Nickel(II) complexes with dithiadiiminoamine and dithiabis(thiosemicarbazone) ligands †
Pavlishchuk, Vitaly V.; Kolotilov, Sergey V.; Addison, Anthony W.; Butcher, Raymond J.; Sinn, Ekkehard; Journal of the Chemical Society, Dalton Transactions  (2000) 335–; doi:10.1039/a906294g

data_7008887
_publ_section_title
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 Nickel(II) complexes with dithiadiiminoamine and
 dithiabis(thiosemicarbazone) ligands&#x200A;&#x2020;
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_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              335
_journal_paper_doi               10.1039/a906294g
_journal_year                    2000
_chemical_formula_sum            'C12 H27 Cl2 N4 Ni O8.5 S2'
_chemical_formula_weight         557.11
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.888(2)
_cell_length_b                   19.831(3)
_cell_length_c                   13.2864(16)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      4.96
_cell_volume                     4449.7(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5007
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.41
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  0.4374
_exptl_absorpt_correction_T_min  0.4107
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale_purple
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.74
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5007
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.301
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+4.0131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                2991
_reflns_number_total             5007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a906294g.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pccn
_cod_original_formula_sum        'C12 H27 Cl2 N4 Ni O8.50 S2'
_cod_database_code               7008887