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_7154777
_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 Cl3 N6 O3'
_chemical_formula_sum            'C42 H45 Cl3 N6 O3'
_chemical_formula_weight         788.19
_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                 92.420(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6060(4)
_cell_length_b                   18.7364(5)
_cell_length_c                   14.7922(4)
_cell_measurement_reflns_used    10919
_cell_measurement_temperature    130(1)
_cell_measurement_theta_max      28.73
_cell_measurement_theta_min      2.90
_cell_volume                     4044.48(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(1)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45026
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         2.90
_diffrn_standards_interval_count 4
_diffrn_standards_interval_time  60
_diffrn_standards_number         45070
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro (Agilent Technologies, 2011)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     997
_refine_ls_number_reflns         18081
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                14047
_reflns_number_total             18081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ob02090e2.cif
_cod_data_source_block           3c
_cod_depositor_comments
'Adding full bibliography for 7154775--7154783.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7154777