Synthesis and Crystal Structure of Aqua Adduct of Dinuclear Ruthenium(II,III) 3,4,5-Tri(ethoxy-d5)benzoate Tetrafluoroborate
ISHIDA, Hideaki; HANDA, Makoto; MIKURIYA, Masahiro; X-ray Structure Analysis Online 30 (2014) 9–; doi:10.2116/xraystruct.30.9

data_1551672
_publ_section_title
;
 Synthesis and Crystal Structure of Aqua Adduct of Dinuclear
 Ruthenium(II,III) 3,4,5-Tri(ethoxy-d5)benzoate Tetrafluoroborate
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              9
_journal_paper_doi               10.2116/xraystruct.30.9
_journal_volume                  30
_journal_year                    2014
_chemical_formula_sum            'C56 H20 B D60 F4 O23 Ru2'
_chemical_formula_weight         1470.51
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 100.789(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.243(4)
_cell_length_b                   10.4850(15)
_cell_length_c                   23.115(3)
_cell_measurement_temperature    90(2)
_cell_volume                     6485.9(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXL'
_computing_publication_material  'Bruker SHELXL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'psi and omega 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  0.0642
_diffrn_reflns_av_sigmaI/netI    0.1301
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18155
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.9783
_exptl_absorpt_correction_T_min  0.7370
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            reddish-brown
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_meas      1.465
_exptl_crystal_density_method    floatation
_exptl_crystal_description       needle
_exptl_crystal_F_000             2916
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6597
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.853
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                3902
_reflns_number_total             6597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            30_9_1.txt
_cod_data_source_block           ru3c2d5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/andrius/struct/COD-crude-data/automatic-downloads/current/J-STAGE/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 6524 2018-11-02 12:15:13Z antanas 
;
_cod_original_cell_volume        6486.1(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1551672