Channel- and layer-type anionic host structures in inclusion compounds of urea, tetraalkylammonium terephthalate/trimesate and water
Feng Xue; Thomas C. W. Mak; Acta Crystallographica Section B 56 (2000) 142–154; doi:10.1107/S0108768199011283

data_2101967
_publ_section_title
;
 Channel- and layer-type anionic host structures in inclusion compounds
 of urea, tetraalkylammonium terephthalate/trimesate and water
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              142
_journal_page_last               154
_journal_paper_doi               10.1107/S0108768199011283
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac
'3[N(C2 H5)4]+,C9 H3 O6 3-,2(C H4 N2 O),7.5(H2 O)'
_chemical_formula_sum            'C35 H86 N7 O15.5'
_chemical_formula_weight         853.11
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                72.460(10)
_cell_angle_beta                 78.320(10)
_cell_angle_gamma                66.950(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2500(10)
_cell_length_b                   14.0340(10)
_cell_length_c                   15.2600(10)
_cell_measurement_reflns_used    118
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     2478.1(4)
_computing_cell_refinement       'MSC bioteX (MSC, 1995)'
_computing_data_collection       'MSC bioteX (MSC, 1995)'
_computing_data_reduction        'MSC bioteX (MSC, 1995)'
_computing_molecular_graphics    'Siemens SHELXTL-PC (Siemens, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .753
_diffrn_measured_fraction_theta_max .753
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
;
Take 36 oscillation photos in the range of 0 - 180\%,
\D\f = 5\%, 10 min. per frame.  Background level -40.
Crystal to detector distance 78.037 mm.
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
;
Rigaku RU-200 rotating-anode generator operated at 50kV and 90mA
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0000
_diffrn_reflns_av_sigmaI/netI    .0654
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6973
_diffrn_reflns_theta_full        25.54
_diffrn_reflns_theta_max         25.54
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    .089
_exptl_absorpt_correction_T_max  1.138
_exptl_absorpt_correction_T_min  .863
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             938
_exptl_crystal_size_max          .60
_exptl_crystal_size_mid          .50
_exptl_crystal_size_min          .40
_refine_diff_density_max         .452
_refine_diff_density_min         -.402
_refine_ls_extinction_coef       .037(4)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         6973
_refine_ls_number_restraints     403
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          .0853
_refine_ls_R_factor_gt           .0723
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+0.6009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .2151
_reflns_number_gt                5849
_reflns_number_total             6973
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hr0043.cif
_cod_data_source_block           compd3
_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 'Empirical' changed to
'empirical' 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:

'_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 'Empirical'
changed to 'empirical' 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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+0.6009P] 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^)+(0.0987P)^2^+0.6009P] 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        2478.1(3)
_cod_original_formula_sum        'C35 H86 N7 O15.50'
_cod_database_code               2101967
_cod_database_fobs_code          2101967