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_7128362
_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_absolute_configuration '-R,R diamine from synthesis'
_chemical_formula_moiety         'C42 H48 N6, 0.75(C H4 O)'
_chemical_formula_sum            'C42.75 H51 N6 O0.75'
_chemical_formula_weight         660.89
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2021-03-27 deposited with the CCDC.	2021-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   20.450(2)
_cell_length_b                   20.450(2)
_cell_length_c                   5.9423(5)
_cell_measurement_reflns_used    5593
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.4280
_cell_measurement_theta_min      1.9560
_cell_volume                     2152.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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   40.00    --  -20.00 -68.00   0.00  125
  2  \w   -100.00  25.00   1.00   70.00    --  -10.00 -68.00 120.00  125
  3  \w   -100.00  25.00   1.00   70.00    --  -10.00 -68.00 240.00  125
  4  \w   -100.00  25.00   1.00   70.00    --  -10.00 -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      -0.0325419000
_diffrn_orient_matrix_UB_12      -0.0358793000
_diffrn_orient_matrix_UB_13      0.0126702000
_diffrn_orient_matrix_UB_21      -0.0229270000
_diffrn_orient_matrix_UB_22      0.0145881000
_diffrn_orient_matrix_UB_23      -0.0410758000
_diffrn_orient_matrix_UB_31      0.0047379000
_diffrn_orient_matrix_UB_32      -0.0094552000
_diffrn_orient_matrix_UB_33      -0.1113483000
_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  0.1107
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            19869
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        21.941
_diffrn_reflns_theta_max         21.941
_diffrn_reflns_theta_min         3.043
_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    0.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (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    1.020
_exptl_crystal_description       needle
_exptl_crystal_F_000             711
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 547 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   6.7(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1724
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0900P)^2^+0.9330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1637
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                1504
_reflns_number_total             1724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01650d2.cif
_cod_data_source_block           MeOH_1-R_100K_publ
_cod_depositor_comments
'Adding full bibliography for 7128359--7128364.cif.'
_cod_original_cell_volume        2152.2(5)
_cod_database_code               7128362
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 N6 O2'
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.978
_reflns_odcompleteness_completeness 99.94
_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, All O(H) groups
2. Restrained distances
 O2-C16
 1.43 with sigma of 0.01
 O1-C15
 1.43 with sigma of 0.01
3. Others
 Fixed Sof: O1(0.16667) H1A(0.16667) C15(0.16667) H15A(0.16667) H15B(0.16667)
 H15C(0.16667) O2(0.08333) H2(0.08333) C16(0.08333) H16B(0.08333) H16C(0.08333)
 H16A(0.08333)
 Fixed X: H16B(0.63521) H16C(0.64635) H16A(0.71844)
 Fixed Y: H16B(0.28156) H16C(0.36479) H16A(0.35365)
 Fixed Z: H16B(0.69215) H16C(0.69215) H16A(0.69215)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C6(H6)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14)
4.d Tetrahedral OH refined with riding coordinates:
 O1(H1A), O2(H2)
4.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_shelx_res_checksum              85225
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.398
_oxdiff_exptl_absorpt_empirical_full_min 0.650