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_1543691
_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         'C60 H106 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
_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
;
2016-05-20 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                85.002(2)
_cell_angle_beta                 80.744(3)
_cell_angle_gamma                80.730(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1736(3)
_cell_length_b                   13.0734(4)
_cell_length_c                   23.8027(7)
_cell_measurement_reflns_used    28327
_cell_measurement_temperature    99.97(13)
_cell_measurement_theta_max      32.5530
_cell_measurement_theta_min      2.2930
_cell_volume                     3380.24(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3590
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -99.00   13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3427  -77.0000 -150.0000 112

  2 omega  -99.00   13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3427  -77.0000  -60.0000 112

  3 omega  -54.00   58.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3427   77.0000  150.0000 112

  4 omega  -54.00   58.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3427   77.0000   60.0000 112

  5 omega   35.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0927  178.0000  120.0000 74

  6 omega  -94.00    9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3427  -57.0000   60.0000 103

  7 omega  -50.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3427   57.0000 -150.0000 75

  8 omega  -50.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3427   57.0000  -60.0000 104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0378915000
_diffrn_orient_matrix_UB_12      -0.0270620000
_diffrn_orient_matrix_UB_13      -0.0126597000
_diffrn_orient_matrix_UB_21      -0.0452995000
_diffrn_orient_matrix_UB_22      0.0448001000
_diffrn_orient_matrix_UB_23      0.0005400000
_diffrn_orient_matrix_UB_31      0.0272687000
_diffrn_orient_matrix_UB_32      0.0171640000
_diffrn_orient_matrix_UB_33      -0.0274704000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            82178
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.260
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.203
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1314
_exptl_crystal_size_max          0.3211
_exptl_crystal_size_mid          0.2745
_exptl_crystal_size_min          0.2315
_refine_diff_density_max         1.091
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         20615
_refine_ls_number_restraints     864
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+1.5770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16562
_reflns_number_total             20615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02024k2.cif
_cod_data_source_block           100k
_cod_depositor_comments
'Adding full bibliography for 1543686--1543702.cif.'
_cod_original_cell_volume        3380.26(18)
_cod_database_code               1543691
_chemical_oxdiff_formula         'Co3 O10 C40 H40'
_reflns_odcompleteness_completeness 92.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.82
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C58A)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59A)=Sof(H59A)=Sof(H59B)=
 Sof(H59C)=Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(H60C)=1-FVAR(1)
 Sof(C58B)=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C59B)=Sof(H59D)=Sof(H59E)=
 Sof(H59F)=Sof(C60B)=Sof(H60D)=Sof(H60E)=Sof(H60F)=FVAR(1)
 Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=
 Sof(H30C)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=1-FVAR(2)
 Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=
 Sof(H30F)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=FVAR(2)
 Sof(Co3B)=Sof(N2B)=Sof(C7B)=Sof(H7C)=Sof(H7D)=Sof(C8B)=Sof(H8D)=Sof(H8E)=
 Sof(H8F)=Sof(C9B)=Sof(H9C)=Sof(H9D)=Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=
 Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(3)
 Sof(Co3A)=Sof(N2A)=Sof(C7A)=Sof(H7A)=Sof(H7B)=Sof(C8A)=Sof(H8A)=Sof(H8B)=
 Sof(H8C)=Sof(C9A)=Sof(H9A)=Sof(H9B)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7A(H7A,H7B), C7B(H7C,H7D), C9A(H9A,
 H9B), C9B(H9C,H9D), C11A(H11A,H11B), C11B(H11C,H11D)
4.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C40(H40), C42(H42)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8A(H8A,H8B,H8C), C8B(H8D,
 H8E,H8F), C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C12A(H12A,H12B,H12C),
 C12B(H12D,H12E,H12F), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F), C30A(H30A,H30B,H30C), C30B(H30D,
 H30E,H30F), C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C),
 C58A(H58A,H58B,H58C), C58B(H58D,H58E,H58F), C59A(H59A,H59B,H59C), C59B(H59D,
 H59E,H59F), C60A(H60A,H60B,H60C), C60B(H60D,H60E,H60F)
;
_shelx_res_checksum              99291
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'