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_7700420
_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            'C21 H22 Cu N4 S4'
_chemical_formula_weight         522.2
_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
_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
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_audit_creation_date             2019-05-17T15:56:54-00:00
_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                78.592(8)
_cell_angle_beta                 80.289(7)
_cell_angle_gamma                77.953(7)
_cell_formula_units_Z            2
_cell_length_a                   9.2020(6)
_cell_length_b                   9.8519(9)
_cell_length_c                   13.1757(13)
_cell_measurement_reflns_used    3306
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      61.31
_cell_measurement_theta_min      5.29
_cell_measurement_wavelength     0.71073
_cell_volume                     1134.93(17)
_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)'
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_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.02
_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, EosS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.070585
_diffrn_orient_matrix_UB_12      0.094721
_diffrn_orient_matrix_UB_13      0.082139
_diffrn_orient_matrix_UB_21      0.156578
_diffrn_orient_matrix_UB_22      -0.005093
_diffrn_orient_matrix_UB_23      0.029052
_diffrn_orient_matrix_UB_31      0.018228
_diffrn_orient_matrix_UB_32      0.131592
_diffrn_orient_matrix_UB_33      -0.083024
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8440
_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        61.606
_diffrn_reflns_theta_max         61.606
_diffrn_reflns_theta_min         3.453
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.924
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             538
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0627P)^2^+0.0075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0
_reflns_number_gt                2912
_reflns_number_total             3493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02071c2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7700420--7700423.cif.'
_cod_original_cell_volume        1134.93(18)
_cod_database_code               7700420
_shelx_estimated_absorpt_t_min   0.439
_shelx_estimated_absorpt_t_max   0.866
_shelx_shelxl_version_number     2018/1