Unprecedented Application of Flexible Bis(pyridyl-tetrazole) Ligands To Construct Helix/Loop Subunits To Modify Polyoxometalate Anions.
Wang, Xiu-Li; Li, Na; Tian, Ai-Xiang; Ying, Jun; Li, Tian-Jiao; Lin, Xiao-Ling; Luan, Jian; Yang, Yang; Inorganic chemistry 53 (2014) 7118–7129; doi:10.1021/ic403153f

data_4340342
_publ_section_title
;
 Unprecedented Application of Flexible Bis(pyridyl-tetrazole) Ligands To
 Construct Helix/Loop Subunits To Modify Polyoxometalate Anions.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7118
_journal_page_last               7129
_journal_paper_doi               10.1021/ic403153f
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C40 H47 Ag3 N25 O64 P2 W18'
_chemical_formula_weight         5596.88
_chemical_name_systematic
; 
 ? 
;
_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                 99.0030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.0496(19)
_cell_length_b                   15.2674(10)
_cell_length_c                   22.9741(15)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.284
_cell_measurement_theta_min      2.5775
_cell_volume                     9717.3(11)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0639
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59351
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    21.938
_exptl_absorpt_correction_T_max  0.072
_exptl_absorpt_correction_T_min  0.027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9880
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         5.456
_refine_diff_density_min         -4.394
_refine_diff_density_rms         0.583
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1360
_refine_ls_number_reflns         23562
_refine_ls_number_restraints     2314
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0698
_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^)+(0.0738P)^2^+641.7980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1839
_reflns_number_gt                15982
_reflns_number_total             24386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic403153f_si_002.cif
_cod_data_source_block           compound-3
_cod_depositor_comments
'Adding full bibliography for 4340340--4340342.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4340342