Bis(3,5-dimethylpyrazole-1-carbodithioato) Nickel(II) and Its Transformation to a Dinuclear Complex: Crystal Structure of [Ni2(μ-3,5-Me2Pz)2(L1)2] (L1= 3,5-dimethylpyrazole-1-carbodithioate)
Sami Mukhopadhyay; Uday Mukhopadhyay; Thomas C. W. Mak; Debashis Ray; Inorganic Chemistry 40 (2001) 1057–1059; doi:10.1021/ic000138i

data_4319265
_publ_section_title
;
 Bis(3,5-dimethylpyrazole-1-carbodithioato) Nickel(II) and Its
 Transformation to a Dinuclear Complex: Crystal Structure of
 [Ni2(\m-3,5-Me2Pz)2(L1)2] (L1= 3,5-dimethylpyrazole-1-carbodithioate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1057
_journal_page_last               1059
_journal_paper_doi               10.1021/ic000138i
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C22 H28 N8 Ni2 S4'
_chemical_formula_weight         650.18
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.748(2)
_cell_length_b                   13.575(3)
_cell_length_c                   23.378(5)
_cell_measurement_reflns_used    BIOTEX
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      BIOTEX
_cell_measurement_theta_min      BIOTEX
_cell_volume                     2766.5(11)
_computing_cell_refinement       BIOTEX
_computing_data_collection       BIOTEX
_computing_data_reduction        BIOTEX
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'RIGAKU RAXIS-IIC'
_diffrn_measurement_method       'Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation anod 50kV 90mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1600
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5064
_diffrn_reflns_theta_max         27.23
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.0000(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.450
_refine_ls_goodness_of_fit_obs   1.543
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         1558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.448
_refine_ls_restrained_S_obs      1.543
_refine_ls_R_factor_all          0.1699
_refine_ls_R_factor_obs          0.0843
_refine_ls_shift/esd_max         -0.032
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3274
_refine_ls_wR_factor_obs         0.2010
_reflns_number_observed          2336
_reflns_number_total             5064
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000138i.cif
_cod_data_source_block           drpzdt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319265