Variable electronic structure and spin distribution in bis(2,2'-bipyridine)-metal complexes (M = Ru or Os) of 4,5-dioxido- and 4,5-diimido-pyrene.
Chatterjee, Madhumita; Mondal, Sudipta; Hazari, Arijit Singha; Záliš, Stanislav; Kaim, Wolfgang; Lahiri, Goutam Kumar; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4191–4201; doi:10.1039/d1dt00282a

data_7706732
_publ_section_title
;
 Variable electronic structure and spin distribution in
 bis(2,2'-bipyridine)-metal complexes (M = Ru or Os) of 4,5-dioxido- and
 4,5-diimido-pyrene.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4191
_journal_page_last               4201
_journal_paper_doi               10.1039/d1dt00282a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C36 H26 N6 Ru, 2(Cl O4)'
_chemical_formula_sum            'C36 H26 Cl2 N6 O8 Ru'
_chemical_formula_weight         842.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-06-07 deposited with the CCDC.	2021-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.022(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7428(4)
_cell_length_b                   16.1774(8)
_cell_length_c                   20.8421(9)
_cell_measurement_reflns_used    5707
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.0680
_cell_measurement_theta_min      1.9580
_cell_volume                     3266.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.9939
_diffrn_measured_fraction_theta_max 0.9939
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -49.00  70.00   0.50    8.00    --  -20.00  72.00  36.00  238
  2  \w    -69.00  15.00   0.50    8.00    --  -20.00   0.00  36.00  168
  3  \w    -54.00   0.00   0.50    8.00    --  -20.00  72.00 -36.00  108
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0150111000
_diffrn_orient_matrix_UB_12      0.0330651000
_diffrn_orient_matrix_UB_13      -0.0219087000
_diffrn_orient_matrix_UB_21      0.0131869000
_diffrn_orient_matrix_UB_22      -0.0261844000
_diffrn_orient_matrix_UB_23      -0.0259822000
_diffrn_orient_matrix_UB_31      -0.0704789000
_diffrn_orient_matrix_UB_32      -0.0119082000
_diffrn_orient_matrix_UB_33      -0.0039430000
_diffrn_radiation_collimation    0.3
_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  0.0713
_diffrn_reflns_av_unetI/netI     0.1098
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21871
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.7131
_exptl_crystal_description       needle
_exptl_crystal_F_000             1700
_refine_diff_density_max         0.8929
_refine_diff_density_min         -1.2679
_refine_diff_density_rms         0.1890
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             10.3635
_refine_ls_goodness_of_fit_ref   1.0491
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    48
_refine_ls_number_parameters     486
_refine_ls_number_reflns         5731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0491
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+2.7338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -9
_reflns_number_gt                4508
_reflns_number_total             5731
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt00282a2.cif
_cod_data_source_block           '[3](ClO4)2'
_cod_depositor_comments
'Adding full bibliography for 7706729--7706732.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7706732
_chemical_oxdiff_formula         'C50 H40 N10 O10 Ru2'
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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), C18(H18), C5(H5), C6(H6), C33(H33), C20(H20), C11(H11), C17(H17),
 C23(H23), C28(H28), C13(H13), C29(H29), C4(H4), C34(H34), C19(H19), C9(H9),
 C30(H30), C25(H25), C35(H35), C24(H24), C26(H26), C36(H36), C8(H8), C12(H12)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.441
_oxdiff_exptl_absorpt_empirical_full_min 0.835