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_7706730
_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 Os, 2(Cl O4)'
_chemical_formula_sum            'C36 H26 Cl2 N6 O8 Os'
_chemical_formula_weight         931.73
_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'
_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                 95.821(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7560(2)
_cell_length_b                   16.2063(4)
_cell_length_c                   20.8243(4)
_cell_measurement_reflns_used    13325
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.9980
_cell_measurement_theta_min      1.9710
_cell_volume                     3275.52(12)
_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 (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  30.00   0.50    8.00    --  -20.00   0.00 -36.00  280
  2  \w    -59.00   2.50   0.50    8.00    --  -20.00  72.00-180.00  123
  3  \w    -36.00  -6.00   0.50    8.00    --  -20.00  72.00 108.00   60
  4  \w    -32.00  -1.00   0.50    8.00    --  -20.00 -72.00-180.00   62
  5  \w   -110.00 -61.50   0.50    8.00    --  -20.00   0.00-108.00   97
;
_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      -0.0208530000
_diffrn_orient_matrix_UB_12      -0.0415793000
_diffrn_orient_matrix_UB_13      -0.0052444000
_diffrn_orient_matrix_UB_21      -0.0282484000
_diffrn_orient_matrix_UB_22      0.0102345000
_diffrn_orient_matrix_UB_23      -0.0317161000
_diffrn_orient_matrix_UB_31      0.0641192000
_diffrn_orient_matrix_UB_32      -0.0090390000
_diffrn_orient_matrix_UB_33      -0.0117502000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18744
_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         1.966
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64094
_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_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0479P)^2^+4.3957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4981
_reflns_number_total             5769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00282a2.cif
_cod_data_source_block           '[4](ClO4)2'
_cod_depositor_comments
'Adding full bibliography for 7706729--7706732.cif.'
_cod_original_cell_volume        3275.52(13)
_cod_database_code               7706730
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.296
_reflns_odcompleteness_completeness 90.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C5(H5), C4(H4), C20(H20), C27(H27), C28(H28), C23(H23),
 C30(H30), C25(H25), C6(H6), C24(H24), C35(H35), C33(H33), C11(H11), C18(H18),
 C19(H19), C29(H29), C26(H26), C13(H13), C34(H34), C36(H36), C17(H17), C12(H12),
  C8(H8), C9(H9)
;
_shelx_res_checksum              83966
_shelx_hkl_checksum              259
_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 1.425
_oxdiff_exptl_absorpt_empirical_full_min 0.829