Constructing monocrystalline covalent organic networks by polymerization
Beaudoin, Daniel; Maris, Thierry; Wuest, James D.; Nature Chemistry 5 (2013) 830–834; doi:10.1038/nchem.1730

data_1516319
_publ_section_title
;
 Constructing monocrystalline covalent organic networks by polymerization
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              830
_journal_page_last               834
_journal_paper_doi               10.1038/nchem.1730
_journal_volume                  5
_journal_year                    2013
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C25 H16 N4 O4'
_chemical_formula_sum            'C25 H16 N4 O4'
_chemical_formula_weight         436.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           117
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 -2ab'
_symmetry_space_group_name_H-M   'P -4 b 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1545(15)
_cell_length_b                   13.1545(15)
_cell_length_c                   7.9818(9)
_cell_measurement_reflns_used    2539
_cell_measurement_temperature    100
_cell_measurement_theta_max      51.40
_cell_measurement_theta_min      4.75
_cell_volume                     1381.2(3)
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection       'APEX2  (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Quazar MX'
_diffrn_radiation_source         'Incoatec I\muS Microsource '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17740
_diffrn_reflns_theta_full        70.41
_diffrn_reflns_theta_max         70.41
_diffrn_reflns_theta_min         4.75
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.9762
_exptl_absorpt_correction_T_min  0.8200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
Attempts to  model disordered solvent molecules
were unsuccessful. PLATON/SQUEEZE  was used to correct
the data for the presence of the disordered solvent.
A potential solvent volume of 504.2 \%A^3^, 
36.5 % of the total unit-cell volume, was found.
158 electrons per unit cell worth of scattering were located
in the void. The reported structure is based on the 
PLATON/SQUEEZE corrected data. The actual solvent content is
unknown, so several quantities calculated like empirical formula, density, 
absorption coefficient, F(000) etc. may be incorrect.

Ref:  Sluis, P. van der & Spek, A.L. (1990). Acta Cryst. A46, 194-201.
;
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Friedel Pairs merged'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1684P)^2^+0.2477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2344
_refine_ls_wR_factor_ref         0.2417
_reflns_number_gt                640
_reflns_number_total             751
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nchem.1730-s3.cif
_cod_data_source_block           jw1616
_cod_original_sg_symbol_H-M      P-4b2
_cod_database_code               1516319