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_7116621
_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_name_full               Chem.Commun.
_journal_page_first              4227
_journal_paper_doi               10.1039/C4cc10400E
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C78 H92 O6'
_chemical_formula_weight         1125.52
_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                72.532(10)
_cell_angle_beta                 84.273(10)
_cell_angle_gamma                89.557(8)
_cell_formula_units_Z            2
_cell_length_a                   13.3230(14)
_cell_length_b                   16.3491(14)
_cell_length_c                   17.448(2)
_cell_measurement_reflns_used    1997
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.9200
_cell_measurement_theta_min      3.3360
_cell_volume                     3606.2(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.2889
_diffrn_reflns_av_sigmaI/netI    0.6725
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30898
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_correction_T_min  0.9793
_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    1.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       0.111(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         12654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.4219
_refine_ls_R_factor_gt           0.1584
_refine_ls_shift/su_max          1.837
_refine_ls_shift/su_mean         0.039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1945P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3448
_refine_ls_wR_factor_ref         0.4984
_reflns_number_gt                2835
_reflns_number_total             12654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc10400e2.cif
_cod_data_source_block           gnu010
_cod_original_cell_volume        3606.1(7)
_cod_database_code               7116621