Cleavage of Ni-(μ2-S)-Ni Bridges in Dinuclear Nickel(II) Dithiolate Pincer Complexes and Related Reactions
Deguang Huang; Liang Deng; Jibin Sun; R. H. Holm; Inorganic Chemistry 48 (2009) 6159–6166; doi:10.1021/ic900494u

data_4302521
_publ_section_title
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Cleavage of Ni-(\m2-S)-Ni Bridges in Dinuclear Nickel(II) Dithiolate Pincer
Complexes and Related Reactions
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6159
_journal_page_last               6166
_journal_paper_doi               10.1021/ic900494u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C16 H36 N, C7 H3 Br N Ni O2 S2'
_chemical_formula_sum            'C23 H39 Br N2 Ni O2 S2'
_chemical_formula_weight         578.30
_chemical_name_common            '[Ni(pdtc)Br](Bu4N)'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 111.4640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5520(10)
_cell_length_b                   22.8926(17)
_cell_length_c                   9.2961(7)
_cell_measurement_reflns_used    5623
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.35
_cell_volume                     2684.0(3)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'SMART V5.632 (Bruker AXS, 2001)'
_computing_data_reduction
;
SAINT V7.34A (Bruker AXS, 2006), SADABS (Bruker AXS, 2004)              
;
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001b)'
_computing_publication_material  'SHELXTL v6.12 (Bruker AXS, 2001b)'
_computing_structure_refinement  'SHELXTL v6.12 (Bruker AXS, 2001b)'
_computing_structure_solution    'SHELXTL v6.12 (Bruker AXS, 2001b)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans, 0.3 degree'
_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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9025
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.389
_exptl_absorpt_correction_T_max  0.7626
_exptl_absorpt_correction_T_min  0.7012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         3209
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.405
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+2.3283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                2925
_reflns_number_total             3209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900494u_si_001_04.cif
_cod_data_source_block           compound8
_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 
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_cod_database_code               4302521