#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:55:18 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223893 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/04/7700421.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_7700421
loop_
_publ_author_name
'Bilyj, Jessica K.'
'Silajew, Nicole V.'
'Hanson, Graeme R.'
'Harmer, Jeffrey R.'
'Bernhardt, Paul V.'
_publ_section_title
;
 Trivalent copper stabilised by acetylacetone dithiocarbazate Schiff base
 ligands: structural, spectroscopic and electrochemical properties.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15501
_journal_page_last               15514
_journal_paper_doi               10.1039/c9dt02071c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C9 H12 Cu N4 O S4'
_chemical_formula_weight         384.01
_space_group_IT_number           62
_space_group_name_Hall           '-P 2c 2n'
_space_group_name_H-M_alt        'P n a m'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2c 2n'
_symmetry_space_group_name_H-M   'P n a m'
_atom_sites_solution_hydrogens   geom
_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             2019-05-17T15:33:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-05-17 deposited with the CCDC.    2019-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3466(5)
_cell_length_b                   12.2444(4)
_cell_length_c                   6.9842(3)
_cell_measurement_reflns_used    1329
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      62.35
_cell_measurement_theta_min      4.42
_cell_measurement_wavelength     1.5418
_cell_volume                     1483.44(9)
_computing_cell_refinement
'CrysalisPro  Version 1.171.36.28 (Agilent Technologies, 2013)'
_computing_data_collection
'CrysalisPro  Version 1.171.36.28 (Agilent Technologies, 2013)'
_computing_data_reduction
'CrysalisPro  Version 1.171.36.28 (Agilent Technologies, 2013)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.07
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type
'Agilent Technologies Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.044361
_diffrn_orient_matrix_UB_12      -0.10886
_diffrn_orient_matrix_UB_13      -0.007222
_diffrn_orient_matrix_UB_21      -0.076895
_diffrn_orient_matrix_UB_22      0.062935
_diffrn_orient_matrix_UB_23      -0.003418
_diffrn_orient_matrix_UB_31      0.00263
_diffrn_orient_matrix_UB_32      0.002584
_diffrn_orient_matrix_UB_33      -0.220514
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3990
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_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        62.499
_diffrn_reflns_theta_max         62.499
_diffrn_reflns_theta_min         4.42
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.324
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0323
_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)+(0.0337P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0
_reflns_number_gt                958
_reflns_number_total             1283
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02071c2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7700420--7700423.cif.'
_cod_original_sg_symbol_H-M      Pnam
_cod_database_code               7700421
_shelx_shelxl_version_number     2018/1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x-1/2, -y-1/2, 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
C1 C 0.5864(3) 0.5771(4) 0.25 0.0505(11) Uani 1 2 d S T P
C2 C 0.3911(2) 0.5624(4) 0.25 0.0517(11) Uani 1 2 d S T P
C3 C 0.3243(3) 0.4856(4) 0.25 0.0569(13) Uani 1 2 d S T P
C4 C 0.3276(2) 0.3632(4) 0.25 0.0521(12) Uani 1 2 d S T P
C5 C 0.4492(3) 0.1461(4) 0.25 0.0554(12) Uani 1 2 d S T P
C6 C 0.3718(3) 0.6807(4) 0.25 0.0641(14) Uani 1 2 d S T P
H6A H 0.315608 0.689601 0.25 0.096 Uiso 1 2 calc R U P
H6B H 0.393434 0.715204 0.364568 0.096 Uiso 0.5 1 calc R U P
H6C H 0.393434 0.715204 0.135432 0.096 Uiso 0.5 1 calc R U P
C7 C 0.2517(2) 0.3058(5) 0.25 0.0711(16) Uani 1 2 d S T P
H7A H 0.20998 0.359807 0.25 0.107 Uiso 1 2 calc R U P
H7B H 0.247602 0.259952 0.135432 0.107 Uiso 0.5 1 calc R U P
H7C H 0.247602 0.259952 0.364568 0.107 Uiso 0.5 1 calc R U P
C8 C 0.6072(3) 0.8009(4) 0.25 0.0736(16) Uani 1 2 d S T P
H8A H 0.643622 0.862062 0.25 0.11 Uiso 1 2 calc R U P
H8B H 0.5747 0.80481 0.135432 0.11 Uiso 0.5 1 calc R U P
H8C H 0.5747 0.80481 0.364568 0.11 Uiso 0.5 1 calc R U P
C9 C 0.3441(4) -0.0207(5) 0.25 0.120(3) Uani 1 2 d S T P
H9A H 0.334908 -0.099653 0.25 0.18 Uiso 1 2 calc R U P
H9B H 0.320834 0.011766 0.364568 0.18 Uiso 0.5 1 calc R U P
H9C H 0.320834 0.011766 0.135432 0.18 Uiso 0.5 1 calc R U P
O1 O 0.2608(2) 0.5255(3) 0.25 0.1085(18) Uani 1 2 d S T P
Cu1 Cu 0.49832(3) 0.37348(5) 0.25 0.0489(2) Uani 1 2 d S T P
N1 N 0.5160(2) 0.6104(3) 0.25 0.0578(10) Uani 1 2 d S T P
N2 N 0.46140(19) 0.5269(3) 0.25 0.0510(10) Uani 1 2 d S T P
N3 N 0.39250(18) 0.3111(3) 0.25 0.0479(9) Uani 1 2 d S T P
N4 N 0.3844(2) 0.1996(3) 0.25 0.0549(10) Uani 1 2 d S T P
S1 S 0.61817(6) 0.44345(10) 0.25 0.0604(4) Uani 1 2 d S T P
S2 S 0.54026(6) 0.20045(10) 0.25 0.0716(4) Uani 1 2 d S T P
S3 S 0.65947(7) 0.67458(11) 0.25 0.0632(4) Uani 1 2 d S T P
S4 S 0.44532(9) 0.00500(11) 0.25 0.0857(5) 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 0.0181 0.0091 '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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
N1 C1 S1 127.1(4)
N1 C1 S3 118.3(4)
S1 C1 S3 114.7(3)
N2 C2 C6 122.7(4)
N2 C2 C3 121.3(4)
C6 C2 C3 116.0(4)
O1 C3 C2 117.0(4)
O1 C3 C4 116.1(4)
C2 C3 C4 126.9(4)
N3 C4 C7 122.4(4)
N3 C4 C3 121.6(4)
C7 C4 C3 116.0(4)
N4 C5 S2 126.9(3)
N4 C5 S4 118.0(3)
S2 C5 S4 115.1(3)
N2 Cu1 N3 93.76(14)
N2 Cu1 S2 179.87(11)
N3 Cu1 S2 86.37(11)
N2 Cu1 S1 86.43(11)
N3 Cu1 S1 179.81(11)
S2 Cu1 S1 93.44(5)
C1 N1 N2 114.3(4)
C2 N2 N1 113.1(4)
C2 N2 Cu1 128.5(3)
N1 N2 Cu1 118.4(3)
C4 N3 N4 113.6(3)
C4 N3 Cu1 127.9(3)
N4 N3 Cu1 118.4(3)
C5 N4 N3 114.4(4)
C1 S1 Cu1 93.79(15)
C5 S2 Cu1 93.87(16)
C1 S3 C8 102.9(2)
C5 S4 C9 102.4(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.289(6)
C1 S1 1.727(5)
C1 S3 1.741(4)
C2 N2 1.294(6)
C2 C6 1.486(6)
C2 C3 1.493(7)
C3 O1 1.206(6)
C3 C4 1.500(7)
C4 N3 1.294(6)
C4 C7 1.492(6)
C5 N4 1.300(6)
C5 S2 1.714(5)
C5 S4 1.730(5)
C8 S3 1.793(6)
C9 S4 1.784(7)
Cu1 N2 1.984(3)
Cu1 N3 1.988(3)
Cu1 S2 2.2401(13)
Cu1 S1 2.2487(12)
N1 N2 1.394(5)
N3 N4 1.373(5)
