Bis(iminodiethylenediammonium) di-μ~5~-hydrogenphosphato-pentamolybdate(VI) tetrahydrate
Feng Geng; Guo-Hua Han; Bi-Zhou Lin; Acta Crystallographica Section C 62 (2006) m355–m357; doi:10.1107/S0108270106023092

data_2015496
_publ_section_title
;
 Bis(iminodiethylenediammonium)
 di-\m~5~-hydrogenphosphato-pentamolybdate(VI) tetrahydrate
;
_journal_coeditor_code           GZ3012
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m355
_journal_page_last               m357
_journal_paper_doi               10.1107/S0108270106023092
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C4 H15 N3)2 [Mo5 O15 (H P O4)2], 4H2 O'
_chemical_formula_moiety         '2C4 H15 N3 2+, H2 Mo5 O23 P2 4-, 4H2 O'
_chemical_formula_sum            'C8 H40 Mo5 N6 O27 P2'
_chemical_formula_weight         1194.10
_chemical_name_systematic
;
Bis(aminodiethylammonium) di-\m~5~-hydrogenphosphato-pentamolybdate(VI)
tetrahydrate
;
_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                95.650(6)
_cell_angle_beta                 95.734(6)
_cell_angle_gamma                111.408(5)
_cell_formula_units_Z            2
_cell_length_a                   10.3497(14)
_cell_length_b                   10.9934(15)
_cell_length_c                   15.751(2)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1642.4(4)
_computing_cell_refinement
;
TEXSAN (Molecular Structure Corporation, 1987)
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1987)
;
_computing_data_reduction
;
TEXSAN
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Rigaku AFC-5R'
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25131
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        0.16
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.062
_exptl_absorpt_correction_T_max  0.8524
_exptl_absorpt_correction_T_min  0.7338
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.934
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         6733
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                6371
_reflns_number_total             6733
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3012.cif
_cod_data_source_block           I
_cod_database_code               2015496
_cod_database_fobs_code          2015496