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_7008888
_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            'C10 H20 Cl2 N6 Ni O9 S4'
_chemical_formula_weight         626.17
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 97.399(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6487(16)
_cell_length_b                   14.789(3)
_cell_length_c                   21.618(5)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.53
_cell_measurement_theta_min      2.94
_cell_volume                     2425.0(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            4607
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.417
_exptl_absorpt_correction_T_max  0.9558
_exptl_absorpt_correction_T_min  0.8300
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            pale_purple
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       long_needle
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.95
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         4267
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.128
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+4.5244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1281
_reflns_number_gt                3038
_reflns_number_total             4267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a906294g.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        2425.1(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7008888