Optical Resolution, Determination of Absolute Configuration, and Photoracemization of cis-RuL2(CN)2 (L = 2,2'-Bipyridine and Its Analogues).
Aihara, Yusuke; Sato, Kyohei; Shinozaki, Kazuteru; Inorganic chemistry 55 (2016) 8387–8395; doi:10.1021/acs.inorgchem.6b00772

data_4347914
_publ_section_title
;
 Optical Resolution, Determination of Absolute Configuration, and
 Photoracemization of cis-RuL2(CN)2 (L = 2,2'-Bipyridine and Its
 Analogues).
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8387
_journal_page_last               8395
_journal_paper_doi               10.1021/acs.inorgchem.6b00772
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C38 H48 N6 Ru, 2(C H Cl3), C6 H14'
_chemical_formula_sum            'C46 H64 Cl6 N6 Ru'
_chemical_formula_weight         1014.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2569(19)
_cell_length_b                   18.666(3)
_cell_length_c                   18.731(2)
_cell_measurement_reflns_used    13527
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      3.10
_cell_volume                     5334.3(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1062
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52887
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.346
_diffrn_reflns_theta_min         3.081
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.594
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 3576 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         11993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0850
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+6.8535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.1998
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                10928
_reflns_number_total             11993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00772_si_002.cif
_cod_data_source_block           AiharaNo2
_cod_database_code               4347914
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2013-4
_shelx_res_checksum              38913
_shelx_hkl_checksum              16987