The synthesis of flexible tetrapyridylethanes from pyridylpyrylium dications
Le Poul, Pascal; Le Poul, Nicolas; Golhen, Stephane; Robin-Le Guen, Françoise; Caro, Bertrand; New J. Chem. 40 (2016) 5666–; doi:10.1039/C5NJ03257A

data_7055451
_publ_section_title
;
 The synthesis of flexible tetrapyridylethanes from pyridylpyrylium
 dications
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              5666
_journal_paper_doi               10.1039/C5NJ03257A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_sum            'C58 H42 N4'
_chemical_formula_weight         794.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-15 deposited with the CCDC.
2016-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 76.691(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9142(17)
_cell_length_b                   13.574(2)
_cell_length_c                   14.539(2)
_cell_measurement_reflns_used    3880
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1
_cell_volume                     2096.1(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-97 (Altomare al, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1898
_diffrn_reflns_av_unetI/netI     0.2232
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7210
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.258
_diffrn_reflns_theta_min         5.194
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.018
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.2867
_refine_ls_R_factor_gt           0.0919
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1344P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2180
_refine_ls_wR_factor_ref         0.3083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1096
_reflns_number_total             3743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03257a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7055451.cif.'
_cod_database_code               7055451
_shelxl_version_number           2013-4
_shelx_res_checksum              94001