Self-Exfoliated Guanidinium-Based Ionic Covalent Organic Nanosheets (iCONs).
Mitra, Shouvik; Kandambeth, Sharath; Biswal, Bishnu P.; Khayum M, Abdul; Choudhury, Chandan K.; Mehta, Mihir; Kaur, Gagandeep; Banerjee, Subhrashis; Prabhune, Asmita; Verma, Sandeep; Roy, Sudip; Kharul, Ulhas K.; Banerjee, Rahul; Journal of the American Chemical Society 138 (2016) 2823–2828; doi:10.1021/jacs.5b13533

data_4130071
_publ_section_title
;
 Self-Exfoliated Guanidinium-Based Ionic Covalent Organic Nanosheets
 (iCONs).
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2823
_journal_page_last               2828
_journal_paper_doi               10.1021/jacs.5b13533
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C H6 N6, Br'
_chemical_formula_sum            'C H6 Br N6'
_chemical_formula_weight         182.02
_chemical_name_systematic        GT-Br
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-21
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled Nov  7 2012 10:34:12, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   7.7196(5)
_cell_length_b                   7.7196(5)
_cell_length_c                   6.2784(6)
_cell_measurement_reflns_used    419
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.2370
_cell_measurement_theta_min      4.4340
_cell_volume                     324.02(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1640
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9940
_diffrn_measured_fraction_theta_max 0.8852
_diffrn_measurement_details
;
  1 omega   69.00   97.00   1.0000    5.9450
omega____ theta____ kappa____ phi______ frames
    -       19.9032  178.0000 -180.0000 28

  2 omega  -42.00   50.00   1.0000    5.9450
omega____ theta____ kappa____ phi______ frames
    -       19.9032  -77.0000  -30.0000 92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0649387000
_diffrn_orient_matrix_UB_12      0.1051419000
_diffrn_orient_matrix_UB_13      -0.0023880000
_diffrn_orient_matrix_UB_21      -0.0782185000
_diffrn_orient_matrix_UB_22      0.0144438000
_diffrn_orient_matrix_UB_23      0.0388880000
_diffrn_orient_matrix_UB_31      0.0300006000
_diffrn_orient_matrix_UB_32      -0.0027804000
_diffrn_orient_matrix_UB_33      0.1059939000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            707
_diffrn_reflns_theta_full        29.07
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.254
_exptl_absorpt_correction_T_max  0.286
_exptl_absorpt_correction_T_min  0.243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             178
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1369
_reflns_number_gt                231
_reflns_number_total             280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b13533_si_002.cif
_cod_data_source_block           TG-Br
_cod_original_cell_volume        324.02(5)
_cod_database_code               4130071
_chemical_oxdiff_formula         'C12 H14 N1 Br1'
_reflns_odcompleteness_completeness 99.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H of N3, H1 of N1
2. Others
 Fixed Sof: H(0.5)
3.a Rotating group:
 N3(H)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1)
;