Polymorphism and pseudopolymorphism in calixarenes: acetonitrile clathrates of p-But-calix[n]arenes (n = 6 and 8)
Dale, Sophie H.; Elsegood, Mark R. J.; Redshaw, Carl; CrystEngComm 5 (2003) 368–; doi:10.1039/b308407h

data_7216288
_publ_section_title
;
 Polymorphism and pseudopolymorphism in calixarenes: acetonitrile
 clathrates of p-But-calix[n]arenes (n = 6 and 8)
;
_journal_issue                   65
_journal_name_full               CrystEngComm
_journal_page_first              368
_journal_paper_doi               10.1039/b308407h
_journal_volume                  5
_journal_year                    2003
_chemical_formula_sum            'C96 H124 N4 O8'
_chemical_formula_weight         1461.99
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 92.251(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.419(2)
_cell_length_b                   21.8067(14)
_cell_length_c                   21.1486(13)
_cell_measurement_reflns_used    7547
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.16
_cell_volume                     17704.4(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            63586
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'octahedral prism'
_exptl_crystal_F_000             6336
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.00055(6)
_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   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         15584
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1669
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+66.3018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.2365
_reflns_number_gt                7431
_reflns_number_total             15584
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b308407h.txt
_cod_data_source_block           3
_cod_original_cell_volume        17704.7(19)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7216288