New organic‒inorganic frameworks incorporating iso- and heteropolymolybdate units and a 3,3',5,5'-tetramethyl-4,4'-bi-1<i>H</i>-pyrazole-2,2'-diium multiple hydrogen-bond donor
Lukashuk, Liliana V.; Lysenko, Andrey B.; Krautscheid, Harald; Domasevitch, Konstantin V.; Acta Crystallographica Section C 67 (2011) m378–m383; doi:10.1107/S0108270111047159

data_2018324
_publ_section_title
;
 New organic--inorganic frameworks incorporating iso- and
 heteropolymolybdate units and a
 3,3',5,5'-tetramethyl-4,4'-bi-1<i>H</i>-pyrazole-2,2'-diium multiple
 hydrogen-bond donor
;
_journal_coeditor_code           KU3054
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m378
_journal_page_last               m383
_journal_paper_doi               10.1107/S0108270111047159
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C10 H16 N4)2 [Mo8 O26] , 2H2 O'
_chemical_formula_moiety         '2(C10 H16 N4 2+), Mo8 O26 4-, 2(H2 O)'
_chemical_formula_sum            'C20 H36 Mo8 N8 O28'
_chemical_formula_weight         1604.09
_chemical_name_systematic
;
Poly[bis(3,3',5,5'-tetramethyl-4,4'-bi-1<i>H</i>-pyrazole-2,2'-diium)
\g-octamolybdate(VI) dihydrate]
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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           SHELXL97
_cell_angle_alpha                106.242(8)
_cell_angle_beta                 106.063(9)
_cell_angle_gamma                106.102(8)
_cell_formula_units_Z            1
_cell_length_a                   8.0821(8)
_cell_length_b                   11.2521(11)
_cell_length_c                   12.9231(13)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      1.78
_cell_volume                     1000.9(2)
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f oscillation scans'
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9228
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.530
_exptl_absorpt_correction_T_max  0.8233
_exptl_absorpt_correction_T_min  0.7184
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.735
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                3837
_reflns_number_total             4505
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ku3054.cif
_cod_data_source_block           I
_cod_database_code               2018324
_cod_database_fobs_code          2018324