Room-temperature monoclinic and low-temperature triclinic phase-transition structures of <i>meso</i>-octamethylcalix[4]pyrrole‒dimethyl sulfoxide (1/1)
Lynch, Vincent M.; Gale, Philip A.; Sessler, Jonathan L.; Madeiros, David; Acta Crystallographica Section C 57 (2001) 1426–1428; doi:10.1107/S0108270101015931

data_2012371
_publ_section_title
;
 Room-temperature monoclinic and low-temperature triclinic
 phase-transition structures of
 <i>meso</i>-octamethylcalix[4]pyrrole--dimethyl sulfoxide (1/1)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1426
_journal_page_last               1428
_journal_paper_doi               10.1107/S0108270101015931
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C28 H36 N4, C2 H6 O1 S1'
_chemical_formula_moiety         'C28 H36 N4, C2 H6 O1 S1'
_chemical_formula_sum            'C30 H42 N4 O S'
_chemical_formula_weight         506.74
_chemical_name_systematic
;
meso-octamethylcalix[4]pyrrole dimethyl sulfoxide solvate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.71(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.411(2)
_cell_length_b                   23.586(6)
_cell_length_c                   12.482(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      10.9
_cell_measurement_theta_min      8.8
_cell_volume                     2919.7(12)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'XP in SHELXTL/PC'
_computing_structure_refinement  'XL in SHELXTL/PC'
_computing_structure_solution    'XS in SHELXTL/PC (Sheldrick, 1998)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full .994
_diffrn_measured_fraction_theta_max .994
_diffrn_measurement_device       'Siemens P3'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0466
_diffrn_reflns_av_sigmaI/netI    .1509
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6290
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 96
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    .139
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'trapezoidal prism'
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          .34
_exptl_crystal_size_mid          .34
_exptl_crystal_size_min          .24
_refine_diff_density_max         .164
_refine_diff_density_min         -.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5109
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      .969
_refine_ls_R_factor_all          .2078
_refine_ls_R_factor_gt           .0707
_refine_ls_shift/su_max          .016
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0482P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .1103
_refine_ls_wR_factor_ref         .1522
_reflns_number_gt                2069
_reflns_number_total             5109
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fr1336.cif
_cod_data_source_block           monoclinicI
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2012371