Amine guest size and hydrogen-bonding influence the structures of p-tert-butylcalix[4]arene inclusions
Brouwer, Eric B.; Udachin, Kostantin A.; Enright, Gary D.; Ripmeester, John A.; Chemical Communications  (2000) 1905–; doi:10.1039/b001274m

data_7110900
_publ_section_title
;
 Amine guest size and hydrogen-bonding influence the structures of
 p-tert-butylcalix[4]arene inclusions
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1905
_journal_paper_doi               10.1039/b001274m
_journal_year                    2000
_chemical_formula_sum            'C51 H77 N3.5 O4'
_chemical_formula_weight         803.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.1070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.8406(12)
_cell_length_b                   39.310(2)
_cell_length_c                   13.3090(8)
_cell_measurement_temperature    173(2)
_cell_volume                     9866.1(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(1)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            85570
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.068
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3516
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.00039(10)
_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   1.202
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1165
_refine_ls_number_reflns         16869
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.2057
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          3.542
_refine_ls_shift/su_mean         0.102
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1720
_reflns_number_gt                5447
_reflns_number_total             16869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001274msup1.cif
_cod_data_source_block           ku18
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9866.2(10)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C51 H77 N3.50 O4'
_cod_database_code               7110900