Combination between lacunary polyoxometalates and high-nuclear transition metal clusters under hydrothermal conditions: I. from isolated cluster to 1-D chain.
Zheng, Shou-Tian; Yuan, Da-Qiang; Jia, Hong-Peng; Zhang, Jie; Yang, Guo-Yu; Chemical communications (Cambridge, England)  (2007) 1858–1860; doi:10.1039/b617191e

data_7101879
_publ_section_title
;
 Combination between lacunary polyoxometalates and high-nuclear
 transition metal clusters under hydrothermal conditions: I. from
 isolated cluster to 1-D chain.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1858
_journal_page_last               1860
_journal_paper_doi               10.1039/b617191e
_journal_year                    2007
_chemical_formula_moiety         'C12 H46 N9 Ni6 P W9 O39, 4(H2 O)'
_chemical_formula_sum            'C12 H54 N9 Ni6 O43 P W9'
_chemical_formula_weight         3050.52
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4477(3)
_cell_length_b                   19.4046(3)
_cell_length_c                   16.22210(10)
_cell_measurement_reflns_used    304
_cell_measurement_temperature    274(2)
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      2.48
_cell_volume                     5177.46(13)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      274(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'phi and omega 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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29016
_diffrn_reflns_theta_full        26.51
_diffrn_reflns_theta_max         26.51
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.171
_exptl_absorpt_correction_T_max  0.11
_exptl_absorpt_correction_T_min  0.023
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    3.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5528
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.276
_refine_diff_density_min         -1.620
_refine_diff_density_rms         0.314
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5419
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+124.9408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                4708
_reflns_number_total             5419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b617191e.txt
_cod_data_source_block           4
_cod_original_sg_symbol_Hall     -P2ac2n
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7101879