Cyclometallation and NN bond cleavage of 2-(arylazo)phenols by osmium. Synthesis, structure and redox properties †
Majumder, Kanchana; Peng, Shie-Ming; Bhattacharya, Samaresh; Journal of the Chemical Society, Dalton Transactions  (2001) 284–; doi:10.1039/b007486l

data_7010260
_publ_section_title
;
 Cyclometallation and N&#xE006;N bond cleavage of 2-(arylazo)phenols by
 osmium. Synthesis, structure and redox properties&#x200A;&#x2020;
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              284
_journal_paper_doi               10.1039/b007486l
_journal_year                    2001
_chemical_formula_sum            'C38.5 H31.5 Cl2 N3 O2 Os P'
_chemical_formula_weight         860.24
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 112.731(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   40.4327(2)
_cell_length_b                   10.9195(2)
_cell_length_c                   17.5688(3)
_cell_measurement_reflns_used    6551
_cell_measurement_temperature    295(2)
_cell_volume                     7154.24(19)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\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  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19051
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.797
_exptl_absorpt_correction_T_max  0.7195
_exptl_absorpt_correction_T_min  0.5139
_exptl_absorpt_correction_type   ' empirical used sadabs'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3396
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.342
_refine_diff_density_min         -1.944
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.00007(3)
_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_all   1.021
_refine_ls_goodness_of_fit_obs   1.117
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.117
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_obs          0.0564
_refine_ls_shift/esd_max         0.018
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1456
_refine_ls_wR_factor_obs         0.1353
_reflns_number_observed          5205
_reflns_number_total             7104
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b007486l.txt
_cod_data_source_block           ic6515
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7154.2(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C38.50 H31.50 Cl2 N3 O2 Os P'
_cod_database_code               7010260