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_7049038
_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         'C32 H39 O4 Os P2, C24 H20 B'
_chemical_formula_sum            'C56 H59 B O4 Os P2'
_chemical_formula_weight         1058.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-10-18 deposited with the CCDC.    2019-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.281(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0342(8)
_cell_length_b                   16.7169(9)
_cell_length_c                   18.2980(10)
_cell_measurement_reflns_used    9734
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.44
_cell_volume                     5049.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            92143
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.355
_diffrn_reflns_theta_min         2.242
_exptl_absorpt_coefficient_mu    2.633
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       plate
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.034
_refine_diff_density_max         2.107
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         12600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0208P)^2^+8.3228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10634
_reflns_number_total             12602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00223e2.cif
_cod_data_source_block           cx112_p_sq
_cod_depositor_comments
'Adding full bibliography for 7049037--7049039.cif.'
_cod_database_code               7049038
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.589
_shelx_estimated_absorpt_t_max   0.916
_shelx_res_checksum              75798
_shelx_fab_checksum              89689