Constitutional isomers of brominated-functionalized copillar[5]arenes: synthesis, characterization, and crystal structures
Al-Azemi, Talal F.; Vinodh, Mickey; Alipour, Fatemeh H.; Mohamod, Abdirahman A.; RSC Advances 9 (2019) 13814–; doi:10.1039/C9RA02313E

data_7232716
_publ_section_title
;
 Constitutional isomers of brominated-functionalized copillar[5]arenes:
 synthesis, characterization, and crystal structures
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              13814
_journal_paper_doi               10.1039/C9RA02313E
_journal_volume                  9
_journal_year                    2019
_chemical_formula_sum            'C55 H62 Br6 N2 O10'
_chemical_formula_weight         1390.52
_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   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-11-22 deposited with the CCDC.    2019-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                94.870(7)
_cell_angle_beta                 102.695(7)
_cell_angle_gamma                97.465(7)
_cell_formula_units_Z            2
_cell_length_a                   11.7192(7)
_cell_length_b                   11.9722(6)
_cell_length_c                   22.1105(16)
_cell_measurement_reflns_used    11140
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      3.00
_cell_volume                     2980.0(3)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0911
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28910
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.447
_diffrn_reflns_theta_min         2.998
_exptl_absorpt_coefficient_mu    4.096
_exptl_absorpt_correction_T_max  0.518
_exptl_absorpt_correction_T_min  0.270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       Block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.618
_refine_diff_density_min         -2.110
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         13556
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1599
_refine_ls_R_factor_gt           0.0900
_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^)+(0.1594P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2517
_refine_ls_wR_factor_ref         0.3121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6774
_reflns_number_total             13556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra02313e2.cif
_cod_data_source_block           4b
_cod_database_code               7232716
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.495
_shelx_estimated_absorpt_t_max   0.560
_shelx_res_checksum              80212