π-Conjugated Heterotriangulene Macrocycles by Solution and Surface-supported Synthesis toward Honeycomb Networks
Florian Schlütter; Frédéric Rossel; Milan Kivala; Volker Enkelmann; Jean-Paul Gisselbrecht; Pascal Ruffieux; Roman Fasel; Klaus Müllen; Journal of the American Chemical Society 135 (2013) 4550–4557; doi:10.1021/ja400857g

data_4119493
_publ_contact_author_address
; 

 Max-Planck-Institute for Polymer Research 

 Ackermannweg 10 

 D-55021 Mainz 

 Germany 

;
_publ_contact_author_email       ve@mpip-mainz.mpg.de
_publ_contact_author_fax         '+49 379100'
_publ_contact_author_name        'Volker Enkelmann'
_publ_contact_author_phone       '+49 379133'
_publ_section_title
;
 \p-Conjugated Heterotriangulene Macrocycles by Solution and
 Surface-supported Synthesis toward Honeycomb Networks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4550
_journal_page_last               4557
_journal_paper_doi               10.1021/ja400857g
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C82 H76 Cl3 N3'
_chemical_formula_sum            'C82 H76 Cl3 N3'
_chemical_formula_weight         1209.88
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             12-07-17
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 101.689(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   49.2578(9)
_cell_length_b                   15.0524(6)
_cell_length_c                   19.1141(7)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    120
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     13878.2(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            45947
_diffrn_reflns_theta_full        26.935
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.838
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       prism
_exptl_crystal_F_000             5120
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;

;
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9293
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         9185
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1409
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.000567
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;

 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 

 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 

 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 

 Method = Robust Weighting (Prince, 1982) 

 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 

 A~i~ are: 

 3.33 3.26 1.77 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2382
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0587
_reflns_limit_h_max              62
_reflns_limit_h_min              -63
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                9185
_reflns_number_total             15855
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            ja400857g_si_002.cif
_cod_data_source_block           fscyc
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4119493