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_7700422
_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 H13 Cu N4 S4'
_chemical_formula_weight         369.01
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
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_audit_creation_date             2019-05-17T15:44:36-00:00
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;
2019-05-17 deposited with the CCDC.    2019-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                106.962(6)
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_cell_angle_gamma                90.272(6)
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_cell_length_b                   8.7981(6)
_cell_length_c                   11.6005(9)
_cell_measurement_reflns_used    1891
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      61.99
_cell_measurement_theta_min      4.18
_cell_measurement_wavelength     1.54184
_cell_volume                     704.04(11)
_computing_cell_refinement
'CrysalisPro  Version 1.171.36.28 (Agilent Technologies, 2013)'
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'CrysalisPro  Version 1.171.36.28 (Agilent Technologies, 2013)'
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'CrysalisPro  Version 1.171.36.28 (Agilent Technologies, 2013)'
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_diffrn_ambient_temperature      190(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.07
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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      -0.088468
_diffrn_orient_matrix_UB_12      0.082139
_diffrn_orient_matrix_UB_13      -0.100727
_diffrn_orient_matrix_UB_21      -0.189484
_diffrn_orient_matrix_UB_22      -0.021367
_diffrn_orient_matrix_UB_23      0.019994
_diffrn_orient_matrix_UB_31      0.043595
_diffrn_orient_matrix_UB_32      0.163225
_diffrn_orient_matrix_UB_33      0.103782
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4546
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_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        62.468
_diffrn_reflns_theta_max         62.468
_diffrn_reflns_theta_min         4.19
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.63
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.381
_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            brown
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.875
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0738P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.106
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0
_reflns_number_gt                1939
_reflns_number_total             2215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02071c2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7700420--7700423.cif.'
_cod_original_cell_volume        704.04(10)
_cod_database_code               7700422
_shelx_shelxl_version_number     2018/1