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_4086982
_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
'C233 H210 Ag14 F6 N8 O7 P12 S2, 4(C F3 O3 S), 3(C4 H10 O), 2(C3 H6 O)'
_chemical_formula_sum            'C255 H252 Ag14 F18 N8 O24 P12 S6'
_chemical_formula_weight         6228.81
_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-2014/6
_cell_angle_alpha                98.669(2)
_cell_angle_beta                 91.245(2)
_cell_angle_gamma                93.451(2)
_cell_formula_units_Z            1
_cell_length_a                   16.8626(7)
_cell_length_b                   17.5460(8)
_cell_length_c                   22.2763(9)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.21
_cell_measurement_theta_min      2.99
_cell_volume                     6500.6(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0246
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            100626
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.604
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             3126
_exptl_crystal_size_max          0.568
_exptl_crystal_size_mid          0.551
_exptl_crystal_size_min          0.142
_refine_diff_density_max         2.856
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1554
_refine_ls_number_reflns         25449
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+29.4558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20642
_reflns_number_total             25449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            8_9.cif
_cod_data_source_block           8
_cod_database_code               4086982
_shelx_estimated_absorpt_t_min   0.543
_shelx_estimated_absorpt_t_max   0.845
_shelxl_version_number           2014/6
_shelx_res_checksum              58718
_shelx_hkl_checksum              66125