Poly[tris(<i>p</i>-xylylenediaminium) [tetradeca-μ-oxo-hexadecanonamolybdate(VI)] dihydrate]
Nelson, James H.; Narducci Sarjeant, Amy; Norquist, Alexander J.; Acta Crystallographica Section E 63 (2007) m1442–m1444; doi:10.1107/S1600536807018557

data_2213187
_publ_section_title
;
 Poly[tris(<i>p</i>-xylylenediaminium)
 [tetradeca-\m-oxo-hexadecanonamolybdate(VI)] dihydrate]
;
_journal_coeditor_code           BV2050
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1442
_journal_page_last               m1444
_journal_paper_doi               10.1107/S1600536807018557
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C8 H14 N2)3 [Mo9 O30] , 2H2 O'
_chemical_formula_moiety         '3C8 H14 N2 2+ , Mo9 O30 6- , 2H2 O'
_chemical_formula_sum            'C24 H46 Mo9 N6 O32'
_chemical_formula_weight         1794.13
_chemical_name_systematic
;
Poly[tris(<i>p</i>-xylylenediaminium) [tetradeca-\m-oxo-
hexadecanonamolybdate(VI)] dihydrate]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 105.908(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.850(3)
_cell_length_b                   13.656(3)
_cell_length_c                   21.441(4)
_cell_measurement_reflns_used    13373
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      32.1051
_cell_measurement_theta_min      3.7626
_cell_volume                     4744.7(16)
_computing_cell_refinement       'CrysAlis RED'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2004)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2004)'
_computing_molecular_graphics    'ATOMS (Dowty, 2002)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Oxford CrysAlis CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49286
_diffrn_reflns_theta_full        29.573
_diffrn_reflns_theta_max         32.144
_diffrn_reflns_theta_min         3.826
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.399
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'(multifaceted crystal model; Clark & Reid, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.511
_exptl_crystal_description       plate
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.8603
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4638
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.000880
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial (Watkin, 1994; Prince,
1982),
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)],
where A~i~ are the Chebychev coefficients listed below and x = Fcalc/Fmax
Method = robust weighting (Prince, 1982)
W = [weight] * [1-(\dF/6*\sF)^2^]^2^
A~i~ are: 0.344E+05 -0.492E+05 0.417E+05 -0.161E+05 0.755E+04
Prince, E. (1982). <i>Mathematical Techniques in Crystallography and
Materials Science</i>. New York: Springer-Verlag.
Watkin, D. (1994). <i>Acta Cryst.</i> A<b>50</b>, 411--437.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0468
_refine_ls_wR_factor_gt          0.0468
_refine_ls_wR_factor_ref         0.0468
_reflns_number_gt                4638
_reflns_number_total             7576
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            bv2050.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2213187
_cod_database_fobs_code          2213187