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_4070843
_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            'C55 H83 B N2 Os P2'
_chemical_formula_weight         1035.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 101.286(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.467(3)
_cell_length_b                   13.713(3)
_cell_length_c                   14.322(3)
_cell_measurement_reflns_used    12683
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     2593.7(10)
_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 1.000
_diffrn_measured_fraction_theta_max 0.933
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32985
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.09
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.556
_exptl_absorpt_correction_T_max  0.705
_exptl_absorpt_correction_T_min  0.586
_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    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.411
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         12561
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          3.360
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0573
_reflns_number_gt                11389
_reflns_number_total             12561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7010722-file002.cif
_cod_data_source_block           mae241as
_cod_original_cell_volume        2593.8(9)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4070843