Selective functionalization of methylene bridges of calix[6]arenes. Isolation and identification of stable conformers of methyl ether of p-tert-butylcalix[6]arene
Shafali Arora; Shivali Sharma; Venus S. Mithu; Chang Hee-Lee; Kamaljit Singh; Chem.Commun. 51 (2015) 4227–; doi:10.1039/C4cc10400E

data_7116620
_publ_section_title
;
 Selective functionalization of methylene bridges of calix[6]arenes.
 Isolation and identification of stable conformers of methyl ether of
 p-tert-butylcalix[6]arene
;
_journal_coden_Cambridge         182
_journal_name_full               Chem.Commun.
_journal_page_first              4227
_journal_paper_doi               10.1039/C4cc10400E
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C39 H52 Cl3 O3'
_chemical_formula_weight         675.16
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-07-19 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                109.657(6)
_cell_angle_beta                 95.088(4)
_cell_angle_gamma                107.141(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8070(4)
_cell_length_b                   13.8699(9)
_cell_length_c                   16.6745(11)
_cell_measurement_reflns_used    4115
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      69.4040
_cell_measurement_theta_min      5.0750
_cell_volume                     1996.1(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Micro-Focus (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13422
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         71.31
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    2.322
_exptl_absorpt_correction_T_max  0.9129
_exptl_absorpt_correction_T_min  0.8360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.419
_refine_diff_density_rms         '0.049 ata_global'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0734
_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^)+(0.1498P)^2^+0.3566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2175
_refine_ls_wR_factor_ref         0.2544
_reflns_number_gt                5143
_reflns_number_total             7557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc10400e2.cif
_cod_data_source_block           gndu009
_cod_database_code               7116620