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_7128360
_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(C8 H10)'
_chemical_formula_sum            'C58 H68 N6'
_chemical_formula_weight         849.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-10-23
_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                104.5050(4)
_cell_angle_beta                 91.5770(5)
_cell_angle_gamma                105.6390(5)
_cell_formula_units_Z            2
_cell_length_a                   11.19190(7)
_cell_length_b                   15.18470(8)
_cell_length_c                   15.73550(8)
_cell_measurement_reflns_used    31076
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.7188703978
_cell_measurement_theta_min      1.40837131993
_cell_volume                     2480.11(3)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.6.4-g47a579eb-release'
_computing_data_collection       'Diamond I19 GDA, (Diamond, RAL, Didcot, UK)'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.6.4-g47a579eb-release
pointless (Evans, P., 2006)
XIA2 0.5.340-g5578c4a7-dials-1.6 (Winter, G., 2010)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean PILATUS_2M_S_N_24_0107_Diamond
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1264
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32622
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.847
_diffrn_reflns_theta_min         1.302
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.040: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         10349
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0674
_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^)+(0.1218P)^2^+0.5184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1899
_refine_ls_wR_factor_ref         0.1955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9404
_reflns_number_total             10349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01650d2.cif
_cod_data_source_block           2oX_1-rac_100K_publ
_cod_depositor_comments
'Adding full bibliography for 7128359--7128364.cif.'
_cod_original_cell_volume        2480.11(2)
_cod_database_code               7128360
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.994
_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. Restrained distances
 C57-C53 = C58-C54
 1.49 with sigma of 0.01
 C62-C65 = C66-C61
 1.49 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C63, C62, C60, C59, C64, C61, C66, C65
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C50, C43, C44, C48, C49, C45, C47, C46
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C62)=Sof(C61)=Sof(C60)=Sof(H1ca)=Sof(C59)=Sof(H2ca)=Sof(C64)=Sof(H3ca)=
 Sof(C63)=Sof(H4ca)=Sof(C66)=Sof(H5ca)=Sof(H6ca)=Sof(H7ca)=Sof(C65)=Sof(H8ca)=
 Sof(H9ca)=Sof(H0da)=1-FVAR(1)
 Sof(C53)=Sof(C54)=Sof(C55)=Sof(H1da)=Sof(C56)=Sof(H2da)=Sof(C51)=Sof(H3da)=
 Sof(C52)=Sof(H4da)=Sof(C57)=Sof(H5da)=Sof(H6da)=Sof(H7da)=Sof(C58)=Sof(H8da)=
 Sof(H9da)=Sof(H0ea)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C5(Hb), C15(Hd), C4(Hg), C34(Hi), C29(Hn), C20(Hu)
5.b Secondary CH2 refined with riding coordinates:
 C16(Hj,Hk), C17(Hs,Ht), C19(Hv,Hw), C30(Hx,Hy), C2(Hz,H0aa), C32(H1aa,H2aa),
 C3(H5aa,H6aa), C18(H0ba,H1ba), C6(H2ba,H3ba), C33(H4ba,H5ba), C1(H7ba,H8ba),
 C31(H9ba,H0ca)
5.c Aromatic/amide H refined with riding coordinates:
 C42(H), C21(Ha), C37(Hc), C14(He), C9(Hf), C39(Hh), C27(Hl), C35(Hm), C28(Ho),
  C11(Hp), C38(Hq), C41(Hr), C7(H3aa), C13(H4aa), C23(H7aa), C25(H8aa),
 C10(H9aa), C24(H6ba), C48(H48), C45(H45), C46(H46), C47(H47), C60(H1ca),
 C59(H2ca), C64(H3ca), C63(H4ca), C55(H1da), C56(H2da), C51(H3da), C52(H4da)
5.d Fitted hexagon refined as free rotating group:
 C62(C61,C60,C59,C64,C63), C53(C54,C55,C56,C51,C52)
5.e Idealised Me refined as rotating group:
 C49(H49a,H49b,H49c), C50(H50a,H50b,H50c), C66(H5ca,H6ca,H7ca), C65(H8ca,H9ca,
 H0da), C57(H5da,H6da,H7da), C58(H8da,H9da,H0ea)
;
_shelx_res_checksum              52639
_olex2_submission_special_instructions 'No special instructions were received'