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_2108438
_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         'H2 O, C N S, C3 H6 N6, C3 H7 N6'
_chemical_formula_sum            'C7 H15 N13 O S'
_chemical_formula_weight         329.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                63.474(6)
_cell_angle_beta                 71.339(7)
_cell_angle_gamma                63.549(6)
_cell_formula_units_Z            4
_cell_length_a                   11.1348(9)
_cell_length_b                   12.1287(11)
_cell_length_c                   13.1868(12)
_cell_measurement_reflns_used    2499
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      56.16
_cell_measurement_theta_min      3.79
_cell_volume                     1410.2(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.699
_diffrn_measured_fraction_theta_max 0.699
_diffrn_measurement_device_type  'Bruker Apex2 CCD diffractometer'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.699
_diffrn_reflns_Laue_measured_fraction_max 0.699
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4143
_diffrn_reflns_point_group_measured_fraction_full 0.699
_diffrn_reflns_point_group_measured_fraction_max 0.699
_diffrn_reflns_theta_full        51.544
_diffrn_reflns_theta_max         51.544
_diffrn_reflns_theta_min         3.790
_exptl_absorpt_coefficient_mu    2.315
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.886731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2004/1 (Bruker,2004) was used for absorption correction. R(int) was 0.0321 before and 0.0251 after correction. The Ratio of minimum to maximum transmission is 0.8867. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       irregular
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         2169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0736
_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^)+(0.1590P)^2^+1.9008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2152
_refine_ls_wR_factor_ref         0.2293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1753
_reflns_number_total             2169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            px5012sup1.cif
_cod_data_source_block           10
_cod_database_code               2108438
_cod_database_fobs_code          2108438
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(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.a Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 N23(H23), N33(H33)
3.c X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B), N14(H14A,H14B), N15(H15A,H15B),
 N16(H16A,H16B), N24(H24A,H24B), N25(H25A,H25B), N26(H26A,H26B), N34(H34A,H34B),
  N35(H35A,H35B), N36(H36A,H36B)
;
_olex2_submission_special_instructions 'No special instructions were received'