Osmium NHC Complexes from Alcohol-Functionalized Imidazoles and Imidazolium Salts
Eguillor, Beatriz; Esteruelas, Miguel A.; García-Raboso, Jorge; Oliván, Montserrat; Oñate, Enrique; Pastor, Isidro M.; Peñafiel, Itziar; Yus, Miguel; Organometallics 30 (2011) 1658–; doi:10.1021/om101173e

data_4064191
_publ_section_title
;
 Osmium NHC Complexes from Alcohol-Functionalized Imidazoles and
 Imidazolium Salts
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1658
_journal_paper_doi               10.1021/om101173e
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C29 H54 N2 O Os P2, C1.25 H3'
_chemical_formula_sum            'C30.25 H57 N2 O Os P2'
_chemical_formula_weight         716.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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            16
_cell_length_a                   35.231(9)
_cell_length_b                   35.231(9)
_cell_length_c                   11.818(4)
_cell_measurement_reflns_used    4674
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     14669(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.939
_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  0.1102
_diffrn_reflns_av_sigmaI/netI    0.1638
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            47362
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.87
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.586
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.694
_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            brown
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5864
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         9055
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                4622
_reflns_number_total             9055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101173e_si_002.cif
_cod_data_source_block           mae424as
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               4064191