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_4089094
_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         '2(C62 H47 Au Cu P4), 2(F6 P), C H2 Cl2'
_chemical_formula_sum            'C125 H96 Au2 Cl2 Cu2 F12 P10'
_chemical_formula_weight         2727.62
_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                98.904(18)
_cell_angle_beta                 98.603(12)
_cell_angle_gamma                91.20(4)
_cell_formula_units_Z            1
_cell_length_a                   10.788(12)
_cell_length_b                   17.03(2)
_cell_length_c                   17.42(2)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.31
_cell_volume                     3123(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0821
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            135948
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.597
_diffrn_reflns_theta_min         1.198
_exptl_absorpt_coefficient_mu    2.912
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             1354
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.071
_refine_diff_density_max         2.377
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         20814
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+1.0106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15716
_reflns_number_total             20814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00701_si_002.cif
_cod_data_source_block           8
_cod_database_code               4089094
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.562
_shelx_estimated_absorpt_t_max   0.820
_shelx_res_checksum              44377
_shelx_hkl_checksum              88106
_shelx_fab_checksum              87418