Computational Modelling of Solvent Effects in a Prolific Solvatomorphic Porous Organic Cage
McMahon, David P.; Stephenson, Andrew; Chong, Samantha Y.; Little, Marc; Jones, James T. A.; Cooper, Andrew I.; Day, Graeme Matthew; Faraday Discussions  (2018) –; doi:10.1039/C8FD00031J

data_1549250
_publ_section_title
;
 Computational Modelling of Solvent Effects in a Prolific Solvatomorphic
 Porous Organic Cage
;
_journal_name_full               'Faraday Discussions'
_journal_paper_doi               10.1039/C8FD00031J
_journal_year                    2018
_chemical_formula_moiety         '2(C48 H48 N12), 7.75(C H2 Cl2)'
_chemical_formula_sum            'C103.75 H111.5 Cl15.5 N24'
_chemical_formula_weight         2244.14
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-11
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-09-21 deposited with the CCDC.
2018-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.3987(16)
_cell_length_b                   21.3987(16)
_cell_length_c                   21.3164(18)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.378
_cell_measurement_theta_min      2.323
_cell_volume                     8453.2(11)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30840
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.411
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1293 before and 0.0924 after correction.
The Ratio of minimum to maximum transmission is 0.7514.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             3496
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.116
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details
;
 Flack x determined using 2631 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.33(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         7407
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0912
_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^)+(0.1970P)^2^+12.4680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2501
_refine_ls_wR_factor_ref         0.2591
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.933
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                6606
_reflns_number_total             7407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8fd00031j5.cif
_cod_data_source_block           2_CC1_7_75_CH2Cl2_R3
_cod_original_cell_volume        8453.2(15)
_cod_original_formula_sum        'C103.75 H111.50 Cl15.50 N24'
_cod_database_code               1549250
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl10-C36 = Cl9-C36
 1.74 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl10) = Uanis(C36) = Uanis(Cl9)
4. Others
 Sof(Cl9)=Sof(Cl10)=Sof(C36)=Sof(H36A)=Sof(H36B)=0.33333*FVAR(2)
 Fixed Sof: Cl1(0.5) Cl2(0.5) C34(0.5) H34A(0.5) H34B(0.5) Cl3(0.5) Cl4(0.5)
 C35(0.5) H35A(0.5) H35B(0.5) Cl5(0.33333) H37A(0.33333) H37B(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C32(H32A,H32B), C13(H13A,
 H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C34(H34A,H34B),
 C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B), C36(H36A,H36B)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C29(H29),
 C31(H31), C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12)
;
_shelx_res_checksum              29012
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'