A pyrovanadate-templated silver(I)-ethynide cluster circumscribed by macrocyclic polyoxovanadate(V)
Yun-Peng Xie; Thomas Mak; Chem.Commun. 48 (2012) 1123–; doi:10.1039/c2cc16756e

data_7107232
_publ_section_title
;
 A pyrovanadate-templated silver(I)-ethynide cluster circumscribed by
 macrocyclic polyoxovanadate(V)
;
_journal_name_full               Chem.Commun.
_journal_page_first              1123
_journal_paper_doi               10.1039/c2cc16756e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C204 H342 Ag44 N10 O110 V36'
_chemical_formula_weight         11275.00
_chemical_name_systematic
;
?
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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                   20.250(3)
_cell_length_b                   20.250(3)
_cell_length_c                   84.201(19)
_cell_measurement_temperature    293(2)
_cell_volume                     34528(11)
_computing_cell_refinement       SAINT(Bruker,2001)
_computing_data_collection       APEX2(Bruker,2003)
_computing_data_reduction        APEX2(Bruker,2003)
_computing_molecular_graphics    'SHELXL-97 (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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1402
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       110
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            303614
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    3.417
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orang
_exptl_crystal_density_diffrn    2.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             21648
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.260
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.232
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.55(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         20693
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1355
_refine_ls_R_factor_gt           0.0981
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+1866.1066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2236
_refine_ls_wR_factor_ref         0.2448
_reflns_number_gt                14768
_reflns_number_total             20693
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc16756e.txt
_cod_data_source_block           22
_cod_original_cell_volume        34526(10)
_cod_original_sg_symbol_H-M      I-42d
_cod_database_code               7107232