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_7033752
_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 C54 Cl6 F34 Fe N6 O6 S6, 0.25(C14 H32)'
_chemical_formula_sum            'C57.5 H8 B2 Cl6 F34 Fe N6 O6 S6'
_chemical_formula_weight         2007.23
_chemical_name_systematic
;
 ?
;
_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'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2014-12-18
_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                 101.479(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.188(19)
_cell_length_b                   8.114(5)
_cell_length_c                   30.93(2)
_cell_measurement_temperature    100
_cell_volume                     7179(8)
_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_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  apex
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1136
_diffrn_reflns_av_unetI/netI     0.1604
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            26864
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         1.424
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_description       plate
_exptl_crystal_F_000             3932
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9481
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1593
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4703
_reflns_number_total             9481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03628j2.cif
_cod_data_source_block           tg1
_cod_depositor_comments
'Adding full bibliography for 7033751--7033755.cif.'
_cod_original_formula_sum        'C57.50 H8 B2 Cl6 F34 Fe N6 O6 S6'
_cod_database_code               7033752
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.834
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C28-C29 = C29-C30 = C30-C31 = C31-C32 = C32-C33 = C33-C34
 1.5 with sigma of 0.01
 C28-C30 = C29-C31 = C30-C32 = C31-C33 = C32-C34
 2.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(C28) = Uiso(C29) = Uiso(C30) = Uiso(C31) = Uiso(C32) = Uiso(C33) =
Uiso(C34)
4. Others
 Fixed Sof: C28(0.25) H28B(0.25) H28C(0.25) H28A(0.25) C29(0.25) H29B(0.25)
 H29A(0.25) C30(0.25) H30B(0.25) H30A(0.25) C31(0.25) H31A(0.25) H31B(0.25)
 C32(0.25) H32B(0.25) H32A(0.25) C33(0.25) H33B(0.25) H33A(0.25) C34(0.25)
 H34B(0.25) H34A(0.25) H34C(0.25)
5.a Riding coordinates:
 C28(H28B,H28C,H28A), C29(H29B,H29A), C30(H30B,H30A), C31(H31A,H31B), C32(H32B,
 H32A), C33(H33B,H33A), C34(H34B,H34A,H34C)
;
_shelx_res_checksum              57613
_olex2_submission_special_instructions 'No special instructions were received'