Non-innocence and mixed valency in tri- and tetranuclear ruthenium complexes of a heteroquinone bridging ligand
Ansari, Mohd. Asif; Mandal, Abhishek; Beyer, Katharina; Paretzki, Alexa; Schwederski, Brigitte; Kaim, W.; Lahiri, Goutam Kumar; Dalton Trans.  (2017) –; doi:10.1039/C7DT03509H

data_7044579
_publ_section_title
;
 Non-innocence and mixed valency in tri- and tetranuclear ruthenium
 complexes of a heteroquinone bridging ligand
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03509H
_journal_year                    2017
_chemical_formula_sum            'C102 H100 N8 O32.5 Ru6'
_chemical_formula_weight         2564.31
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-02 deposited with the CCDC.
2017-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                106.199(2)
_cell_angle_beta                 103.748(2)
_cell_angle_gamma                100.635(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7442(2)
_cell_length_b                   14.8795(3)
_cell_length_c                   17.1035(3)
_cell_measurement_reflns_used    27978
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      75.0380
_cell_measurement_theta_min      2.8280
_cell_volume                     2685.21(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18456
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         2.826
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.355
_exptl_absorpt_correction_T_max  -0.010
_exptl_absorpt_correction_T_min  10000000.000
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.027
_refine_diff_density_max         2.038
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.014(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1332
_refine_ls_number_reflns         18456
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1344P)^2^+7.5560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.932
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                17513
_reflns_number_total             18456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03509h2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        2685.20(9)
_cod_original_formula_sum        'C102 H100 N8 O32.50 Ru6'
_cod_database_code               7044579
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.826
_shelx_res_checksum              21172