Synthesis and Reactions of Mono- and Dinuclear Ni(I) Thiolate Complexes
Mikinao Ito; Tsuyoshi Matsumoto; Kazuyuki Tatsumi; Inorganic Chemistry 48 (2009) 2215–2223; doi:10.1021/ic802276w

data_4301631
_publ_section_title
;
Synthesis and Reactions of Mono- and Dinuclear Ni(I) Thiolate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2215
_journal_page_last               2223
_journal_paper_doi               10.1021/ic802276w
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C66 H48 Ni2 O P S2 '
_chemical_formula_sum            'C66 H48 Ni2 O P S2'
_chemical_formula_weight         1069.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 108.320(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.538(4)
_cell_length_b                   17.614(3)
_cell_length_c                   18.475(4)
_cell_measurement_reflns_used    10283
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     5417.9(19)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42228
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2220.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     669
_refine_ls_number_reflns         12369
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0478P)^2^+5.6601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                10659
_reflns_number_total             12369
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic802276w_si_002_03.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        5417.8(19)
_cod_original_formula_sum        'C66 H48 Ni2 O P S2 '
_cod_database_code               4301631