Metallo-supramolecular assembly of protic pincer-type complexes: encapsulation of dinitrogen and carbon disulfide into multiproton-responsive diruthenium cage
Toda, Tatsuro; Suzuki, Satoshi; Kuwata, Shigeki; Chemical Communications  (2018) –; doi:10.1039/C8CC08384C

data_7122667
_publ_section_title
;
 Metallo-supramolecular assembly of protic pincer-type complexes:
 encapsulation of dinitrogen and carbon disulfide into
 multiproton-responsive diruthenium cage
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08384C
_journal_year                    2018
_chemical_formula_moiety
'C108 H112 Br K N8 P4 Ru2, C6 H6, 0.5(C5 H12)'
_chemical_formula_sum            'C116.5 H124 Br K N8 P4 Ru2'
_chemical_formula_weight         2081.35
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-11-23 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                92.417(2)
_cell_angle_beta                 101.754(2)
_cell_angle_gamma                104.9134(18)
_cell_formula_units_Z            2
_cell_length_a                   14.936(3)
_cell_length_b                   16.296(3)
_cell_length_c                   22.411(4)
_cell_measurement_reflns_used    12027
_cell_measurement_temperature    93
_cell_measurement_theta_max      28.89
_cell_measurement_theta_min      2.57
_cell_volume                     5134.6(17)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            57664
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         3.045
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2162.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene/pentane'
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.60
_refine_diff_density_min         -1.17
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1199
_refine_ls_number_reflns         22894
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0803P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16333
_reflns_number_total             22894
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c8cc08384c2.cif
_cod_data_source_block           compound2-C6H6-C5H12
_cod_original_cell_volume        5134.7(16)
_cod_database_code               7122667
_shelx_res_checksum              24332
_shelx_hkl_checksum              68294
_shelx_fab_checksum              29144