Low-Nuclearity Alkynyl d10Clusters Supported by Chelating Multidentate Phosphines
Belyaev, Andrey; Dau, Thuy Minh; Jänis, Janne; Grachova, Elena V.; Tunik, Sergey P.; Koshevoy, Igor O.; Organometallics 35 (2016) 3763–; doi:10.1021/acs.organomet.6b00701

data_4089100
_publ_section_title
;
 Low-Nuclearity Alkynyl d10Clusters Supported by Chelating Multidentate
 Phosphines
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              3763
_journal_paper_doi               10.1021/acs.organomet.6b00701
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C114 H88 Ag2 Au O4 P6, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C116 H90 Ag2 Au Cl2 F3 O7 P6 S'
_chemical_formula_weight         2354.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                91.07(4)
_cell_angle_beta                 95.03(5)
_cell_angle_gamma                100.96(5)
_cell_formula_units_Z            1
_cell_length_a                   11.49(3)
_cell_length_b                   14.45(3)
_cell_length_c                   15.54(3)
_cell_measurement_reflns_used    9276
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.33
_cell_volume                     2522(10)
_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.4.03 (Brandenburg, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       '62mm x 62mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II DUO CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48833
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.814
_exptl_absorpt_coefficient_mu    2.070
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             1182
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.064
_refine_diff_density_max         3.009
_refine_diff_density_min         -1.809
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         9210
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+23.6543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7685
_reflns_number_total             9210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00701_si_002.cif
_cod_data_source_block           14
_cod_database_code               4089100
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.607
_shelx_estimated_absorpt_t_max   0.879
_shelx_res_checksum              19139
_shelx_hkl_checksum              87808
_shelx_fab_checksum              74281