Structural Interconversion and Regulation of Optical Properties of Stable Hypercoordinate Dipyrrin-Silicon Complexes
Naoya Sakamoto; Chusaku Ikeda; Masaki Yamamura; Tatsuya Nabeshima; Journal of the American Chemical Society 133 (2011) 4726–4729; doi:10.1021/ja2001924

data_4105879
_publ_contact_author_address
;
 Graduate School of Pure and Applied Sciences,
 University of Tsukuba, Tsukuba, Ibaraki, 305-8571, Japan.
;
_publ_contact_author_email       NABESIMA@CHEM.TSUKUBA.AC.JP
_publ_contact_author_name        'Tatsuya Nabeshima'
_publ_section_title
;
 Structural Interconversion and Regulation of Optical Properties of Stable
 Hypercoordinate Dipyrrin-Silicon Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4726
_journal_page_last               4729
_journal_paper_doi               10.1021/ja2001924
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C30 H23 N2 O2.5 Si'
_chemical_formula_weight         479.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.661(2)
_cell_angle_beta                 76.871(3)
_cell_angle_gamma                87.781(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6726(12)
_cell_length_b                   10.9105(9)
_cell_length_c                   11.2603(12)
_cell_measurement_temperature    120(2)
_cell_volume                     1161.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'MAC Science DIP-2030'
_diffrn_measurement_method       IP
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11621
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  0.9733
_exptl_absorpt_correction_T_min  0.9351
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_F_000             502
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1617
_reflns_number_gt                3488
_reflns_number_total             5296
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2001924_si_002.cif
_cod_data_source_block           319da
_cod_original_formula_sum        'C30 H23 N2 O2.50 Si'
_cod_database_code               4105879