Dinuclear cobalt complexes with a redox active biphenyl bridging ligand [Co<sub>2</sub>(BP)(tqa)<sub>2</sub>](PF<sub>6</sub>)<sub>2</sub> (H<sub>4</sub>BP = 4,4'-bis(3-<i>tert</i>-butyl-1,2-catechol), tqa = tris(2-quinolylmethyl)amine): structure and magnetic properties.
Suenaga, Yusaku; Mibu, Takuto; Okubo, Takashi; Maekawa, Masahiko; Kuroda-Sowa, Takayoshi; Sugimoto, Kunihisa; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9833–9841; doi:10.1039/d1dt00995h

data_7707696
_publ_section_title
;
 Dinuclear cobalt complexes with a redox active biphenyl bridging ligand
 [Co<sub>2</sub>(BP)(tqa)<sub>2</sub>](PF<sub>6</sub>)<sub>2</sub>
 (H<sub>4</sub>BP = 4,4'-bis(3-<i>tert</i>-butyl-1,2-catechol), tqa =
 tris(2-quinolylmethyl)amine): structure and magnetic properties.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9833
_journal_page_last               9841
_journal_paper_doi               10.1039/d1dt00995h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C80 H70 Co2 N8 O4, 2(C3 H6 O), 2(F6 P)'
_chemical_formula_sum            'C98 H106 Co2 F12 N8 O10 P2'
_chemical_formula_weight         1963.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-05-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
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2021-05-31 deposited with the CCDC.	2021-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.376(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2480(3)
_cell_length_b                   41.0134(12)
_cell_length_c                   12.2659(5)
_cell_measurement_reflns_used    10791
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.3690
_cell_measurement_theta_min      1.9810
_cell_volume                     4526.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_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     -7.00  24.92   0.38   79.79    --   16.00 -82.00  90.00   84
  2  \w    -57.00  28.12   0.38   79.79    --   16.00 -57.00-180.00  224
  3  \w    -16.00  38.34   0.38   79.79    --   16.00  82.00 -30.00  143
  4  \w    -48.00 -15.70   0.38   79.79    --   16.00  38.00  30.00   85
  5  \w     -2.00  95.28   0.38   79.79    --   16.00  38.00  30.00  256
  6  \w     -8.00  58.12   0.38   79.79    --   16.00 -77.00 150.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0046785000
_diffrn_orient_matrix_UB_12      -0.0047044000
_diffrn_orient_matrix_UB_13      -0.0564258000
_diffrn_orient_matrix_UB_21      -0.0149573000
_diffrn_orient_matrix_UB_22      0.0163855000
_diffrn_orient_matrix_UB_23      -0.0174366000
_diffrn_orient_matrix_UB_31      0.0771938000
_diffrn_orient_matrix_UB_32      0.0028801000
_diffrn_orient_matrix_UB_33      0.0071936000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32482
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.975
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       needle
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         10397
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0636
_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^)+(0.1075P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6921
_reflns_number_total             10397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00995h2.cif
_cod_data_source_block           m7-41-l3tqapf6-ace-hex-2mm-r.t.
_cod_depositor_comments
'Adding full bibliography for 7707696--7707697.cif.'
_cod_database_code               7707696
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C82 H82 N8 O6 P2 F12 Co2'
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.791
_reflns_odcompleteness_completeness 98.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Restrained distances
 P1A-F1A \\sim P1B-F1B
 with sigma of 0.02
 P1A-F2A \\sim P1B-F2B
 with sigma of 0.02
 P1A-F4A \\sim F4B-P1B
 with sigma of 0.02
 P1A-F5A \\sim F5B-P1B
 with sigma of 0.02
 P1A-F6A \\sim P1B-F6B
 with sigma of 0.02
 P1A-F1A \\sim P1A-F2A \\sim P1A-F3A \\sim P1A-F4A \\sim P1A-F5A \\sim P1A-F6A
 with sigma of 0.02
 C7A-C8A \\sim C7B-C8B
 with sigma of 0.02
 C7A-C9A \\sim C7B-C9B
 with sigma of 0.02
 C7A-C10A \\sim C7B-C10B
 with sigma of 0.02
 C7A-C8A \\sim C7A-C9A \\sim C7A-C10A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P1A \\sim F1A \\sim F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(P1B) = Uanis(F1B) = Uanis(F2B) = Uanis(F3B) = Uanis(F4B) = Uanis(F5B) =
Uanis(F6B)
Uanis(C7A) = Uanis(C8A) = Uanis(C9A) = Uanis(C10A)
Uanis(C7B) = Uanis(C8B) = Uanis(C9B) = Uanis(C10B)
4. Rigid body (RIGU) restrains
 P1A, F1A, F2A, F3A, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(P1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(1)
 Sof(P1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(1)
 Sof(C7B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=
 Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(2)
 Sof(C7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C30(H30A,H30B), C40(H40A,H40B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C32(H32), C33(H33),
  C34(H34), C35(H35), C37(H37), C38(H38)
6.c Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C8B(H8BA,H8BB,
 H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), C41(H41A,H41B,H41C),
 C43(H43A,H43B,H43C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17095
_shelx_hkl_checksum              96295
_shelx_fab_checksum              79953
_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 5.493
_oxdiff_exptl_absorpt_empirical_full_min 0.435