Two different three-dimensional hydrogen-bonded framework structures in two hydrated adducts <i>meso</i>-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane‒terephthalic acid‒water (1/1/4) and (1/1/6)
Lough, Alan J.; Gregson, Richard M.; Ferguson, George; Glidewell, Christopher; Acta Crystallographica Section B 56 (2000) 85–93; doi:10.1107/S0108768199011544

data_2101956
_publ_section_title
;Two different three-dimensional hydrogen-bonded framework structures in two
 hydrated adducts
 <i>meso</i>-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane--terephthalic
 acid--water (1/1/4) and (1/1/6)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              85
_journal_page_last               93
_journal_paper_doi               10.1107/S0108768199011544
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C16 H38 N4,C8 H4 O4,4H2 O'
_chemical_formula_sum            'C24 H50 N4 O8'
_chemical_formula_weight         522.68
_chemical_name_systematic
;
Meso-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetra-
azacyclotetradecane--terephthalic acid--water (1/1/4).
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 110.549(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3213(4)
_cell_length_b                   14.0499(4)
_cell_length_c                   16.0491(6)
_cell_measurement_reflns_used    6427
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      4.08
_cell_volume                     2812.67(16)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD server software (Nonius, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'NRCVAX96, ORTEP (Johnson, 1976), PLATON (Spek, 1999)'
_computing_publication_material
'NRCVAX96, SHELXL97  and WordPerfect macro PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement
'NRCVAX96 (Gabe et al., 1989)and SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full .996
_diffrn_measured_fraction_theta_max .996
_diffrn_measurement_device_type  Kappa-CCD
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .082
_diffrn_reflns_av_sigmaI/netI    .0716
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32836
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.08
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .092
_exptl_absorpt_correction_T_max  .9909
_exptl_absorpt_correction_T_min  .9686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .10
_refine_diff_density_max         .233
_refine_diff_density_min         -.202
_refine_ls_extinction_coef       .0036(7)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997a)'
_refine_ls_goodness_of_fit_ref   .914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6427
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      .914
_refine_ls_R_factor_all          .0840
_refine_ls_R_factor_gt           .0412
_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^)+(0.0512P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .0988
_reflns_number_gt                4031
_reflns_number_total             6427
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            bm0023.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_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:

'_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2101956
_cod_database_fobs_code          2101956