Modular assembly of porous organic cage crystals: isoreticular quasiracemates and ternary co-crystal
Tothadi, Srinu; Little, Marc A.; Hasell, Tom; Briggs, Michael E.; Chong, Samantha Y.; Liu, Ming; Cooper, Andrew I.; CrystEngComm  (2017) –; doi:10.1039/C7CE00783C

data_7228322
_publ_section_title
;
 Modular assembly of porous organic cage crystals: isoreticular
 quasiracemates and ternary co-crystal
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00783C
_journal_year                    2017
_chemical_formula_moiety
'0.75(C72 H84 N12), 0.75(C66 H72 N12), 0.50(C60 H72 N12), 11.92(H2O)'
_chemical_formula_sum            'C133.5 H176.84 N24 O11.92'
_chemical_formula_weight         2308.50
_space_group_crystal_system      cubic
_space_group_IT_number           196
_space_group_name_Hall           'F 2 2 3'
_space_group_name_H-M_alt        'F 2 3'
_symmetry_space_group_name_Hall  'F 2 2 3'
_symmetry_space_group_name_H-M   'F 2 3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-04-26 deposited with the CCDC.
2017-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.1722(10)
_cell_length_b                   24.1722(10)
_cell_length_c                   24.1722(10)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.259
_cell_measurement_theta_min      2.599
_cell_volume                     14123.7(10)
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32931
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.950
_diffrn_reflns_theta_max         28.180
_diffrn_reflns_theta_min         2.598
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1188 before and 0.0640 after correction.
The Ratio of minimum to maximum transmission is 0.9179.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       prism
_exptl_crystal_F_000             4965
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 893 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.259
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2259
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      2.261
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0941
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2475
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2031
_reflns_number_total             2259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00783c2.cif
_cod_data_source_block           CC3-S_CC4-S_CC13-S_Ternary_Cocrystal_100K
_cod_original_cell_volume        14123.7(18)
_cod_original_formula_sum        'C133.50 H176.84 N24 O11.92'
_cod_database_code               7228322
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.517(10) 0.483(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Shared sites
{C18A, C18B}
{C12A, C12B}
4. Restrained distances
 C6-C5 = C7-C5
 1.54 with sigma of 0.01
 C9-C8
 1.39 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C13B) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uiso(C18A) = Uiso(C18B)
Uanis(C12A) = Uanis(C12B)
6. Rigid body (RIGU) restrains
 C18B, N3, C18A, C17, C16, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: N2(0.5) C9(0.5) C10(0.5) H10(0.5) C8(0.5) H8(0.5) C11(0.5)
 H11(0.5) C12A(0.25) H12A(0.25) H12B(0.25) H5BC(0.5) H5BD(0.5) H5AA(0.5)
 H5AB(0.5) C7(0.25) H7A(0.5) H7B(0.5) N3(0.5) C16(0.5) C15(0.5) H15(0.5)
 C17(0.5) H17(0.5) C18A(0.25) C6(0.5) H6A(0.5) H6B(0.5) O6(0.11111) C19(0.25)
 C20(0.25) O5(0.11111) C13B(0.25) C18B(0.25) C12B(0.25) C12(0.125) O4(0.25)
 O1(0.02083) O3(0.33333) O2(0.08333) O12(0.08333)
 Fixed X: O3(0.35988)
 Fixed Y: O3(0.61608)
 Fixed Z: O3(0.8721)
8.a Ternary CH refined with riding coordinates:
 C11(H11)
8.b Secondary CH2 refined with riding coordinates:
 C12A(H12A,H12B), C5(H5BC,H5BD), C5(H5AA,H5AB), C7(H7A,H7B), C6(H6A,H6B)
8.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C1(H1), C8(H8), C15(H15), C17(H17)
;
_shelx_res_checksum              11803
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'