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_4086493
_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         'C76 H56 B2 N14 Pb2 Pt2'
_chemical_formula_sum            'C76 H56 B2 N14 Pb2 Pt2'
_chemical_formula_weight         1991.52
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2011-06-28T18:58:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.11
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.489
_cell_length_b                   16.711
_cell_length_c                   15.655
_cell_measurement_reflns_used    4400
_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                     3234.580
_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 0.99
_diffrn_measured_fraction_theta_max 0.99
_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      0.173613E-1
_diffrn_orient_matrix_UB_12      0.434616E-1
_diffrn_orient_matrix_UB_13      0.436707E-1
_diffrn_orient_matrix_UB_21      0.777875E-1
_diffrn_orient_matrix_UB_22      -0.24283E-2
_diffrn_orient_matrix_UB_23      -0.85499E-2
_diffrn_orient_matrix_UB_31      -0.137747E-1
_diffrn_orient_matrix_UB_32      0.41065E-1
_diffrn_orient_matrix_UB_33      -0.467249E-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  0.0408
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16363
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.44
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    9.559
_exptl_absorpt_correction_T_max  0.1018
_exptl_absorpt_correction_T_min  0.0594
_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    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.018
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.325
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+0.5578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                5130
_reflns_number_total             5862
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om6b00162_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        3234.5(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4086493