High yielding self-assembly favored by preorganization.
Zhang, Chi; Jiao, Tianyu; Tong, Lu; Wang, Hongye; Pan, Yuanjiang; Li, Hao; Chemical communications (Cambridge, England) 56 (2020) 3903–3906; doi:10.1039/d0cc00898b

data_7126093
_publ_section_title
;
 High yielding self-assembly favored by preorganization.
;
_journal_issue                   27
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3903
_journal_page_last               3906
_journal_paper_doi               10.1039/d0cc00898b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '3(C H Cl3), C60 H51 N3'
_chemical_formula_sum            'C63 H54 Cl9 N3'
_chemical_formula_weight         1172.14
_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     dual
_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
;
2020-02-03 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                71.662(16)
_cell_angle_beta                 84.799(18)
_cell_angle_gamma                86.827(16)
_cell_formula_units_Z            4
_cell_length_a                   11.337(6)
_cell_length_b                   20.266(11)
_cell_length_c                   26.705(16)
_cell_measurement_reflns_used    2562
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      51.96
_cell_measurement_theta_min      7.58
_cell_volume                     5798(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      169.98
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1208
_diffrn_reflns_av_unetI/netI     0.1536
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            56473
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.736
_diffrn_reflns_theta_min         3.042
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.814
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1395 before and 0.0704 after correction. The Ratio of minimum to maximum transmission is 0.6476. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.379
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.00020(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1364
_refine_ls_number_reflns         21752
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.2248
_refine_ls_R_factor_gt           0.1250
_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^)+(0.1000P)^2^+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2868
_refine_ls_wR_factor_ref         0.3581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9737
_reflns_number_total             21752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00898b2.cif
_cod_data_source_block           190925zc_1_0m
_cod_depositor_comments
'Adding full bibliography for 7126091--7126093.cif.'
_cod_original_cell_volume        5797(6)
_cod_database_code               7126093
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.872
_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
 Cl2-C121 = Cl1-C121 = Cl3-C121
 1.78 with sigma of 0.01
 Cl4-C122 = Cl5-C122 = Cl6-C122
 1.78 with sigma of 0.01
 Cl17-C126 = Cl16-C126 = Cl18-C126
 1.78 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C121 \\sim Cl1 \\sim Cl2 \\sim Cl3: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C122 \\sim Cl4 \\sim Cl5 \\sim Cl6: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C126 \\sim Cl16 \\sim Cl18 \\sim Cl17: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C126 \\sim Cl16 \\sim Cl17 \\sim Cl18: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C126) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C121(H121), C122(H122), C123(H123), C124(H124), C125(H125), C126(H126)
4.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C38(H38A,H38B), C53(H53A,H53B), C77(H77A,H77B), C98(H98A,
 H98B), C113(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20),
 C23(H23), C26(H26), C28(H28), C30(H30), C33(H33), C34(H34), C36(H36), C39(H39),
  C41(H41), C42(H42), C43(H43), C45(H45), C47(H47), C48(H48), C49(H49),
 C51(H51), C52(H52), C55(H55), C56(H56), C59(H59), C71(H71), C72(H72), C73(H73),
  C75(H75), C76(H76), C79(H79), C80(H80), C83(H83), C86(H86), C88(H88),
 C90(H90), C92(H92), C94(H94), C95(H95), C99(H99), C101(H101), C102(H102),
 C103(H103), C105(H105), C107(H107), C108(H108), C109(H109), C111(H111),
 C112(H112), C115(H115), C116(H116), C119(H119)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C),
 C37(H37A,H37B,H37C), C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C84(H84A,H84B,H84C), C97(H97A,H97B,H97C),
 C120(H12A,H12B,H12C)
;
_shelx_res_checksum              90299
_olex2_submission_special_instructions 'No special instructions were received'