Synthesis of Group 14 Dipyridinometalloles with Enhanced Electron-Deficient Properties and Solid-State Phosphorescence
Ohshita, Joji; Murakami, Kazuya; Tanaka, Daiki; Ooyama, Yousuke; Mizumo, Tomonobu; Kobayashi, Norifumi; Higashimura, Hideyuki; Nakanishi, Takayuki; Hasegawa, Yasuchika; Organometallics 33 (2014) 517–; doi:10.1021/om401019b

data_4082334
_publ_section_title
;
 Synthesis of Group 14 Dipyridinometalloles with Enhanced
 Electron-Deficient Properties and Solid-State Phosphorescence
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              517
_journal_paper_doi               10.1021/om401019b
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C24 H20 N2 O2 Si'
_chemical_formula_sum            'C24 H20 N2 O2 Si'
_chemical_formula_weight         396.52
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.8537(16)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.1171(7)
_cell_length_b                   10.9863(7)
_cell_length_c                   15.6860(7)
_cell_measurement_reflns_used    14393
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.23
_cell_volume                     2057.3(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19625
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             832.00
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4693
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.8407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                3719
_reflns_number_total             4693
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om401019b_si_001.cif
_cod_data_source_block           murakami2
_cod_original_cell_volume        2057.34(19)
_cod_database_code               4082334