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_4334138
_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            'C43 H48 Cl O4 Os P3'
_chemical_formula_weight         947.37
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 110.671(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
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_cell_length_c                   24.423(9)
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_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.37
_cell_volume                     4093(3)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART1000 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
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_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
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_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
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_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
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_exptl_absorpt_coefficient_mu    3.339
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_exptl_absorpt_correction_T_min  0.4466
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.507
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         9831
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0458
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_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+7.1838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                7951
_reflns_number_total             9831
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302483e_si_001_2.cif
_cod_data_source_block           md_2b
_cod_original_cell_volume        4093(2)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4334138