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_7710443
_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         'C40 H37 O14 Ru2'
_chemical_formula_sum            'C40 H37 O14 Ru2'
_chemical_formula_weight         943.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-25
_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                86.133(4)
_cell_angle_beta                 83.120(4)
_cell_angle_gamma                78.119(4)
_cell_formula_units_Z            2
_cell_length_a                   12.1135(5)
_cell_length_b                   13.4028(6)
_cell_length_c                   14.5460(8)
_cell_measurement_reflns_used    17776
_cell_measurement_temperature    100.5(7)
_cell_measurement_theta_max      27.3610
_cell_measurement_theta_min      2.0720
_cell_volume                     2292.15(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.5(7)
_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   -349.73  10.27   1.00    3.00   6.61  -9.84 -31.50    --   360
  2  \w    -65.46  -0.46   1.00    3.00    --  -19.34  94.56 145.16   65
  3  \w    -60.89   0.11   1.00    3.00    --  -14.77  94.56 -34.84   61
  4  \w   -100.81  15.19   1.00    3.00    --   -9.84 -59.25 -51.92  116
  5  \w    -65.46  -0.46   1.00    3.00    --  -19.34  94.56   1.16   65
  6  \f    -10.27 349.73   1.00    3.00  81.02  -9.84  31.50    --   360
  7  \w    -65.46  -0.46   1.00    3.00    --  -19.34  94.56  73.16   65
  8  \f   -339.92  20.08   1.00    3.00  15.81  -9.84 -59.25    --   360
  9  \w   -100.81  15.19   1.00    3.00    --   -9.84 -59.25 164.08  116
 10  \w    -51.04  -0.04   1.00    3.00    --   -4.92  94.56 -34.84   51
;
_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      0.0145590000
_diffrn_orient_matrix_UB_12      0.0403848000
_diffrn_orient_matrix_UB_13      -0.0299631000
_diffrn_orient_matrix_UB_21      -0.0543832000
_diffrn_orient_matrix_UB_22      0.0303765000
_diffrn_orient_matrix_UB_23      0.0123570000
_diffrn_orient_matrix_UB_31      0.0212964000
_diffrn_orient_matrix_UB_32      0.0194089000
_diffrn_orient_matrix_UB_33      0.0369674000
_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  0.1176
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            100536
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.554
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0
_refine_diff_density_max         7.590
_refine_diff_density_min         -1.813
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.255
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.1037
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2791
_refine_ls_wR_factor_ref         0.2976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6479
_reflns_number_total             8069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01466a2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2292.16(19)
_cod_database_code               7710443
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   0.849
_reflns_odcompleteness_completeness 79.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.80
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C17(H17), C8(H8), C18(H18), C10(H10), C9(H9), C20(H20), C19(H19),
 C38(H38), C23(H23), C28(H28)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C016(H01A,H01B,H01C), C21(H21A,H21B,H21C), C30(H30A,H30B,
 H30C), C37(H37A,H37B,H37C), C32(H32A,H32B,H32C), C26(H26A,H26B,H26C), C35(H35A,
 H35B,H35C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              47173
_shelx_hkl_checksum              45429
_shelx_fab_checksum              99701
_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 2.061
_oxdiff_exptl_absorpt_empirical_full_min 0.355