Readily prepared inclusion forming chiral calixsalens.
Janiak, Agnieszka; Petryk, Małgorzata; Barbour, Leonard J.; Kwit, Marcin; Organic & biomolecular chemistry 14 (2015) 669–673; doi:10.1039/c5ob02090e

data_7154778
_publ_section_title
;
 Readily prepared inclusion forming chiral calixsalens.
;
_journal_issue                   2
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              669
_journal_page_last               673
_journal_paper_doi               10.1039/c5ob02090e
_journal_volume                  14
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C42 H45 Br3 N6 O3'
_chemical_formula_sum            'C42 H45 Br3 N6 O3'
_chemical_formula_weight         921.57
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-07 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.8320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5208(2)
_cell_length_b                   19.0262(3)
_cell_length_c                   14.9678(2)
_cell_measurement_reflns_used    50674
_cell_measurement_temperature    130(1)
_cell_measurement_theta_max      76.55
_cell_measurement_theta_min      2.95
_cell_volume                     4133.12(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(1)
_diffrn_detector_area_resol_mean 10.5357
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0125
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            61556
_diffrn_reflns_theta_full        76.55
_diffrn_reflns_theta_max         76.55
_diffrn_reflns_theta_min         2.95
_diffrn_standards_number         61611
_exptl_absorpt_coefficient_mu    3.983
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.4 (release 09-12-2010 CrysAlis171 .NET)
(compiled Dec  9 2010,10:47:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         17091
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+3.9677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                17015
_reflns_number_total             17091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ob02090e2.cif
_cod_data_source_block           3d
_cod_depositor_comments
'Adding full bibliography for 7154775--7154783.cif.'
_cod_original_cell_volume        4133.13(10)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7154778