Three multi-nuclear clusters and one infinite chain induced by a pendant 4-butyl-1H-pyrazole ligand for modification of Keggin anions.
Tian, Ai-xiang; Ning, Ya-li; Ying, Jun; Hou, Xue; Li, Tian-jiao; Wang, Xiu-li; Dalton transactions (Cambridge, England : 2003) 44 (2015) 386–394; doi:10.1039/c4dt02821j

data_7032974
_publ_section_title
;
 Three multi-nuclear clusters and one infinite chain induced by a pendant
 4-butyl-1H-pyrazole ligand for modification of Keggin anions.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              386
_journal_page_last               394
_journal_paper_doi               10.1039/c4dt02821j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C34 H70 Cu6 N12 O88 P2 W22'
_chemical_formula_weight         6543
_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                90.000(5)
_cell_angle_beta                 123.633(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   25.202(5)
_cell_length_b                   13.227(5)
_cell_length_c                   21.533(5)
_cell_measurement_reflns_used    4687
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      2.41
_cell_volume                     5976(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17534
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         26.80
_diffrn_reflns_theta_min         1.14
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    22.232
_exptl_absorpt_correction_T_max  0.069
_exptl_absorpt_correction_T_min  0.026
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8  March, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5588
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
The free water molecules were highly disordered and could not be modeled properly, thus the SQUEEZE routine of PLATON was applied to remove the contributions to the scattering from the solvent molecules. The reported refinements are of the guest-free structures using the *.hkp files produced via the SQUEEZE routine. 
;
_refine_diff_density_max         2.468
_refine_diff_density_min         -2.692
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6615
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.836
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                4963
_reflns_number_total             6670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02821j2.cif
_cod_data_source_block           compound-1
_cod_depositor_comments
'Adding full bibliography for 7032974--7032977.cif.'
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7032974