Accessing the rich carbon nitride materials chemistry by heat treatments of ammonium thiocyanate, NH~4~SCN
Larsen, Finn Krebs; Hasen Mamakhel, Aref; Overgaard, Jacob; Jørgensen, Jens-Erik; Kato, Kenichi; Brummerstedt Iversen, Bo; Acta Crystallographica Section B 75 (2019) –; doi:10.1107/S2052520619005791

data_2108436
_publ_section_title
;
 Accessing the rich carbon nitride materials chemistry by heat treatments
 of ammonium thiocyanate, NH~4~SCN
;
_journal_coeditor_code           PX5012SUP1
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619005791
_journal_volume                  75
_journal_year                    2019
_chemical_formula_moiety         'C6 H9.67 N11'
_chemical_formula_sum            'C6 H9.67 N11'
_chemical_formula_weight         235.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.025(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.534(3)
_cell_length_b                   28.13(2)
_cell_length_c                   10.698(5)
_cell_measurement_reflns_used    796
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      16.1
_cell_measurement_theta_min      3.03
_cell_volume                     1055.5(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex2 CCD diffractometer'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.1299
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8793
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        16.270
_diffrn_reflns_theta_max         16.270
_diffrn_reflns_theta_min         1.142
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             491
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.077(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1107
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0641
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.2139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                759
_reflns_number_total             1107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            px5012sup1.cif
_cod_data_source_block           3
_cod_database_code               2108436
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H8(0.66666)
4.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N8(H8)
4.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N5(H5A,H5B), N7(H7A,H7B), N10(H10A,H10B)
;
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108436