Metal-Only Lewis Pairs Based on Zerovalent Osmium
Bissert, Robin; Braunschweig, Holger; Dewhurst, Rian D.; Schneider, Christoph; Organometallics 35 (2016) 2567–; doi:10.1021/acs.organomet.6b00495

data_4088853
_publ_section_title
;
 Metal-Only Lewis Pairs Based on Zerovalent Osmium
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              2567
_journal_paper_doi               10.1021/acs.organomet.6b00495
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C27 H33 N2 O3 Os P'
_chemical_formula_sum            'C27 H33 N2 O3 Os P'
_chemical_formula_weight         654.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_secondary   iterative
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.66(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4461(18)
_cell_length_b                   12.090(3)
_cell_length_c                   16.857(6)
_cell_measurement_reflns_used    9387
_cell_measurement_temperature    121(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      2.43
_cell_volume                     3132.6(14)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      121(2)
_diffrn_detector                 'CMOS area detector (Photon 100)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            3506
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.787
_diffrn_reflns_theta_min         2.398
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_exptl_absorpt_coefficient_mu    4.147
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.062
_platon_squeeze_details
;
The unit cell contains one molecule 
which have been treated as a diffuse contribution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON. 
;
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.308
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.320
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0174
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+10.0290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3323
_reflns_number_total             3506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00495_si_002.cif
_cod_data_source_block           1d
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4088853
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.577
_shelx_estimated_absorpt_t_max   0.783
_shelx_res_checksum              53731