Chiral-at-Metal Phosphorescent Square-Planar Pt(II)-Complexes from an Achiral Organometallic Ligand.
Schulte, Thorben R.; Holstein, Julian J.; Krause, Lennard; Michel, Reent; Stalke, Dietmar; Sakuda, Eri; Umakoshi, Keisuke; Longhi, Giovanna; Abbate, Sergio; Clever, Guido H.; Journal of the American Chemical Society 139 (2017) 6863–6866; doi:10.1021/jacs.7b03963

data_4131309
_publ_section_title
;
 Chiral-at-Metal Phosphorescent Square-Planar Pt(II)-Complexes from an
 Achiral Organometallic Ligand.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6863
_journal_page_last               6866
_journal_paper_doi               10.1021/jacs.7b03963
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C42 H24 N2 Pt'
_chemical_formula_sum            'C42 H24 N2 Pt'
_chemical_formula_weight         751.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.984(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5938(12)
_cell_length_b                   9.2189(6)
_cell_length_c                   18.8427(14)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.07
_cell_measurement_theta_min      2.50
_cell_volume                     3033.5(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v4.2.3'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker D8 Venture CMOS with Photon 100'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            152787
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.251
_diffrn_reflns_theta_min         2.451
_diffrn_source_type              'INCOATEC microfocus sealed tube'
_exptl_absorpt_coefficient_mu    4.660
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 6281 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.142(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         19280
_refine_ls_number_restraints     649
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0122P)^2^+4.2888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0487
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                15142
_reflns_number_total             19280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03963_si_004.cif
_cod_data_source_block           tsk9
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4131309
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.468
_shelx_estimated_absorpt_t_max   0.800
_shelx_res_checksum              37816
_shelx_hkl_checksum              98815