Structural and Photophysical Study on Alkynyl Cyclometalated Pt2Pb2and Pt2Pb Clusters
Díez, Álvaro; Lalinde, Elena; Moreno, M. Teresa; Ruiz, Santiago; Organometallics  (2016) –; doi:10.1021/acs.organomet.6b00162

data_4086495
_publ_section_title
;
 Structural and Photophysical Study on Alkynyl Cyclometalated Pt2Pb2and
 Pt2Pb Clusters
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00162
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C71 H42 B F12 N8 Pb Pt2, C16 H36 N, 2(C H Cl3)'
_chemical_formula_sum            'C89 H80 B Cl6 F12 N9 Pb Pt2'
_chemical_formula_weight         2324.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-06-28T12:01:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.901(1)
_cell_angle_beta                 82.966(1)
_cell_angle_gamma                84.314(1)
_cell_formula_units_Z            2
_cell_length_a                   12.7567(3)
_cell_length_b                   15.2714(4)
_cell_length_c                   22.8713(4)
_cell_measurement_reflns_used    8041
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_cell_measurement_wavelength     0.71073
_cell_volume                     4398.97(17)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.612792E-1
_diffrn_orient_matrix_UB_12      -0.142795E-1
_diffrn_orient_matrix_UB_13      0.232168E-1
_diffrn_orient_matrix_UB_21      -0.361346E-1
_diffrn_orient_matrix_UB_22      0.391367E-1
_diffrn_orient_matrix_UB_23      0.31995E-1
_diffrn_orient_matrix_UB_31      -0.351426E-1
_diffrn_orient_matrix_UB_32      -0.509653E-1
_diffrn_orient_matrix_UB_33      0.194754E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            67295
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.27
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    5.34
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.097
_refine_diff_density_min         -1.576
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         17861
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+16.6972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.107
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                14485
_reflns_number_total             17861
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om6b00162_si_002.cif
_cod_data_source_block           3
_cod_database_code               4086495