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_1543701
_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             2016-06-16
_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                84.771(12)
_cell_angle_beta                 81.525(15)
_cell_angle_gamma                81.41(2)
_cell_formula_units_Z            2
_cell_length_a                   10.472(3)
_cell_length_b                   12.763(3)
_cell_length_c                   23.102(2)
_cell_measurement_reflns_used    1486
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      16.8610
_cell_measurement_theta_min      1.7680
_cell_volume                     3012.2(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      air
_diffrn_ambient_temperature      295(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3590
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.382
_diffrn_measured_fraction_theta_max 0.382
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -25.00  11.00   1.00   60.00    --   18.53  81.00 151.00   36
  2  \w     -4.00  69.00   1.00   60.00    --   18.53 -97.00-143.00   73
  3  \w    -25.00  14.00   1.00   60.00    --   18.53  77.00 -30.00   39
  4  \w     60.00 112.00   1.00   60.00    --   18.53 178.00 -90.00   52
  5  \w    -48.00  31.00   1.00   60.00    --   18.53  26.00  -7.00   79
  6  \w    -15.00  62.00   1.00   60.00    --   18.53 -67.00  23.00   77
  7  \w    -28.00  16.00   1.00   60.00    --   18.53  38.00-180.00   44
  8  \w   -114.00 -68.00   1.00   60.00    --  -19.47-178.00 -90.00   46
  9  \w     12.00  40.00   1.00   60.00    --  -19.47-114.00-135.00   28
 10  \w    -33.00  13.00   1.00   60.00    --  -19.47  26.00  -7.00   46
 11  \w     -8.00  20.00   1.00   60.00    --  -19.47  19.00-180.00   28
 12  \w    -49.00 -19.00   1.00   60.00    --  -19.47  19.00-180.00   30
 13  \w   -112.00 -87.00   1.00   60.00    --  -19.47-145.00  72.00   25
 14  \w    -38.00 -13.00   1.00   60.00    --  -19.47  77.00 -30.00   25
 15  \w     -1.00  26.00   1.00   60.00    --  -19.47 -39.00  12.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0565755000
_diffrn_orient_matrix_UB_12      0.0208848000
_diffrn_orient_matrix_UB_13      0.0044841000
_diffrn_orient_matrix_UB_21      0.0203078000
_diffrn_orient_matrix_UB_22      0.0032182000
_diffrn_orient_matrix_UB_23      -0.0307108000
_diffrn_orient_matrix_UB_31      -0.0341603000
_diffrn_orient_matrix_UB_32      0.0522310000
_diffrn_orient_matrix_UB_33      -0.0022738000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_av_unetI/netI     0.1120
_diffrn_reflns_Laue_measured_fraction_full 0.382
_diffrn_reflns_Laue_measured_fraction_max 0.382
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14705
_diffrn_reflns_point_group_measured_fraction_full 0.382
_diffrn_reflns_point_group_measured_fraction_max 0.382
_diffrn_reflns_theta_full        20.810
_diffrn_reflns_theta_max         20.810
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.350
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1314
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         2410
_refine_ls_number_restraints     663
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1710
_refine_ls_R_factor_gt           0.1064
_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^)+(0.1880P)^2^+39.0920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2665
_refine_ls_wR_factor_ref         0.3361
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1377
_reflns_number_total             2410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02024k2.cif
_cod_data_source_block           p3_b
_cod_depositor_comments
'Adding full bibliography for 1543686--1543702.cif.'
_cod_original_cell_volume        3012.4(12)
_cod_database_code               1543701
_chemical_oxdiff_formula         'Co3 N2 O12 C60 H106'
_reflns_odcompleteness_completeness 38.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     20.77
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C40(H40), C42(H42)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), 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), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              30127
_shelx_shelxl_version_number     2014/7
_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 1.517
_oxdiff_exptl_absorpt_empirical_full_min 0.792