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_7706729
_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 H24 N4 O2 Ru, Cl O4, 2(C6 H6)'
_chemical_formula_sum            'C48 H36 Cl N4 O6 Ru'
_chemical_formula_weight         901.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-07 deposited with the CCDC.	2021-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.578(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.1871(4)
_cell_length_b                   25.7337(6)
_cell_length_c                   19.8582(5)
_cell_measurement_reflns_used    23905
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.1490
_cell_measurement_theta_min      2.0450
_cell_volume                     8263.6(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -110.00  70.00   0.50    8.00    --  -20.00   0.00  36.00  360
  2  \w    -79.00   9.00   0.50    8.00    --  -20.00 -72.00-108.00  176
  3  \w    -53.00 -21.00   0.50    8.00    --  -20.00  72.00  36.00   64
  4  \w   -110.00-104.50   0.50    8.00    --  -20.00   0.00 -36.00   11
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0327515000
_diffrn_orient_matrix_UB_12      0.0102428000
_diffrn_orient_matrix_UB_13      0.0185396000
_diffrn_orient_matrix_UB_21      -0.0195830000
_diffrn_orient_matrix_UB_22      -0.0246580000
_diffrn_orient_matrix_UB_23      -0.0007661000
_diffrn_orient_matrix_UB_31      0.0216434000
_diffrn_orient_matrix_UB_32      -0.0068253000
_diffrn_orient_matrix_UB_33      0.0305602000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47058
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.886
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80381
_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    1.449
_exptl_crystal_description       plate
_exptl_crystal_F_000             3688
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         14533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+42.2655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12741
_reflns_number_total             14533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00282a2.cif
_cod_data_source_block           '[1](ClO4)'
_cod_depositor_comments
;
Adding full bibliography for 7706729--7706732.cif.

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C36 H24 N4 O2 Ru), 2(Cl O4), 4(C6 H6)'
_cod_original_formula_sum        'C96 H72 Cl2 N8 O12 Ru2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1802.65
_cod_database_code               7706729
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C25 H32 N8 O10 Cl1 Ru1'
_reflns_odcompleteness_completeness 99.93
_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:
 C30(H30), C33(H33), C34(H34), C23(H23), C8(H8), C29(H29), C35(H35), C66(H66),
 C60(H60), C64(H64), C59(H59), C6(H6), C36(H36), C61(H61), C62(H62), C28(H28),
 C27(H27), C20(H20), C54(H54), C13(H13), C53(H53), C24(H24), C56(H56), C69(H69),
  C9(H9), C65(H65), C45(H45), C55(H55), C63(H63), C17(H17), C12(H12), C18(H18),
 C25(H25), C49(H49), C4(H4), C26(H26), C72(H72), C40(H40), C71(H71), C42(H42),
 C70(H70), C11(H11), C02G(H02G), C5(H5), C41(H41), C19(H19), C44(H44), C47(H47),
  C02N(H02N), C48(H48), C02Q(H02Q), C02R(H02R), C02S(H02S), C02T(H02T),
 C73(H73), C85(H85), C74(H74), C89(H89), C77(H77), C90(H90), C78(H78), C88(H88),
  C79(H79), C76(H76), C86(H86), C84(H84), C87(H87), C82(H82), C81(H81),
 C83(H83), C75(H75), C80(H80)
;
_shelx_res_checksum              20808
_shelx_hkl_checksum              1321
_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 1.564
_oxdiff_exptl_absorpt_empirical_full_min 0.739