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_7228323
_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_absolute_configuration syn
_chemical_formula_moiety         'C78 H108 N12, C48 H48 N12'
_chemical_formula_sum            'C126 H156 N24'
_chemical_formula_weight         2006.74
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-02-25
_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                   24.586(3)
_cell_length_b                   24.586(3)
_cell_length_c                   24.586(3)
_cell_measurement_reflns_used    7720
_cell_measurement_temperature    400(2)
_cell_measurement_theta_max      2.343
_cell_measurement_theta_min      25.367
_cell_volume                     14862(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      400(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26336
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        20.700
_diffrn_reflns_theta_max         20.790
_diffrn_reflns_theta_min         2.343
_diffrn_source                   'Rotating Anode'
_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    0.054
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0658 before and 0.0597 after correction.
The Ratio of minimum to maximum transmission is 0.9017.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.897
_exptl_crystal_description       prism
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.119
_refine_diff_density_min         -0.064
_refine_diff_density_rms         0.018
_refine_ls_abs_structure_details
;
 Flack x determined using 368 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.5(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1321
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0740P)^2^+9.6730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1655
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                971
_reflns_number_total             1321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00783c2.cif
_cod_data_source_block           FT-RCC3-R_CC1-S_Cocrystal_400K
_cod_original_cell_volume        14861(5)
_cod_database_code               7228323
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C5-C5_$1 = C6-C5 = C7-C6 = C7-C7_$1
 1.54 with sigma of 0.015
3. 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
4. Others
 Fixed Sof: H4A(0.5) H4B(0.5)
5.a Ternary CH refined with riding coordinates:
 C5(H5)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C9(H9), C11(H11)
;
_shelx_res_checksum              18456
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'