Ultramacrocyclization in water via external templation
Chen, Qiong; Lei, Ye; Wu, Guangcheng; Li, Qing; Pan, Yuanjiang; Li, Hao; Chemical Science 13 (2022) 798–803; doi:10.1039/D1SC06236K

data_1565915
_publ_section_title
;
 Ultramacrocyclization in water via external templation
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              798
_journal_page_last               803
_journal_paper_doi               10.1039/D1SC06236K
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         '2(Cl), C49 H48 N6 O7, 4.5(H2 O)'
_chemical_formula_sum            'C49 H57 Cl2 N6 O11.5'
_chemical_formula_weight         984.90
_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   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc28cq2g
_audit_creation_date             2021-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-15 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                74.272(7)
_cell_angle_beta                 81.268(8)
_cell_angle_gamma                78.693(8)
_cell_formula_units_Z            4
_cell_length_a                   10.3120(12)
_cell_length_b                   20.687(2)
_cell_length_c                   26.395(3)
_cell_measurement_reflns_used    9208
_cell_measurement_temperature    184(2)
_cell_measurement_theta_max      51.41
_cell_measurement_theta_min      3.18
_cell_volume                     5285.6(10)
_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      183.95
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.984
_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  0.1519
_diffrn_reflns_av_unetI/netI     0.1958
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            66904
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.175
_diffrn_reflns_theta_min         3.182
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.3544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1733 before and 0.1065 after correction. The Ratio of minimum to maximum transmission is 0.4720. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.685
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         19978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.2236
_refine_ls_R_factor_gt           0.1263
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3271
_refine_ls_wR_factor_ref         0.4007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7967
_reflns_number_total             19978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06236k2.cif
_cod_data_source_block           210710cq_159c_0m
_cod_depositor_comments
'Adding full bibliography for 1565914--1565917.cif.'
_cod_original_cell_volume        5285.7(10)
_cod_original_formula_sum        'C49 H57 Cl2 N6 O11.50'
_cod_database_code               1565915
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.949
_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 O(H,H) groups
2. Others
 Fixed Sof: Cl17(0.5)
3.a Free rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B), O20(H20A,
 H20B), O21(H21A,H21B), O22(H22A,H22B), O23(H23A,H23B), O13(H13A,H13B)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
  C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,
 H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C13(H13), C14(H14), C16(H16),
 C17(H17), C19(H19), C20(H20), C22(H22), C25(H25), C26(H26), C38(H38), C39(H39),
  C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C49(H49), C50(H50), C52(H52), C54(H54), C55(H55), C58(H58), C59(H59),
  C63(H63), C64(H64), C66(H66), C67(H67), C69(H69), C70(H70), C72(H72),
 C75(H75), C76(H76), C87(H87), C88(H88), C90(H90), C91(H91), C92(H92), C93(H93),
  C94(H94), C95(H95), C96(H96), C97(H97), C98(H98), C99(H99)
;
_shelx_res_checksum              64291
_shelx_hkl_checksum              62895
_shelx_fab_checksum              21271
_olex2_submission_special_instructions 'No special instructions were received'