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_4344063
_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, C4 H8 O'
_chemical_formula_sum            'C42 H35 Cl4 N4 O5 P Ru2'
_chemical_formula_weight         1050.65
_chemical_name_systematic        Ru2(chp)4(PPh3)*THF
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 99.490(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5005(14)
_cell_length_b                   32.007(3)
_cell_length_c                   13.4954(11)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      68.191
_cell_measurement_theta_min      3.596
_cell_volume                     4047.6(8)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\ \w and 0.6\ \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            66660
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.318
_diffrn_reflns_theta_min         2.761
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.275
_exptl_absorpt_correction_T_max  0.7879
_exptl_absorpt_correction_T_min  0.3460
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0731 before and 0.0501 after correction.
The Ratio of minimum to maximum transmission is 0.4391.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2104
_exptl_crystal_preparation       'hexane/THF liquid diffusion'
_exptl_crystal_recrystallization_method 'hexane/THF liquid diffusion'
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         7292
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0221
_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^)+(0.0199P)^2^+4.0524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6498
_reflns_number_total             7292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01241_si_002.cif
_cod_data_source_block           berry477
_cod_depositor_comments
'Adding full bibliography for 4344062--4344067.cif.'
_cod_database_code               4344063
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.019) H3(0.024) H4(0.024) H7(0.019) H8(0.024) H9(0.023)
 H12(0.018) H13(0.02) H14(0.02) H17(0.024) H18(0.029) H19(0.027) H22(0.019)
 H23(0.025) H24(0.025) H25(0.022) H26(0.018) H28(0.018) H29(0.024) H30(0.024)
 H31(0.02) H32(0.017) H34(0.017) H35(0.025) H36(0.027) H37(0.022) H38(0.016)
 H39A(0.027) H39B(0.027) H40A(0.033) H40B(0.033) H40C(0.033) H40D(0.033)
 H41A(0.04) H41B(0.04) H42A(0.043) H42B(0.043) H41C(0.046) H41D(0.046)
 H42C(0.054) H42D(0.054)
 Fixed X: H2(-0.1596) H3(-0.2985) H4(-0.3106) H7(-0.1945) H8(-0.4226) H9(-
 0.4987) H12(0.3677) H13(0.2705) H14(0.0567) H17(0.382) H18(0.401) H19(0.271)
 H22(0.0768) H23(-0.0225) H24(0.017) H25(0.1545) H26(0.2618) H28(0.1716)
 H29(0.2742) H30(0.5185) H31(0.6588) H32(0.5557) H34(0.4634) H35(0.6729)
 H36(0.7579) H37(0.6301) H38(0.4245) H39A(1.1218) H39B(1.0301) H40A(0.9344)
 H40B(0.8207) H40C(0.9455) H40D(0.8453) H41A(0.9654) H41B(0.7956) H42A(0.8174)
 H42B(0.9522) H41C(0.7389) H41D(0.7965) H42C(0.9018) H42D(1.0139)
 Fixed Y: H2(0.506) H3(0.5005) H4(0.4357) H7(0.3702) H8(0.3452) H9(0.3275)
 H12(0.2946) H13(0.2286) H14(0.2104) H17(0.4278) H18(0.3814) H19(0.318)
 H22(0.507) H23(0.5684) H24(0.5874) H25(0.5445) H26(0.4843) H28(0.3847)
 H29(0.3455) H30(0.3513) H31(0.3975) H32(0.438) H34(0.4158) H35(0.4401)
 H36(0.5071) H37(0.5503) H38(0.5254) H39A(0.2836) H39B(0.3119) H40A(0.2397)
 H40B(0.2777) H40C(0.238) H40D(0.2696) H41A(0.2458) H41B(0.2532) H42A(0.3246)
 H42B(0.3117) H41C(0.2949) H41D(0.2522) H42C(0.32) H42D(0.2831)
 Fixed Z: H2(0.0469) H3(-0.1103) H4(-0.1966) H7(0.4186) H8(0.3666) H9(0.1953)
 H12(0.3601) H13(0.3718) H14(0.2636) H17(-0.0473) H18(-0.1767) H19(-0.1898)
 H22(0.2416) H23(0.293) H24(0.4626) H25(0.5809) H26(0.5294) H28(0.4614)
 H29(0.6004) H30(0.6618) H31(0.5865) H32(0.4499) H34(0.21) H35(0.162)
 H36(0.2075) H37(0.3008) H38(0.3546) H39A(0.5089) H39B(0.4232) H40A(0.4533)
 H40B(0.4376) H40C(0.4869) H40D(0.4141) H41A(0.629) H41B(0.5981) H42A(0.6131)
 H42B(0.6961) H41C(0.5441) H41D(0.6012) H42C(0.682) H42D(0.6711)
;
_shelx_res_checksum              40238
_shelx_hkl_checksum              11674
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_submission_original_sample_id Berry477
_olex2_submission_special_instructions 'No special instructions were received'