(NH~4~)~2~(NH~3~(CH~2~)~6~NH~3~)~4~[H~2~W~12~O~42~]·8H~2~O: a novel ammonium 1,6-hexanediammonium dodecatungstate
Gainsford, Graeme J.; Robinson, Natalie; Tallon, J. L.; Acta Crystallographica Section E 58 (2002) m521–m523; doi:10.1107/S1600536802015799

data_2201640
_publ_section_title
;
 (NH~4~)~2~(NH~3~(CH~2~)~6~NH~3~)~4~[H~2~W~12~O~42~]&#x00B7;8H~2~O: a
 novel ammonium 1,6-hexanediammonium dodecatungstate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m521
_journal_page_last               m523
_journal_paper_doi               10.1107/S1600536802015799
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '2(N H4) 4(C6 H18 N2) [H2 W12 O42] .8H2 O'
_chemical_formula_sum            'C24 H98 N10 O50 W12'
_chemical_formula_weight         3533.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.99(3)
_cell_angle_beta                 84.85(3)
_cell_angle_gamma                87.69(3)
_cell_formula_units_Z            1
_cell_length_a                   10.987(2)
_cell_length_b                   10.980(2)
_cell_length_c                   14.681(3)
_cell_measurement_reflns_used    340
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      3.8
_cell_volume                     1758.6(6)
_computing_cell_refinement       DENZO
_computing_data_collection       'DENZO (Otinowski & Minor, 1997)'
_computing_data_reduction        DENZO
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 4000
_diffrn_measured_fraction_theta_full 0.839
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_device_type  'Quantum4 CCD detector'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_monochromator  none
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.9204
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_sigmaI/netI    0.058
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3953
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         2.9
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    37.816
_exptl_absorpt_correction_T_max  0.389
_exptl_absorpt_correction_T_min  0.033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1582
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.74
_refine_diff_density_min         -2.77
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.039
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0454P)^2^+33.4374P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.103
_refine_ls_wR_factor_ref         0.103
_reflns_number_gt                3937
_reflns_number_total             3953
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            tk6077.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (8 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (6 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2019-10-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C12 H49 N5 O25 W6'
_cod_original_formula_weight         1766.66
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2201640
_cod_database_fobs_code          2201640