Polycyclic aromatic azomethine ylides: a unique entry to extended polycyclic heteroaromatics
Berger, Reinhard; Wagner, Manfred; Feng, Xinliang; Müllen, Klaus; Chem. Sci. 6 (2015) 436–; doi:10.1039/C4SC02793K

data_1518099
_publ_section_title
;
 Polycyclic aromatic azomethine ylides: a unique entry to extended
 polycyclic heteroaromatics
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              436
_journal_paper_doi               10.1039/C4SC02793K
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C38 H19 F10 N, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C38.5 H20 Cl F10 N'
_chemical_formula_weight         722.00
_space_group_IT_number           2
_symmetry_cell_setting           monoclinic
_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                87.227(2)
_cell_angle_beta                 75.478(3)
_cell_angle_gamma                67.501(3)
_cell_formula_units_Z            4
_cell_length_a                   12.6166(15)
_cell_length_b                   16.350(2)
_cell_length_c                   16.738(2)
_cell_measurement_reflns_used    7903
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.7
_cell_measurement_theta_min      2.4
_cell_volume                     3083.7(6)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'SAINT (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SMART APEX2'
_diffrn_measurement_method       'CCD scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14687
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.35
_diffrn_source                   'sealed Tube'
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14688
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+1.3995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0984
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                10629
_reflns_number_total             14688
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4sc02793k2.cif
_cod_data_source_block           aw014rc
_cod_depositor_comments
;
Adding full bibliography for 1518098--1518099.cif.

2019-07-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        3083.5(6)
_cod_original_formula_moiety     '2(C38 H19 F10 N), C H2 Cl2'
_cod_original_formula_sum        'C77 H40 Cl2 F20 N2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1444.01
_cod_database_code               1518099