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_2108435
_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         'C N S, C6 H10 N11, C3 H6 N6'
_chemical_formula_sum            'C10 H16 N18 S'
_chemical_formula_weight         420.47
_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   geom
_audit_creation_date             2016-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                64.634(4)
_cell_angle_beta                 78.716(5)
_cell_angle_gamma                87.703(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8299(11)
_cell_length_b                   9.8507(11)
_cell_length_c                   10.2105(12)
_cell_measurement_reflns_used    1147
_cell_measurement_temperature    15(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      2.2
_cell_volume                     875.04(18)
_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      15.0
_diffrn_measured_fraction_theta_full 0.854
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       phi-scan
_diffrn_radiation_wavelength     0.4428
_diffrn_reflns_av_R_equivalents  0.1358
_diffrn_reflns_av_unetI/netI     0.1574
_diffrn_reflns_Laue_measured_fraction_full 0.854
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17124
_diffrn_reflns_point_group_measured_fraction_full 0.854
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        15.407
_diffrn_reflns_theta_max         21.654
_diffrn_reflns_theta_min         1.894
_exptl_absorpt_coefficient_mu    0.076
_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_density_diffrn    1.596
_exptl_crystal_description       irregular
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   1.0
_exptl_transmission_factor_min   0.89
_refine_diff_density_max         1.451
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         7199
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1615
_refine_ls_R_factor_gt           0.0805
_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^)+(0.1212P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2335
_refine_ls_wR_factor_ref         0.2648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3650
_reflns_number_total             7199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            px5012sup1.cif
_cod_data_source_block           2
_cod_database_code               2108435
_cod_database_fobs_code          2108435
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N15) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. 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
4.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N8(H8)
4.b X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N11(H11A,H11B), N10(H10A,H10B), N1(H1A,H1B), N17(H17A,H17B),
 N12(H12A,H12B), N14(H14A,H14B)
;
_shelx_shelxl_version_number     2014/7