Soluble Silver Acetylide for the Construction and Structural Conversion of All-Alkynyl-Stabilized High-Nuclearity Homoleptic Silver Clusters
Zhang, Rui; Hao, Xiang; Li, Xiumin; Zhou, Zhengyang; Sun, Junliang; Cao, Rui; Crystal Growth & Design 15 (2015) 2505–; doi:10.1021/acs.cgd.5b00286

data_4513115
_publ_section_title
;
 Soluble Silver Acetylide for the Construction and Structural Conversion
 of All-Alkynyl-Stabilized High-Nuclearity Homoleptic Silver Clusters
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2505
_journal_paper_doi               10.1021/acs.cgd.5b00286
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C256 H336 Ag16'
_chemical_formula_weight         5139.15
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.8070(9)
_cell_length_b                   25.8070(9)
_cell_length_c                   20.5657(10)
_cell_measurement_reflns_used    9637
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.17
_cell_measurement_theta_min      2.27
_cell_volume                     13696.8(9)
_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  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            158423
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.465
_diffrn_reflns_theta_min         2.232
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_T_max  0.7847
_exptl_absorpt_correction_T_min  0.7606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             5248
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_refine_diff_density_max         2.386
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Flack x determined using 4376 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.105(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         14097
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1414P)^2^+23.3794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.2105
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                10690
_reflns_number_total             14097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b00286_si_003.cif
_cod_data_source_block           2_sq
_cod_original_cell_volume        13696.8(12)
_cod_database_code               4513115
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.761
_shelx_estimated_absorpt_t_max   0.785
_shelx_res_checksum              36884
_shelx_hkl_checksum              24026
_shelx_fab_checksum              29329