The behaviour of two diamino-derived host compounds in cyclohexanone and isomeric methylcyclohexanones
Trollip, Danica B.; Barton, Benita; Caira, Mino R.; Hosten, Eric C.; CrystEngComm 27 (2025) 3279–3294; doi:10.1039/D5CE00298B

data_7250335
_publ_section_title
;
 The behaviour of two diamino-derived host compounds in cyclohexanone and
 isomeric methylcyclohexanones
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              3279
_journal_page_last               3294
_journal_paper_doi               10.1039/D5CE00298B
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C45 H38 N2, C7 H12 O'
_chemical_formula_sum            'C52 H50 N2 O'
_chemical_formula_weight         718.94
_chemical_melting_point          'onset of decomp. 385.6 K'
_chemical_name_common            none
_chemical_name_systematic
'N,N'-Bis(5-phenyl-5-dibenzo[a,d]cycloheptenyl)propane-1,3-diamine3-methylcyclohexanone clathrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-04-07 deposited with the CCDC.	2025-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                99.086(2)
_cell_angle_beta                 102.942(2)
_cell_angle_gamma                101.262(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8102(7)
_cell_length_b                   15.3893(11)
_cell_length_c                   15.4064(12)
_cell_measurement_reflns_used    5878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.50
_cell_volume                     1951.6(3)
_computing_cell_refinement
'SAINT V8.40A, Bruker AXS Inc.: Madison (WI), USA.'
_computing_data_collection       'Apex3 v2019.1-0, Bruker (2019).'
_computing_data_reduction
'SAINT V8.40A, Bruker AXS Inc.: Madison (WI), USA.'
_computing_molecular_graphics
'POV-Ray in interface X-Seed (LJ Barbour, 1999)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean n/a
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE SCXRD diffractometer'
_diffrn_measurement_method       'omega-and phi-scans, width 1.0 deg.'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1215
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            56222
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.162
_diffrn_reflns_theta_min         2.154
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       needle
_exptl_crystal_F_000             768
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 3-methylcyclohexanone'
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         8636
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0561P)^2^+0.6783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5033
_reflns_number_total             8636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00298b2.cif
_cod_data_source_block           DB32REV
_cod_depositor_comments
'Adding full bibliography for 7250335--7250339.cif.'
_cod_database_code               7250335
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              92599
_shelx_hkl_checksum              37866