Metal-Assisted Unusual Hydroxylation at the Carbon Atom of the Triazine Ring in Dinuclear Ruthenium(II) and Osmium(II) Complexes Bridged by 2,4,6-Tris(2-pyridyl)-1,3,5-triazine: Synthesis, Structural Characterization, Stereochemistry, and Electrochemical Studies
Parimal Paul; Beena Tyagi; Anvarhusen K. Bilakhiya; Parthasarathi Dastidar; Eringathodi Suresh; Inorganic Chemistry 39 (2000) 14–22; doi:10.1021/ic990938x

data_4300148
_publ_section_title
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Metal-Assisted Unusual Hydroxylation at the Carbon Atom of the Triazine
Ring in Dinuclear Ruthenium(II) and Osmium(II) Complexes Bridged by
2,4,6-Tris(2-pyridyl)-1,3,5-triazine: Synthesis, Structural
Characterization, Stereochemistry, and Electrochemical Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14
_journal_page_last               22
_journal_paper_doi               10.1021/ic990938x
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C58 H47 F18 N14 O2 P3 Ru2'
_chemical_formula_weight         1609.15
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.84(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.584(7)
_cell_length_b                   14.309(4)
_cell_length_c                   41.044(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      7
_cell_volume                     14420(7)
_computing_cell_refinement       'CAD-4 PC '
_computing_data_collection       'CAD-4 PC '
_computing_data_reduction        NRCVAX
_computing_molecular_graphics    'ORTEP, PLUTON '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.473
_diffrn_measured_fraction_theta_max 0.473
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometr '
_diffrn_measurement_method       'omega-two theta'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1675
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9910
_diffrn_reflns_theta_full        22.91
_diffrn_reflns_theta_max         22.91
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        nil
_diffrn_standards_interval_time  1h
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.581
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             6432
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.365
_refine_diff_density_min         -1.756
_refine_diff_density_rms         0.311
_refine_ls_extinction_coef       0.0041(5)
_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   1.679
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         9910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.679
_refine_ls_R_factor_all          0.2677
_refine_ls_R_factor_gt           0.1796
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4789
_refine_ls_wR_factor_ref         0.5029
_reflns_number_gt                5554
_reflns_number_total             9910
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2000P)^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^)+(0.2000P)^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 
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_cod_database_code               4300148