Trivalent copper stabilised by acetylacetone dithiocarbazate Schiff base ligands: structural, spectroscopic and electrochemical properties.
Bilyj, Jessica K.; Silajew, Nicole V.; Hanson, Graeme R.; Harmer, Jeffrey R.; Bernhardt, Paul V.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15501–15514; doi:10.1039/c9dt02071c

data_7700421
_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
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_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       '\k-geometry diffractometer'
_diffrn_measurement_device_type
'Agilent Technologies Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w 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/[\s^2^(Fo^2^)+(0.0337P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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