New synthetic route for organic polyoxometallic clusters: synthetic and structural investigations on the first dumb-bell shaped polyoxozirconium hydroxide with the [Zr9(μ5-O)2(μ3-O)4(μ-O)4(μ-OH)8] core structure
Bai, Guangcai; Ma, Qingjun; Roesky, Herbert W.; Vidovic, Denis; Herbst-Irmer, Regine; Chemical Communications (Cambridge, United Kingdom)  (2003) 898–899; doi:10.1039/b212281b

data_7113559
_publ_section_title
;
 New synthetic route for organic polyoxometallic clusters: synthetic and
 structural investigations on the first dumb-bell shaped polyoxozirconium
 hydroxide with the [Zr9(\m5-O)2(\m3-O)4(\m-O)4(\m-OH)8] core structure
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   7
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              898
_journal_page_last               899
_journal_paper_doi               10.1039/b212281b
_journal_year                    2003
_chemical_formula_sum            'C101 H152 O18 Zr9'
_chemical_formula_weight         2475.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 102.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.269(4)
_cell_length_b                   16.745(3)
_cell_length_c                   31.219(6)
_cell_measurement_reflns_used    996
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      49.326
_cell_measurement_theta_min      12.474
_cell_volume                     10357(4)
_computing_cell_refinement       'Bruker AXS SAINT (V.5.00, Madison 1997)'
_computing_data_collection       'Siemens SMART (V.5.050, Siemens 1998)'
_computing_data_reduction        'Bruker AXS SAINT (V.5.00, Madison 1997)'
_computing_molecular_graphics    'Bruker AXS Shelxtl (Madison 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type
'STOE-Siemens-Huber four circle diffractometer'
_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  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            80494
_diffrn_reflns_theta_full        24.93
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         6.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5048
_exptl_crystal_size_max          0.3mm
_exptl_crystal_size_mid          0.2mm
_exptl_crystal_size_min          0.05mm
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1196
_refine_ls_number_reflns         16554
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0425P)^2^+47.2628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                11951
_reflns_number_total             16554
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7104040
_cod_data_source_file            b212281b.txt
_cod_data_source_block           compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        10357(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C80 H128 O18 Zr9, 3(C7 H8)'
_cod_database_code               7113559