Pentamethylcyclopentadienyl osmium complexes that contain diazoalkane, dioxygen and allenylidene ligands: preparation and reactivity.
Albertin, Gabriele; Antoniutti, Stefano; Castro, Jesús; Sibilla, Francesca; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3116–3131; doi:10.1039/c9dt00223e

data_7049037
_publ_section_title
;
 Pentamethylcyclopentadienyl osmium complexes that contain diazoalkane,
 dioxygen and allenylidene ligands: preparation and reactivity.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3116
_journal_page_last               3131
_journal_paper_doi               10.1039/c9dt00223e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C43 H53 O3 Os P2, C24 H20 B'
_chemical_formula_sum            'C67 H73 B O3 Os P2'
_chemical_formula_weight         1189.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-10-18 deposited with the CCDC.    2019-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                92.982(3)
_cell_angle_beta                 99.500(3)
_cell_angle_gamma                94.337(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5543(8)
_cell_length_b                   16.5381(13)
_cell_length_c                   16.6482(13)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.51
_cell_volume                     2851.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HeliosTM multilayer optics'
_diffrn_radiation_source         'Incoatec high brillance I\muS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45360
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.376
_diffrn_reflns_theta_min         2.409
_exptl_absorpt_coefficient_mu    2.338
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.075
_refine_diff_density_max         2.963
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         14113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+2.1953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11171
_reflns_number_total             14113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00223e2.cif
_cod_data_source_block           cx137_a
_cod_depositor_comments
'Adding full bibliography for 7049037--7049039.cif.'
_cod_database_code               7049037
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.688
_shelx_estimated_absorpt_t_max   0.844
_shelx_res_checksum              4072