Synthesis, Structure, and Properties of Corona[6]arenes and Their Assembly with Anions in the Crystalline State.
Zhao, Meng-Yao; Wang, De-Xian; Wang, Mei-Xiang; The Journal of organic chemistry 83 (2018) 1502–1509; doi:10.1021/acs.joc.7b03136

data_4033395
_publ_section_title
;
 Synthesis, Structure, and Properties of Corona[6]arenes and Their
 Assembly with Anions in the Crystalline State.
;
_journal_issue                   3
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1502
_journal_page_last               1509
_journal_paper_doi               10.1021/acs.joc.7b03136
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C32 H22 N10 O6, C16 H36 N, Br'
_chemical_formula_sum            'C48 H58 Br N11 O6'
_chemical_formula_weight         964.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 90.118(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2331(17)
_cell_length_b                   25.605(4)
_cell_length_c                   16.613(2)
_cell_measurement_reflns_used    12990
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4700
_cell_measurement_theta_min      1.4612
_cell_volume                     4778.3(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37582
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         1.461
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.497
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.159
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         10875
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0696
_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^)+(0.0561P)^2^+4.2043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9060
_reflns_number_total             10875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b03136_si_006.cif
_cod_data_source_block           mx6217
_cod_depositor_comments
'Adding full bibliography for 4033391--4033399.cif.'
_cod_database_code               4033395
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.658
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C38-C40A
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C40A) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C39A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40D)=
 Sof(H40E)=Sof(H40F)=1-FVAR(1)
 Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 Sof(H40C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,
 H38B), C38(H38C,H38D), C39(H39A,H39B), C41(H41A,H41B), C42(H42A,H42B),
 C43(H43A,H43B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C39A(H39C,H39D)
5.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C40(H40A,H40B,H40C)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15), C16(H16),
 C20(H20), C21(H21), C23(H23), C24(H24), C28(H28), C29(H29), C31(H31), C32(H32)
5.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C36(H36A,H36B,H36C), C44(H44A,H44B,H44C), C48(H48A,H48B,
 H48C), C40A(H40D,H40E,H40F)
;
_shelx_res_checksum              38970
_shelx_hkl_checksum              74563
_olex2_submission_special_instructions 'No special instructions were received'