Model Studies of Methyl CoM Reductase: Methane Formation via CH3-S Bond Cleavage of Ni(I) Tetraazacyclic Complexes Having Intramolecular Methyl Sulfide Pendants
Jun-ichi Nishigaki; Tsuyoshi Matsumoto; Kazuyuki Tatsumi; Inorganic Chemistry 51 (2012) 5173–5187; doi:10.1021/ic300017k

data_4329078
_publ_section_title
;
 Model Studies of Methyl CoM Reductase: Methane Formation via CH3-S Bond
 Cleavage of Ni(I) Tetraazacyclic Complexes Having Intramolecular Methyl
 Sulfide Pendants
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5173
_journal_page_last               5187
_journal_paper_doi               10.1021/ic300017k
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'2(C32 H12 B F24), C16 H36 N4 Ni S2, 4(C4 H8 O) '
_chemical_formula_sum            'C96 H92 B2 F48 N4 Ni O4 S2'
_chemical_formula_weight         2422.17
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                71.676(5)
_cell_angle_beta                 70.960(4)
_cell_angle_gamma                86.426(6)
_cell_formula_units_Z            1
_cell_length_a                   12.3465(15)
_cell_length_b                   13.3250(15)
_cell_length_c                   17.4185(18)
_cell_measurement_reflns_used    6121
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2568.9(5)
_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    SIR92
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.080
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31408
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1230.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.79
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     734
_refine_ls_number_reflns         11685
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1200P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2392
_reflns_number_gt                8465
_reflns_number_total             11685
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic300017k_si_002_16.cif
_cod_data_source_block           RRSS-[Ni(mtc)](BArF4)2_Complex7b
_cod_original_formula_sum        'C96 H92 B2 F48 N4 Ni O4 S2 '
_cod_database_code               4329078