Crystal structure of 5,11,17,23-tetra(tert-butyl)-25,26,27,28-tetrahexoxycalix[4]arene, C68H104O4
Patel, Chintan R.; Samipillai, Marivel; Friedrich, Holger B.; Kruger, Hendrik G.; Govender, Thavendran; Maguire, Glenn E. M.; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 397–402; doi:10.1515/ncrs-2016-0286

data_8106548
_publ_section_title
;
 Crystal structure of
 5,11,17,23-tetra(tert-butyl)-25,26,27,28-tetrahexoxycalix[4]arene,
 C68H104O4
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              397
_journal_page_last               402
_journal_paper_doi               10.1515/ncrs-2016-0286
_journal_volume                  232
_journal_year                    2017
_chemical_formula_sum            'C136 H207.5 O8'
_chemical_formula_weight         1970.51
_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'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 92.4000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4442(12)
_cell_length_b                   16.8522(11)
_cell_length_c                   38.048(3)
_cell_measurement_reflns_used    159821
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      1.07
_cell_volume                     12456.5(15)
_computing_molecular_graphics    'ORTEP-3 (Furrigia, 2012)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa Duo Apex II Diffractometer'
_diffrn_measurement_method       '0.5\% \f scans and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            159808
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.394
_diffrn_reflns_theta_min         1.071
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_description       block
_exptl_crystal_F_000             4350
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.460
_exptl_crystal_size_min          0.400
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.937
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1457
_refine_ls_number_reflns         31202
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+4.2685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                22557
_reflns_number_total             31202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2016-0286_suppl.cif
_cod_data_source_block           hexcalix
_cod_original_cell_volume        12456.4(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C136 H207.50 O8'
_cod_database_code               8106548
_shelx_estimated_absorpt_t_min   0.971
_shelx_estimated_absorpt_t_max   0.975