Azo Anion Radical Complexes of Osmium and Related Nonradical Species
Kausikisankar Pramanik; Maya Shivakumar; Prasanta Ghosh; Animesh Chakravorty; Inorganic Chemistry 39 (2000) 195–199; doi:10.1021/ic9908322

data_4300107
_publ_section_title
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Azo Anion Radical Complexes of Osmium and Related Nonradical Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              195
_journal_page_last               199
_journal_paper_doi               10.1021/ic9908322
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C47 H38 Br N4 O Os P2'
_chemical_formula_weight         1006.86
_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   'riding model'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.67(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.215(4)
_cell_length_b                   17.634(7)
_cell_length_c                   22.473(8)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     4012(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       w
_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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.1264
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7446
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.83
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.303
_exptl_absorpt_correction_T_max  0.180
_exptl_absorpt_correction_T_min  0.117
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          O.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.891
_refine_diff_density_min         -2.122
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.032
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.066
_refine_ls_R_factor_all          0.1697
_refine_ls_R_factor_obs          0.0866
_refine_ls_shift/esd_max         0.067
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1259P)^2^+64.7145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2689
_refine_ls_wR_factor_obs         0.2012
_reflns_number_observed          3862
_reflns_number_total             6940
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1259P)^2^+64.7145P] 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^)+(0.1259P)^2^+64.7145P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

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 2.4.5 from 2014-11-21.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4300107