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_4088916
_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         'C52 H80 K O34 Si8, F'
_chemical_formula_sum            'C52 H80 F K O34 Si8'
_chemical_formula_weight         1531.98
_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             2016-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                73.882(13)
_cell_angle_beta                 79.293(13)
_cell_angle_gamma                88.688(14)
_cell_formula_units_Z            1
_cell_length_a                   8.445(3)
_cell_length_b                   14.704(5)
_cell_length_c                   16.727(5)
_cell_measurement_reflns_used    5493
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2
_cell_measurement_theta_min      2.5
_cell_volume                     1959.8(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29209
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.980
_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    0.272
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.847
_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    1.298
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.903
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8934
_refine_ls_number_restraints     1165
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+2.5805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1979
_refine_ls_wR_factor_ref         0.2067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7413
_reflns_number_total             8934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00565_si_002.cif
_cod_data_source_block           compound1
_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               4088916
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2A-O8A
 1.2 with sigma of 0.01
 C1-O7A
 1.455 with sigma of 0.01
 O7A-C2A
 1.34 with sigma of 0.01
 C2A-C3A
 1.49 with sigma of 0.01
 C3A-C5A
 1.318 with sigma of 0.01
 C3A-C4A
 1.506 with sigma of 0.01
 C2B-O8B
 1.2 with sigma of 0.01
 C1-O7B
 1.455 with sigma of 0.01
 O7B-C2B
 1.34 with sigma of 0.01
 C2B-C3B
 1.49 with sigma of 0.01
 C3B-C5B
 1.318 with sigma of 0.01
 C3B-C4B
 1.506 with sigma of 0.01
 C16-O13
 1.455 with sigma of 0.01
 C16-O13
 1.455 with sigma of 0.01
 C18A-C19A
 1.5 with sigma of 0.01
 C18-C19
 1.5 with sigma of 0.01
 C18A-C20A
 1.32 with sigma of 0.01
 C18-C20
 1.32 with sigma of 0.01
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
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(H1BC)=Sof(H1BD)=Sof(O7B)=Sof(O8B)=Sof(C2B)=Sof(C3B)=Sof(C4B)=Sof(H4BA)=
 Sof(H4BB)=Sof(H4BC)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(O7A)=Sof(O8A)=Sof(C2A)=Sof(C3A)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=FVAR(1)
 Sof(H16C)=Sof(H16D)=Sof(O13A)=Sof(O14A)=Sof(C17A)=Sof(C18A)=Sof(C19A)=
 Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(H20C)=Sof(H20D)=1-FVAR(2)
 Sof(H16A)=Sof(H16B)=Sof(O13)=Sof(O14)=Sof(C17)=Sof(C18)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C6(H6A,H6B), C11(H11A,H11B), C16(H16A,H16B),
 C16(H16C,H16D), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
  C25(H25A,H25B), C26(H26A,H26B)
7.b Me refined with riding coordinates:
 C4A(H4AA,H4AB,H4AC), C4B(H4BA,H4BB,H4BC)
7.c X=CH2 refined with riding coordinates:
 C9(H9A,H9B), C14(H14A,H14B), C5A(H5AA,H5AB), C20(H20A,H20B), C5B(H5BA,H5BB),
 C20A(H20C,H20D)
7.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C19A(H19D,H19E,
 H19F)
;
_shelx_res_checksum              4075
_shelx_hkl_checksum              77151
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'