4,9-Diazonia-1,12-dodecanediammonium Dilithium <i>cyclo</i>-Hexaphosphate Tetrahydrate
Gharbi, A.; Jouini, A.; Acta Crystallographica Section C 52 (1996) 1342–1344; doi:10.1107/S0108270196000558

data_2004972
_publ_section_title
;
 4,9-Diazonia-1,12-dodecanediammonium Dilithium
 <i>cyclo</i>-Hexaphosphate Tetrahydrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1342
_journal_page_last               1344
_journal_paper_doi               10.1107/S0108270196000558
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety
'[N H3 (C H2)3 N H (C H2)4 N H (C H2)3 N H3] Li2 P6 O18, 4H2 O'
_chemical_formula_structural
'[N H3 (C H2)3 N H (C H2)4 N H (C H2)3 N H3] Li2 P6 O18, 4H2 O'
_chemical_formula_sum            'C10 H38 Li2 N4 O22 P6'
_chemical_formula_weight         766.14
_chemical_name_common
'Spermine dilithium cyclohexaphosphate tetrahydrate'
_chemical_name_systematic
;
4,9,12-triazoniadoceylammonium Dilithiumcyclohexaphosphate
Tetrahydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 116.440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.040(2)
_cell_length_b                   7.936(2)
_cell_length_c                   20.444(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      10
_cell_volume                     3056.5(9)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'MOLEN (Fair, 1990)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0115
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2776
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0.85
_diffrn_standards_interval_count '0.90 + 0.35tan(\q)'
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_meas      1.556
_exptl_crystal_density_method    'pycnometry (toluene)'
_exptl_crystal_description       'Multifaced prism'
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.434
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   0.906
_refine_ls_goodness_of_fit_obs   0.881
_refine_ls_hydrogen_treatment    refiso
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         2691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_restrained_S_obs      0.881
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_obs          0.0326
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0583P)^2^ + 3.771P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1092
_refine_ls_wR_factor_obs         0.0948
_reflns_number_observed          2196
_reflns_number_total             2691
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            du1143.cif
_cod_data_source_block           spermine
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'none' was changed to '?' - the value
is undefined or not given.

'_geom_bond_publ_flag' value 'N' changed
to 'n' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (24
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (58 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2004972