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_4035390
_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), C60 H57 N15'
_chemical_formula_sum            'C62 H59 Cl6 N15'
_chemical_formula_weight         1226.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.885(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5704(8)
_cell_length_b                   25.7255(10)
_cell_length_c                   16.0579(9)
_cell_measurement_reflns_used    4807
_cell_measurement_temperature    169.8
_cell_measurement_theta_max      29.5991
_cell_measurement_theta_min      2.8387
_cell_volume                     6009.5(6)
_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)'
_diffrn_ambient_temperature      169.8
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -6.00   39.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8433   88.0000  -50.0000 45

  2 omega  -87.00   -4.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183  -38.0000  120.0000 83

  3 omega  -61.00   -2.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183  -38.0000    0.0000 59
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0346565000
_diffrn_orient_matrix_UB_12      0.0077685000
_diffrn_orient_matrix_UB_13      -0.0404670000
_diffrn_orient_matrix_UB_21      -0.0237313000
_diffrn_orient_matrix_UB_22      -0.0236657000
_diffrn_orient_matrix_UB_23      -0.0010663000
_diffrn_orient_matrix_UB_31      -0.0247583000
_diffrn_orient_matrix_UB_32      0.0118169000
_diffrn_orient_matrix_UB_33      0.0244440000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24664
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.344
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         2.844
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92970
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         10975
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0726P)^2^+3.4146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6831
_reflns_number_total             10975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b01421_si_002.cif
_cod_data_source_block           160719_ty_2z
_cod_database_code               4035390
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'c10 h10 n2 Cl3'
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.854
_reflns_odcompleteness_completeness 99.60
_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 C(H,H,H,H) groups, All N(H) groups
2. Restrained distances
 N14-H14
 0.88 with sigma of 0.02
 N1-H1
 0.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N7A) = Uanis(N7)
4. Others
 Sof(H21c)=Sof(H21d)=Sof(H22c)=Sof(H22d)=Sof(N7A)=Sof(H7A)=1-FVAR(1)
 Sof(N7)=Sof(H7)=Sof(H21a)=Sof(H21b)=Sof(H22a)=Sof(H22b)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C61(H61), C62(H62)
5.b Secondary CH2 refined with riding coordinates:
 C51(H51a,H51b), C1(H1a,H1b), C53(H53a,H53b), C42(H42a,H42b), C2(H2a,H2b),
 C23(H23a,H23b), C41(H41a,H41b), C52(H52a,H52b), C20(H20a,H20b), C50(H50a,H50b),
  C21(H21a,H21b), C21(H21c,H21d), C22(H22a,H22b), C22(H22c,H22d)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C35(H35), C48(H48), C5(H5), C15(H15), C36(H36), C18(H18),
 C29(H29), C19(H19), C39(H39), C27(H27), C57(H57), C17(H17), C9(H9), C56(H56),
 C38(H38), C3(H3), C47(H47), C54(H54), C14(H14a), C30(H30), C26(H26), C24(H24),
 C40(H40), C44(H44), C49(H49), C59(H59), C60(H60), C45(H45), N7(H7), N7A(H7A)
;
_shelx_res_checksum              7209
_shelx_hkl_checksum              72018
_olex2_submission_special_instructions 'No special instructions were received'