Influence of the Anion of the Salt Used on the Coordination Mode of an N-Heterocyclic Carbene Ligand to Osmium
Baya, Miguel; Eguillor, Beatriz; Esteruelas, Miguel A.; Oliván, Montserrat; Oñate, Enrique; Organometallics 26 (2007) 6556–; doi:10.1021/om700746h

data_4073936
_publ_section_title
;
 Influence of the Anion of the Salt Used on the Coordination Mode of an
 N-Heterocyclic Carbene Ligand to Osmium
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              6556
_journal_paper_doi               10.1021/om700746h
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C30 H46 Br Cl2 N6 Os P'
_chemical_formula_weight         862.71
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL-97
_cell_angle_alpha                89.303(5)
_cell_angle_beta                 86.032(6)
_cell_angle_gamma                86.220(6)
_cell_formula_units_Z            2
_cell_length_a                   8.664(3)
_cell_length_b                   11.597(4)
_cell_length_c                   16.999(5)
_cell_measurement_reflns_used    2153
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      2
_cell_volume                     1700.1(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      105(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.910
_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  0.0882
_diffrn_reflns_av_sigmaI/netI    0.1230
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20937
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         1.76
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    5.159
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.540
_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            red
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.276
_refine_diff_density_min         -2.848
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         8037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1369
_reflns_number_gt                5821
_reflns_number_total             8037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700746h-file002.cif
_cod_data_source_block           mae268as
_cod_original_cell_volume        1700.2(9)
_cod_database_code               4073936