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_7706731
_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 Os, Cl O4, 0.5(C6 H6)'
_chemical_formula_sum            'C39 H27 Cl N4 O6 Os'
_chemical_formula_weight         873.29
_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
_audit_creation_date             2019-02-21
_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                 92.6620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2362(2)
_cell_length_b                   25.7702(4)
_cell_length_c                   19.8131(3)
_cell_measurement_reflns_used    41148
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.1030
_cell_measurement_theta_min      1.9080
_cell_volume                     8281.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -63.00  70.00   0.50    8.00    --  -20.00   0.00-108.00  266
  2  \w    -85.50  19.00   0.50    8.00    --  -20.00 -72.00 108.00  209
  3  \w    -73.00 -43.00   0.50    8.00    --  -20.00 -72.00-108.00   60
  4  \w   -110.00   0.50   0.50    8.00    --  -20.00   0.00-180.00  221
;
_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      0.0245605000
_diffrn_orient_matrix_UB_12      -0.0226355000
_diffrn_orient_matrix_UB_13      -0.0024017000
_diffrn_orient_matrix_UB_21      0.0325065000
_diffrn_orient_matrix_UB_22      0.0123988000
_diffrn_orient_matrix_UB_23      0.0189208000
_diffrn_orient_matrix_UB_31      -0.0159256000
_diffrn_orient_matrix_UB_32      -0.0095459000
_diffrn_orient_matrix_UB_33      0.0303415000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58560
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_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    3.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             3440
_refine_diff_density_max         2.015
_refine_diff_density_min         -2.837
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.311
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         14538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.311
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0002P)^2^+155.1254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12969
_reflns_number_total             14538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00282a2.cif
_cod_data_source_block           '[2](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 Os), 2(Cl O4), C6 H6'
_cod_original_formula_sum        'C78 H54 Cl2 N8 O12 Os2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1746.59
_cod_database_code               7706731
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 91.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C14) = Uanis(N2) = Uanis(C39) = Uanis(C52) = Uanis(C40) =
Uanis(C43) = Uanis(C42) = Uanis(C46) = Uanis(C44) = Uanis(C50) = Uanis(C37) =
Uanis(C6) = Uanis(C10) = Uanis(C63)
3.a Aromatic/amide H refined with riding coordinates:
 C62(H62), C71(H71), C72(H72), C34(H34), C24(H24), C30(H30), C27(H27),
 C26(H26), C20(H20), C59(H59), C9(H9), C25(H25), C4(H4), C60(H60), C8(H8),
 C70(H70), C49(H49), C33(H33), C69(H69), C53(H53), C45(H45), C40(H40), C56(H56),
  C47(H47), C36(H36), C55(H55), C65(H65), C66(H66), C63(H63), C23(H23),
 C17(H17), C61(H61), C18(H18), C28(H28), C19(H19), C35(H35), C11(H11), C29(H29),
  C48(H48), C6(H6), C54(H54), C44(H44), C12(H12), C64(H64), C5(H5), C41(H41),
 C13(H13), C77(H77), C42(H42), C76(H76), C73(H73), C74(H74), C78(H78), C75(H75)
;
_shelx_res_checksum              76802
_shelx_hkl_checksum              58609
_shelx_fab_checksum              60295
_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 1.276
_oxdiff_exptl_absorpt_empirical_full_min 0.856