Resorcinarene configuration and inclusion behaviour: Isolation of a guest free form of pyrogall[4]arene
Brown, Philip O.; Enright, Gary D.; Ripmeester, John A.; CrystEngComm 8 (2006) 381–; doi:10.1039/b603883b

data_7203389
_publ_section_title
;
 Resorcinarene configuration and inclusion behaviour: Isolation of a
 guest free form of pyrogall[4]arene
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              381
_journal_paper_doi               10.1039/b603883b
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety
'2(C32 H32 O12), 1(C13 H16 N4 S1), 1(SO4 2-), 1(H2 O)'
_chemical_formula_sum            'C77 H82 N4 O29 S2'
_chemical_formula_weight         1591.59
_chemical_name_common
;
2*(methylpyrogall(4)arene)1*(1,3-bis(3-pyridylmethyl)-2-
thiourea)1*(SO4 2-)1*H2O clathrate
;
_chemical_name_systematic
;
2*(methylpyrogall[4]arene)1*(1,3-bis(3-pyridylmethyl)-2-thiourea)1*(SO4 2-)1*H2O
clathrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.0560(10)
_cell_angle_beta                 82.3200(10)
_cell_angle_gamma                83.1340(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5012(6)
_cell_length_b                   18.1017(12)
_cell_length_c                   21.8277(14)
_cell_measurement_temperature    173(2)
_cell_volume                     3486.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.1032
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44480
_diffrn_reflns_theta_full        29.64
_diffrn_reflns_theta_max         29.64
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.9728
_exptl_absorpt_correction_T_min  0.9214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1376
_refine_ls_number_reflns         19416
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                9855
_reflns_number_total             19416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603883b.txt
_cod_data_source_block           sadf
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap+geom' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203389