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_4329077
_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         'C14 H32 N4 Ni, C F3 O3 S '
_chemical_formula_sum            'C15 H32 F3 N4 Ni O3 S'
_chemical_formula_weight         464.20
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   18.709(3)
_cell_length_b                   11.982(2)
_cell_length_c                   9.4404(17)
_cell_measurement_reflns_used    7144
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4
_cell_volume                     2116.3(6)
_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_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.022
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15972
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.063
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             980.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.34
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1433 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.141(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3989
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                3754
_reflns_number_total             3989
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic300017k_si_002_15.cif
_cod_data_source_block           RSRS-[Ni(tmc)]OTf
_cod_original_cell_volume        2116.2(7)
_cod_original_formula_sum        'C15 H32 F3 N4 Ni O3 S '
_cod_database_code               4329077