Bis- and mono(m-benzoic acid)-functionalized pillar[5]arenes
Ke, Wen; Wu, Xin-Lang; chen, yi; Hu, Wen-Jing; Liu, Yahu; Jia, Xueshun; Li, Jiu-Sheng; Jiang, Biao; Org. Biomol. Chem.  (2017) –; doi:10.1039/C7OB00984D

data_7155636
_publ_section_title
;
 Bis- and mono(m-benzoic acid)-functionalized pillar[5]arenes
;
_journal_name_full               'Org. Biomol. Chem.'
_journal_paper_doi               10.1039/C7OB00984D
_journal_year                    2017
_chemical_formula_sum            'C68 H78 N O13.5'
_chemical_formula_weight         1125.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-21 deposited with the CCDC.
2017-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                102.2970(10)
_cell_angle_beta                 100.4640(10)
_cell_angle_gamma                91.103(2)
_cell_formula_units_Z            4
_cell_length_a                   13.2049(4)
_cell_length_b                   20.8347(6)
_cell_length_c                   22.0840(6)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.39
_cell_measurement_theta_min      2.71
_cell_volume                     5827.0(3)
_computing_cell_refinement       HKL3000
_computing_data_collection       'local program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean '8192 x 8192 pixels'
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'marXperts MX300 CCD Detector'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.82673
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.908
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_number            12571
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.546
_diffrn_reflns_theta_max         25.546
_diffrn_reflns_theta_min         1.118
_diffrn_source                   'SSRF BL17B'
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       block
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1508
_refine_ls_number_reflns         12571
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+3.3280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1948
_refine_ls_wR_factor_ref         0.2002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11505
_reflns_number_total             12571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ob00984d2.cif
_cod_data_source_block           1_a
_cod_depositor_comments
;

2017-10-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C136 H156 N2 O27'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2250.62
_cod_database_code               7155636
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              71627