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_4035878
_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         'C30 H19 N9 O7 S, 2(C2 H3 N)'
_chemical_formula_sum            'C34 H25 N11 O7 S'
_chemical_formula_weight         731.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.99410(19)
_cell_length_b                   11.75950(8)
_cell_length_c                   24.61960(16)
_cell_measurement_reflns_used    5771
_cell_measurement_temperature    173.2(3)
_cell_measurement_theta_max      76.5120
_cell_measurement_theta_min      4.0150
_cell_volume                     6946.63(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 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_environment      N~2~
_diffrn_ambient_temperature      173.2(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -51.00  -1.00   1.00    4.76    --  -40.81 -19.00  60.00   50
  2  \w     10.00  49.00   1.00    4.76    --   40.81 -99.00  30.00   39
  3  \w     38.00  64.00   1.00   19.04    --  112.00-111.00  60.00   26
  4  \w     88.00 114.00   1.00   19.04    --  112.00-111.00  60.00   26
  5  \w    100.00 136.00   1.00   19.04    --  112.00 -45.00  60.00   36
  6  \w     87.00 133.00   1.00   19.04    --  112.00  30.00-120.00   46
  7  \w     85.00 151.00   1.00   19.04    --  112.00  30.00-180.00   66
  8  \w     42.00  93.00   1.00   19.04    --  112.00 -95.00-120.00   51
  9  \w     41.00  71.00   1.00   19.04    --  112.00-111.00 -60.00   30
 10  \w     48.00  84.00   1.00   19.04    --  112.00 -45.00  60.00   36
 11  \w    111.00 171.00   1.00   19.04    --  112.00 111.00  90.00   60
 12  \w    -41.00 -13.00   1.00    4.76    --  -40.81 -57.00-120.00   28
 13  \w   -112.00 -86.00   1.00    4.76    --  -40.81 -57.00-120.00   26
 14  \w   -121.00 -55.00   1.00    4.76    --  -40.81 -19.00  60.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0257527000
_diffrn_orient_matrix_UB_12      -0.0658476000
_diffrn_orient_matrix_UB_13      0.0478813000
_diffrn_orient_matrix_UB_21      0.0345063000
_diffrn_orient_matrix_UB_22      0.0717056000
_diffrn_orient_matrix_UB_23      0.0402082000
_diffrn_orient_matrix_UB_31      -0.0476437000
_diffrn_orient_matrix_UB_32      0.0875429000
_diffrn_orient_matrix_UB_33      0.0031075000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22650
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.929
_diffrn_reflns_theta_min         3.591
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0620P)^2^+1.2860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1246
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5543
_reflns_number_total             7254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b03136_si_002.cif
_cod_data_source_block           zmy20170522-424
_cod_original_cell_volume        6946.63(8)
_cod_database_code               4035878
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C27(H27), C5(H5), C26(H26), C8(H8),
 C7(H7), C29(H29), C4(H4), C30(H30), C23(H23), C24(H24), C21(H21), C20(H20)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.586
_oxdiff_exptl_absorpt_empirical_full_min 0.629