Creating porosity in a trianglimine macrocycle by heterochiral pairing.
He, Donglin; Clowes, Rob; Little, Marc A.; Liu, Ming; Cooper, Andrew I.; Chemical communications (Cambridge, England) 57 (2021) 6141–6144; doi:10.1039/d1cc01650d

data_7128363
_publ_section_title
;
 Creating porosity in a trianglimine macrocycle by heterochiral pairing.
;
_journal_issue                   50
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6141
_journal_page_last               6144
_journal_paper_doi               10.1039/d1cc01650d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C42 H48 N6, 2(0.5(C8 H10))'
_chemical_formula_sum            'C50 H58 N6'
_chemical_formula_weight         743.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-27 deposited with the CCDC.	2021-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.506(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.2103(4)
_cell_length_b                   14.0669(2)
_cell_length_c                   25.3934(4)
_cell_measurement_reflns_used    31055
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.7840
_cell_measurement_theta_min      2.1380
_cell_volume                     8791.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  15.00   1.00    5.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00    5.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00    5.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00    5.00    --  -20.00 -30.00  90.00  125
;
_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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0046428000
_diffrn_orient_matrix_UB_12      0.0445487000
_diffrn_orient_matrix_UB_13      0.0112939000
_diffrn_orient_matrix_UB_21      0.0282405000
_diffrn_orient_matrix_UB_22      0.0045088000
_diffrn_orient_matrix_UB_23      0.0110644000
_diffrn_orient_matrix_UB_31      0.0034186000
_diffrn_orient_matrix_UB_32      0.0231797000
_diffrn_orient_matrix_UB_33      -0.0238428000
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            70247
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.075
_diffrn_reflns_theta_min         1.778
_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
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.537
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         15555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+5.3816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11060
_reflns_number_total             15555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01650d2.cif
_cod_data_source_block           1pX_1-rac_100K_publ
_cod_depositor_comments
'Adding full bibliography for 7128359--7128364.cif.'
_cod_database_code               7128363
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C42H48N6
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.965
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C14(H14), C23(H23), C28(H28), C37(H37), C42(H42)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C15(H15), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22), C29(H29), C31(H31), C32(H32), C33(H33), C35(H35),
  C36(H36), C43(H43), C45(H45), C47(H47), C49(H49)
2.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              62056
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.490
_oxdiff_exptl_absorpt_empirical_full_min 0.767