First cage-like pentanuclear Co(ii)-silsesquioxane.
Bilyachenko, A. N.; Yalymov, A. I.; Levitsky, M. M.; Korlyukov, A. A.; Es'kova, M. A.; Long, J.; Larionova, J.; Guari, Y.; Shul'pina, L. S.; Ikonnikov, N. S.; Trigub, A. L.; Zubavichus, Y. V.; Golub, I. E.; Shubina, E. S.; Shul'pin, G. B.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 13663–13666; doi:10.1039/c6dt02026g

data_7039859
_publ_section_title
;
 First cage-like pentanuclear Co(ii)-silsesquioxane.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13663
_journal_page_last               13666
_journal_paper_doi               10.1039/c6dt02026g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C78.5 H97.5 Co5 N4.5 Na O28 S2.5 Si10, C2 H6 O S'
_chemical_formula_sum            'C80.5 H103.5 Co5 N4.5 Na O29 S3.5 Si10'
_chemical_formula_weight         2308.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-05-17 deposited with the CCDC.
2016-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.6119(4)
_cell_length_b                   27.1456(5)
_cell_length_c                   37.5545(8)
_cell_measurement_reflns_used    7621
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.001
_cell_measurement_theta_min      4.938
_cell_volume                     19993.1(7)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1963
_diffrn_reflns_av_unetI/netI     0.1481
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            74758
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.025
_diffrn_reflns_theta_min         4.938
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.888
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.2729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1643 before and 0.0936 after correction.
The Ratio of minimum to maximum transmission is 0.3625.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       irregular
_exptl_crystal_F_000             9536
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.447
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1185
_refine_ls_number_reflns         17521
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1694
_refine_ls_R_factor_gt           0.0986
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0885P)^2^+249.9917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10749
_reflns_number_total             17521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02026g2.cif
_cod_data_source_block           yaai168
_cod_depositor_comments          'Adding full bibliography for 7039859.cif.'
_cod_original_formula_sum        'C80.50 H103.50 Co5 N4.50 Na O29 S3.50 Si10'
_cod_database_code               7039859
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 S0AA-O5AA
 1.52 with sigma of 0.01
 S0AA-C4AA
 1.75 with sigma of 0.01
 S0AA-C5AA
 1.75 with sigma of 0.01
 C5AA-C4AA
 2.368 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uiso(O0AA) = Uiso(O5AA)
Uiso(C5AA) = Uiso(C4AA)
4. Rigid body (RIGU) restrains
 S0AA, C7AA, O0AA, C4AA, O5AA, C5AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O5AA)=1-FVAR(1)
 Sof(O0AA)=FVAR(1)
 Fixed Sof: O22(0.5) S1(0.5) C7BA(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C2AA(0.5)
 H2AA(0.5) H2AB(0.5) H2AC(0.5) C6AA(0.5) H6AA(0.5) N5(0.5) C0BA(0.5) H0BA(0.5)
 H0BB(0.5) H0BC(0.5) C5CA(0.5) H5CA(0.5) H5CB(0.5) H5CC(0.5) O21(0.5) S5(0.5)
 O27(0.5) C9AA(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5) C5BA(0.5) H5BA(0.5) H5BB(0.5)
 H5BC(0.5) S6(0.5) O1A(0.5) C8AA(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) C1CA(0.5)
 H1CA(0.5) H1CB(0.5) H1CC(0.5) C4AA(0.62494) H4AA(0.62494) H4AB(0.62494)
 H4AC(0.62494) C5AA(0.37506) H5AA(0.37506) H5AB(0.37506) H5AC(0.37506)
 Fixed Uiso: O27(0.07) C5BA(0.07) C4AA(0.15) C5AA(0.15)
6.a Riding coordinates:
 O0(H0)
6.b Free rotating group:
 S5(O27,C9AA), S6(O1A,C8AA)
6.c Me refined with riding coordinates:
 C3CA(H3CA,H3CB,H3CC), C6CA(H6CA,H6CB,H6CC), C71(H71A,H71B,H71C), C72(H72A,
 H72B,H72C), C66(H66A,H66B,H66C), C65(H65A,H65B,H65C), C7BA(H7BA,H7BB,H7BC),
 C2AA(H2AA,H2AB,H2AC), C69(H69A,H69B,H69C), C68(H68A,H68B,H68C), C63(H63A,H63B,
 H63C), C62(H62A,H62B,H62C), C0BA(H0BA,H0BB,H0BC), C5CA(H5CA,H5CB,H5CC),
 C9AA(H9AA,H9AB,H9AC), C5BA(H5BA,H5BB,H5BC), C8AA(H8AA,H8AB,H8AC), C1CA(H1CA,
 H1CB,H1CC)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C56(H56), C48(H48), C3(H3), C20(H20), C12(H12), C14(H14), C8(H8),
 C32(H32), C24(H24), C46(H46), C60(H60), C4(H4), C16(H16), C30(H30), C21(H21),
 C54(H54), C52(H52), C22(H22), C51(H51), C44(H44), C33(H33), C50(H50), C39(H39),
  C18(H18), C5(H5), C41(H41), C27(H27), C6(H6), C35(H35), C58(H58), C15(H15),
 C36(H36), C45(H45), C10(H10), C40(H40), C29(H29), C23(H23), C53(H53), C42(H42),
  C34(H34), C57(H57), C9(H9), C17(H17), C38(H38), C47(H47), C28(H28), C26(H26),
 C11(H11), C59(H59), C70(H70), C67(H67), C64(H64), C61(H61), C6AA(H6AA)
6.e Idealised Me refined as rotating group:
 C7AA(H7AA,H7AB,H7AC), C4AA(H4AA,H4AB,H4AC), C5AA(H5AA,H5AB,H5AC)
;
_olex2_submission_special_instructions 'No special instructions were received'