Osmium Models of Intermediates Involved in Catalytic Reactions of Alkylidenecyclopropanes
Esteruelas, Miguel A.; López, Ana M.; López, Fernando; Mascareñas, José L.; Mozo, Silvia; Oñate, Enrique; Saya, Luc\?ía; Organometallics 32 (2013) 4851–; doi:10.1021/om400597q

data_4081330
_publ_section_title
;
 Osmium Models of Intermediates Involved in Catalytic Reactions of
 Alkylidenecyclopropanes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4851
_journal_paper_doi               10.1021/om400597q
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C56 H47 B Cl2 F24 N Os P'
_chemical_formula_weight         1492.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 91.2683(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.056(2)
_cell_length_b                   17.482(2)
_cell_length_c                   34.820(5)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2.3
_cell_volume                     11597(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX DUO 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  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            46134
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.17
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.435
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.665
_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            orange
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             5888
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.117
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         10788
_refine_ls_number_restraints     416
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+608.6609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.1819
_reflns_number_gt                9190
_reflns_number_total             10788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400597q_si_002.cif
_cod_data_source_block           enriquen20b
_cod_original_cell_volume        11597(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4081330