Hydrogen Atom and Hydride Transfer in the Reactions of Chromium(IV) and Chromium(V) Complexes with Rhodium Hydrides. Crystal Structure of a Superoxorhodium(III) Product
Andreja Bakac; Ilia A. Guzei; Inorganic Chemistry 39 (2000) 736–740; doi:10.1021/ic991098p

data_4300196
_publ_contact_author_address
;
   Department of Chemistry
   Iowa State University of Science and Technology
   Ames, Iowa, 50011
   USA
;
_publ_contact_author_email       iguzei@iastate.edu
_publ_contact_author_fax         +515-294-5717
_publ_contact_author_name
;
Ilia A. Guzei
;
_publ_contact_author_phone       +515-294-6419
_publ_section_title
;
Hydrogen Atom and Hydride Transfer in the Reactions of Chromium(IV) and
Chromium(V) Complexes with Rhodium Hydrides. Crystal Structure of a
Superoxorhodium(III) Product
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              736
_journal_page_last               740
_journal_paper_doi               10.1021/ic991098p
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C20 H41 F6 N5 O9 Rh S2'
_chemical_formula_weight         776.61
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
manual editing of the .cif file created by SHELXL-97 
;
_cell_angle_alpha                72.8420(10)
_cell_angle_beta                 82.0820(10)
_cell_angle_gamma                75.4140(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4257(5)
_cell_length_b                   13.4119(7)
_cell_length_c                   13.6140(7)
_cell_measurement_temperature    173(2)
_cell_volume                     1587.69(14)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6457
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.8572
_exptl_absorpt_correction_T_min  0.7127
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark_orange
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             798
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.324
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6457
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1031P)^2^+2.8739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                5531
_reflns_number_total             6457
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4300196