Trisodium bis{1-[iminio(morpholino)methyl]guanidinium} bis[hexahydrogenhexamolybdoaluminate(III)] chloride icosahydrate
Wang, Feng; Cao, Rui-Ge; Pan, Yi-Bing; Liu, Shu-Xia; Acta Crystallographica Section E 64 (2008) m1069–m1070; doi:10.1107/S1600536808022745

data_2218962
_publ_section_title
;
 Trisodium bis{1-[iminio(morpholino)methyl]guanidinium}
 bis[hexahydrogenhexamolybdoaluminate(III)] chloride icosahydrate
;
_journal_coeditor_code           CV2425
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1069
_journal_page_last               m1070
_journal_paper_doi               10.1107/S1600536808022745
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac
'Na3 (C6 H15 N5 O)2 [Al (O H)6 Mo6 O18]2 Cl, 20H2 O'
_chemical_formula_moiety
'3(Na +), 2(C6 H15 N5 O 2+), 2(Al H18 Mo6 O30 3-), Cl -, 8(H2 O)'
_chemical_formula_sum            'C12 H82 Al2 Cl Mo12 N10 Na3 O70'
_chemical_formula_weight         2796.54
_chemical_name_systematic
;
Trisodium bis{1-[iminio(morpholino)methyl]guanidinium}
bis[hexahydrogenhexamolybdoaluminate(III)] chloride icosahydrate
;
_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                81.6980(10)
_cell_angle_beta                 75.3140(10)
_cell_angle_gamma                77.0570(10)
_cell_formula_units_Z            1
_cell_length_a                   10.1070(6)
_cell_length_b                   11.3869(7)
_cell_length_c                   17.2548(10)
_cell_measurement_reflns_used    6444
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      1.84
_cell_volume                     1864.03(19)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART'
_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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9902
_diffrn_reflns_theta_full        25.60
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.154
_exptl_absorpt_correction_T_max  0.624
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.291
_refine_ls_extinction_coef       0.0137(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         6882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0443P)^2^+4.9534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                6108
_reflns_number_total             6882
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2425.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               2218962
_cod_database_fobs_code          2218962