Elliptic Column Consolidated by Acetylide Dianion, Cyanide, and Trifluoroacetate in a Novel Quadruple Salt of Silver(I)
Quan-Ming Wang; Thomas C. W. Mak; Journal of the American Chemical Society 123 (2001) 1501–1502; doi:10.1021/ja0028727

data_4115444
_publ_section_title
;
 Elliptic Column Consolidated by Acetylide Dianion, Cyanide, and
 Trifluoroacetate in a Novel Quadruple Salt of Silver(I)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1501
_journal_page_last               1502
_journal_paper_doi               10.1021/ja0028727
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C37 H18 Ag24 B2 F53 N3 O39'
_chemical_formula_weight         4746.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 103.804(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.372(3)
_cell_length_b                   25.257(3)
_cell_length_c                   15.9775(16)
_cell_measurement_temperature    293(2)
_cell_volume                     10335(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34846
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    4.596
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.337
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.050
_exptl_crystal_description       prism
_exptl_crystal_F_000             8752
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.898
_refine_diff_density_min         -2.075
_refine_diff_density_rms         0.235
_refine_ls_extinction_coef       0.000012(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   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         12465
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1996
_refine_ls_wR_factor_ref         0.2311
_reflns_number_gt                6230
_reflns_number_total             12465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0028727.cif
_cod_data_source_block           f5
_cod_original_cell_volume        10334.8(19)
_cod_database_code               4115444