Gram-scale synthesis of two-dimensional polymer crystals and their structure analysis by X-ray diffraction
Max J. Kory; Michael Worle; Thomas Weber; Payam Payamyar; Stan W. van de Poll; Julia Dshemuchadse; Nils Trapp; Dieter Schluter; Nature Chemistry 6 (2014) 779–784; doi:10.1038/nchem.2007

data_1551377
_publ_section_title
;
 Gram-scale synthesis of two-dimensional polymer crystals and their
 structure analysis by X-ray diffraction
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              779
_journal_page_last               784
_journal_paper_doi               10.1038/nchem.2007
_journal_volume                  6
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_sum            'C168 H88 N26 O18'
_chemical_formula_weight         2758.64
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   19.4393(5)
_cell_length_b                   19.4393(5)
_cell_length_c                   28.547(2)
_cell_measurement_reflns_used    4207
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      29.4655
_cell_measurement_theta_min      4.1849
_cell_volume                     9342.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector_area_resol_mean 8.1188
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            24699
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         4.19
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             4266
_exptl_crystal_preparation
;
irradiated for 48 h with a bluie LED tempered 
for 72 h at 60 deg. C and 120 deg. C for 12 h, followed by an 
irradiation for 10 h and tempering at
140 deg. C for 4 h and an irradiation for 4h, 
finally depolymerized at 180 deg C for three days 
;
_exptl_crystal_recrystallization_method 'crystallized from o-cyanopyridine'
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9295
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.2333
_refine_ls_R_factor_gt           0.1195
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3079
_refine_ls_wR_factor_ref         0.3914
_reflns_number_gt                3908
_reflns_number_total             9295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2007-s6.cif
_cod_data_source_block           5
_cod_original_cell_volume        9342.1(8)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               1551377