Chemically Induced Cyclometalation of 2-(Arylazo)phenols. Synthesis, Characterization, and Redox Properties of a Family of Organoosmium Complexes
Parna Gupta; Ray J. Butcher; Samaresh Bhattacharya; Inorganic Chemistry 42 (2003) 5405–5411; doi:10.1021/ic0343713

data_4314103
_publ_section_title
;
 Chemically Induced Cyclometalation of 2-(Arylazo)phenols. Synthesis,
 Characterization, and Redox Properties of a Family of Organoosmium
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5405
_journal_page_last               5411
_journal_paper_doi               10.1021/ic0343713
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C50 H40 N2 O2 Os P2'
_chemical_formula_weight         952.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 108.136(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.262(3)
_cell_length_b                   19.353(5)
_cell_length_c                   18.410(4)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      12.44
_cell_measurement_theta_min      2.70
_cell_volume                     4151.8(18)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9593
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.41
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.191
_exptl_absorpt_correction_T_max  0.8661
_exptl_absorpt_correction_T_min  0.5627
_exptl_absorpt_correction_type   Shelxa
_exptl_crystal_colour            dichroic_yellow-gr
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.73
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00037(8)
_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   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         9162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.8609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                6923
_reflns_number_total             9162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0343713si20030407_085524.cif
_cod_data_source_block           sb-s1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4151.9(16)
_cod_database_code               4314103