Tris(morpholinium) hexa-μ~3~-hydroxido-hexa-μ~2~-oxido-dodecaoxidohexamolybdenum(VI)chromate(III) tetrahydrate
Yang, Yan-Yan; Song, Yu; Liu, Li-Ye; Qu, Xiao-Shu; Acta Crystallographica Section E 67 (2011) m776–; doi:10.1107/S1600536811018149

data_2230360
_publ_section_title
;
 Tris(morpholinium)
 hexa-\m~3~-hydroxido-hexa-\m~2~-oxido-dodecaoxidohexamolybdenum(VI)chromate(III)
 tetrahydrate
;
_journal_coeditor_code           HY2428
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m776
_journal_paper_doi               10.1107/S1600536811018149
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C4 H10 N O)3 [H6 Cr Mo6 O24], 4H2 O'
_chemical_formula_moiety         '3(C4 H10 N O +), Cr H6 Mo6 O24 3-, 4(H2 O)'
_chemical_formula_sum            'C12 H44 Cr Mo6 N3 O31'
_chemical_formula_weight         1354.14
_chemical_name_systematic
;
Tris(morpholinium) hexa-\m~3~-hydroxido-hexa-\m~2~-oxido-
dodecaoxidohexamolybdenum(VI)chromate(III) 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                110.3920(10)
_cell_angle_beta                 102.9210(10)
_cell_angle_gamma                90.6350(10)
_cell_formula_units_Z            1
_cell_length_a                   7.9474(4)
_cell_length_b                   9.9654(5)
_cell_length_c                   13.7404(7)
_cell_measurement_reflns_used    3855
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      2.75
_cell_volume                     989.47(9)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0136
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5458
_diffrn_reflns_theta_full        26.09
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    2.204
_exptl_absorpt_correction_T_max  0.380
_exptl_absorpt_correction_T_min  0.324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             661
_exptl_crystal_size_max          0.529
_exptl_crystal_size_mid          0.495
_exptl_crystal_size_min          0.439
_refine_diff_density_max         1.175
_refine_diff_density_min         -0.545
_refine_ls_extinction_coef       0.0147(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3855
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+2.0824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                3562
_reflns_number_total             3855
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2428.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C12 H44 Cr1 Mo6 N3 O31'
_cod_database_code               2230360
_cod_database_fobs_code          2230360