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_4344062
_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         'C24 H20 Cl4 N4 O5 Ru2, 2.35(C4 H8 O)'
_chemical_formula_sum            'C33.41 H38.83 Cl4 N4 O7.35 Ru2'
_chemical_formula_weight         958.07
_chemical_name_common            Ru2(chp)4(THF)*2.4THF
_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                 98.481(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.311(2)
_cell_length_b                   17.1328(19)
_cell_length_c                   18.565(2)
_cell_measurement_reflns_used    9424
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      69.46
_cell_measurement_theta_min      3.21
_cell_volume                     7333.5(13)
_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      100.01
_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 0.995
_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    '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  0.0301
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58260
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.775
_diffrn_reflns_theta_min         3.214
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.809
_exptl_absorpt_correction_T_max  0.5962
_exptl_absorpt_correction_T_min  0.1624
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0671 before and 0.0371 after correction.
The Ratio of minimum to maximum transmission is 0.2724.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3857
_exptl_crystal_recrystallization_method 'THF/Hexanes, -20 deg C'
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.773
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         6900
_refine_ls_number_restraints     559
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0273P)^2^+29.9650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6487
_reflns_number_total             6900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01241_si_002.cif
_cod_data_source_block           berry319
_cod_depositor_comments
'Adding full bibliography for 4344062--4344067.cif.'
_cod_original_cell_volume        7333.7(13)
_cod_database_code               4344062
_shelx_estimated_absorpt_t_max   0.515
_shelx_estimated_absorpt_t_min   0.145
_olex2_refinement_description
;
1. Others
 Fixed Sof: O7(0.5) C29(0.5) H29A(0.5) H29B(0.5) C30(0.5) H30A(0.5) H30B(0.5)
 C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 Fixed Uiso: H2(0.034) H3(0.04) H4(0.042) H7(0.037) H8(0.047) H9(0.053)
 H12(0.045) H13(0.054) H14(0.053) H17(0.063) H18(0.079) H19(0.072) H21A(0.021)
 H21B(0.021) H22A(0.027) H22B(0.027) H23A(0.034) H23B(0.034) H24A(0.031)
 H24B(0.031) H21C(0.035) H21D(0.035) H22C(0.041) H22D(0.041) H23C(0.046)
 H23D(0.046) H24C(0.034) H24D(0.034) H25A(0.051) H25B(0.051) H26A(0.065)
 H26B(0.065) H27A(0.054) H27B(0.054) H28A(0.06) H28B(0.06) H25C(0.066)
 H25D(0.066) H26C(0.059) H26D(0.059) H27C(0.068) H27D(0.068) H28C(0.059)
 H28D(0.059) H29A(0.078) H29B(0.078) H30A(0.053) H30B(0.053) H31A(0.075)
 H31B(0.075) H32A(0.057) H32B(0.057) H33A(0.049) H33B(0.049) H34A(0.054)
 H34B(0.054) H35A(0.081) H35B(0.081) H36A(0.078) H36B(0.078) H33C(0.071)
 H33D(0.071) H34C(0.066) H34D(0.066) H35C(0.08) H35D(0.08) H36C(0.079)
 H36D(0.079) H37A(0.07) H37B(0.07) H38A(0.059) H38B(0.059) H39A(0.063)
 H39B(0.063) H40A(0.064) H40B(0.064) H37C(0.068) H37D(0.068) H38C(0.068)
 H38D(0.068) H39C(0.065) H39D(0.065) H40C(0.073) H40D(0.073)
 Fixed X: H2(0.3682) H3(0.3475) H4(0.3127) H7(0.5153) H8(0.5115) H9(0.4222)
 H12(0.3479) H13(0.271) H14(0.1998) H17(0.1984) H18(0.111) H19(0.1003)
 H21A(0.4206) H21B(0.4817) H22A(0.4193) H22B(0.4884) H23A(0.482) H23B(0.4301)
 H24A(0.4055) H24B(0.3606) H21C(0.43) H21D(0.4901) H22C(0.4987) H22D(0.4297)
 H23C(0.4415) H23D(0.4922) H24C(0.4142) H24D(0.37) H25A(0.3962) H25B(0.3912)
 H26A(0.2978) H26B(0.298) H27A(0.3083) H27B(0.2749) H28A(0.3545) H28B(0.3817)
 H25C(0.4444) H25D(0.4104) H26C(0.4016) H26D(0.3582) H27C(0.2924) H27D(0.3411)
 H28C(0.29) H28D(0.2939) H29A(0.5447) H29B(0.476) H30A(0.5322) H30B(0.4649)
 H31A(0.4378) H31B(0.4935) H32A(0.494) H32B(0.5532) H33A(0.3997) H33B(0.4177)
 H34A(0.431) H34B(0.4692) H35A(0.543) H35B(0.5024) H36A(0.5565) H36B(0.5466)
 H33C(0.4043) H33D(0.4277) H34C(0.4426) H34D(0.4903) H35C(0.5526) H35D(0.5017)
 H36C(0.552) H36D(0.4925) H37A(0.4237) H37B(0.4676) H38A(0.4603) H38B(0.5077)
 H39A(0.5759) H39B(0.535) H40A(0.5574) H40B(0.4937) H37C(0.4037) H37D(0.4378)
 H38C(0.4492) H38D(0.4976) H39C(0.5525) H39D(0.4974) H40C(0.561) H40D(0.5378)
 Fixed Y: H2(1.1708) H3(1.1649) H4(1.0469) H7(0.8716) H8(0.7622) H9(0.6966)
 H12(0.7345) H13(0.6492) H14(0.6669) H17(1.0578) H18(1.074) H19(1.0277)
 H21A(0.9277) H21B(0.9538) H22A(1.0275) H22B(1.0284) H23A(1.1257) H23B(1.1519)
 H24A(1.124) H24B(1.0952) H21C(0.949) H21D(0.9736) H22C(1.0544) H22D(1.0556)
 H23C(1.1763) H23D(1.1456) H24C(1.1411) H24D(1.1172) H25A(0.3879) H25B(0.2958)
 H26A(0.29) H26B(0.3767) H27A(0.4345) H27B(0.3572) H28A(0.3089) H28B(0.3948)
 H25C(0.3594) H25D(0.4142) H26C(0.4267) H26D(0.4687) H27C(0.3854) H27D(0.3196)
 H28C(0.3579) H28D(0.2723) H29A(0.3002) H29B(0.3086) H30A(0.2065) H30B(0.2049)
 H31A(0.2844) H31B(0.2451) H32A(0.3923) H32B(0.3467) H33A(0.3507) H33B(0.2601)
 H34A(0.3471) H34B(0.2698) H35A(0.3577) H35B(0.4277) H36A(0.3092) H36B(0.3987)
 H33C(0.3446) H33D(0.2565) H34C(0.3545) H34D(0.288) H35C(0.3835) H35D(0.4478)
 H36C(0.3937) H36D(0.4424) H37A(0.5351) H37B(0.6075) H38A(0.5102) H38B(0.5783)
 H39A(0.4937) H39B(0.4272) H40A(0.4228) H40B(0.3978) H37C(0.5067) H37D(0.5871)
 H38C(0.5059) H38D(0.5669) H39C(0.4549) H39D(0.4007) H40C(0.499) H40D(0.4119)
 Fixed Z: H2(0.4399) H3(0.558) H4(0.6024) H7(0.4502) H8(0.5227) H9(0.5223)
 H12(0.1527) H13(0.1469) H14(0.224) H17(0.1516) H18(0.195) H19(0.3116)
 H21A(0.1377) H21B(0.1831) H22A(0.0606) H22B(0.0866) H23A(0.1713) H23B(0.1087)
 H24A(0.2363) H24B(0.167) H21C(0.1503) H21D(0.1991) H22C(0.1048) H22D(0.0778)
 H23C(0.1322) H23D(0.1944) H24C(0.2569) H24D(0.1854) H25A(0.533) H25B(0.5479)
 H26A(0.49) H26B(0.5242) H27A(0.4174) H27B(0.3846) H28A(0.349) H28B(0.3626)
 H25C(0.5019) H25D(0.5516) H26C(0.4059) H26D(0.454) H27C(0.3869) H27D(0.3811)
 H28C(0.5083) H28D(0.4735) H29A(0.6594) H29B(0.6345) H30A(0.736) H30B(0.6999)
 H31A(0.7869) H31B(0.8354) H32A(0.8221) H32B(0.8144) H33A(0.2876) H33B(0.2927)
 H34A(0.1804) H34B(0.2014) H35A(0.2125) H35B(0.2338) H36A(0.3247) H36B(0.3453)
 H33C(0.2789) H33D(0.2756) H34C(0.1754) H34D(0.1996) H35C(0.2362) H35D(0.2262)
 H36C(0.3538) H36D(0.3418) H37A(0.453) H37B(0.4537) H38A(0.5656) H38B(0.5641)
 H39A(0.5398) H39B(0.5666) H40A(0.4353) H40B(0.451) H37C(0.4621) H37D(0.4544)
 H38C(0.5752) H38D(0.5568) H39C(0.5652) H39D(0.5358) H40C(0.4513) H40D(0.4314)
;
_shelx_res_checksum              28019
_shelx_hkl_checksum              23868
_olex2_submission_original_sample_id Berry319
_olex2_submission_special_instructions 'No special instructions were received'