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_1549252
_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), 11.32(C H Cl3)'
_chemical_formula_sum            'C107.33 H107.33 Cl33.97 N24'
_chemical_formula_weight         2937.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-04
_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                73.378(2)
_cell_angle_beta                 72.980(2)
_cell_angle_gamma                76.700(2)
_cell_formula_units_Z            2
_cell_length_a                   17.1487(11)
_cell_length_b                   18.3913(11)
_cell_length_c                   24.7171(15)
_cell_measurement_reflns_used    9327
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.855
_cell_measurement_theta_min      2.344
_cell_volume                     7050.9(8)
_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)'
_diffrn_ambient_temperature      150
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            117695
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.382
_diffrn_reflns_theta_min         0.886
_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    0.704
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.4830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1000 before and 0.0786 after correction.
The Ratio of minimum to maximum transmission is 0.6476.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             2994
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.197
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1707
_refine_ls_number_reflns         28822
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0798
_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^)+(0.1374P)^2^+10.4733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2284
_refine_ls_wR_factor_ref         0.2512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22595
_reflns_number_total             28822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8fd00031j5.cif
_cod_data_source_block           cc1_chcl3_150k
_cod_database_code               1549252
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl16-C100 = Cl17-C100
 1.74 with sigma of 0.015
 Cl15-C99 = Cl13-C99 = Cl14-C99
 1.74 with sigma of 0.015
 Cl16-C100 = Cl17-C100 = Cl18-C100
 1.74 with sigma of 0.015
 Cl46-C108 = Cl47-C108 = Cl48-C108
 1.74 with sigma of 0.015
 Cl44-C107 = Cl43-C107 = Cl45-C107
 1.74 with sigma of 0.015
 Cl55-C113 = Cl57-C113 = Cl56-C113
 1.74 with sigma of 0.015
 Cl49-C109 = Cl54-C109 = Cl51-C109 = Cl52-C109 = Cl50-C109 = Cl53-C109
 1.74 with sigma of 0.015
 Cl21-C105 = Cl20-C105 = Cl19-C105
 1.74 with sigma of 0.015
 Cl11-C98 = Cl10-C98 = Cl9-C98 = Cl8-C98 = Cl7-C98
 1.74 with sigma of 0.015
 Cl10-C98 = Cl9-C98 = Cl12-C98 = Cl11-C98 = Cl7-C98 = Cl8-C98
 1.74 with sigma of 0.015
3. Uiso/Uaniso restraints and constraints
Uiso(Cl45) = Uiso(C107) = Uiso(Cl43) = Uiso(Cl44)
4. Rigid body (RIGU) restrains
 C109, Cl52, Cl53, Cl54, Cl49, Cl50, Cl51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl13, Cl14, Cl15, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl16, Cl17, Cl18, C100
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl19, Cl20, Cl21, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl22, Cl23, Cl24, C104
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl46, Cl47, Cl48, C108
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C98, Cl7, Cl9, Cl11, Cl8, Cl10, Cl12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H98A)=Sof(Cl8)=Sof(Cl10)=Sof(Cl12)=Sof(Cl16)=Sof(Cl17)=Sof(Cl18)=
 Sof(C100)=Sof(H100)=1-FVAR(1)
 Sof(H98)=Sof(Cl7)=Sof(Cl9)=Sof(Cl11)=Sof(Cl13)=Sof(Cl14)=Sof(Cl15)=Sof(C99)=
 Sof(H99)=FVAR(1)
 Sof(Cl19)=Sof(Cl20)=Sof(Cl21)=Sof(C105)=Sof(H105)=1-FVAR(2)
 Sof(Cl22)=Sof(Cl23)=Sof(Cl24)=Sof(C104)=Sof(H104)=FVAR(2)
 Sof(Cl37)=Sof(Cl38)=Sof(Cl39)=Sof(C111)=Sof(H111)=1-FVAR(3)
 Sof(Cl34)=Sof(Cl35)=Sof(Cl36)=Sof(C112)=Sof(H112)=0.5*FVAR(4)
 Sof(Cl40)=Sof(Cl41)=Sof(Cl42)=Sof(C110)=Sof(H110)=FVAR(3)
 Fixed Sof: H109(0.5) H10A(0.5) Cl52(0.5) Cl53(0.5) Cl54(0.5) Cl49(0.5)
 Cl50(0.5) Cl51(0.5) Cl43(0.25) Cl44(0.25) Cl45(0.25) C107(0.25) H107(0.25)
 Cl46(0.5) Cl47(0.5) Cl48(0.5) C108(0.5) H108(0.5) Cl55(0.25) Cl56(0.25)
 C113(0.25) H113(0.25) Cl57(0.25)
6.a Ternary CH refined with riding coordinates:
 C98(H98), C98(H98A), C109(H109), C109(H10A), C102(H102), C107(H107),
 C110(H110), C106(H106), C99(H99), C97(H97), C105(H105), C104(H104), C101(H101),
  C103(H103), C111(H111), C100(H100), C108(H108), C112(H112), C113(H113)
6.b Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,
 H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B),
 C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C48(H48A,H48B)
6.c Aromatic/amide H refined with riding coordinates:
 C50(H50), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C59(H59),
 C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C70(H70), C72(H72),
  C73(H73), C74(H74), C75(H75), C77(H77), C79(H79), C81(H81), C82(H82),
 C83(H83), C84(H84), C1(H1), C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C29(H29), C31(H31), C33(H33), C34(H34),
 C35(H35), C36(H36)
;
_shelx_res_checksum              88599
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'