A reexamination of the low-temperature crystal structure of the <i>p-tert</i>-butylcalix[4]arene‒toluene inclusion compound. Differences in spatial averaging with Cu and Mo<i>K</i>α radiation
Enright, Gary D.; Brouwer, Eric B.; Udachin, Konstantin A.; Ratcliffe, Christopher I.; Ripmeester, John A.; Acta Crystallographica Section B 58 (2002) 1032–1035; doi:10.1107/S0108768102018803

data_2103461
_publ_section_title
;
 A reexamination of the low-temperature crystal structure of the
 <i>p-tert</i>-butylcalix[4]arene--toluene inclusion compound.
 Differences in spatial averaging with Cu and Mo<i>K</i>\a radiation
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1032
_journal_page_last               1035
_journal_paper_doi               10.1107/S0108768102018803
_journal_volume                  58
_journal_year                    2002
_chemical_formula_sum            'C51 H64 O4'
_chemical_formula_weight         741.02
_chemical_name_common            t-butycalix[4]arene:toluene
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 89.91(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8141(18)
_cell_length_b                   13.890(3)
_cell_length_c                   17.8060(17)
_cell_measurement_reflns_used    'all reflections'
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.69
_cell_measurement_theta_min      1.47
_cell_volume                     4405.9(11)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction
'SAINT (Bruker, 1997), SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    various
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51325
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   'empirical (SADABS; Bruker,1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .26
_exptl_crystal_size_min          .18
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         11537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+1.4935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                9480
_reflns_number_total             11537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            an0621.cif
_cod_data_source_block           newcell
_cod_original_cell_volume        4405.9(15)
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               2103461
_cod_database_fobs_code          2103461