Assembly of an undeca-nuclear nickel substituted POM through polycarboxylate ligand.
Zheng, Yun-Yun; Wen, Ru; Kong, Xiang-Jian; Long, La-Sheng; Huang, Rong-Bin; Zheng, Lan-Sun; Dalton transactions (Cambridge, England : 2003) 41 (2012) 9871–9875; doi:10.1039/c2dt12507b

data_7019671
_publ_section_title
;
 Assembly of an undeca-nuclear nickel substituted POM through
 polycarboxylate ligand.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9871
_journal_page_last               9875
_journal_paper_doi               10.1039/c2dt12507b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C24 H103 N15 Ni12 O99 P2 W18'
_chemical_formula_weight         6261.97
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 105.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   38.794(8)
_cell_length_b                   20.940(4)
_cell_length_c                   17.201(3)
_cell_measurement_reflns_used    8498
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.09
_cell_volume                     13456(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
'teXsan (Molecular Structure Corporation, Rigaku Corporation, 1999)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 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      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method       \w
_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  0.2083
_diffrn_reflns_av_sigmaI/netI    0.1690
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57640
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    17.071
_exptl_absorpt_correction_T_max  0.505
_exptl_absorpt_correction_T_min  0.148
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             11368
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
SQUEEZE removed 2 disordered (H2en)2+ and
7 disordered water molecules per formula unit. This valueis
calculated based upon elemental analysis data and the squeeze void count electrons.
;
_refine_diff_density_max         4.677
_refine_diff_density_min         -2.758
_refine_diff_density_rms         0.476
_refine_ls_extinction_coef       0.000094(13)
_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   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         13580
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0885
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1193P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2325
_refine_ls_wR_factor_ref         0.2516
_reflns_number_gt                8498
_reflns_number_total             13580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12507b.txt
_cod_data_source_block           compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        13457(5)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7019671