Isomeric Diruthenium Complexes of a Heterocyclic and Quinonoid Bridging Ligand: Valence and Spin Alternatives for the Metal/Ligand/Metal Arrangement.
Ansari, Mohd Asif; Mandal, Abhishek; Paretzki, Alexa; Beyer, Katharina; Kaim, Wolfgang; Lahiri, Goutam Kumar; Inorganic chemistry 55 (2016) 12357–12365; doi:10.1021/acs.inorgchem.6b02245

data_4349278
_publ_section_title
;
 Isomeric Diruthenium Complexes of a Heterocyclic and Quinonoid Bridging
 Ligand: Valence and Spin Alternatives for the Metal/Ligand/Metal
 Arrangement.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12357
_journal_page_last               12365
_journal_paper_doi               10.1021/acs.inorgchem.6b02245
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C38 H36 N4 O10 Ru2, C2 H3 N'
_chemical_formula_sum            'C40 H39 N5 O10 Ru2'
_chemical_formula_weight         951.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   34.064(6)
_cell_length_b                   60.772(10)
_cell_length_c                   8.0360(13)
_cell_measurement_reflns_used    13084
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      3.1
_cell_volume                     16636(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  AFC12
_diffrn_measurement_method       Rigaku
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       67
_diffrn_reflns_limit_k_min       -72
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            40863
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.097
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       plate
_exptl_crystal_F_000             7712
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 2934 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.018(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7339
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0346P)^2^+61.8269P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7010
_reflns_number_total             7339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02245_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4349278
_shelxl_version_number           2012-9
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.852
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C31(H31), C15(H15), C16(H16), C7(H7), C4(H4), C5(H5), C14(H14),
 C6(H6), C21(H21), C26(H26), C36(H36)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C38(H38A,H38B,
 H38C), C33(H33A,H33B,H33C), C28(H28A,H28B,H28C), C23(H23A,H23B,H23C), C19(H19A,
 H19B,H19C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              23501
_shelx_hkl_checksum              4306
_olex2_submission_special_instructions 'No special instructions were received'