Revelation of Varying Coordination Modes and Noninnocence of Deprotonated 2,2'-Bipyridine-3,3'-diol in {Os(bpy)2} Frameworks.
Ghosh, Prabir; Ray, Ritwika; Das, Ankita; Lahiri, Goutam Kumar; Inorganic chemistry 53 (2014) 10695–10707; doi:10.1021/ic501852a

data_4341133
_publ_section_title
;
 Revelation of Varying Coordination Modes and Noninnocence of Deprotonated
 2,2'-Bipyridine-3,3'-diol in {Os(bpy)2} Frameworks.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10695
_journal_page_last               10707
_journal_paper_doi               10.1021/ic501852a
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C32.5 H24.5 Cl2.5 N4 O6 Os'
_chemical_formula_weight         845.88
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.293(3)
_cell_angle_beta                 98.983(4)
_cell_angle_gamma                107.565(3)
_cell_formula_units_Z            4
_cell_length_a                   12.791(5)
_cell_length_b                   12.816(5)
_cell_length_c                   20.033(7)
_cell_measurement_reflns_used    8335
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      3.03
_cell_volume                     3028(2)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36404
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    4.486
_exptl_absorpt_correction_T_max  0.4673
_exptl_absorpt_correction_T_min  0.4673
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       neddle
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.324
_refine_diff_density_min         -1.909
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         10349
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0909P)^2^+76.3606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1816
_reflns_number_gt                9207
_reflns_number_total             10349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501852a_si_004.cif
_cod_data_source_block           '[4]ClO4'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Numerical'
changed to 'numerical' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4341133--4341136.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4341133