Synthesis and Reactivity of the Methoxozirconium Pentatungstate (nBu4N)6[{(μ-MeO)ZrW5O18}2]: Insights into Proton-Transfer Reactions, Solution Dynamics, and Assembly of {ZrW5O18}2- Building Blocks
R. John Errington; Sagar S. Petkar; Paul S. Middleton; William McFarlane; William Clegg; Robert A. Coxall; Ross W. Harrington; Journal of the American Chemical Society 129 (2007) 12181–12196; doi:10.1021/ja0725495

data_4109974
_publ_section_title
;
 Synthesis and Reactivity of the Methoxozirconium Pentatungstate
 (nBu4N)6[{(\m-MeO)ZrW5O18}2]: Insights into Proton-Transfer Reactions,
 Solution Dynamics, and Assembly of {ZrW5O18}2- Building Blocks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12181
_journal_page_last               12196
_journal_paper_doi               10.1021/ja0725495
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         '6 C16 H36 N +, H2 O38 W10 Zr2 6-, C2 H3 N'
_chemical_formula_sum            'C98 H221 N7 O38 W10 Zr2'
_chemical_formula_weight         4126.75
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 123.664(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   42.705(9)
_cell_length_b                   16.063(4)
_cell_length_c                   24.531(10)
_cell_measurement_reflns_used    265
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.50
_cell_measurement_theta_min      2.50
_cell_volume                     14006(8)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48162
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.90
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.385
_exptl_absorpt_correction_T_max  0.188
_exptl_absorpt_correction_T_min  0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_description       block
_exptl_crystal_F_000             7940
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.195
_refine_diff_density_min         -2.276
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         11842
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+847.7634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1622
_reflns_number_gt                8312
_reflns_number_total             11842
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0725495si20070418_010810_2.cif
_cod_data_source_block           rje392_anion3
_cod_original_cell_volume        14006(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4109974