Molecular design of cage iron(ii) and cobalt(ii,iii) complexes with a second fluorine-enriched superhydrophobic shell.
Belov, Alexander S.; Zelinskii, Genrikh E.; Varzatskii, Oleg A.; Belaya, Irina G.; Vologzhanina, Anna V.; Dolganov, Alexander V.; Novikov, Valentin V.; Voloshin, Yan Z.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 3773–3784; doi:10.1039/c4dt03628j

data_7033754
_publ_section_title
;
 Molecular design of cage iron(ii) and cobalt(ii,iii) complexes with a
 second fluorine-enriched superhydrophobic shell.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3773
_journal_page_last               3784
_journal_paper_doi               10.1039/c4dt03628j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'B2 C60 Co F53 N6 O6 S6'
_chemical_formula_sum            'C60 B2 Co F53 N6 O6 S6'
_chemical_formula_weight         2180.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             2014-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2014-12-21 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.062(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.529(4)
_cell_length_b                   8.1068(11)
_cell_length_c                   28.045(4)
_cell_measurement_reflns_used    3148
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.60
_cell_volume                     6861.9(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            24922
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.602
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_description       prism
_exptl_crystal_F_000             4240
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.933
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         6669
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+46.4465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5534
_reflns_number_total             6669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03628j2.cif
_cod_data_source_block           gz20
_cod_depositor_comments
'Adding full bibliography for 7033751--7033755.cif.'
_cod_original_cell_volume        6861.8(15)
_cod_database_code               7033754
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.794
_olex2_refinement_description
;
1. Restrained angles
 C17-C20-F12A
 fixed at 110 with sigma of 0.02
 C17-C20-C16B
 fixed at 110 with sigma of 0.02
 C17-C20-C16B
 fixed at 110 with sigma of 0.02
 C16B-C20-C17
 fixed at 110 with sigma of 0.02
 C16B-C20-C17
 fixed at 110 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(F11A) \\sim Ueq, Uanis(F11B) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.007
Uiso(C16A) = Uiso(C16B)
Uanis(F10A) = Uanis(F11B) = Uanis(F12A)
Uanis(F12B) = Uanis(F10B) = Uanis(F11B)
3. Same fragment restrains
{C8, F3, F4, F5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C16A, F10A, F11A, F12A}
{C24, F17, F18, F19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C16B, F10B, F11B, F12B}
4. Others
 Fixed Sof: C16A(0.5) F10A(0.5) F11A(0.5) F12A(0.5) C16B(0.5) F11B(0.5)
 F12B(0.5)
;
_shelx_res_checksum              40324
_olex2_submission_special_instructions 'No special instructions were received'