1,4,8,11-Tetraazoniacyclotetradecane tetrakis(phenylphosphonate) dihydrate forms hydrogen-bonded sheets
Bowes, Katharine F.; Ferguson, George; Lough, Alan J.; Glidewell, Christopher; Acta Crystallographica Section C 59 (2003) o461–o463; doi:10.1107/S010827010301182X

data_2013506
_publ_section_title
;
 1,4,8,11-Tetraazoniacyclotetradecane tetrakis(phenylphosphonate)
 dihydrate forms hydrogen-bonded sheets
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o461
_journal_page_last               o463
_journal_paper_doi               10.1107/S010827010301182X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C10 H28 N4 4+, 4C6 H6 O3 P 1-, 2H2 O'
_chemical_formula_moiety         'C10 H28 N4 4+, 4C6 H6 O3 P 1-, 2H2 O'
_chemical_formula_sum            'C34 H56 N4 O14 P4'
_chemical_formula_weight         868.71
_chemical_name_systematic
;
1,4,8,11-Tetraazoniacyclotetradecane tetrakis-phenylphosphonate
dihydrate
;
_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'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.5130(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.0678(3)
_cell_length_b                   8.7475(2)
_cell_length_c                   17.6106(5)
_cell_measurement_reflns_used    4536
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.60
_cell_volume                     2013.00(9)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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'
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_diffrn_reflns_av_R_equivalents  0.042
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_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
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_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14531
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO--SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.279
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_refine_ls_extinction_coef       0.0054(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4536
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+0.9176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                3866
_reflns_number_total             4536
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1643.cif
_cod_data_source_block           I
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2013506
_cod_database_fobs_code          2013506