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_4089092
_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         'C62 H47 Cu2 P4, F6 P, C3 H6 O'
_chemical_formula_sum            'C65 H53 Cu2 F6 O P5'
_chemical_formula_weight         1246.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.118(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9071(8)
_cell_length_b                   30.125(2)
_cell_length_c                   17.9273(14)
_cell_measurement_reflns_used    9353
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.35
_cell_measurement_theta_min      2.70
_cell_volume                     5686.6(7)
_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.3.2g (Brandenburg, 2011)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (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 0.998
_diffrn_measured_fraction_theta_max 0.987
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78314
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.666
_diffrn_reflns_theta_min         2.513
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       block
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.468
_exptl_crystal_size_min          0.402
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.288
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         20604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0714P)^2^+4.9125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15941
_reflns_number_total             20604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00701_si_002.cif
_cod_data_source_block           6
_cod_original_cell_volume        5686.5(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089092
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.606
_shelx_estimated_absorpt_t_max   0.756
_shelx_res_checksum              37651
_shelx_hkl_checksum              98467