Synthesis and Dimer Cleavage Reactions of the N2S Thiolate Bridged Dimer [(mmp-dach)2Ni2]Cl2
Craig A. Grapperhaus; John A. Bellefeuille; Joseph H. Reibenspies; Marcetta Y. Darensbourg; Inorganic Chemistry 38 (1999) 3698–3703; doi:10.1021/ic990106z

data_4322182
_publ_section_title
;
 Synthesis and Dimer Cleavage Reactions of the N2S Thiolate Bridged Dimer
 [(mmp-dach)2Ni2]Cl2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3698
_journal_page_last               3703
_journal_paper_doi               10.1021/ic990106z
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C86 H72 B2 F48 N4 Ni2 O S2'
_chemical_formula_weight         2292.64
_chemical_name_systematic
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;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.06(3)
_cell_angle_beta                 74.12(3)
_cell_angle_gamma                86.48(3)
_cell_formula_units_Z            1
_cell_length_a                   13.009(3)
_cell_length_b                   13.626(3)
_cell_length_c                   16.031(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2614.1(11)
_computing_cell_refinement       'P3VAX (SIEMENS, 1990)'
_computing_data_collection       'P3VAX (SIEMENS, 1990)'
_computing_data_reduction        'XDISK (SIEMENS, 1990)'
_computing_molecular_graphics    'XP (SIEMENS, 1990)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'Siemens R3M'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9491
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1154
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0065(15)
_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_ref   1.075
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         9054
_refine_ls_number_restraints     1232
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.808
_refine_ls_shift/su_mean         0.072
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1357P)^2^+1.2051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2153
_refine_ls_wR_factor_ref         0.2375
_reflns_number_gt                6653
_reflns_number_total             9054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990106z.cif
_cod_data_source_block           md199
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1357P)^2^+1.2051P] 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^)+(0.1357P)^2^+1.2051P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2614.1(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4322182