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_1543686
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-17
_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                84.9760(10)
_cell_angle_beta                 80.6660(10)
_cell_angle_gamma                80.6530(10)
_cell_formula_units_Z            2
_cell_length_a                   11.12620(10)
_cell_length_b                   13.0303(2)
_cell_length_c                   23.6869(2)
_cell_measurement_reflns_used    37000
_cell_measurement_temperature    20
_cell_measurement_theta_max      20
_cell_measurement_theta_min      1
_cell_volume                     3337.00(7)
_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      20.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  synchrotron
_diffrn_radiation_wavelength     0.4997
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32261
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        17.447
_diffrn_reflns_theta_max         18.934
_diffrn_reflns_theta_min         1.116
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction in RAPID AUTO, Rigaku software
;
_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    1.218
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1314
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   1
_exptl_transmission_factor_min   0.6471
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         15267
_refine_ls_number_restraints     864
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11880
_reflns_number_total             15267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02024k2.cif
_cod_data_source_block           20k
_cod_depositor_comments
'Adding full bibliography for 1543686--1543702.cif.'
_cod_database_code               1543686
_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(H7Ba)=Sof(H7Bb)=Sof(C8B)=Sof(H8Ba)=Sof(H8Bb)=
 Sof(H8Bc)=Sof(C9B)=Sof(H9Ba)=Sof(H9Bb)=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(H7Aa)=Sof(H7Ab)=Sof(C8A)=Sof(H8Aa)=Sof(H8Ab)=
 Sof(H8Ac)=Sof(C9A)=Sof(H9Aa)=Sof(H9Ab)=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(H7Aa,H7Ab), C7B(H7Ba,H7Bb),
 C9A(H9Aa,H9Ab), C9B(H9Ba,H9Bb), 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(H8Aa,H8Ab,H8Ac),
 C8B(H8Ba,H8Bb,H8Bc), 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              8121
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'