Controllable Self-Assembly of Macrocycles in Water for Isolating Aromatic Hydrocarbon Isomers.
Wu, Guangcheng; Wang, Cai-Yun; Jiao, Tianyu; Zhu, Huangtianzhi; Huang, Feihe; Li, Hao; Journal of the American Chemical Society 140 (2018) 5955–5961; doi:10.1021/jacs.8b01651

data_4132110
_publ_section_title
;
 Controllable Self-Assembly of Macrocycles in Water for Isolating Aromatic
 Hydrocarbon Isomers.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5955
_journal_page_last               5961
_journal_paper_doi               10.1021/jacs.8b01651
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'H2 O7 P2, C37 H38 N6 O2, 8.5(H2 O)'
_chemical_formula_sum            'C37 H57 N6 O17.5 P2'
_chemical_formula_weight         927.82
_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_creation_date             2018-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                101.1010(10)
_cell_angle_beta                 110.0030(10)
_cell_angle_gamma                92.8250(10)
_cell_formula_units_Z            4
_cell_length_a                   13.6131(3)
_cell_length_b                   18.1837(4)
_cell_length_c                   19.2192(4)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.90
_cell_measurement_theta_min      3.408
_cell_volume                     4352.48(17)
_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      170.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0612
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            53096
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.966
_diffrn_reflns_theta_min         3.029
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1074 before and 0.0670 after correction. The Ratio of minimum to maximum transmission is 0.8050. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.082
_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     1127
_refine_ls_number_reflns         16503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0675
_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^)+(0.1091P)^2^+3.2811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.2023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11409
_reflns_number_total             16503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01651_si_002.cif
_cod_data_source_block           mjl18014_0m_pl_pl
_cod_depositor_comments
;

2020-07-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C74 H114 N12 O35 P4'
_cod_original_formula_weight         1855.65
_cod_original_formula_moiety         'H4 O14 P4, 2(C37 H38 N6 O2), 17(H2 O)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4352.47(17)
_cod_database_code               4132110
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.970
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O4(H4), O7(H7B), O14(H2A), N1(H1), N6(H6), N7(H7A), N12(H12A), O19(H19A,H19B),
  O20(H20A,H20B), O21(H21C,H21D), O22(H22C,H22D), O23(H23C,H23D), O24(H24C,
 H24D), O25(H25C,H25D), O26(H26C,H26D), O27(H27C,H27D), O28(H28A,H28B),
 O29(H29A,H29B), O30(H30A,H30B), O31(H31A,H31B), O32(H32A,H32B), O33(H33A,H33B),
  O34(H34A,H34B), O35(H35A,H35B)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C14(H14A,H14B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C46(H46A,H46B),
  C51(H51A,H51B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,
 H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6A), C7(H7), C8(H8), C11(H11), C12(H12), C15(H15), C19(H19),
 C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36), C37(H37), C39(H39), C43(H43), C44(H44), C45(H45), C48(H48),
 C49(H49), C52(H52), C56(H56), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69),
  C70(H70), C71(H71), C72(H72), C73(H73), C74(H74)
2.d Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_shelx_res_checksum              89130
_shelx_hkl_checksum              28565
_olex2_submission_special_instructions 'No special instructions were received'