#------------------------------------------------------------------------------
#$Date: 2024-07-05 20:39:15 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293202 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/32/7063245.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_7063245
loop_
_publ_author_name
'Cebotari, Diana'
'Calancea, Sergiu'
'Garbuz, Olga'
'Balan, Greta'
'Marrot, Jérôme'
'Shova, Sergiu'
'Guérineau, Vincent'
'Touboul, David'
'Tsapkov, Victor'
'Gulea, Aurelian'
'Floquet, Sébastien'
_publ_section_title
;
 Synthesis, structure and biological properties of a series of
 dicopper(bis-thiosemicarbazone) complexes
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12043
_journal_page_last               12053
_journal_paper_doi               10.1039/D4NJ00342J
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety
'C28.147 H34 Cu4 N12 O4 S4, 2(Cl O4), 2(Cl O3.5), 2(H2 O), 4(C2 H6 O)'
_chemical_formula_sum            'C36.15 H62 Cl4 Cu4 N12 O25 S4'
_chemical_formula_weight         1588.97
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-03 deposited with the CCDC.	2024-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                102.963(9)
_cell_angle_beta                 95.669(9)
_cell_angle_gamma                99.977(9)
_cell_formula_units_Z            1
_cell_length_a                   9.0820(11)
_cell_length_b                   11.3880(11)
_cell_length_c                   16.0107(16)
_cell_measurement_reflns_used    3515
_cell_measurement_temperature    160.05(10)
_cell_measurement_theta_max      26.1040
_cell_measurement_theta_min      1.9150
_cell_volume                     1572.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  11.00   1.00   30.00    --  -15.44  45.00  50.00   25
  2  ω      1.00  67.00   1.00   30.00    --   17.94  45.00  50.00   66
  3  ω    -50.00  35.00   1.00   30.00    --   17.94 -45.00 -99.00   85
  4  ω    -71.00 -42.00   1.00   30.00    --  -15.44-178.00 -60.00   29
  5  ω    -71.00 -39.00   1.00   30.00    --  -15.44-178.00  30.00   32
  6  ω     10.00  39.00   1.00   30.00    --   17.94  77.00-120.00   29
  7  ω    -51.00  34.00   1.00   30.00    --   17.94 -38.00-180.00   85
  8  ω      0.00  27.00   1.00   30.00    --   17.94  77.00 -30.00   27
  9  ω     -9.00  37.00   1.00   30.00    --   17.94  77.00 120.00   46
 10  ω     -4.00  35.00   1.00   30.00    --   17.94  77.00-180.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0162938000
_diffrn_orient_matrix_UB_12      0.0628243000
_diffrn_orient_matrix_UB_13      0.0229010000
_diffrn_orient_matrix_UB_21      0.0740866000
_diffrn_orient_matrix_UB_22      0.0061599000
_diffrn_orient_matrix_UB_23      -0.0112212000
_diffrn_orient_matrix_UB_31      -0.0258085000
_diffrn_orient_matrix_UB_32      0.0165224000
_diffrn_orient_matrix_UB_33      -0.0382053000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0882
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12761
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.873
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       plate
_exptl_crystal_F_000             811
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.027
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5542
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0934
_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)+(0.1244P)²+13.7792P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2290
_refine_ls_wR_factor_ref         0.2540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3945
_reflns_number_total             5542
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4nj00342j2.cif
_cod_data_source_block           shi_5018_roru_auto
_cod_depositor_comments
'Adding full bibliography for 7063243--7063248.cif.'
_cod_database_code               7063245
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H30N6O8S2Cu2
_chemical_oxdiff_usercomment     DC_251
_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.
;
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.626
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O14-C18
 2.5 with sigma of 0.01
 O14X-C18X
 2.5 with sigma of 0.01
 O14X-C17X = O14-C17 = O13X-C15X = O13-C15
 1.4 with sigma of 0.01
 C18-C17 = C18X-C17X
 1.52 with sigma of 0.01
 C16-C15 = C16X-C15X
 1.52 with sigma of 0.01
 C16-O13
 2.5 with sigma of 0.01
 O13X-C16X
 2.5 with sigma of 0.01
 C10X-C8X \\sim C8X-C9X
 with sigma of 0.01
 C9-C10 \\sim C10-C8
 with sigma of 0.01
 C9X-C10X \\sim C10X-C8X
 with sigma of 0.01
 C7-C8 \\sim C7-C10X \\sim C7-C10 \\sim C7-C9X \\sim C7-C9 \\sim C7-C8X
 with sigma of 0.01
 C10-C8 \\sim C8-C9
 with sigma of 0.01
 Cl2-O8 \\sim Cl2-O9 \\sim Cl2-O10 \\sim Cl2-O7 \\sim Cl2-O12 \\sim Cl2-O11
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C7 \\sim C9X \\sim C10 \\sim C10X \\sim C8 \\sim C8X \\sim C9: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(C16X) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C18X)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C15X) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C9X) = Uanis(C9) = Uanis(C8X) = Uanis(C8) = Uanis(C10X) = Uanis(C10)
Uanis(C16) = Uanis(C16X)
Uanis(O14X) = Uanis(O14)
Uanis(C17X) = Uanis(C17)
Uanis(C18X) = Uanis(C18)
Uanis(O13X) = Uanis(O13)
Uanis(C15) = Uanis(C15X)
4. Others
 Sof(C10X)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C8X)=Sof(H8XA)=Sof(H8XB)=
 Sof(H8XC)=Sof(C9)=Sof(C9X)=Sof(H9XA)=Sof(H9XB)=Sof(H9XC)=1-FVAR(1)
 Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(1)
 Sof(O12)=1-FVAR(2)
 Sof(O11)=FVAR(2)
 Sof(O14)=Sof(H14)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=1-FVAR(3)
 Sof(C17X)=Sof(H17C)=Sof(H17D)=Sof(O14X)=Sof(H14X)=Sof(C18X)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=FVAR(3)
 Sof(O13)=Sof(H13A)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=1-FVAR(4)
 Sof(O13X)=Sof(H13X)=Sof(C15X)=Sof(H15C)=Sof(H15D)=Sof(C16X)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=FVAR(4)
 Fixed Sof: H2A(0.5) H5(0.5) O9(0.5) O8(0.5) O10(0.5)
5.a Riding coordinates:
 O2(H2), O40(H40A,H40B), N2(H2A), N5(H5), N6(H6A,H6B), O14(H14), N3(H3A,H3B),
 O13(H13A), C18(H18A,H18B,H18C), C10X(H10A,H10B,H10C), C8X(H8XA,H8XB,H8XC),
 C16(H16A,H16B,H16C), C9(H9A,H9B,H9C), C10(H10D,H10E,H10F), C8(H8A,H8B,H8C),
 O14X(H14X), C18X(H18D,H18E,H18F), O13X(H13X), C16X(H16D,H16E,H16F)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C17X(H17C,H17D), C15X(H15C,H15D)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C11(H11)
5.d Idealised Me refined as rotating group:
 C9X(H9XA,H9XB,H9XC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.846
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 0.79530(12) 0.45564(9) 0.53404(7) 0.0224(3) Uani 1 1 d . . . . .
Cu2 Cu 0.59350(12) 0.64053(9) 0.53913(7) 0.0231(3) Uani 1 1 d . . . . .
S1 S 0.9012(3) 0.3316(2) 0.43756(15) 0.0246(5) Uani 1 1 d . . . . .
S2 S 0.4777(3) 0.7337(2) 0.44908(15) 0.0271(5) Uani 1 1 d . . . . .
Cl1 Cl 0.8744(3) 1.0588(3) 0.71596(17) 0.0519(8) Uani 1 1 d . . . . .
Cl2 Cl 0.3282(3) 0.5010(3) 0.7741(2) 0.0544(8) Uani 1 1 d D . . . .
O1 O 0.7228(7) 0.5782(5) 0.6187(4) 0.0222(13) Uani 1 1 d . . . . .
O2 O 0.6535(7) 0.5080(5) 0.4621(4) 0.0272(14) Uani 1 1 d . . . . .
H2 H 0.687558 0.532636 0.420155 0.041 Uiso 1 1 d R U . . .
O40 O 1.2218(8) 1.1009(7) 0.6209(5) 0.0432(18) Uani 1 1 d . . . . .
H40A H 1.134550 1.073338 0.634197 0.065 Uiso 1 1 d R U . . .
H40B H 1.278250 1.122378 0.670107 0.065 Uiso 1 1 d R U . . .
N1 N 0.9140(8) 0.4134(7) 0.6256(5) 0.0238(17) Uani 1 1 d . . . . .
N2 N 0.9974(9) 0.3231(7) 0.5997(5) 0.0284(18) Uani 1 1 d . . . . .
H2A H 1.046580 0.294395 0.638275 0.034 Uiso 0.5 1 d R U P . .
N4 N 0.5573(9) 0.7618(7) 0.6339(5) 0.0259(17) Uani 1 1 d . . . . .
N5 N 0.4667(9) 0.8422(7) 0.6127(6) 0.0310(19) Uani 1 1 d . . . . .
H5 H 0.438439 0.895371 0.653905 0.037 Uiso 0.5 1 d R U P . .
N6 N 0.3404(9) 0.9132(7) 0.5117(6) 0.0317(19) Uani 1 1 d . . . . .
H6A H 0.313924 0.966470 0.553533 0.038 Uiso 1 1 d R U . . .
H6B H 0.310984 0.911240 0.457273 0.038 Uiso 1 1 d R U . . .
O14 O 1.3593(17) 0.9556(12) 0.7555(7) 0.051(3) Uani 0.86(3) 1 d D . P A 1
H14 H 1.363205 1.033234 0.772934 0.076 Uiso 0.86(3) 1 d R U P A 1
N3 N 1.0836(9) 0.1970(7) 0.4915(5) 0.0321(19) Uani 1 1 d . . . . .
H3A H 1.133573 0.170520 0.531052 0.039 Uiso 1 1 d R U . . .
H3B H 1.088103 0.167690 0.436292 0.039 Uiso 1 1 d R U . . .
C1 C 0.7586(10) 0.6103(8) 0.7028(6) 0.024(2) Uani 1 1 d . . . . .
C13 C 0.6055(10) 0.7795(8) 0.7137(7) 0.028(2) Uani 1 1 d . . . . .
H13 H 0.576424 0.845206 0.752212 0.034 Uiso 1 1 calc R U . . .
O5 O 0.9675(11) 1.1754(7) 0.7353(5) 0.062(2) Uani 1 1 d . . . . .
O4 O 0.8159(10) 1.0280(8) 0.7875(5) 0.061(2) Uani 1 1 d . . . . .
C6 C 0.8490(10) 0.5518(8) 0.7494(6) 0.025(2) Uani 1 1 d . . . . .
C12 C 1.0011(10) 0.2811(8) 0.5152(6) 0.025(2) Uani 1 1 d . . . . .
C2 C 0.7006(10) 0.7097(8) 0.7524(6) 0.024(2) Uani 1 1 d . . . . .
C14 C 0.4243(10) 0.8369(8) 0.5304(6) 0.024(2) Uani 1 1 d . . . . .
C11 C 0.9197(10) 0.4531(8) 0.7070(6) 0.027(2) Uani 1 1 d . . . . .
H11 H 0.974673 0.415179 0.743312 0.033 Uiso 1 1 calc R U . . .
O7 O 0.2364(9) 0.3806(7) 0.7591(7) 0.073(3) Uani 1 1 d D . . . .
C3 C 0.7377(11) 0.7437(9) 0.8431(6) 0.031(2) Uani 1 1 d . . . . .
C5 C 0.8777(12) 0.5877(9) 0.8389(6) 0.035(2) Uani 1 1 d . . . . .
C4 C 0.8249(12) 0.6845(10) 0.8877(6) 0.037(2) Uani 1 1 d . . . . .
O3 O 0.9760(16) 0.9679(12) 0.6889(9) 0.122(5) Uani 1 1 d . . . . .
O13 O 0.4108(16) 0.2059(14) 0.7716(9) 0.076(5) Uani 0.79(2) 1 d D . P B 2
H13A H 0.365050 0.261101 0.756822 0.114 Uiso 0.79(2) 1 d R U P B 2
O12 O 0.253(3) 0.5590(17) 0.7162(11) 0.060(8) Uiso 0.51(5) 1 d D . P C 1
C15 C 0.5670(17) 0.255(2) 0.7877(11) 0.079(7) Uani 0.79(2) 1 d D U P B 2
H15A H 0.586245 0.326520 0.762222 0.095 Uiso 0.79(2) 1 calc R U P B 2
H15B H 0.619025 0.192057 0.756965 0.095 Uiso 0.79(2) 1 calc R U P B 2
C17 C 1.269(2) 0.8872(19) 0.8030(10) 0.085(7) Uani 0.86(3) 1 d D . P A 1
H17A H 1.237242 0.800869 0.768542 0.102 Uiso 0.86(3) 1 calc R U P A 1
H17B H 1.175836 0.920863 0.810120 0.102 Uiso 0.86(3) 1 calc R U P A 1
O9 O 0.4667(17) 0.511(2) 0.8277(13) 0.094(7) Uiso 0.5 1 d D . P C 2
C7 C 0.8611(14) 0.7251(10) 0.9859(7) 0.058(3) Uani 1 1 d D U . . .
O8 O 0.266(2) 0.5638(19) 0.8466(11) 0.092(7) Uiso 0.5 1 d D . P C .
C18 C 1.345(3) 0.888(3) 0.8922(11) 0.122(9) Uani 0.86(3) 1 d D U P A 1
H18A H 1.383048 0.811902 0.891029 0.182 Uiso 0.86(3) 1 d R U P A 1
H18B H 1.278638 0.899302 0.936659 0.182 Uiso 0.86(3) 1 d R U P A 1
H18C H 1.430568 0.957852 0.905609 0.182 Uiso 0.86(3) 1 d R U P A 1
O10 O 0.441(2) 0.474(2) 0.7200(14) 0.104(8) Uiso 0.5 1 d D . P C 1
C10X C 0.941(3) 0.8599(16) 1.0155(16) 0.091(5) Uani 0.537(13) 1 d D U P D 2
H10A H 0.876226 0.911804 0.995538 0.137 Uiso 0.537(13) 1 d R U P D 2
H10B H 1.035366 0.870184 0.991048 0.137 Uiso 0.537(13) 1 d R U P D 2
H10C H 0.962506 0.884214 1.078908 0.137 Uiso 0.537(13) 1 d R U P D 2
C8X C 0.710(2) 0.717(2) 1.0209(15) 0.091(5) Uani 0.537(13) 1 d D U P D 2
H8XA H 0.726483 0.761558 1.081932 0.137 Uiso 0.537(13) 1 d R U P D 2
H8XB H 0.664203 0.630188 1.015602 0.137 Uiso 0.537(13) 1 d R U P D 2
H8XC H 0.641903 0.753018 0.987562 0.137 Uiso 0.537(13) 1 d R U P D 2
C16 C 0.638(2) 0.295(3) 0.8824(14) 0.139(11) Uani 0.79(2) 1 d D U P B 2
H16A H 0.748800 0.316455 0.891462 0.209 Uiso 0.79(2) 1 d R U P B 2
H16B H 0.604990 0.220575 0.902142 0.209 Uiso 0.79(2) 1 d R U P B 2
H16C H 0.598090 0.362905 0.915272 0.209 Uiso 0.79(2) 1 d R U P B 2
C9 C 0.810(3) 0.6160(19) 1.0239(15) 0.091(5) Uani 0.537(13) 1 d D U P D 1
H9A H 0.834359 0.641100 1.087151 0.137 Uiso 0.463(13) 1 d R U P D 1
H9B H 0.859639 0.548200 1.001131 0.137 Uiso 0.463(13) 1 d R U P D 1
H9C H 0.700259 0.588900 1.007641 0.137 Uiso 0.463(13) 1 d R U P D 1
O6 O 0.7714(15) 1.0376(17) 0.6496(8) 0.141(6) Uani 1 1 d . . . . .
C10 C 1.034(2) 0.757(2) 1.0033(18) 0.091(5) Uani 0.463(13) 1 d D U P D 1
H10D H 1.073139 0.818540 0.972822 0.137 Uiso 0.463(13) 1 d R U P D 1
H10E H 1.072329 0.681730 0.982782 0.137 Uiso 0.463(13) 1 d R U P D 1
H10F H 1.067128 0.788990 1.065682 0.137 Uiso 0.463(13) 1 d R U P D 1
C8 C 0.802(3) 0.8341(19) 1.0323(17) 0.091(5) Uani 0.463(13) 1 d D U P D 1
H8A H 0.842936 0.856987 1.093981 0.137 Uiso 0.463(13) 1 d R U P D 1
H8B H 0.691326 0.813897 1.025651 0.137 Uiso 0.463(13) 1 d R U P D 1
H8C H 0.833797 0.903188 1.006671 0.137 Uiso 0.463(13) 1 d R U P D 1
C9X C 0.954(3) 0.652(2) 1.0300(15) 0.091(5) Uani 0.537(13) 1 d D U P D 2
H9XA H 1.056200 0.664148 1.014840 0.137 Uiso 0.537(13) 1 calc R U P D 2
H9XB H 0.906535 0.564149 1.010728 0.137 Uiso 0.537(13) 1 calc R U P D 2
H9XC H 0.958119 0.679312 1.092884 0.137 Uiso 0.537(13) 1 calc R U P D 2
O11 O 0.335(4) 0.5667(17) 0.7084(10) 0.065(8) Uiso 0.49(5) 1 d D . P C 2
C17X C 1.336(10) 0.964(13) 0.842(6) 0.085(7) Uani 0.14(3) 1 d D . P A 2
H17C H 1.273139 0.880212 0.817784 0.102 Uiso 0.14(3) 1 calc R U P A 2
H17D H 1.265975 1.020114 0.857954 0.102 Uiso 0.14(3) 1 calc R U P A 2
O14X O 1.409(11) 0.999(8) 0.775(4) 0.051(3) Uani 0.14(3) 1 d D . P A 2
H14X H 1.421852 1.075578 0.781596 0.076 Uiso 0.14(3) 1 d R U P A 2
C18X C 1.434(17) 0.962(16) 0.924(6) 0.122(9) Uani 0.14(3) 1 d D U P A 2
H18D H 1.541112 0.998903 0.927451 0.182 Uiso 0.14(3) 1 d R U P A 2
H18E H 1.424761 0.880513 0.935351 0.182 Uiso 0.14(3) 1 d R U P A 2
H18F H 1.388641 1.014744 0.967071 0.182 Uiso 0.14(3) 1 d R U P A 2
O13X O 0.489(8) 0.216(6) 0.767(4) 0.076(5) Uani 0.21(2) 1 d D . P B 1
H13X H 0.455672 0.288239 0.765790 0.114 Uiso 0.21(2) 1 d R U P B 1
C15X C 0.569(8) 0.229(6) 0.849(4) 0.079(7) Uani 0.21(2) 1 d D U P B 1
H15C H 0.672941 0.217068 0.841196 0.095 Uiso 0.21(2) 1 calc R U P B 1
H15D H 0.521597 0.160837 0.873057 0.095 Uiso 0.21(2) 1 calc R U P B 1
C16X C 0.581(13) 0.349(8) 0.916(5) 0.139(11) Uani 0.21(2) 1 d D U P B 1
H16D H 0.658643 0.421115 0.917730 0.209 Uiso 0.21(2) 1 d R U P B 1
H16E H 0.614263 0.308425 0.960860 0.209 Uiso 0.21(2) 1 d R U P B 1
H16F H 0.486203 0.374655 0.927920 0.209 Uiso 0.21(2) 1 d R U P B 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 S1 173.62(19) . . ?
O2 Cu1 S1 102.9(2) . . ?
O2 Cu1 O1 78.1(3) . . ?
O2 Cu1 N1 168.0(3) . . ?
N1 Cu1 S1 88.4(2) . . ?
N1 Cu1 O1 91.1(3) . . ?
S2 Cu2 O2 91.67(15) . 2_666 ?
O1 Cu2 S2 171.23(19) . . ?
O1 Cu2 O2 97.1(2) . 2_666 ?
O2 Cu2 S2 103.6(2) . . ?
O2 Cu2 O1 77.5(3) . . ?
O2 Cu2 O2 87.9(2) . 2_666 ?
N4 Cu2 S2 88.2(2) . . ?
N4 Cu2 O1 90.6(3) . . ?
N4 Cu2 O2 93.2(3) . 2_666 ?
N4 Cu2 O2 168.1(3) . . ?
C12 S1 Cu1 94.4(3) . . ?
C14 S2 Cu2 94.7(3) . . ?
O5 Cl1 O4 113.6(5) . . ?
O5 Cl1 O3 105.8(7) . . ?
O4 Cl1 O3 105.2(7) . . ?
O6 Cl1 O5 114.2(8) . . ?
O6 Cl1 O4 112.3(7) . . ?
O6 Cl1 O3 104.6(10) . . ?
O7 Cl2 O12 104.7(10) . . ?
O7 Cl2 O8 99.5(11) . . ?
O7 Cl2 O10 100.2(12) . . ?
O12 Cl2 O8 91.9(13) . . ?
O9 Cl2 O7 110.6(11) . . ?
O9 Cl2 O8 91.2(13) . . ?
O10 Cl2 O12 94.1(15) . . ?
O10 Cl2 O8 157.2(14) . . ?
O11 Cl2 O7 121.8(10) . . ?
O11 Cl2 O9 116.3(16) . . ?
O11 Cl2 O8 111.5(14) . . ?
Cu1 O1 Cu2 99.8(3) . . ?
C1 O1 Cu1 128.5(5) . . ?
C1 O1 Cu2 131.7(5) . . ?
Cu1 O2 Cu2 104.2(3) . . ?
Cu1 O2 H2 115.1 . . ?
Cu2 O2 H2 109.9 . . ?
H40A O40 H40B 102.4 . . ?
N2 N1 Cu1 116.2(5) . . ?
C11 N1 Cu1 128.1(7) . . ?
C11 N1 N2 115.6(8) . . ?
N1 N2 H2A 120.7 . . ?
C12 N2 N1 118.6(7) . . ?
C12 N2 H2A 120.7 . . ?
N5 N4 Cu2 116.0(6) . . ?
C13 N4 Cu2 128.1(7) . . ?
C13 N4 N5 115.8(8) . . ?
N4 N5 H5 120.3 . . ?
C14 N5 N4 119.2(8) . . ?
C14 N5 H5 120.5 . . ?
H6A N6 H6B 120.0 . . ?
C14 N6 H6A 120.0 . . ?
C14 N6 H6B 119.9 . . ?
C17 O14 H14 111.9 . . ?
H3A N3 H3B 120.0 . . ?
C12 N3 H3A 120.0 . . ?
C12 N3 H3B 120.0 . . ?
O1 C1 C6 123.9(8) . . ?
O1 C1 C2 119.3(8) . . ?
C6 C1 C2 116.8(8) . . ?
N4 C13 H13 116.6 . . ?
N4 C13 C2 126.7(9) . . ?
C2 C13 H13 116.6 . . ?
C1 C6 C11 122.4(8) . . ?
C5 C6 C1 120.8(9) . . ?
C5 C6 C11 116.7(8) . . ?
N2 C12 S1 122.0(7) . . ?
N3 C12 S1 120.0(7) . . ?
N3 C12 N2 118.0(8) . . ?
C1 C2 C13 123.5(8) . . ?
C3 C2 C1 119.4(8) . . ?
C3 C2 C13 117.1(8) . . ?
N5 C14 S2 121.3(7) . . ?
N6 C14 S2 120.3(7) . . ?
N6 C14 N5 118.5(9) . . ?
N1 C11 C6 125.6(8) . . ?
N1 C11 H11 117.2 . . ?
C6 C11 H11 117.2 . . ?
C4 C3 C2 122.9(9) . . ?
C6 C5 C4 123.1(9) . . ?
C3 C4 C5 116.9(9) . . ?
C3 C4 C7 120.6(9) . . ?
C5 C4 C7 122.5(9) . . ?
C15 O13 H13A 108.0 . . ?
O13 C15 H15A 108.2 . . ?
O13 C15 H15B 108.2 . . ?
O13 C15 C16 116.2(10) . . ?
H15A C15 H15B 107.4 . . ?
C16 C15 H15A 108.2 . . ?
C16 C15 H15B 108.2 . . ?
O14 C17 H17A 108.5 . . ?
O14 C17 H17B 108.5 . . ?
O14 C17 C18 114.9(10) . . ?
H17A C17 H17B 107.5 . . ?
C18 C17 H17A 108.5 . . ?
C18 C17 H17B 108.5 . . ?
C4 C7 C10X 111.0(12) . . ?
C4 C7 C8X 106.8(13) . . ?
C4 C7 C9 109.3(13) . . ?
C4 C7 C10 104.1(14) . . ?
C10X C7 C8X 106.3(9) . . ?
C9 C7 C10 107.3(9) . . ?
C8 C7 C4 118.1(14) . . ?
C8 C7 C9 109.1(9) . . ?
C8 C7 C10 108.4(9) . . ?
C9X C7 C4 117.1(13) . . ?
C9X C7 C10X 107.8(9) . . ?
C9X C7 C8X 107.4(9) . . ?
C17 C18 H18A 111.2 . . ?
C17 C18 H18B 112.6 . . ?
C17 C18 H18C 104.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.4 . . ?
C7 C10X H10A 110.1 . . ?
C7 C10X H10B 108.8 . . ?
C7 C10X H10C 109.6 . . ?
H10A C10X H10B 109.5 . . ?
H10A C10X H10C 109.5 . . ?
H10B C10X H10C 109.5 . . ?
C7 C8X H8XA 109.3 . . ?
C7 C8X H8XB 109.9 . . ?
C7 C8X H8XC 109.3 . . ?
H8XA C8X H8XB 109.5 . . ?
H8XA C8X H8XC 109.5 . . ?
H8XB C8X H8XC 109.5 . . ?
C15 C16 H16A 114.5 . . ?
C15 C16 H16B 101.4 . . ?
C15 C16 H16C 112.2 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.4 . . ?
C7 C9 H9A 109.7 . . ?
C7 C9 H9B 110.5 . . ?
C7 C9 H9C 108.2 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.4 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10D 110.5 . . ?
C7 C10 H10E 108.6 . . ?
C7 C10 H10F 109.4 . . ?
H10D C10 H10E 109.5 . . ?
H10D C10 H10F 109.5 . . ?
H10E C10 H10F 109.5 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
C7 C8 H8C 108.4 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9X H9XA 109.5 . . ?
C7 C9X H9XB 109.5 . . ?
C7 C9X H9XC 109.5 . . ?
H9XA C9X H9XB 109.5 . . ?
H9XA C9X H9XC 109.5 . . ?
H9XB C9X H9XC 109.5 . . ?
H17C C17X H17D 107.2 . . ?
O14X C17X H17C 108.0 . . ?
O14X C17X H17D 108.0 . . ?
O14X C17X C18X 117.4(12) . . ?
C18X C17X H17C 108.0 . . ?
C18X C17X H17D 108.0 . . ?
C17X O14X H14X 110.6 . . ?
C17X C18X H18D 114.6 . . ?
C17X C18X H18E 113.5 . . ?
C17X C18X H18F 99.9 . . ?
H18D C18X H18E 109.4 . . ?
H18D C18X H18F 109.5 . . ?
H18E C18X H18F 109.5 . . ?
C15X O13X H13X 109.2 . . ?
O13X C15X H15C 107.9 . . ?
O13X C15X H15D 107.9 . . ?
O13X C15X C16X 117.6(12) . . ?
H15C C15X H15D 107.2 . . ?
C16X C15X H15C 107.9 . . ?
C16X C15X H15D 107.9 . . ?
C15X C16X H16D 120.8 . . ?
C15X C16X H16E 88.5 . . ?
C15X C16X H16F 116.6 . . ?
H16D C16X H16E 109.5 . . ?
H16D C16X H16F 109.5 . . ?
H16E C16X H16F 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 S1 2.257(2) . ?
Cu1 O1 1.966(6) . ?
Cu1 O2 1.904(6) . ?
Cu1 N1 1.930(8) . ?
Cu2 S2 2.255(3) . ?
Cu2 O1 1.976(6) . ?
Cu2 O2 2.560(6) 2_666 ?
Cu2 O2 1.918(6) . ?
Cu2 N4 1.906(8) . ?
S1 C12 1.725(10) . ?
S2 C14 1.717(9) . ?
Cl1 O5 1.396(8) . ?
Cl1 O4 1.398(8) . ?
Cl1 O3 1.523(13) . ?
Cl1 O6 1.293(12) . ?
Cl2 O7 1.432(7) . ?
Cl2 O12 1.438(9) . ?
Cl2 O9 1.423(10) . ?
Cl2 O8 1.440(10) . ?
Cl2 O10 1.437(10) . ?
Cl2 O11 1.422(9) . ?
O1 C1 1.305(11) . ?
O2 H2 0.8484 . ?
O40 H40A 0.8657 . ?
O40 H40B 0.8563 . ?
N1 N2 1.394(10) . ?
N1 C11 1.274(12) . ?
N2 H2A 0.8800 . ?
N2 C12 1.336(11) . ?
N4 N5 1.406(10) . ?
N4 C13 1.269(12) . ?
N5 H5 0.8799 . ?
N5 C14 1.321(12) . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8797 . ?
N6 C14 1.314(11) . ?
O14 H14 0.8584 . ?
O14 C17 1.426(9) . ?
N3 H3A 0.8801 . ?
N3 H3B 0.8800 . ?
N3 C12 1.328(11) . ?
C1 C6 1.403(13) . ?
C1 C2 1.441(12) . ?
C13 H13 0.9500 . ?
C13 C2 1.455(13) . ?
C6 C11 1.460(13) . ?
C6 C5 1.384(13) . ?
C2 C3 1.406(13) . ?
C11 H11 0.9500 . ?
C3 C4 1.371(14) . ?
C5 C4 1.387(14) . ?
C4 C7 1.521(15) . ?
O13 H13A 0.8730 . ?
O13 C15 1.406(10) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.522(10) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.524(10) . ?
C7 C10X 1.525(14) . ?
C7 C8X 1.530(14) . ?
C7 C9 1.524(14) . ?
C7 C10 1.531(14) . ?
C7 C8 1.510(14) . ?
C7 C9X 1.514(13) . ?
C18 H18A 0.9798 . ?
C18 H18B 0.9802 . ?
C18 H18C 0.9801 . ?
C10X H10A 0.9800 . ?
C10X H10B 0.9803 . ?
C10X H10C 0.9800 . ?
C8X H8XA 0.9800 . ?
C8X H8XB 0.9800 . ?
C8X H8XC 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9801 . ?
C16 H16C 0.9801 . ?
C9 H9A 0.9802 . ?
C9 H9B 0.9798 . ?
C9 H9C 0.9802 . ?
C10 H10D 0.9800 . ?
C10 H10E 0.9800 . ?
C10 H10F 0.9800 . ?
C8 H8A 0.9798 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9X H9XA 0.9800 . ?
C9X H9XB 0.9800 . ?
C9X H9XC 0.9800 . ?
C17X H17C 0.9900 . ?
C17X H17D 0.9900 . ?
C17X O14X 1.402(10) . ?
C17X C18X 1.521(10) . ?
O14X H14X 0.8462 . ?
C18X H18D 0.9800 . ?
C18X H18E 0.9799 . ?
C18X H18F 0.9799 . ?
O13X H13X 0.9290 . ?
O13X C15X 1.401(10) . ?
C15X H15C 0.9900 . ?
C15X H15D 0.9900 . ?
C15X C16X 1.520(10) . ?
C16X H16D 0.9801 . ?
C16X H16E 0.9796 . ?
C16X H16F 0.9801 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O12 0.85 2.36 3.03(2) 136.6 2_666 yes
O2 H2 O10 0.85 2.40 3.02(2) 129.7 2_666 yes
O2 H2 O11 0.85 2.09 2.688(18) 127.6 2_666 yes
O40 H40A Cl1 0.87 2.81 3.641(8) 161.3 . yes
O40 H40A O5 0.87 2.55 3.198(12) 131.9 . yes
O40 H40A O3 0.87 2.10 2.917(15) 157.6 . yes
O40 H40B O13 0.86 1.88 2.715(14) 166.4 1_665 yes
O40 H40B O13X 0.86 2.27 3.08(5) 156.7 1_665 yes
N2 H2A O5 0.88 2.37 3.035(11) 133.1 1_545 yes
N2 H2A O7 0.88 2.36 3.053(12) 135.4 1_655 yes
N5 H5 O14 0.88 1.88 2.719(13) 158.9 1_455 yes
N5 H5 O14X 0.88 2.10 2.96(7) 163.1 1_455 yes
N6 H6A O40 0.88 2.02 2.877(10) 163.7 1_455 yes
N6 H6B O6 0.88 2.04 2.889(13) 160.8 2_676 yes
O14 H14 O13X 0.86 2.22 2.95(8) 143.1 1_665 yes
N3 H3A O40 0.88 1.96 2.836(11) 173.2 1_545 yes
N3 H3B O3 0.88 2.19 3.011(14) 154.5 2_766 yes
C13 H13 O14 0.95 2.51 3.273(15) 136.9 1_455 yes
C13 H13 O14X 0.95 2.50 3.34(9) 148.0 1_455 yes
C11 H11 O7 0.95 2.47 3.211(13) 134.3 1_655 yes
O13 H13A Cl2 0.87 2.77 3.560(16) 152.1 . yes
O13 H13A O7 0.87 1.94 2.777(17) 160.9 . yes
C15 H15A O9 0.99 2.59 3.15(3) 116.0 . yes
O14X H14X O13 0.85 1.55 2.37(8) 164.5 1_665 yes
O13X H13X Cl2 0.93 2.84 3.77(7) 173.1 . yes
O13X H13X O7 0.93 2.41 3.21(7) 144.5 . yes
O13X H13X O10 0.93 2.41 3.29(8) 156.5 . yes
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 S1 C12 N2 -2.1(7) . . . . ?
Cu1 S1 C12 N3 177.2(7) . . . . ?
Cu1 O1 C1 C6 -6.2(12) . . . . ?
Cu1 O1 C1 C2 175.2(6) . . . . ?
Cu1 N1 N2 C12 6.1(10) . . . . ?
Cu1 N1 C11 C6 -7.6(13) . . . . ?
Cu2 S2 C14 N5 4.5(7) . . . . ?
Cu2 S2 C14 N6 -175.9(7) . . . . ?
Cu2 O1 C1 C6 177.5(6) . . . . ?
Cu2 O1 C1 C2 -1.0(12) . . . . ?
Cu2 N4 N5 C14 -6.0(10) . . . . ?
Cu2 N4 C13 C2 -0.4(14) . . . . ?
O1 C1 C6 C11 3.8(14) . . . . ?
O1 C1 C6 C5 -177.5(8) . . . . ?
O1 C1 C2 C13 -1.4(13) . . . . ?
O1 C1 C2 C3 179.4(8) . . . . ?
N1 N2 C12 S1 -2.1(11) . . . . ?
N1 N2 C12 N3 178.6(7) . . . . ?
N2 N1 C11 C6 176.4(8) . . . . ?
N4 N5 C14 S2 0.0(11) . . . . ?
N4 N5 C14 N6 -179.5(7) . . . . ?
N4 C13 C2 C1 2.3(15) . . . . ?
N4 C13 C2 C3 -178.5(9) . . . . ?
N5 N4 C13 C2 180.0(8) . . . . ?
C1 C6 C11 N1 3.4(14) . . . . ?
C1 C6 C5 C4 -2.3(15) . . . . ?
C1 C2 C3 C4 -1.6(15) . . . . ?
C13 N4 N5 C14 173.7(8) . . . . ?
C13 C2 C3 C4 179.2(9) . . . . ?
C6 C1 C2 C13 179.9(8) . . . . ?
C6 C1 C2 C3 0.7(13) . . . . ?
C6 C5 C4 C3 1.5(16) . . . . ?
C6 C5 C4 C7 -178.2(10) . . . . ?
C2 C1 C6 C11 -177.6(8) . . . . ?
C2 C1 C6 C5 1.1(13) . . . . ?
C2 C3 C4 C5 0.5(16) . . . . ?
C2 C3 C4 C7 -179.8(10) . . . . ?
C11 N1 N2 C12 -177.3(8) . . . . ?
C11 C6 C5 C4 176.4(9) . . . . ?
C3 C4 C7 C10X -57.8(15) . . . . ?
C3 C4 C7 C8X 57.6(14) . . . . ?
C3 C4 C7 C9 123.8(14) . . . . ?
C3 C4 C7 C10 -121.8(14) . . . . ?
C3 C4 C7 C8 -1.6(17) . . . . ?
C3 C4 C7 C9X 178.0(13) . . . . ?
C5 C6 C11 N1 -175.4(9) . . . . ?
C5 C4 C7 C10X 121.9(13) . . . . ?
C5 C4 C7 C8X -122.6(13) . . . . ?
C5 C4 C7 C9 -56.5(15) . . . . ?
C5 C4 C7 C10 57.9(15) . . . . ?
C5 C4 C7 C8 178.1(14) . . . . ?
C5 C4 C7 C9X -2.3(17) . . . . ?
