Preparation, Structure, Bonding, and Preliminary Reactivity of a Six-Coordinate d4Osmium‒Boryl Complex
Esteruelas, Miguel A.; Fernández, Israel; López, Ana M.; Mora, Malka; Oñate, Enrique; Organometallics 31 (2012) 4646–; doi:10.1021/om300407d

data_4078770
_publ_section_title
;
 Preparation, Structure, Bonding, and Preliminary Reactivity of a
 Six-Coordinate d4Osmium--Boryl Complex
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4646
_journal_paper_doi               10.1021/om300407d
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C25 H46 B Cl O3 Os P2'
_chemical_formula_weight         693.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.226(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.246(3)
_cell_length_b                   10.8358(18)
_cell_length_c                   16.886(3)
_cell_measurement_reflns_used    1923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      2
_cell_volume                     2854.2(9)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (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 0.991
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_sigmaI/netI    0.1242
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23666
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.66
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.697
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.678
_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.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.646
_refine_diff_density_min         -2.634
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6795
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                4203
_reflns_number_total             6795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300407d_si_001.cif
_cod_data_source_block           enrique31as
_cod_original_cell_volume        2854.2(8)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4078770