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_4344067
_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         'C40 H24 Cl10 N8 O8 Ru4 Zn, 1.33(C H2 Cl2)'
_chemical_formula_sum            'C41.33 H26.66 Cl12.66 N8 O8 Ru4 Zn'
_chemical_formula_weight         1681.87
_chemical_name_common            '[Ru2(chp)4]2(ZnCl2)*1.33(CH2Cl2)'
_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                 103.80(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.665(16)
_cell_length_b                   22.80(2)
_cell_length_c                   18.894(18)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      0.000
_cell_measurement_theta_min      0.000
_cell_volume                     6135(10)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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 0.986
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0909
_diffrn_reflns_laue_measured_fraction_full 0.986
_diffrn_reflns_laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21354
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.389
_diffrn_reflns_theta_min         1.424
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.950
_exptl_absorpt_correction_T_max  0.9926
_exptl_absorpt_correction_T_min  0.9198
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0511 before and 0.0422 after correction.
The Ratio of minimum to maximum transmission is 0.9267.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.035
_platon_squeeze_details
;
;
_refine_diff_density_max         1.447
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         12297
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      1.348
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0481P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7793
_reflns_number_total             12297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01241_si_002.cif
_cod_data_source_block           berry403
_cod_depositor_comments
'Adding full bibliography for 4344062--4344067.cif.'
_cod_original_cell_volume        6136(11)
_cod_database_code               4344067
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.820
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H7(0.028) H8(0.03) H9(0.03) H7A(0.029) H8A(0.03) H9A(0.03)
 H22(0.035) H23(0.041) H24(0.034) H32(0.058) H33(0.055) H34(0.042) H2(0.031)
 H3(0.035) H4(0.029) H12(0.028) H13(0.028) H14(0.03) H17(0.034) H18(0.041)
 H19(0.033) H27(0.043) H28(0.047) H29(0.033) H37(0.046) H38(0.046) H39(0.032)
 H1SA(0.059) H1SB(0.059) H2SA(0.051) H2SB(0.051)
 Fixed X: H7(0.8729) H8(1.0055) H9(1.1525) H7A(0.8714) H8A(1.0072) H9A(1.1531)
 H22(0.4968) H23(0.3614) H24(0.314) H32(0.5603) H33(0.7309) H34(0.817)
 H2(1.0496) H3(1.2053) H4(1.2896) H12(0.7286) H13(0.7938) H14(0.95) H17(0.9175)
 H18(1.0042) H19(1.096) H27(0.2962) H28(0.4062) H29(0.5658) H37(0.5997)
 H38(0.7036) H39(0.743) H1SA(0.3164) H1SB(0.2837) H2SA(0.9569) H2SB(0.9185)
 Fixed Y: H7(0.7404) H8(0.7979) H9(0.7495) H7A(0.7378) H8A(0.7959) H9A(0.7477)
 H22(0.4304) H23(0.3735) H24(0.3559) H32(0.66) H33(0.6585) H34(0.6074)
 H2(0.5697) H3(0.5412) H4(0.5059) H12(0.5071) H13(0.5285) H14(0.5631)
 H17(0.3447) H18(0.2858) H19(0.3276) H27(0.644) H28(0.7057) H29(0.6829)
 H37(0.3573) H38(0.2997) H39(0.3273) H1SA(0.1732) H1SB(0.1063) H2SA(0.6741)
 H2SB(0.7376)
 Fixed Z: H7(0.2616) H8(0.259) H9(0.2733) H7A(0.2845) H8A(0.2978) H9A(0.3058)
 H22(0.0011) H23(-0.0035) H24(0.1059) H32(0.4623) H33(0.4923) H34(0.4286)
 H2(0.5295) H3(0.5716) H4(0.4864) H12(0.0607) H13(-0.0367) H14(-0.0163)
 H17(0.3372) H18(0.2787) H19(0.205) H27(0.1039) H28(0.0691) H29(0.1056)
 H37(0.4673) H38(0.4208) H39(0.3141) H1SA(0.6624) H1SB(0.6538) H2SA(0.4204)
 H2SB(0.4346)
;
_shelx_res_checksum              25605
_shelx_hkl_checksum              28432
_olex2_submission_special_instructions 'No special instructions were received'