Abnormal and Normal N-Heterocyclic Carbene Osmium Polyhydride Complexes Obtained by Direct Metalation of Imidazolium Salts
Eguillor, Beatriz; Esteruelas, Miguel A.; Oliván, Montserrat; Puerta, Marta; Organometallics 27 (2008) 445–; doi:10.1021/om7010722

data_4070844
_publ_section_title
;
 Abnormal and Normal N-Heterocyclic Carbene Osmium Polyhydride Complexes
 Obtained by Direct Metalation of Imidazolium Salts
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              445
_journal_paper_doi               10.1021/om7010722
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C31 H62 N2 Os P2'
_chemical_formula_weight         714.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.396(5)
_cell_length_b                   13.801(6)
_cell_length_c                   21.640(9)
_cell_measurement_reflns_used    2154
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      2
_cell_volume                     3403(3)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.1519
_diffrn_reflns_av_sigmaI/netI    0.1780
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42952
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.861
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.212
_refine_diff_density_min         -1.382
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         8462
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                5027
_reflns_number_total             8462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7010722-file002.cif
_cod_data_source_block           mae256as
_cod_original_cell_volume        3403(2)
_cod_database_code               4070844