Ethane-1,2-diphosphonic acid as a building block in supramolecular chemistry; a pillared-layer framework and framework-encapsulated cations
Wheatley, Paul S.; Lough, Alan J.; Ferguson, George; Burchell, Colin J.; Glidewell, Christopher; Acta Crystallographica Section B 57 (2001) 95–102; doi:10.1107/S0108768100014841

data_2103561
_publ_section_title
;
 Ethane-1,2-diphosphonic acid as a building block in supramolecular
 chemistry; a pillared-layer framework and framework-encapsulated
 cations
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              95
_journal_page_last               102
_journal_paper_doi               10.1107/S0108768100014841
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         '(C13 H28 N2), (C2 H6 O6 P2), 2.8(H2 O)'
_chemical_formula_sum            'C15 H39.6 N2 O8.8 P2'
_chemical_formula_weight         450.01
_chemical_name_systematic
;
4,4'-trimethylenedipiperidine-ethane-1,2-diphosphonic acid-water
(1/1/2.8).
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 99.942(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1218(2)
_cell_length_b                   20.6215(7)
_cell_length_c                   18.1831(7)
_cell_measurement_reflns_used    13672
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      3.01
_cell_volume                     2260.98(14)
_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
'NRCVAX-96, ORTEP (Johnson, 1976), PLATON (Spek, 2000)'
_computing_publication_material
'NRCVAX-96, SHELXL-97  and WordPerfect macro PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'NRCVAX-96 and SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      120.0(10)
_diffrn_measured_fraction_theta_full .994
_diffrn_measured_fraction_theta_max .994
_diffrn_measurement_device_type  Kappa-CCD
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_av_R_equivalents  .033
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_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
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_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .237
_exptl_absorpt_correction_T_max  .9719
_exptl_absorpt_correction_T_min  .9318
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_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
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_exptl_crystal_density_method    'not measured'
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+1.1810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1139
_reflns_number_gt                4617
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_cod_data_source_block           17
_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/c'
_cod_database_code               2103561
_cod_database_fobs_code          2103561