Thermal deprotonation and condensation of melamine in the presence of indium(III)chloride.
Bayat, Elaheh; Ströbele, Markus; Enseling, David; Jüstel, Thomas; Meyer, H-Jürgen; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10912–10918; doi:10.1039/d4dt01029a

data_7716387
_publ_section_title
;
 Thermal deprotonation and condensation of melamine in the presence of
 indium(III)chloride.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10912
_journal_page_last               10918
_journal_paper_doi               10.1039/d4dt01029a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'3(C12 H8 Cl6 In3 N20), 2(Cl3 H3 In N), 9(H4 N)'
_chemical_formula_sum            'C36 H66 Cl24 In11 N71'
_chemical_formula_weight         3607.41
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-15
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-02-15 deposited with the CCDC.	2024-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.1902(2)
_cell_length_b                   28.1902(2)
_cell_length_c                   28.1902(2)
_cell_measurement_reflns_used    6847
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      75.4330
_cell_measurement_theta_min      3.8160
_cell_volume                     22402.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -37.00  27.00   0.50   11.00    --   42.44 -20.00 -65.00  128
  2  \w    105.00 178.00   0.50   50.00    --  110.13 105.00-126.00  146
  3  \w   -115.00 -63.00   0.50   11.00    --  -42.44-140.00-180.00  104
  4  \w    -51.00 -20.00   0.50   50.00    --  -96.00  45.00  60.00   62
  5  \w    -51.00 -20.00   0.50   50.00    --  -96.00  45.00 -30.00   62
  6  \w    -51.00 -20.00   0.50   50.00    --  -96.00  45.00  90.00   62
  7  \w    -86.00 -24.00   0.50   50.00    --  -96.00 125.00  30.00  124
  8  \w     37.00  71.00   0.50   50.00    --  110.13 -61.00 -90.00   68
  9  \w   -115.00 -19.00   0.50   11.00    --  -42.44 -57.00-120.00  192
 10  \w   -120.00 -19.00   0.50   11.00    --  -42.44 -37.00 -30.00  202
 11  \w   -175.00-124.00   0.50   50.00    --  -96.00 -30.00   0.00  102
 12  \w    -71.00 -22.00   0.50   50.00    --  -96.00  61.00 -90.00   98
 13  \w   -175.00 -72.00   0.50   50.00    --  -96.00 -30.00 120.00  206
 14  \w    -51.00 -20.00   0.50   50.00    --  -96.00  45.00-150.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0137152000
_diffrn_orient_matrix_UB_12      0.0527439000
_diffrn_orient_matrix_UB_13      0.0040659000
_diffrn_orient_matrix_UB_21      0.0042582000
_diffrn_orient_matrix_UB_22      0.0031273000
_diffrn_orient_matrix_UB_23      -0.0544021000
_diffrn_orient_matrix_UB_31      -0.0527182000
_diffrn_orient_matrix_UB_32      0.0139632000
_diffrn_orient_matrix_UB_33      -0.0033556000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            51919
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.155
_diffrn_reflns_theta_min         3.841
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.580
_exptl_absorpt_correction_T_max  0.664
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_description       block
_exptl_crystal_F_000             13808
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.001(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3414
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0553P)^2^+88.7518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3309
_reflns_number_total             3414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01029a2.cif
_cod_data_source_block           ebinring
_cod_depositor_comments          'Adding full bibliography for 7716387.cif.'
_cod_original_cell_volume        22402.4(5)
_cod_database_code               7716387
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C36 H54 Cl24 In11 N69'
_shelx_estimated_absorpt_t_max   0.650
_shelx_estimated_absorpt_t_min   0.385
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.001(13)
 -0.001(13)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All N(H,H,H) groups, All N(H,H,H,H) groups
3. Restrained distances
 N12-H12B
 0.95 with sigma of 0.02
 H12B-H11D
 3.5 with sigma of 0.02
 H12B-H11A
 3.5 with sigma of 0.02
 H12B-H11C
 4 with sigma of 0.02
 H12C-N12
 0.95 with sigma of 0.02
 H12B-H11B
 4 with sigma of 0.02
 N11-H11D
 0.99 with sigma of 0.02
 H12C-H12D
 1.49 with sigma of 0.02
 N12-H12D
 0.95 with sigma of 0.02
 N11-H11C
 0.99 with sigma of 0.02
 H12B-H12D
 1.49 with sigma of 0.02
 H12D-H12C
 1.62 with sigma of 0.002
 H12C-H12B
 1.62 with sigma of 0.002
 H12D-H12B
 1.62 with sigma of 0.002
 H12A-N12
 0.95 with sigma of 0.002
 H12D-H12A
 1.62 with sigma of 0.002
 N11-H11A
 0.99 with sigma of 0.02
 H12A-H12B
 1.62 with sigma of 0.02
 N11-H11B
 0.99 with sigma of 0.02
 H12C-H12A
 1.62 with sigma of 0.002
 H11B-H11C
 1.62 with sigma of 0.02
 H11B-H11D
 1.62 with sigma of 0.02
 H11D-H11A
 1.62 with sigma of 0.02
 H11A-H11D
 1.62 with sigma of 0.002
 H11C-H11A
 1.62 with sigma of 0.002
 H11C-H11D
 1.62 with sigma of 0.002
 H11B-H11A
 1.62 with sigma of 0.002
 H11A-H12D
 2.1 with sigma of 0.02
 H11D-H12A
 2.1 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N11) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.001
Uanis(N12) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Others
 Fixed Sof: Cl5(0.5) Cl6(0.5) N14(0.16667) H14A(0.16667) H14B(0.16667)
 H14C(0.16667) N13(0.16667) H13A(0.16667) H13C(0.16667) H13B(0.16667) N12(0.5)
 H12C(0.5) H12B(0.5) H12D(0.5) H12A(0.5)
6.a X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N10(H10A,H10B)
6.b Idealised Me refined as rotating group:
 N14(H14A,H14B,H14C), N13(H13A,H13C,H13B)
;
_shelx_res_checksum              396
_shelx_hkl_checksum              25692
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.770
_oxdiff_exptl_absorpt_empirical_full_min 0.133