Synthesis and Structures of Novel Molecular Ionic Compounds Based on Encapsulation of Anions and Cations
El Aziz, Youssef; Taylor, Peter G.; Bassindale, Alan R.; Coles, Simon J.; Pitak, Mateusz B.; Organometallics 35 (2016) 4004–; doi:10.1021/acs.organomet.6b00565

data_4088919
_publ_section_title
;
 Synthesis and Structures of Novel Molecular Ionic Compounds Based on
 Encapsulation of Anions and Cations
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              4004
_journal_paper_doi               10.1021/acs.organomet.6b00565
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C60 H56 F72 K O18 Si8, C2 H4 Cl2, F'
_chemical_formula_sum            'C62 H60 Cl2 F73 K O18 Si8'
_chemical_formula_weight         2814.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                69.641(5)
_cell_angle_beta                 83.129(6)
_cell_angle_gamma                61.922(4)
_cell_formula_units_Z            1
_cell_length_a                   13.8521(5)
_cell_length_b                   14.5848(5)
_cell_length_c                   14.9006(10)
_cell_measurement_reflns_used    30328
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.1
_cell_volume                     2486.6(2)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33301
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.133
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1398
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.787
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1036
_refine_ls_number_reflns         11333
_refine_ls_number_restraints     2666
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0630P)^2^+3.6449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9972
_reflns_number_total             11333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00565_si_002.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4088919
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.809
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C18-F27
 1.32 with sigma of 0.01
 C18A-F26A
 1.32 with sigma of 0.01
 C18A-F28A
 1.32 with sigma of 0.01
 F25A-C17A
 1.32 with sigma of 0.01
 C17A-F24A
 1.32 with sigma of 0.01
 C17A-C16
 1.5 with sigma of 0.01
 C18A-C17A
 1.5 with sigma of 0.01
 C17-C18
 1.5 with sigma of 0.01
 C17-C16
 1.5 with sigma of 0.01
 F26A-F28A
 2.145 with sigma of 0.02
 F26A-F27A
 2.145 with sigma of 0.02
 F27A-F28A
 2.145 with sigma of 0.02
 F27-F26
 2.145 with sigma of 0.02
 F27-F28
 2.145 with sigma of 0.02
 F28-F26
 2.145 with sigma of 0.02
 F25A-F24A
 2.15 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(F29A) \\sim Ueq, Uanis(F30A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C9) = Uanis(C9A)
5. 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
6. Others
 Sof(H20C)=Sof(H20D)=Sof(F29B)=Sof(F30B)=Sof(F31B)=Sof(F32B)=Sof(F33B)=
 Sof(F34B)=Sof(F35B)=Sof(F36B)=Sof(F37B)=Sof(C21B)=Sof(C22B)=Sof(C23B)=
 Sof(C24B)=1-FVAR(1)
 Sof(H20A)=Sof(H20B)=Sof(F29A)=Sof(F30A)=Sof(F31A)=Sof(F32A)=Sof(F33A)=
 Sof(F34A)=Sof(F35A)=Sof(F36A)=Sof(F37A)=Sof(C21A)=Sof(C22A)=Sof(C23A)=
 Sof(C24A)=FVAR(1)
 Sof(F24A)=Sof(F25A)=Sof(F26A)=Sof(F27A)=Sof(F28A)=Sof(C17A)=Sof(C18A)=1-FVAR(2)
 Sof(F24)=Sof(F25)=Sof(F26)=Sof(F27)=Sof(F28)=Sof(C17)=Sof(C18)=FVAR(2)
 Sof(H8BC)=Sof(H8BD)=Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=
 Sof(F16A)=Sof(F17A)=Sof(F18A)=Sof(F19A)=Sof(C9A)=Sof(C10A)=Sof(C11A)=Sof(C12A)=
 1-FVAR(3)
 Sof(H8AA)=Sof(H8AB)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=
 Sof(F17)=Sof(F18)=Sof(F19)=Sof(C9)=Sof(C10)=Sof(C11)=Sof(C12)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C7(H7A,H7B), C8(H8AA,H8AB), C8(H8BC,H8BD), C13(H13A,
 H13B), C14(H14A,H14B), C19(H19A,H19B), C20(H20A,H20B), C20(H20C,H20D),
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
  C30(H30A,H30B), C31(H31A,H31B)
;
_shelx_res_checksum              18958
_shelx_hkl_checksum              14449
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'