Tris(propane-1,3-diammonium) di-μ~5~-phosphato-pentamolybdate(VI) tetrahydrate
Hui-Yan Liu; Hai-Ying Wang; Feng Gao; Zai-Sheng Lu; De-Zhong Niu; Acta Crystallographica Section E 62 (2006) m1260–m1262; doi:10.1107/S1600536806016941

data_2209104
_publ_section_title
;
 Tris(propane-1,3-diammonium) di-\m~5~-phosphato-pentamolybdate(VI)
 tetrahydrate
;
_journal_coeditor_code           BT2077
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1260
_journal_page_last               m1262
_journal_paper_doi               10.1107/S1600536806016941
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C3 H12 N2)3 [Mo5 O15 (P O4)2], 4H2 O'
_chemical_formula_moiety         '3C3 H12 N2 2+, Mo5 O23 P2 6-, 4H2 O'
_chemical_formula_sum            'C9 H44 Mo5 N6 O27 P2'
_chemical_formula_weight         1210.14
_chemical_name_systematic
;Tris(propane-1,3-diammonium) di-\m~5~-phosphato-pentamolybdate(VI)
 tetrahydrate
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.398(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.971(3)
_cell_length_b                   15.608(3)
_cell_length_c                   16.750(3)
_cell_measurement_reflns_used    13972
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.272
_cell_volume                     3354.7(12)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART 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     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21375
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    2.021
_exptl_absorpt_correction_T_max  0.7514
_exptl_absorpt_correction_T_min  0.5466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.716
_refine_diff_density_min         -2.466
_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     466
_refine_ls_number_reflns         8130
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0370
_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
'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+2.6086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                7286
_reflns_number_total             8130
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2077.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_cell_volume        3354.5(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2209104
_cod_database_fobs_code          2209104