Precursor Control over the Self-Assembly of Organic Cages via Imine Condensation.
Jiao, Tianyu; Wu, Guangcheng; Chen, Liang; Wang, Cai-Yun; Li, Hao; The Journal of organic chemistry 83 (2018) 12404–12410; doi:10.1021/acs.joc.8b01421

data_4035391
_publ_section_title
;
 Precursor Control over the Self-Assembly of Organic Cages via Imine
 Condensation.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12404
_journal_page_last               12410
_journal_paper_doi               10.1021/acs.joc.8b01421
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         '2(C H Cl3), 2(C Cl3), 2(C66 H63 N9)'
_chemical_formula_sum            'C136 H128 Cl12 N18'
_chemical_formula_weight         2439.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.1980(11)
_cell_length_b                   15.1390(5)
_cell_length_c                   31.8305(11)
_cell_measurement_reflns_used    11425
_cell_measurement_temperature    179.3
_cell_measurement_theta_max      29.5432
_cell_measurement_theta_min      2.8674
_cell_volume                     12624.3(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      179.3
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -70.00   16.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183  -77.0000   60.0000 86

  2 omega  -40.00   64.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183   77.0000 -180.0000 104

  3 omega  -78.00   11.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183  -38.0000 -120.0000 89
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0110327000
_diffrn_orient_matrix_UB_12      -0.0199007000
_diffrn_orient_matrix_UB_13      0.0180372000
_diffrn_orient_matrix_UB_21      -0.0226178000
_diffrn_orient_matrix_UB_22      0.0248327000
_diffrn_orient_matrix_UB_23      -0.0031544000
_diffrn_orient_matrix_UB_31      -0.0099754000
_diffrn_orient_matrix_UB_32      -0.0343766000
_diffrn_orient_matrix_UB_33      -0.0127134000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            76271
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.350
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5096
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.232
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         11489
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0956
_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^)+(0.1754P)^2^+23.2987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2588
_refine_ls_wR_factor_ref         0.3128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7570
_reflns_number_total             11489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b01421_si_001.cif
_cod_data_source_block           160718_ty_2a
_cod_database_code               4035391
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'c10 h10 n2 o8'
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.859
_reflns_odcompleteness_completeness 99.70
_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, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Cl7 \\sim C69 \\sim Cl8: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Others
 Fixed Sof: Cl6(0.75) Cl4(0.75) Cl5(0.75) C68(0.75) Cl7(0.25) Cl8(0.5) C69(0.25)
4.a Riding coordinates:
 N8(H8), N4(H4), N1(H1)
4.b Ternary CH refined with riding coordinates:
 C67(H67)
4.c Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C23(H23A,H23B), C59(H59A,H59B), C58(H58A,H58B), C56(H56A,
 H56B), C25(H25A,H25B), C57(H57A,H57B), C26(H26A,H26B), C2(H2A,H2B), C1(H1A,
 H1B), C48(H48A,H48B), C47(H47A,H47B)
4.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C15(H15), C13(H13), C35(H35), C63(H63), C37(H37), C54(H54),
 C62(H62), C55(H55), C51(H51), C50(H50), C17(H17), C32(H32), C18(H18), C39(H39),
  C6(H6), C60(H60), C27(H27), C9(H9), C33(H33), C53(H53), C8(H8A), C45(H45),
 C3(H3), C22(H22), C5(H5), C41(H41), C65(H65), C20(H20), C66(H66), C21(H21),
 C30(H30), C29(H29), C42(H42), C44(H44), C46(H46)
;
_shelx_res_checksum              26856
_shelx_hkl_checksum              83762
_olex2_submission_special_instructions 'No special instructions were received'