Reactivity of Dioxoosmium(VI) Porphyrins toward Arylhydrazine. Isolation of Hydrazidoosmium and Amidoosmium Porphyrins
Sarana Ka-Yan Leung; Jie-Sheng Huang; Nianyong Zhu; Chi-Ming Che; Inorganic Chemistry 42 (2003) 7266–7272; doi:10.1021/ic034389d

data_4312384
_publ_section_title
;
 Reactivity of Dioxoosmium(VI) Porphyrins toward Arylhydrazine. Isolation
 of Hydrazidoosmium and Amidoosmium Porphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7266
_journal_page_last               7272
_journal_paper_doi               10.1021/ic034389d
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C60 H47 N5 O Os'
_chemical_formula_sum            'C60 H47 N5 O Os'
_chemical_formula_weight         1044.23
_chemical_name_systematic
;
?
;
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 111.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.836(3)
_cell_length_b                   23.880(5)
_cell_length_c                   14.720(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     5190(2)
_computing_cell_refinement       Scalepack
_computing_data_collection       MarControl
_computing_data_reduction        Denzo
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Shelxs-97
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Marresearch Imaging Plate mar300'
_diffrn_measurement_method       Oscillation
_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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0831
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25447
_diffrn_reflns_theta_full        25.52
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    2.501
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.320
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0859P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                5692
_reflns_number_total             8980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034389dsi20030414_042915.cif
_cod_data_source_block           complex_2b
_cod_original_cell_volume        5190.0(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4312384