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_4317723
_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            'C39 H30 Fe0.5 N3 O P2'
_chemical_formula_weight         646.53
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 106.528(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.955(3)
_cell_length_b                   13.213(3)
_cell_length_c                   20.003(5)
_cell_measurement_temperature    273(2)
_cell_volume                     3282.5(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30337
_diffrn_reflns_theta_full        28.67
_diffrn_reflns_theta_max         28.67
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.9929
_exptl_absorpt_correction_T_min  0.8570
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         8066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0478P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                4679
_reflns_number_total             8066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011030l_1.cif
_cod_data_source_block           f16n80m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3282.7(13)
_cod_original_formula_sum        'C39 H30 Fe0.50 N3 O P2'
_cod_database_code               4317723