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_4116957
_publ_section_title
;
 Synthesis, Structural Diversity, Dynamics, and Acidity of the M(II) and
 M(IV) Complexes [MH3(PR3)4]+ (M = Fe, Ru, Os; R = Me, Et)
;
_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            'C36 H59 B Fe P4'
_chemical_formula_weight         682.4
_chemical_name_systematic
; 
 ? 
;
_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                 110.39(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.899(3)
_cell_length_b                   12.702(2)
_cell_length_c                   20.169(4)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      18
_cell_volume                     3817.9(13)
_computing_cell_refinement       'Nicolet P3'
_computing_data_collection       'Nicolet P3'
_computing_data_reduction        SHELXTL-PLUS
_computing_molecular_graphics    'Siemens SHELXTL PLUS'
_computing_publication_material  'Siemens SHELXTL PLUS'
_computing_structure_refinement  'Siemens SHELXTL PLUS'
_computing_structure_solution    'Siemens SHELXTL PLUS'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Siemens-Nicolet P4'
_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_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
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_diffrn_reflns_theta_min         2.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_type   n/a
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       'Yellow Prism'
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_refine_diff_density_max         1.22
_refine_diff_density_min         -0.50
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_refine_ls_structure_factor_coef Fo-Fc
_refine_ls_weighting_details     w=1/[\s^2^(F)+(0.0002)F^2^]
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_obs         5.48
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_reflns_observed_criterion       'F > 4sigma(F)'
_cod_data_source_file            ja963692t_1.cif
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w=1/[\s^2^(F)+(0.0002)F^2^]' 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^(F)+(0.0002)F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct Methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        3818.0(13)
_cod_database_code               4116957