Asymmetrically fused polyoxometalate-silver alkynide composite cluster.
Kurasawa, Mariko; Arisaka, Fumio; Ozeki, Tomoji; Inorganic chemistry 54 (2015) 1650–1654; doi:10.1021/ic502644v

data_4342079
_publ_section_title
;
 Asymmetrically fused polyoxometalate-silver alkynide composite cluster.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1650
_journal_page_last               1654
_journal_paper_doi               10.1021/ic502644v
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'Ag25 P2 W15 Nb3 O62 16(C6 H9) 4(C2 H6 N), 11(C2 H6 N)'
_chemical_formula_sum            'C126 H189 Ag25 N15 Nb3 O62 P2 W15'
_chemical_formula_weight         8701.08
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90.694(1)
_cell_angle_beta                 101.451(1)
_cell_angle_gamma                108.184(2)
_cell_formula_units_Z            2
_cell_length_a                   17.771(1)
_cell_length_b                   19.662(1)
_cell_length_c                   30.509(1)
_cell_measurement_temperature    123(2)
_cell_volume                     9894.8(8)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection
'Crystal Clear (Molecular Structure Corporation, 2001)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       'oscillation method, \w and \p scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.1027
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            73743
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         28.797
_diffrn_reflns_theta_min         2.239
_diffrn_source                   'rotatin anode X-ray tube'
_exptl_absorpt_coefficient_mu    11.337
_exptl_absorpt_correction_T_max  0.4951
_exptl_absorpt_correction_T_min  0.4403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'PLATON MULABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.920
_exptl_crystal_description       plate
_exptl_crystal_F_000             7968
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.115
_refine_diff_density_min         -3.323
_refine_diff_density_rms         0.320
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2263
_refine_ls_number_reflns         47702
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1223
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29295
_reflns_number_total             47702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502644v_si_002.cif
_cod_data_source_block           Ag25P2W15Nb3O62
_cod_depositor_comments          'Adding full bibliography for 4342079.cif.'
_cod_database_code               4342079
_shelx_estimated_absorpt_t_min   0.397
_shelx_estimated_absorpt_t_max   0.660
_shelxl_version_number           2013-3
_shelx_res_checksum              83329
_shelx_hkl_checksum              51789