Electronic Structure of Ru2(II,II) Oxypyridinates: Synthetic, Structural, and Theoretical Insights into Axial Ligand Binding.
Brown, Tristan R.; Dolinar, Brian S.; Hillard, Elizabeth A.; Clérac, Rodolphe; Berry, John F.; Inorganic chemistry 54 (2015) 8571–8589; doi:10.1021/acs.inorgchem.5b01241

data_4344065
_publ_section_title
;
 Electronic Structure of Ru2(II,II) Oxypyridinates: Synthetic, Structural,
 and Theoretical Insights into Axial Ligand Binding.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8571
_journal_page_last               8589
_journal_paper_doi               10.1021/acs.inorgchem.5b01241
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C25 H17 Cl4 N5 O4 Ru2'
_chemical_formula_sum            'C25 H17 Cl4 N5 O4 Ru2'
_chemical_formula_weight         795.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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
_cell_angle_alpha                90
_cell_angle_beta                 107.8400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5485(5)
_cell_length_b                   12.1926(4)
_cell_length_c                   13.7919(4)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.37
_cell_volume                     2648.97(14)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4102
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.533
_diffrn_reflns_theta_min         2.112
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.588
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.363075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0580 before and 0.0426 after correction.
 The Ratio of minimum to maximum transmission is 0.84.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 72448 reflections, Rint = 0.0358
 (37211 with I > 3sig(I), Rint = 0.0324)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.994
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.616
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         4102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+6.9044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3863
_reflns_number_total             4102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01241_si_002.cif
_cod_data_source_block           berry339
_cod_depositor_comments
'Adding full bibliography for 4344062--4344067.cif.'
_cod_database_code               4344065
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.759
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13)
;
_shelx_res_checksum              83574
_shelx_hkl_checksum              65241
_olex2_submission_special_instructions 'No special instructions were received'