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_1549248
_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         'C48 H48 N12, C H2 Cl2, C8 H10'
_chemical_formula_sum            'C57 H60 Cl2 N12'
_chemical_formula_weight         984.07
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 92.088(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.565(4)
_cell_length_b                   10.745(3)
_cell_length_c                   31.067(8)
_cell_measurement_reflns_used    1239
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.0
_cell_measurement_theta_min      2.54
_cell_volume                     5526(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_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)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
scan:
    Number of images: 250
               Slice: -120.0000 - 5.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -68.0000
                 Phi: 0.0000
                 XTD: 40.0000
              2theta: -30.0000
scan:
    Number of images: 250
               Slice: -120.0000 - 5.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -68.0000
                 Phi: 90.0000
                 XTD: 40.0000
              2theta: -30.0000
scan:
    Number of images: 360
               Slice: -120.0000 - 60.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 0.0000
                 XTD: 40.0000
              2theta: -30.0000
scan:
    Number of images: 5
               Slice: -120.0000 - -117.5000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -68.0000
                 Phi: 0.0000
                 XTD: 40.0000
              2theta: -30.0000
;
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.012844
_diffrn_orient_matrix_UB_12      -0.070067
_diffrn_orient_matrix_UB_13      0.024174
_diffrn_orient_matrix_UB_21      -0.019642
_diffrn_orient_matrix_UB_22      0.030466
_diffrn_orient_matrix_UB_23      0.049815
_diffrn_orient_matrix_UB_31      -0.075379
_diffrn_orient_matrix_UB_32      -0.019878
_diffrn_orient_matrix_UB_33      -0.008861
_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  0.0880
_diffrn_reflns_av_unetI/netI     0.1513
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12268
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        20.147
_diffrn_reflns_theta_max         20.147
_diffrn_reflns_theta_min         1.944
_diffrn_source                   Synchrotron
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1094 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.6663.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         5628
_refine_ls_number_restraints     527
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1869
_refine_ls_R_factor_gt           0.0958
_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^)+(0.1624P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2278
_refine_ls_wR_factor_ref         0.2865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2805
_reflns_number_total             5628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8fd00031j5.cif
_cod_data_source_block           CC1_CH2Cl2_o_xylene
_cod_database_code               1549248
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.988
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-C49 = Cl3-C49
 1.74 with sigma of 0.01
 Cl3-C49 = Cl4-C49
 1.74 with sigma of 0.01
 Cl4-Cl3
 2.96 with sigma of 0.02
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: H49B(0.5) H49A(0.5) H49D(0.5) H49C(0.5) Cl1(0.5) Cl2(0.5) Cl3(0.5)
 Cl4(0.5)
5.a Secondary CH2 refined with riding coordinates:
 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), C49(H49B,H49A), C49(H49D,H49C)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), 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),
 C51(H51), C52(H52), C53(H53), C54(H54)
5.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              6243
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'