Preparative and Structural Studies on the Carbonyl Cyanides of Iron, Manganese, and Ruthenium: Fundamentals Relevant to the Hydrogenases
Stephen M. Contakes; Sodio C. N. Hsu; Thomas B. Rauchfuss; Scott R. Wilson; Inorganic Chemistry 41 (2002) 1670–1678; doi:10.1021/ic011030l

data_4317726
_publ_section_title
;
 Preparative and Structural Studies on the Carbonyl Cyanides of Iron,
 Manganese, and Ruthenium: Fundamentals Relevant to the Hydrogenases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1670
_journal_page_last               1678
_journal_paper_doi               10.1021/ic011030l
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C111 H80 Cl9 Mn2 N6 O6 P4'
_chemical_formula_weight         2146.62
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                 99.147(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.008(2)
_cell_length_b                   16.968(2)
_cell_length_c                   19.521(3)
_cell_measurement_temperature    193(2)
_cell_volume                     5234.9(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.2495
_diffrn_reflns_av_sigmaI/netI    0.6364
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27471
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.589
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2198
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.735
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         14593
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      0.735
_refine_ls_R_factor_all          0.3344
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                3413
_reflns_number_total             14593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011030l_4.cif
_cod_data_source_block           pna
_cod_original_cell_volume        5234.9(13)
_cod_database_code               4317726