Tris(ethylenediammonium) penta-μ~2~-oxo-decaoxodi-μ~5~-phosphato-pentamolybdate(VI) trihydrate
Wang, Shu-Xia; Zhu, Miao-Li; Acta Crystallographica Section E 62 (2006) m1395–m1396; doi:10.1107/S1600536806018976

data_2209191
_publ_section_title
;
 Tris(ethylenediammonium)
 penta-\m~2~-oxo-decaoxodi-\m~5~-phosphato-pentamolybdate(VI)
 trihydrate
;
_journal_coeditor_code           HB2054
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1395
_journal_page_last               m1396
_journal_paper_doi               10.1107/S1600536806018976
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C2 H10 N2)3 [Mo5 O15 (P1 O4)2], 3H2 O'
_chemical_formula_moiety         '3C2 H10 N2 2+, Mo5 O23 P2 6-, 3H2 O'
_chemical_formula_sum            'C6 H36 Mo5 N6 O26 P2'
_chemical_formula_weight         1150.05
_chemical_name_systematic
;
Tris(ethylenediammonium) di-\m~5~-phosphato-penta-\m~2~-oxo-
decaoxopentamolybdenum(VI) trihydrate
;
_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                78.611(7)
_cell_angle_beta                 80.228(6)
_cell_angle_gamma                67.198(6)
_cell_formula_units_Z            2
_cell_length_a                   9.014(4)
_cell_length_b                   10.699(4)
_cell_length_c                   17.543(7)
_cell_measurement_reflns_used    6589
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.25
_cell_volume                     1520.8(11)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1999)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2000)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       \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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6233
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.219
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.709
_refine_ls_extinction_coef       0.0064(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         5211
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0123P)^2^+3.1377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0695
_reflns_number_gt                5075
_reflns_number_total             5211
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2054.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Triclinic' changed to 'triclinic'
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_database_code               2209191
_cod_database_fobs_code          2209191