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_4109981
_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
'7 C16 H36 N +, H3 O56 W15 Zr3 7-, 3.5 C2 H3 N'
_chemical_formula_sum            'C119 H265.5 N10.5 O56 W15 Zr3'
_chemical_formula_weight         5771.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 93.722(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   66.456(6)
_cell_length_b                   15.6607(14)
_cell_length_c                   32.988(3)
_cell_measurement_reflns_used    17909
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.96
_cell_measurement_theta_min      3.47
_cell_volume                     34260(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6900
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.1060
_diffrn_reflns_limit_h_max       78
_diffrn_reflns_limit_h_min       -66
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            80097
_diffrn_reflns_theta_full        24.25
_diffrn_reflns_theta_max         24.25
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.274
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_description       plate
_exptl_crystal_F_000             21848
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.911
_refine_diff_density_min         -1.689
_refine_diff_density_rms         0.212
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.029(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3665
_refine_ls_number_reflns         55335
_refine_ls_number_restraints     15205
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+166.6899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                43160
_reflns_number_total             55335
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0725495si20070418_010810_9.cif
_cod_data_source_block           rje307_anion9
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C119 H265.50 N10.50 O56 W15 Zr3'
_cod_database_code               4109981