Synthesis and identification of a trimethylenemethane derivative pi-extended with three pyridinyl radicals.
Matsumoto, Kouzou; Inokuchi, Daisuke; Hirao, Yasukazu; Kurata, Hiroyuki; Sato, Kazunobu; Takui, Takeji; Kubo, Takashi; Organic letters 12 (2010) 836–839; doi:10.1021/ol902937k

data_1503427
_publ_section_title
;
 Synthesis and identification of a trimethylenemethane derivative
 pi-extended with three pyridinyl radicals.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              836
_journal_page_last               839
_journal_paper_doi               10.1021/ol902937k
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C56.30 H46.30 Cl3.90 F12 N3 P2 '
_chemical_formula_sum            'C56.3 H46.3 Cl3.9 F12 N3 P2'
_chemical_formula_weight         1193.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.919(13)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.276(5)
_cell_length_b                   17.432(5)
_cell_length_c                   18.466(5)
_cell_measurement_reflns_used    27044
_cell_measurement_temperature    200.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.2
_cell_volume                     5558(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2004
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49171
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2437.60
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.38
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.305
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     699
_refine_ls_number_reflns         12553
_refine_ls_R_factor_gt           0.0975
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3416
_reflns_number_gt                8475
_reflns_number_total             12553
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol902937k_si_002.cif
_cod_data_source_block           '_inokuchi1023'
_cod_original_formula_sum        'C56.30 H46.30 Cl3.90 F12 N3 P2 '
_cod_database_code               1503427