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_4086494
_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         'C40 H32 B N7 O2 Pb Pt, 0.5(C H2 Cl2) '
_chemical_formula_sum            'C40.5 H33 B Cl N7 O2 Pb Pt'
_chemical_formula_weight         1098.28
_chemical_name_common            'Compound X'
_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   constr
_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      2.4.3
_audit_creation_date             2016-04-01T00:56:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                91.8073(8)
_cell_angle_beta                 101.3520(14)
_cell_angle_gamma                106.0196(14)
_cell_formula_units_Z            4
_cell_length_a                   12.6780(2)
_cell_length_b                   13.1485(3)
_cell_length_c                   24.0521(6)
_cell_measurement_reflns_used    16275
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_cell_measurement_wavelength     0.71073
_cell_volume                     3762.60(14)
_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 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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_UB_11      -0.065518
_diffrn_orient_matrix_UB_12      -0.065386
_diffrn_orient_matrix_UB_13      -0.006375
_diffrn_orient_matrix_UB_21      -0.036561
_diffrn_orient_matrix_UB_22      0.027976
_diffrn_orient_matrix_UB_23      -0.034481
_diffrn_orient_matrix_UB_31      0.037791
_diffrn_orient_matrix_UB_32      -0.035433
_diffrn_orient_matrix_UB_33      -0.02416
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14246
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         0.867
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.3
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9800
_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    1.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.66
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     964
_refine_ls_number_reflns         14246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+30.6623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0
_reflns_number_gt                11822
_reflns_number_total             14246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00162_si_002.cif
_cod_data_source_block           2
_cod_database_code               4086494