Synthesis, Structural Diversity, Dynamics, and Acidity of the M(II) and M(IV) Complexes [MH3(PR3)4]+ (M = Fe, Ru, Os; R = Me, Et)
Dmitry G. Gusev; Rainer Hübener; Peter Burger; Olli Orama; Heinz Berke; Journal of the American Chemical Society 119 (1997) 3716–3731; doi:10.1021/ja963692t

data_4116958
_publ_section_title
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 Synthesis, Structural Diversity, Dynamics, and Acidity of the M(II) and
 M(IV) Complexes [MH3(PR3)4]+ (M = Fe, Ru, Os; R = Me, Et)
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3716
_journal_page_last               3731
_journal_paper_doi               10.1021/ja963692t
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C56 H75 B F24 Fe P4'
_chemical_formula_weight         1394.70
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.93(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.136(2)
_cell_length_b                   14.205(3)
_cell_length_c                   37.117(6)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      4
_cell_volume                     6321(2)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        SHELXTL-Plus
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Nicolet R3'
_diffrn_measurement_method       '\w 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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.1394
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            14414
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.17
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.112
_refine_ls_hydrogen_treatment    'H1,H2,H3 refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         13754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_restrained_S_obs      1.112
_refine_ls_R_factor_all          0.1650
_refine_ls_R_factor_obs          0.0729
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+12.7302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1772
_refine_ls_wR_factor_obs         0.1275
_reflns_number_observed          7189
_reflns_number_total             13761
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja963692t_2.cif
_cod_data_source_block           1b
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+12.7302P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+12.7302P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6321.1(20)
_cod_database_code               4116958