Gram Scale Synthesis of Benzophenanthroline and Its Blue Phosphorescent Platinum Complex.
Saris, Patrick J. G.; Thompson, Mark E.; Organic letters 18 (2016) 3960–3963; doi:10.1021/acs.orglett.6b01693

data_1555633
_publ_section_title
;
 Gram Scale Synthesis of Benzophenanthroline and Its Blue Phosphorescent
 Platinum Complex.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              3960
_journal_page_last               3963
_journal_paper_doi               10.1021/acs.orglett.6b01693
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C33 H32 N2 O2 Pt'
_chemical_formula_sum            'C33 H32 N2 O2 Pt'
_chemical_formula_weight         683.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 96.051(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.7670(8)
_cell_length_b                   26.604(4)
_cell_length_c                   17.464(2)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.4656
_cell_measurement_theta_min      2.8012
_cell_volume                     2664.5(6)
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_collection
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22972
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.53
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    5.300
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_crystal_colour            'clear yellow-orange'
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.153
_refine_diff_density_min         -2.063
_refine_ls_abs_structure_details
;
Flack x determined using 2852 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         7753
_refine_ls_number_restraints     347
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                6540
_reflns_number_total             7753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01693_si_003.cif
_cod_data_source_block           I
_cod_database_code               1555633
_shelx_res_checksum              53956
_shelx_hkl_checksum              66674