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_4344064
_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         'C38 H27 Cl4 N4 O4 P Ru2, 0.5(C7 H8)'
_chemical_formula_sum            'C41.5 H31 Cl4 N4 O4 P Ru2'
_chemical_formula_weight         1024.61
_chemical_name_common            Ru2(chp)4(PPh3)0.5toluene
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                82.934(9)
_cell_angle_beta                 79.593(13)
_cell_angle_gamma                87.230(7)
_cell_formula_units_Z            2
_cell_length_a                   9.314(2)
_cell_length_b                   9.601(3)
_cell_length_c                   22.177(6)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100.00(1)
_cell_measurement_theta_max      30.71
_cell_measurement_theta_min      2.22
_cell_volume                     1935.0(9)
_computing_cell_refinement       'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008-2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.745
_diffrn_reflns_theta_min         1.880
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.1965
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0953 before and 0.0797 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1022
_exptl_crystal_recrystallization_method ether/toluene
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.400
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         11934
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+2.5247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11375
_reflns_number_total             11934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01241_si_002.cif
_cod_data_source_block           berry469
_cod_depositor_comments
'Adding full bibliography for 4344062--4344067.cif.'
_cod_original_cell_volume        1935.1(9)
_cod_original_formula_sum        'C41.50 H31 Cl4 N4 O4 P Ru2'
_cod_database_code               4344064
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.707
_olex2_refinement_description
;
1. Others
 Fixed Sof: C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C40(0.5) C41(0.5) H41(0.5)
 C42(0.5) H42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C45(0.5) H45(0.5)
 Fixed Uiso: H2(0.032) H3(0.044) H4(0.043) H7(0.022) H8(0.029) H9(0.026)
 H12(0.026) H13(0.032) H14(0.028) H17(0.027) H18(0.032) H19(0.032) H22(0.025)
 H23(0.029) H24(0.029) H25(0.026) H26(0.021) H28(0.021) H29(0.026) H30(0.027)
 H31(0.024) H32(0.02) H34(0.023) H35(0.029) H36(0.031) H37(0.031) H38(0.024)
 H39A(0.062) H39B(0.062) H39C(0.062) H41(0.05) H42(0.055) H43(0.058) H44(0.058)
 H45(0.046)
 Fixed X: H2(0.6452) H3(0.857) H4(0.8774) H7(0.0176) H8(0.069) H9(0.2458) H12(-
 0.069) H13(-0.1461) H14(-0.0271) H17(0.6161) H18(0.6984) H19(0.6352)
 H22(0.3512) H23(0.3341) H24(0.1214) H25(-0.0739) H26(-0.0549) H28(-0.072) H29(-
 0.3035) H30(-0.3788) H31(-0.2181) H32(0.0106) H34(0.2929) H35(0.4043)
 H36(0.4629) H37(0.4063) H38(0.2858) H39A(0.2829) H39B(0.3073) H39C(0.2039)
 H41(0.0853) H42(-0.1187) H43(-0.2217) H44(-0.1178) H45(0.0862)
 Fixed Y: H2(0.5859) H3(0.6536) H4(0.6335) H7(0.7522) H8(0.9681) H9(0.985)
 H12(0.146) H13(0.2216) H14(0.408) H17(-0.0025) H18(-0.0656) H19(0.0759)
 H22(0.3858) H23(0.4851) H24(0.4618) H25(0.3374) H26(0.2319) H28(0.3493)
 H29(0.2831) H30(0.0517) H31(-0.1134) H32(-0.0457) H34(-0.0042) H35(-0.2244)
 H36(-0.2977) H37(-0.151) H38(0.0651) H39A(0.1702) H39B(0.0248) H39C(0.1459)
 H41(0.1954) H42(0.1064) H43(-0.1025) H44(-0.2218) H45(-0.1324)
 Fixed Z: H2(0.3377) H3(0.2698) H4(0.1637) H7(0.3179) H8(0.2627) H9(0.1706)
 H12(0.2071) H13(0.1145) H14(0.0477) H17(0.2393) H18(0.1415) H19(0.0545)
 H22(0.4301) H23(0.5222) H24(0.5969) H25(0.5796) H26(0.4891) H28(0.3349)
 H29(0.3251) H30(0.3572) H31(0.3983) H32(0.4115) H34(0.3104) H35(0.3298)
 H36(0.427) H37(0.5055) H38(0.4874) H39A(0.0002) H39B(0.0413) H39C(0.0709) H41(-
 0.0564) H42(-0.0848) H43(-0.032) H44(0.0494) H45(0.0778)
;
_shelx_res_checksum              89880
_shelx_hkl_checksum              55039
_olex2_submission_special_instructions 'No special instructions were received'