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_4344066
_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         'C21.87 H14.8 Cl4.07 N4.93 O4 Ru2, C2 H3 N'
_chemical_formula_sum            'C23.87 H17.8 Cl4.07 N5.93 O4 Ru2'
_chemical_formula_weight         798.02
_chemical_name_common            Ru2(chp)4(MeCN).93(Cl).7*MeCN
_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   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                74.106(9)
_cell_angle_beta                 86.577(16)
_cell_angle_gamma                78.911(9)
_cell_formula_units_Z            2
_cell_length_a                   9.404(3)
_cell_length_b                   9.486(3)
_cell_length_c                   16.400(4)
_cell_measurement_reflns_used    9353
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.27
_cell_volume                     1380.7(7)
_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 1.000
_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    '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_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39066
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.554
_diffrn_reflns_theta_min         1.291
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  0.9664
_exptl_absorpt_correction_T_min  0.8269
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0605 before and 0.0312 after correction.
The Ratio of minimum to maximum transmission is 0.8556.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             783
_exptl_crystal_preparation       'Ru2(chp)4Cl solid + FeCl2/MeCN (hot)'
_exptl_crystal_recrystallization_method 'Reaction tube, no stirring'
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         8449
_refine_ls_number_restraints     362
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0262P)^2^+1.2538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7444
_reflns_number_total             8449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01241_si_002.cif
_cod_data_source_block           berry511
_cod_depositor_comments
'Adding full bibliography for 4344062--4344067.cif.'
_cod_original_cell_volume        1380.8(7)
_cod_original_formula_sum        'C23.87 H17.80 Cl4.07 N5.93 O4 Ru2'
_cod_database_code               4344066
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.026) H3(0.03) H4(0.027) H7(0.026) H8(0.028) H9(0.026)
 H12(0.031) H13(0.035) H14(0.031) H17(0.025) H18(0.029) H19(0.028) H24A(0.065)
 H24B(0.065) H24C(0.065)
 Fixed X: H2(-0.0776) H3(-0.0087) H4(0.2184) H7(-0.0406) H8(-0.0762)
 H9(0.0646) H12(0.5981) H13(0.7504) H14(0.7329) H17(0.4969) H18(0.7353)
 H19(0.8317) H22A(-0.0251) H22B(-0.0786) H22C(-0.1695) H22D(-0.1754) H22E(-
 0.1178) H22F(-0.2259) H22G(-0.169) H22H(-0.0535) H22I(-0.1774) H24A(0.2993)
 H24B(0.4553) H24C(0.344)
 Fixed Y: H2(1.0316) H3(1.2627) H4(1.2827) H7(0.5435) H8(0.7181) H9(0.9083)
 H12(0.1971) H13(0.1838) H14(0.3868) H17(0.6524) H18(0.6875) H19(0.7379)
 H22A(0.2251) H22B(0.2012) H22C(0.3276) H22D(0.3397) H22E(0.2346) H22F(0.3894)
 H22G(0.3504) H22H(0.1855) H22I(0.2949) H24A(0.0207) H24B(0.0068) H24C(0.1623)
 Fixed Z: H2(0.8071) H3(0.7593) H4(0.6905) H7(0.5933) H8(0.4628) H9(0.4241)
 H12(0.8063) H13(0.6919) H14(0.5699) H17(1.0045) H18(0.9814) H19(0.8422)
 H22A(1.0371) H22B(0.9519) H22C(0.9916) H22D(0.9909) H22E(0.9299) H22F(0.8941)
 H22G(1.0061) H22H(0.9928) H22I(0.9113) H24A(0.8655) H24B(0.9042) H24C(0.8855)
;
_shelx_res_checksum              69530
_shelx_hkl_checksum              48603
_olex2_submission_original_sample_id Berry511
_olex2_submission_special_instructions 'No special instructions were received'