#------------------------------------------------------------------------------
#$Date: 2024-07-05 19:42:27 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293112 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/57/7715752.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_7715752
loop_
_publ_author_name
'Geoghegan, Blaise L.'
'Bilyj, Jessica K.'
'Bernhardt, Paul V.'
'DeBeer, Serena'
'Cutsail, 3rd, George E'
_publ_section_title
;
 X-ray absorption and emission spectroscopy of N₂S₂
 Cu(II)/(III) complexes.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7828
_journal_page_last               7838
_journal_paper_doi               10.1039/d4dt00085d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C9 H14 Cu N4 S4'
_chemical_formula_weight         370.02
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2022-08-05T10:35:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2022-09-01 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   46.877(9)
_cell_length_b                   6.9630(14)
_cell_length_c                   8.8140(18)
_cell_measurement_reflns_used    6678
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.27
_cell_measurement_theta_min      3.85
_cell_measurement_wavelength     0.7108
_cell_volume                     2876.9(10)
_computing_cell_refinement       'CrysalisPro (Agilent Technologies,     )'
_computing_data_collection       'CrysalisPro (Agilent Technologies,     )'
_computing_data_reduction        'CrysalisPro (Agilent Technologies,     )'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.02
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Dectris Eiger 9M'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.016045
_diffrn_orient_matrix_UB_12      -0.045568
_diffrn_orient_matrix_UB_13      0.037321
_diffrn_orient_matrix_UB_21      0.098656
_diffrn_orient_matrix_UB_22      -0.017447
_diffrn_orient_matrix_UB_23      -0.007141
_diffrn_orient_matrix_UB_31      0.028609
_diffrn_orient_matrix_UB_32      0.034575
_diffrn_orient_matrix_UB_33      0.04552
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            35983
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         0.869
_diffrn_source                   Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.085
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1512
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeCN'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.087
_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_constraints    0
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0601P)²+2.4243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1095
_reflns_Friedel_coverage         0
_reflns_number_gt                2636
_reflns_number_total             3366
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00085d2.cif
_cod_data_source_block           PB1_Pnma
_cod_depositor_comments
'Adding full bibliography for 7715751--7715752.cif.'
_cod_database_code               7715752
_shelx_shelxl_version_number     2018/1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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
C1A C 0.09469(10) 0.25 0.3935(5) 0.0402(11) Uani 1 2 d S T P . .
H1A1 H 0.09578 0.363792 0.326377 0.048 Uiso 0.5 1 calc R U P . .
H1A2 H 0.09578 0.136208 0.326377 0.048 Uiso 0.5 1 calc R U P . .
C2A C 0.12180(10) 0.25 0.4852(5) 0.0373(10) Uani 1 2 d S T P . .
C3A C 0.14880(10) 0.25 0.3933(6) 0.0437(12) Uani 1 2 d S T P . .
H3A1 H 0.144039 0.25 0.285029 0.066 Uiso 1 2 calc R U P . .
H3A2 H 0.15998 0.364917 0.417456 0.066 Uiso 0.5 1 calc R U P . .
H3A3 H 0.15998 0.135083 0.417456 0.066 Uiso 0.5 1 calc R U P . .
C4A C 0.14981(10) 0.25 0.8387(5) 0.0373(10) Uani 1 2 d S T P . .
C5A C 0.06536(10) 0.25 0.4584(5) 0.0391(11) Uani 1 2 d S T P . .
C6A C 0.04190(11) 0.25 0.3431(5) 0.0484(13) Uani 1 2 d S T P . .
H6A1 H 0.050151 0.25 0.24097 0.073 Uiso 1 2 calc R U P . .
H6A2 H 0.03009 0.135083 0.356471 0.073 Uiso 0.5 1 calc R U P . .
H6A3 H 0.03009 0.364917 0.356471 0.073 Uiso 0.5 1 calc R U P . .
C7A C 0.02597(10) 0.25 0.7834(5) 0.0338(10) Uani 1 2 d S T P . .
C8A C 0.20721(11) 0.25 0.7731(6) 0.0485(13) Uani 1 2 d S T P . .
H8A1 H 0.226864 0.25 0.810975 0.073 Uiso 1 2 calc R U P . .
H8A2 H 0.204011 0.135083 0.711211 0.073 Uiso 0.5 1 calc R U P . .
H8A3 H 0.204012 0.364917 0.711211 0.073 Uiso 0.5 1 calc R U P . .
C9A C -0.01134(11) 0.25 1.0326(5) 0.0444(12) Uani 1 2 d S T P . .
H9A1 H -0.031192 0.25 1.067488 0.067 Uiso 1 2 calc R U P . .
H9A2 H -0.001633 0.135083 1.070745 0.067 Uiso 0.5 1 calc R U P . .
H9A3 H -0.001633 0.364917 1.070745 0.067 Uiso 0.5 1 calc R U P . .
N1A N 0.12177(8) 0.25 0.6309(4) 0.0384(9) Uani 1 2 d S T P . .
N2A N 0.14938(8) 0.25 0.6932(4) 0.0388(9) Uani 1 2 d S T P . .
N3A N 0.06023(8) 0.25 0.6014(4) 0.0336(8) Uani 1 2 d S T P . .
N4A N 0.03086(8) 0.25 0.6390(4) 0.0386(9) Uani 1 2 d S T P . .
Cu1A Cu 0.08867(2) 0.25 0.76692(6) 0.03496(17) Uani 1 2 d S T P . .
S1A S 0.12016(3) 0.25 0.95959(13) 0.0424(3) Uani 1 2 d S T P . .
S2A S 0.18258(3) 0.25 0.93269(14) 0.0424(3) Uani 1 2 d S T P . .
S3A S 0.05141(3) 0.25 0.92654(13) 0.0453(3) Uani 1 2 d S T P . .
S4A S -0.01054(3) 0.25 0.82774(14) 0.0391(3) Uani 1 2 d S T P . .
C1B C -0.14420(10) 0.25 -0.0373(5) 0.0405(11) Uani 1 2 d S T P . .
H1B1 H -0.141907 0.13632 -0.103608 0.049 Uiso 0.5 1 calc R U P . .
H1B2 H -0.141907 0.36368 -0.103608 0.049 Uiso 0.5 1 calc R U P . .
C2B C -0.11929(11) 0.25 0.0637(5) 0.0392(11) Uani 1 2 d S T P . .
C3B C -0.09073(11) 0.25 -0.0137(6) 0.0446(12) Uani 1 2 d S T P . .
H3B1 H -0.093465 0.25 -0.123905 0.067 Uiso 1 2 calc R U P . .
H3B2 H -0.080044 0.364917 0.016203 0.067 Uiso 0.5 1 calc R U P . .
H3B3 H -0.080044 0.135083 0.016203 0.067 Uiso 0.5 1 calc R U P . .
C4B C -0.09749(10) 0.25 0.4341(5) 0.0343(10) Uani 1 2 d S T P . .
C5B C -0.17458(11) 0.25 0.0105(5) 0.0382(11) Uani 1 2 d S T P . .
C6B C -0.19599(12) 0.25 -0.1151(5) 0.0488(13) Uani 1 2 d S T P . .
H6B1 H -0.186062 0.25 -0.212927 0.073 Uiso 1 2 calc R U P . .
H6B2 H -0.207967 0.135083 -0.107319 0.073 Uiso 0.5 1 calc R U P . .
H6B3 H -0.207967 0.364917 -0.107319 0.073 Uiso 0.5 1 calc R U P . .
C7B C -0.21959(10) 0.25 0.3113(5) 0.0380(11) Uani 1 2 d S T P . .
C8B C -0.03815(10) 0.25 0.4151(5) 0.0430(11) Uani 1 2 d S T P . .
H8B1 H -0.019956 0.25 0.469834 0.065 Uiso 1 2 calc R U P . .
H8B2 H -0.039359 0.135083 0.351188 0.065 Uiso 0.5 1 calc R U P . .
H8B3 H -0.039359 0.364917 0.351189 0.065 Uiso 0.5 1 calc R U P . .
C9B C -0.27167(12) 0.25 0.1681(7) 0.0638(17) Uani 1 2 d S T P . .
H9B1 H -0.292508 0.25 0.177304 0.096 Uiso 1 2 calc R U P . .
H9B2 H -0.265546 0.364917 0.112786 0.096 Uiso 0.5 1 calc R U P . .
H9B3 H -0.265546 0.135083 0.112786 0.096 Uiso 0.5 1 calc R U P . .
N1B N -0.12135(8) 0.25 0.2115(4) 0.0366(9) Uani 1 2 d S T P . .
N2B N -0.09480(8) 0.25 0.2875(4) 0.0401(10) Uani 1 2 d S T P . .
N3B N -0.18200(9) 0.25 0.1518(4) 0.0385(9) Uani 1 2 d S T P . .
N4B N -0.21181(8) 0.25 0.1720(5) 0.0389(9) Uani 1 2 d S T P . .
Cu1B Cu -0.15701(2) 0.25 0.33047(6) 0.03462(17) Uani 1 2 d S T P . .
S1B S -0.12887(3) 0.25 0.53686(13) 0.0388(3) Uani 1 2 d S T P . .
S2B S -0.06690(3) 0.25 0.54804(13) 0.0398(3) Uani 1 2 d S T P . .
S3B S -0.19727(3) 0.25 0.46919(13) 0.0453(3) Uani 1 2 d S T P . .
S4B S -0.25590(3) 0.25 0.35454(16) 0.0510(4) Uani 1 2 d S T P . .
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 0 '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'
Cu Cu 0.3201 1.2651 '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
C5A C1A C2A 124.9(4) . . ?
N1A C2A C3A 122.7(5) . . ?
N1A C2A C1A 122.4(4) . . ?
C3A C2A C1A 114.9(4) . . ?
N2A C4A S2A 119.2(4) . . ?
N2A C4A S1A 126.6(4) . . ?
S2A C4A S1A 114.2(3) . . ?
N3A C5A C1A 123.4(4) . . ?
N3A C5A C6A 121.9(4) . . ?
C1A C5A C6A 114.7(4) . . ?
N4A C7A S3A 126.4(4) . . ?
N4A C7A S4A 113.1(3) . . ?
S3A C7A S4A 120.5(3) . . ?
C2A N1A N2A 112.9(4) . . ?
C2A N1A Cu1A 127.8(3) . . ?
N2A N1A Cu1A 119.3(3) . . ?
C4A N2A N1A 113.9(4) . . ?
C5A N3A N4A 114.3(4) . . ?
C5A N3A Cu1A 126.8(3) . . ?
N4A N3A Cu1A 118.9(3) . . ?
C7A N4A N3A 113.7(4) . . ?
N1A Cu1A N3A 94.73(16) . . ?
N1A Cu1A S3A 178.84(12) . . ?
N3A Cu1A S3A 86.43(11) . . ?
N1A Cu1A S1A 86.69(12) . . ?
N3A Cu1A S1A 178.59(11) . . ?
S3A Cu1A S1A 92.15(5) . . ?
C4A S1A Cu1A 93.53(16) . . ?
C4A S2A C8A 101.1(2) . . ?
C7A S3A Cu1A 94.54(16) . . ?
C7A S4A C9A 104.0(2) . . ?
C2B C1B C5B 126.2(4) . . ?
N1B C2B C1B 123.0(4) . . ?
N1B C2B C3B 121.3(4) . . ?
C1B C2B C3B 115.7(4) . . ?
N2B C4B S1B 127.2(4) . . ?
N2B C4B S2B 119.4(3) . . ?
S1B C4B S2B 113.4(2) . . ?
N3B C5B C1B 122.1(4) . . ?
N3B C5B C6B 122.2(5) . . ?
C1B C5B C6B 115.7(4) . . ?
N4B C7B S3B 126.5(4) . . ?
N4B C7B S4B 119.2(4) . . ?
S3B C7B S4B 114.3(3) . . ?
C2B N1B N2B 114.0(4) . . ?
C2B N1B Cu1B 126.4(3) . . ?
N2B N1B Cu1B 119.6(3) . . ?
C4B N2B N1B 112.7(4) . . ?
C5B N3B N4B 112.9(4) . . ?
C5B N3B Cu1B 127.8(4) . . ?
N4B N3B Cu1B 119.4(3) . . ?
C7B N4B N3B 113.8(4) . . ?
N3B Cu1B N1B 94.54(16) . . ?
N3B Cu1B S1B 179.31(12) . . ?
N1B Cu1B S1B 86.15(11) . . ?
N3B Cu1B S3B 86.30(12) . . ?
N1B Cu1B S3B 179.17(11) . . ?
S1B Cu1B S3B 93.01(5) . . ?
C4B S1B Cu1B 94.34(15) . . ?
C4B S2B C8B 104.0(2) . . ?
C7B S3B Cu1B 94.00(17) . . ?
C7B S4B C9B 101.6(3) . . ?
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
C1A C5A 1.489(7) . ?
C1A C2A 1.506(7) . ?
C2A N1A 1.284(6) . ?
C2A C3A 1.503(6) . ?
C4A N2A 1.283(6) . ?
C4A S2A 1.745(5) . ?
C4A S1A 1.751(5) . ?
C5A N3A 1.283(6) . ?
C5A C6A 1.498(6) . ?
C7A N4A 1.293(6) . ?
C7A S3A 1.736(5) . ?
C7A S4A 1.756(5) . ?
C8A S2A 1.820(5) . ?
C9A S4A 1.806(5) . ?
N1A N2A 1.406(5) . ?
N1A Cu1A 1.961(4) . ?
N3A N4A 1.416(5) . ?
N3A Cu1A 1.976(4) . ?
Cu1A S3A 2.2427(14) . ?
Cu1A S1A 2.2503(13) . ?
C1B C2B 1.468(7) . ?
C1B C5B 1.485(7) . ?
C2B N1B 1.306(6) . ?
C2B C3B 1.502(6) . ?
C4B N2B 1.299(6) . ?
C4B S1B 1.727(5) . ?
C4B S2B 1.750(4) . ?
C5B N3B 1.293(6) . ?
C5B C6B 1.494(7) . ?
C7B N4B 1.281(6) . ?
C7B S3B 1.741(5) . ?
C7B S4B 1.744(5) . ?
C8B S2B 1.786(5) . ?
C9B S4B 1.802(6) . ?
N1B N2B 1.414(5) . ?
N1B Cu1B 1.973(4) . ?
N3B N4B 1.409(6) . ?
N3B Cu1B 1.963(4) . ?
Cu1B S1B 2.2471(13) . ?
Cu1B S3B 2.2487(14) . ?
