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_7010261
_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            'C49 H39 Br Cl N2 O Os P2'
_chemical_formula_weight         1039.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.742(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2703(2)
_cell_length_b                   19.1253(1)
_cell_length_c                   19.2075(3)
_cell_measurement_reflns_used    7482
_cell_measurement_temperature    295(2)
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_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  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19163
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        0
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_exptl_absorpt_correction_T_max  0.5643
_exptl_absorpt_correction_T_min  0.3187
_exptl_absorpt_correction_type   'empirical used sadabs'
_exptl_crystal_colour            black
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_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
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_refine_diff_density_min         -3.374
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.00053(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_goodness_of_fit_obs   1.112
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         8690
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.112
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_obs          0.0571
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+18.8233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1610
_refine_ls_wR_factor_obs         0.1494
_reflns_number_observed          6696
_reflns_number_total             8690
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b007486l.txt
_cod_data_source_block           IC5981
_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^)+(0.0830P)^2^+18.8233P] 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^)+(0.0830P)^2^+18.8233P] 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        4293.1(1)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010261