Magnetism and variable temperature and pressure crystal structures of a linear oligonuclear cobalt bis-semiquinonate.
Overgaard, Jacob; Møller, Louise H; Borup, Mette A.; Tricoire, Maxime; Walsh, James P. S.; Diehl, Marcel; Rentschler, Eva; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12924–12932; doi:10.1039/c6dt02024k

data_1543697
_publ_section_title
;
 Magnetism and variable temperature and pressure crystal structures of a
 linear oligonuclear cobalt bis-semiquinonate.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12924
_journal_page_last               12932
_journal_paper_doi               10.1039/c6dt02024k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'0.5(C60 H102 Co3 N2 O12), 0.5(C60 H105 Co3 N2 O12)'
_chemical_formula_sum            'C60 H106 Co3 N2 O12'
_chemical_formula_weight         1224.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-06 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                99.402(6)
_cell_angle_beta                 105.188(7)
_cell_angle_gamma                96.155(6)
_cell_formula_units_Z            4
_cell_length_a                   14.6567(16)
_cell_length_b                   17.3207(17)
_cell_length_c                   23.808(2)
_cell_measurement_reflns_used    4919
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.309
_cell_measurement_theta_min      2.224
_cell_volume                     5682.7(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.424
_diffrn_measured_fraction_theta_max 0.424
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.1115
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.424
_diffrn_reflns_Laue_measured_fraction_max 0.424
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30706
_diffrn_reflns_point_group_measured_fraction_full 0.424
_diffrn_reflns_point_group_measured_fraction_max 0.424
_diffrn_reflns_theta_full        16.416
_diffrn_reflns_theta_max         16.416
_diffrn_reflns_theta_min         0.952
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.6087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0952 before and 0.0756 after correction.
The Ratio of minimum to maximum transmission is 0.8181.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2628
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         5177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0830P)^2^+28.5530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3640
_reflns_number_total             5177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02024k2.cif
_cod_data_source_block           co3sq2_p1_0m
_cod_depositor_comments
'Adding full bibliography for 1543686--1543702.cif.'
_cod_original_cell_volume        5682.6(10)
_cod_database_code               1543697
_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.a Secondary CH2 refined with riding coordinates:
 C7A(H7Aa,H7Ab), C9A(H9Aa,H9Ab), C11A(H11a,H11c), C1B(H1Ba,H1Bb), C3B(H3Ba,
 H3Bb), C5B(H5Ba,H5Bb), C7B(H7Ba,H7Bb), C9B(H9Ba,H9Bb)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C5A(H5A), C15A(H15A), C17A(H17A), C40A(H40A), C42A(H42A),
 C11B(H11B), C15B(H15B), C17B(H17B), C40B(H40B), C42B(H42B)
2.c Idealised Me refined as rotating group:
 C2A(H2Aa,H2Ab,H2Ac), C4A(H4Aa,H4Ab,H4Ac), C6A(H6Aa,H6Ab,H6Ac), C8A(H8Aa,H8Ab,
 H8Ac), C10A(H10d,H10e,H10f), C12A(H12d,H12e,H12f), C20A(H20d,H20e,H20f),
 C21A(H21d,H21e,H21f), C22A(H22d,H22e,H22f), C24A(H24d,H24e,H24f), C25A(H25d,
 H25e,H25f), C26A(H26d,H26e,H26f), C29A(H29d,H29e,H29f), C30A(H30d,H30e,H30f),
 C31A(H31d,H31e,H31f), C34A(H34d,H34e,H34f), C35A(H35d,H35e,H35f), C36A(H36d,
 H36e,H36f), C44A(H44d,H44e,H44f), C45A(H45d,H45e,H45f), C46A(H46d,H46e,H46f),
 C48A(H48d,H48e,H48f), C49A(H49d,H49e,H49f), C50A(H50d,H50e,H50f), C53A(H53d,
 H53e,H53f), C54A(H54d,H54e,H54f), C55A(H55d,H55e,H55f), C58A(H58d,H58e,H58f),
 C59A(H59d,H59e,H59f), C60A(H60d,H60e,H60f), C2B(H2Ba,H2Bb,H2Bc), C4B(H4Ba,H4Bb,
 H4Bc), C6B(H6Ba,H6Bb,H6Bc), C8B(H8Ba,H8Bb,H8Bc), C10B(H10a,H10b,H10c),
 C12B(H12a,H12b,H12c), C20B(H20a,H20b,H20c), C21B(H21a,H21b,H21c), C22B(H22a,
 H22b,H22c), C24B(H24a,H24b,H24c), C25B(H25a,H25b,H25c), C26B(H26a,H26b,H26c),
 C29B(H29a,H29b,H29c), C30B(H30a,H30b,H30c), C31B(H31a,H31b,H31c), C34B(H34a,
 H34b,H34c), C35B(H35a,H35b,H35c), C36B(H36a,H36b,H36c), C44B(H44a,H44b,H44c),
 C45B(H45a,H45b,H45c), C46B(H46a,H46b,H46c), C48B(H48a,H48b,H48c), C49B(H49a,
 H49b,H49c), C50B(H50a,H50b,H50c), C53B(H53a,H53b,H53c), C54B(H54a,H54b,H54c),
 C55B(H55a,H55b,H55c), C58B(H58a,H58b,H58c), C59B(H59a,H59b,H59c), C60B(H60a,
 H60b,H60c)
;
_shelx_res_checksum              11835
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'