Silver Alkynyl-Phosphine Clusters: An Electronic Effect of the Alkynes Defines Structural Diversity
Chen, Yi-Ting; Krytchankou, Ilya S.; Karttunen, Antti J.; Grachova, Elena V.; Tunik, Sergey P.; Chou, Pi-Tai; Koshevoy, Igor O.; Organometallics 36 (2017) 480–; doi:10.1021/acs.organomet.6b00866

data_4086989
_publ_section_title
;
 Silver Alkynyl-Phosphine Clusters: An Electronic Effect of the Alkynes
 Defines Structural Diversity
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              480
_journal_paper_doi               10.1021/acs.organomet.6b00866
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety
'2(C107 H92 Ag7 F9 N3 O9 P6 S3), 2(C F3 O3 S), 3(C3 H6 O)'
_chemical_formula_sum            'C225 H202 Ag14 F24 N6 O27 P12 S8'
_chemical_formula_weight         6016.21
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.0625(6)
_cell_length_b                   23.0625(6)
_cell_length_c                   39.8602(11)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      38.36
_cell_measurement_theta_min      2.34
_cell_volume                     18360.4(8)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'Diamond v.4.01 (Brandenburg, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '62mm x 62mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            63611
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.000
_diffrn_reflns_theta_min         2.284
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_T_max  0.640
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             8976
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.382
_exptl_crystal_size_min          0.372
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 5225 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         12870
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0478P)^2^+30.5731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.909
_reflns_Friedel_fraction_max     0.817
_reflns_number_gt                12064
_reflns_number_total             12870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            6_7.cif
_cod_data_source_block           7
_cod_original_cell_volume        18360.4(11)
_cod_database_code               4086989
_shelx_estimated_absorpt_t_min   0.601
_shelx_estimated_absorpt_t_max   0.640
_shelxl_version_number           2014/6
_shelx_res_checksum              41794
_shelx_hkl_checksum              39201