Bidirectional noninnocence of hinge like deprotonated bis-lawsone on selective ruthenium platform. A function of varying ancillary ligands
Lahiri, Goutam Kumar; Bera, Sudip Kumar; Arya, Yogita; Jimenez-Aparicio, Reyes; Priego, Jose Luis; Dalton Transactions  (2022) –; doi:10.1039/D2DT01466A

data_7710444
_publ_section_title
;
 Bidirectional noninnocence of hinge like deprotonated bis-lawsone on
 selective ruthenium platform. A function of varying ancillary ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01466A
_journal_year                    2022
_chemical_formula_moiety         'C60 H40 N8 O6 Ru2, 2(Cl O4)'
_chemical_formula_sum            'C60 H40 Cl2 N8 O14 Ru2'
_chemical_formula_weight         1370.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-04-25 deposited with the CCDC.	2022-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9906(7)
_cell_length_b                   20.0361(9)
_cell_length_c                   14.8190(6)
_cell_measurement_reflns_used    3840
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.1420
_cell_measurement_theta_min      2.0150
_cell_volume                     5638.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f     39.35 187.85   0.50   16.00  81.90  -8.96  31.50    --   297
  2  \w    -31.91  81.59   0.50   16.00    --   -9.01  49.32 -46.88  227
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0414678000
_diffrn_orient_matrix_UB_12      -0.0033334000
_diffrn_orient_matrix_UB_13      0.0174411000
_diffrn_orient_matrix_UB_21      -0.0020174000
_diffrn_orient_matrix_UB_22      -0.0361356000
_diffrn_orient_matrix_UB_23      -0.0088945000
_diffrn_orient_matrix_UB_31      0.0238307000
_diffrn_orient_matrix_UB_32      -0.0089576000
_diffrn_orient_matrix_UB_33      0.0294574000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1047
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36529
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.018
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic bluish blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.155
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0843
_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^)+(0.0624P)^2^+45.6721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.1985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3696
_reflns_number_total             4969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01466a2.cif
_cod_data_source_block           '[1](ClO4)2'
_cod_database_code               7710444
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.822
_reflns_odcompleteness_completeness 84.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.27
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C27(H27), C30(H30), C3(H3), C11(H11), C2(H2), C29(H29), C14(H14), C28(H28),
 C1(H1), C12(H12), C10(H10), C13(H13), C17(H17), C20(H20), C4(H4), C9(H9),
 C7(H7), C19(H19), C18(H18), C8(H8)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67435
_shelx_hkl_checksum              82514
_shelx_fab_checksum              25477
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.375
_oxdiff_exptl_absorpt_empirical_full_min 0.830