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_4088920
_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         '0.5(C72 H112 N16 O36 Rb2 Si16), F'
_chemical_formula_sum            'C36 H56 F N8 O18 Rb Si8'
_chemical_formula_weight         1218.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1086(5)
_cell_length_b                   19.1296(6)
_cell_length_c                   18.9252(13)
_cell_measurement_reflns_used    33122
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      3.0
_cell_volume                     5469.8(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41196
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.028
_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    1.157
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.850
_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    1.479
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.063
_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     326
_refine_ls_number_reflns         6267
_refine_ls_number_restraints     290
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0382P)^2^+3.4721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5247
_reflns_number_total             6267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00565_si_002.cif
_cod_data_source_block           compound9
_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               4088920
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.785
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Rigid bond restraints
 O9, C13, H13A, H13B, C14, O7, H14A, H14B, O8, C18, Rb01, C15, H18A, H18B, C16,
  H15A, H15B, C17, H16A, H16B, H17A, H17B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O9 \\sim C13 \\sim H13A \\sim H13B \\sim C14 \\sim O7 \\sim H14A \\sim H14B
\\sim O8 \\sim C18 \\sim Rb01 \\sim C15 \\sim H18A \\sim H18B \\sim C16 \\sim
H15A \\sim H15B \\sim C17 \\sim H16A \\sim H16B \\sim H17A \\sim H17B: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C17, C13, H13A, H13B, C14, O7, H14A, H14B, O8, C18, Rb01, C15, H18A, H18B, O9,
  C16, H15A, H15B, H16A, H16B, H17A, H17B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
  C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B)
;
_shelx_res_checksum              50590
_shelx_hkl_checksum              23829
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'