A Novel Dumbbell-like Polyoxometalate Assembled of Copper(II)-Disubstituted Monovacant Keggin Polyoxoanions with a Tetranuclear Copper Cluster.
Miao, Hao; Xu, Xiao; Ju, Wei-Wei; Wan, Hong-Xiang; Zhang, Yu; Zhu, Dun-Ru; Xu, Yan; Inorganic chemistry 53 (2014) 2757–2759; doi:10.1021/ic5000827

data_4337652
_publ_section_title
;
 A Novel Dumbbell-like Polyoxometalate Assembled of
 Copper(II)-Disubstituted Monovacant Keggin Polyoxoanions with a
 Tetranuclear Copper Cluster.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2757
_journal_page_last               2759
_journal_paper_doi               10.1021/ic5000827
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C84 H106 Cu8 N16 O96 P2 W22'
_chemical_formula_weight         7490.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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           SHELXL-97
_cell_angle_alpha                75.420(3)
_cell_angle_beta                 77.176(3)
_cell_angle_gamma                73.647(3)
_cell_formula_units_Z            1
_cell_length_a                   12.585(3)
_cell_length_b                   13.220(3)
_cell_length_c                   24.903(6)
_cell_measurement_reflns_used    4571
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.21
_cell_volume                     3796.3(16)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\w 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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26054
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    17.805
_exptl_absorpt_correction_T_max  0.2238
_exptl_absorpt_correction_T_min  0.1629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    3.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3380
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.791
_refine_diff_density_min         -2.296
_refine_diff_density_rms         0.360
_refine_ls_extinction_coef       0.000053(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         13063
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1309
_reflns_number_gt                8434
_reflns_number_total             13063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5000827_si_002.cif
_cod_data_source_block           mh-13-3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/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_sg_symbol_H-M      'P-1   '
_cod_database_code               4337652