Halogen bonded analogues of deep cavity cavitands
N. Kodiah Beyeh; Mario Cetina; Kari Rissanen; Chem.Commun. 50 (2014) 1959–; doi:10.1039/c3cc49010f

data_7111958
_publ_section_title
;
 Halogen bonded analogues of deep cavity cavitands
;
_journal_name_full               Chem.Commun.
_journal_page_first              1959
_journal_paper_doi               10.1039/c3cc49010f
_journal_volume                  50
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C64 H96 N4 O8, 5.5 (C Br Cl3), 4.75 (Br), 2.5(O)'
_chemical_formula_sum            'C69.5 H96 Br10.25 Cl16.5 N4 O10.5'
_chemical_formula_weight         2559.5
_chemical_name_systematic
;
 ?
;
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-18T11:23:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.783(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7068(4)
_cell_length_b                   31.1489(9)
_cell_length_c                   18.8860(5)
_cell_measurement_reflns_used    19653
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407
_cell_volume                     10415.6(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker-Nonius Kappa Apex II Diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            76288
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         1.323
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.415
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. SADABS 2008/2; University of G\"ottingen: G\"ottingen,
        Germany, 2008.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       plate
_exptl_crystal_F_000             5057
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.171
_refine_diff_density_min         -2.307
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         18449
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.1835
_refine_ls_R_factor_gt           0.1163
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1959P)^2^+108.2777P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3326
_refine_ls_wR_factor_ref         0.3863
_reflns_number_gt                10680
_reflns_number_total             18449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc49010f.txt
_cod_data_source_block           1_7_4
_cod_original_cell_volume        10415.5(5)
_cod_original_formula_sum        'C69.50 H96 Br10.25 Cl16.50 N4 O10.50'
_cod_database_code               7111958