Route for the Elaboration of Functionalized Hybrid 3d-Substituted Trivacant Keggin Anions
Guillaume Rousseau; Olivier Oms; Anne Dolbecq; Jérôme Marrot; Pierre Mialane; Inorganic Chemistry 50 (2011) 7376–7378; doi:10.1021/ic2011088

data_4325954
_publ_contact_author
; 
      Pr P. Mialane
      Institut Lavoisier de Versailles, ILV, UMR CNRS 8180
      Universit\'e de Versailles Saint-Quentin-en-Yvelines
      45 Avenue des Etats Unis
      78035 Versailles Cedex
      France
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_publ_contact_author_email       mialane@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_phone       '(33) 1 39 25 43 83 '
_publ_section_title
;
 Route for the Elaboration of Functionalized Hybrid 3d-Substituted
 Trivacant Keggin Anions
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7376
_journal_page_last               7378
_journal_paper_doi               10.1021/ic2011088
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C8 H18 Cu4 K3 N2 Na O50 Si W9'
_chemical_formula_weight         3019.43
_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                   22.313(3)
_cell_length_b                   18.798(3)
_cell_length_c                   12.0022(16)
_cell_measurement_reflns_used    8966
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.12
_cell_volume                     5034.2(12)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'CCDC area detector'
_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  0.1552
_diffrn_reflns_av_sigmaI/netI    0.1218
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10799
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    22.523
_exptl_absorpt_correction_T_max  0.6615
_exptl_absorpt_correction_T_min  0.3989
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.984
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5376
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.234
_refine_diff_density_min         -4.279
_refine_diff_density_rms         0.578
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0784P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1588
_reflns_number_gt                3100
_reflns_number_total             4349
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic2011088_si_002_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        5034.1(11)
_cod_database_code               4325954