2,9,18-Trioxo-3,5,8,19-tetraaza-[5^5,13^][11]metaphane monohydrate
Kim, Tae Ho; Yang, Sun Young; Lee, Shim Sung; Kim, Jae Sang; Kim, Jineun; Acta Crystallographica Section E 57 (2001) o1200–o1202; doi:10.1107/S1600536801019183

data_2200724
_publ_section_title
;
 2,9,18-Trioxo-3,5,8,19-tetraaza-[5^5,13^][11]metaphane monohydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1200
_journal_page_last               o1202
_journal_paper_doi               10.1107/S1600536801019183
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C18 H24 N4 O3, H2 O'
_chemical_formula_moiety         'C18 H24 N4 O3, H2 O'
_chemical_formula_sum            'C18 H26 N4 O4'
_chemical_formula_weight         362.43
_chemical_name_systematic
;
3,5,8,19-Tetraaza-2,9,18-trione-[5^5,13^][11]metacyclophane monohydrate
;
_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'
_audit_creation_method           SHELXTL
_cell_angle_alpha                90
_cell_angle_beta                 94.748(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3436(8)
_cell_length_b                   13.4554(12)
_cell_length_c                   14.2888(12)
_cell_measurement_reflns_used    11459
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.08
_cell_volume                     1790.3(3)
_computing_cell_refinement       SAINT
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SHELXTL (Siemens, 1996)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full .970
_diffrn_measured_fraction_theta_max .970
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0635
_diffrn_reflns_av_sigmaI/netI    .0533
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11459
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  360
_diffrn_standards_number         156
_exptl_absorpt_coefficient_mu    .096
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .25
_refine_diff_density_max         .207
_refine_diff_density_min         -.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          .0786
_refine_ls_R_factor_gt           .0434
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.0871P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1164
_reflns_number_gt                2794
_reflns_number_total             4316
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6084.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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               2200724
_cod_database_fobs_code          2200724