2_655 . ?
C1 C2 C1 119.4(4) . 2_655 ?
C1 C2 C3 119.7(3) . . ?
C3 C2 Cu1 120.9(3) . . ?
C3 C2 C1 107.5(3) . 2_655 ?
C2 C3 Cu2 120.5(3) . . ?
C2 C3 C8 107.7(3) . 18_545 ?
C4 C3 Cu2 68.5(2) . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 C8 119.7(3) . 18_545 ?
C8 C3 Cu2 117.1(3) 18_545 . ?
C3 C4 Cu2 69.8(2) . . ?
C3 C4 C6 120.4(3) . . ?
C3 C4 C9 119.2(3) . . ?
C6 C4 Cu2 114.1(3) . . ?
C9 C4 Cu2 121.8(3) . . ?
C9 C4 C6 107.9(3) . . ?
C6 C5 Cu3 69.6(2) . . ?
C6 C5 C7 120.2(3) . 18_545 ?
C6 C5 C9 119.3(3) . 18_545 ?
C7 C5 Cu3 114.9(3) 18_545 . ?
C9 C5 Cu3 122.1(3) 18_545 . ?
C9 C5 C7 107.3(3) 18_545 18_545 ?
C4 C6 Cu3 117.5(3) . . ?
C5 C6 Cu3 68.7(2) . . ?
C5 C6 C4 119.7(3) . . ?
C5 C6 C7 119.5(3) . . ?
C7 C6 Cu3 120.6(3) . . ?
C7 C6 C4 107.3(3) . . ?
C5 C7 Cu4 116.8(3) 17 . ?
C6 C7 Cu4 119.9(3) . . ?
C6 C7 C5 108.1(3) . 17 ?
C8 C7 Cu4 68.5(2) . . ?
C8 C7 C5 119.5(3) . 17 ?
C8 C7 C6 119.9(3) . . ?
C3 C8 Cu4 114.7(3) 17 . ?
C7 C8 Cu4 70.2(2) . . ?
C7 C8 C3 120.5(3) . 17 ?
C7 C8 C10 118.6(3) . 18_545 ?
C10 C8 Cu4 121.5(3) 18_545 . ?
C10 C8 C3 107.8(3) 18_545 17 ?
C5 C9 C4 109.2(3) 17 . ?
C10 C9 C4 121.2(3) . . ?
C10 C9 C5 121.2(3) . 17 ?
C1 C10 C8 108.9(3) . 17 ?
C9 C10 C1 121.3(3) . . ?
C9 C10 C8 121.4(3) . 17 ?
O1 C11 O2 124.6(4) . . ?
O1 C11 C12 117.6(4) . . ?
O2 C11 C12 117.7(4) . . ?
C11 C12 H12A 108.4 . . ?
C11 C12 H12B 108.4 . . ?
C11 C12 C13 115.5(4) . . ?
H12A C12 H12B 107.5 . . ?
C13 C12 H12A 108.4 . . ?
C13 C12 H12B 108.4 . . ?
C12 C13 H13A 108.7 . . ?
C12 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C14 C13 C12 114.3(4) . . ?
C14 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
C13 C14 H14A 108.2 . . ?
C13 C14 H14B 108.2 . . ?
C13 C14 C15 116.4(4) . . ?
H14A C14 H14B 107.3 . . ?
C15 C14 H14A 108.2 . . ?
C15 C14 H14B 108.2 . . ?
O3 C15 O4 124.7(4) . . ?
O3 C15 C14 117.2(4) . . ?
O4 C15 C14 118.1(4) . . ?
O5 C16 O6 128.1(10) . . ?
O5 C16 C17 118.9(8) . . ?
O6 C16 C17 113.1(10) . . ?
O5 C16' O6' 130(2) . . ?
O5 C16' C17' 116.6(18) . . ?
O6' C16' C17' 113.2(18) . . ?
C16 C17 H17A 109.7 . . ?
C16 C17 H17B 109.7 . . ?
C16 C17 C18 109.9(7) . . ?
H17A C17 H17B 108.2 . . ?
C18 C17 H17A 109.7 . . ?
C18 C17 H17B 109.7 . . ?
C16' C17' H17C 109.0 . . ?
C16' C17' H17D 109.0 . . ?
C16' C17' C18' 113.0(16) . . ?
H17C C17' H17D 107.8 . . ?
C18' C17' H17C 109.0 . . ?
C18' C17' H17D 109.0 . . ?
C17 C18 H18A 108.6 . . ?
C17 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C19 C18 C17 114.5(6) . . ?
C19 C18 H18A 108.6 . . ?
C19 C18 H18B 108.6 . . ?
C17' C18' H18C 109.4 . . ?
C17' C18' H18D 109.4 . . ?
C17' C18' C19' 111.0(14) . . ?
H18C C18' H18D 108.0 . . ?
C19' C18' H18C 109.4 . . ?
C19' C18' H18D 109.4 . . ?
C18 C19 H19A 105.8 . . ?
C18 C19 H19B 105.8 . . ?
H19A C19 H19B 106.2 . . ?
C20 C19 C18 126.0(8) . . ?
C20 C19 H19A 105.8 . . ?
C20 C19 H19B 105.8 . . ?
C18' C19' H19C 108.4 . . ?
C18' C19' H19D 108.4 . . ?
H19C C19' H19D 107.4 . . ?
C20 C19' C18' 115.6(16) . . ?
C20 C19' H19C 108.4 . . ?
C20 C19' H19D 108.4 . . ?
O7 C20 O8 117.0(5) . . ?
O7 C20 O8' 113.9(6) . . ?
O7 C20 C19 131.3(6) . . ?
O7 C20 C19' 129.1(11) . . ?
C19 C20 O8 111.6(6) . . ?
C19' C20 O8' 116.8(11) . . ?
O9 C21 C22 117.5(4) . . ?
O10 C21 O9 125.5(4) . . ?
O10 C21 C22 117.0(4) . . ?
C21 C22 H22A 108.5 . . ?
C21 C22 H22B 108.5 . . ?
C21 C22 C23 115.2(4) . . ?
H22A C22 H22B 107.5 . . ?
C23 C22 H22A 108.5 . . ?
C23 C22 H22B 108.5 . . ?
C22 C23 H23A 108.4 . . ?
C22 C23 H23B 108.4 . . ?
C22 C23 C24 115.6(5) . . ?
H23A C23 H23B 107.4 . . ?
C24 C23 H23A 108.4 . . ?
C24 C23 H23B 108.4 . . ?
C23 C24 H24A 108.5 . . ?
C23 C24 H24B 108.5 . . ?
H24A C24 H24B 107.5 . . ?
C25 C24 C23 115.2(4) . . ?
C25 C24 H24A 108.5 . . ?
C25 C24 H24B 108.5 . . ?
O11 C25 C24 118.0(4) . . ?
O12 C25 O11 126.4(4) . . ?
O12 C25 C24 115.4(4) . . ?
C29 Cl1' Cl1' 153.9(4) . 13_556 ?
C35 C26 Cl1 123.8(3) . . ?
C35 C26 H26 120.0 . . ?
C35 C26 C27 120.0 . . ?
C27 C26 Cl1 116.2(3) . . ?
C27 C26 H26 120.0 . . ?
C26 C35 C30 120.0 . . ?
C26 C35 C34 124.0(4) . . ?
C30 C35 C34 116.0(4) . . ?
C29 C30 C35 120.0 . . ?
C31 C30 C35 121.4(4) . . ?
C31 C30 C29 118.6(4) . . ?
C30 C29 Cl1' 131.4(4) . . ?
C30 C29 H29 120.0 . . ?
C30 C29 C28 120.0 . . ?
C28 C29 Cl1' 108.5(4) . . ?
C28 C29 H29 120.0 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 C29 120.0 . . ?
C27 C28 H28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27 120.0 . . ?
C30 C31 H31 120.8 . . ?
C30 C31 C32 118.5(6) . . ?
C32 C31 H31 120.8 . . ?
C31 C32 H32 117.7 . . ?
C33 C32 C31 124.6(7) . . ?
C33 C32 H32 117.7 . . ?
C32 C33 H33 122.1 . . ?
C32 C33 C34 115.7(6) . . ?
C34 C33 H33 122.1 . . ?
C35 C34 H34 118.1 . . ?
C33 C34 C35 123.8(6) . . ?
C33 C34 H34 118.1 . . ?
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 1.946(3) . ?
Cu1 O2 1.981(3) 3_665 ?
Cu1 O5 2.328(3) . ?
Cu1 C1 2.003(4) . ?
Cu1 C2 2.029(4) . ?
Cu2 O3 1.950(3) . ?
Cu2 O5 2.398(4) . ?
Cu2 O9 1.950(3) . ?
Cu2 C3 2.019(4) . ?
Cu2 C4 2.001(4) . ?
Cu3 O7 2.409(3) 18_545 ?
Cu3 O10 1.925(3) . ?
Cu3 O12 1.951(3) 18_545 ?
Cu3 C5 2.005(4) . ?
Cu3 C6 2.017(4) . ?
Cu4 O4 1.997(4) 17 ?
Cu4 O7 2.350(3) 18_545 ?
Cu4 O11 1.934(4) . ?
Cu4 C7 2.042(4) . ?
Cu4 C8 2.019(4) . ?
O1 C11 1.248(5) . ?
O2 C11 1.262(5) . ?
O3 C15 1.254(5) . ?
O4 C15 1.260(6) . ?
O5 C16 1.275(14) . ?
O5 C16' 1.24(2) . ?
O6 H6 0.8200 . ?
O6 C16 1.306(12) . ?
O6' H6' 0.8200 . ?
O6' C16' 1.35(3) . ?
O7 C20 1.241(6) . ?
O8 H8 0.8200 . ?
O8 C20 1.426(9) . ?
O8' H8' 0.8200 . ?
O8' C20 1.447(10) . ?
O9 C21 1.260(5) . ?
O10 C21 1.253(6) . ?
O11 C25 1.252(6) . ?
O12 C25 1.247(6) . ?
C1 C2 1.433(5) . ?
C1 C2 1.481(5) 3_665 ?
C1 C10 1.453(5) . ?
C2 C3 1.474(5) . ?
C3 C4 1.431(5) . ?
C3 C8 1.477(5) 18_545 ?
C4 C6 1.478(5) . ?
C4 C9 1.457(5) . ?
C5 C6 1.434(5) . ?
C5 C7 1.485(5) 18_545 ?
C5 C9 1.446(5) 18_545 ?
C6 C7 1.467(5) . ?
C7 C8 1.432(5) . ?
C8 C10 1.460(5) 18_545 ?
C9 C10 1.379(5) . ?
C11 C12 1.520(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.534(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.511(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.516(6) . ?
C16 C17 1.505(13) . ?
C16' C17' 1.43(2) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.526(9) . ?
C17' H17C 0.9700 . ?
C17' H17D 0.9700 . ?
C17' C18' 1.52(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.463(12) . ?
C18' H18C 0.9700 . ?
C18' H18D 0.9700 . ?
C18' C19' 1.61(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.414(10) . ?
C19' H19C 0.9700 . ?
C19' H19D 0.9700 . ?
C19' C20 1.28(2) . ?
C21 C22 1.509(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.513(7) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.535(7) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.521(6) . ?
Cl1 C26 1.578(4) . ?
Cl1' Cl1' 2.397(7) 13_556 ?
Cl1' C29 1.428(5) . ?
C26 H26 0.9300 . ?
C26 C35 1.3900 . ?
C26 C27 1.3900 . ?
C35 C30 1.3900 . ?
C35 C34 1.431(7) . ?
C30 C29 1.3900 . ?
C30 C31 1.379(7) . ?
C29 H29 0.9300 . ?
C29 C28 1.3900 . ?
C28 H28 0.9300 . ?
C28 C27 1.3900 . ?
C27 H27 0.9300 . ?
C31 H31 0.9300 . ?
C31 C32 1.408(10) . ?
C32 H32 0.9300 . ?
C32 C33 1.325(10) . ?
C33 H33 0.9300 . ?
C33 C34 1.403(9) . ?
C34 H34 0.9300 . ?
