Azo Complexes of Osmium(II): Preparation and Reactivity of Organic Azide and Hydrazine Derivatives
Gabriele Albertin; Stefano Antoniutti; Laura Bonaldo; Alessandra Botter; Jesús Castro; Inorganic Chemistry 52 (2013) 2870–2879; doi:10.1021/ic302483e

data_4334137
_publ_section_title
;
 Azo Complexes of Osmium(II): Preparation and Reactivity of Organic Azide
 and Hydrazine Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2870
_journal_page_last               2879
_journal_paper_doi               10.1021/ic302483e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C75 H74 B Cl N O4 Os P3'
_chemical_formula_weight         1382.72
_chemical_name_systematic
; 
 ? 
;
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_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                 94.797(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.554(3)
_cell_length_b                   12.7270(19)
_cell_length_c                   23.939(4)
_cell_measurement_reflns_used    3285
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.55
_cell_measurement_theta_min      2.34
_cell_volume                     6847.5(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1398
_diffrn_reflns_av_sigmaI/netI    0.2327
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44460
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    2.020
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6554
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       plate
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.719
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       0.0035(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         16271
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.2350
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0996P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.2400
_reflns_number_gt                5946
_reflns_number_total             16271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302483e_si_001_1.cif
_cod_data_source_block           pat_8b
_cod_original_cell_volume        6847.5(17)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4334137