The behaviour of tricyclic fused host systems comprising seven-membered B-rings in mixed pyridines
Barton, Benita; Caira, Mino R.; Trollip, Danica B.; Hosten, Eric C.; CrystEngComm 25 (2023) 6317–6328; doi:10.1039/D3CE00811H

data_7247537
_publ_section_title
;
 The behaviour of tricyclic fused host systems comprising seven-membered
 B-rings in mixed pyridines
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              6317
_journal_page_last               6328
_journal_paper_doi               10.1039/D3CE00811H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C44 H40 N2, 2(C5 H5 N)'
_chemical_formula_sum            'C54 H50 N4'
_chemical_formula_weight         754.98
_chemical_melting_point          349.65
_chemical_name_systematic
;
N,N'-Bis(5-phenyl-10,11-dihydro-5-dibenzo[a,d]cycloheptenyl)ethylenediamine
;
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-02-10 deposited with the CCDC.	2023-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                75.212(3)
_cell_angle_beta                 76.005(3)
_cell_angle_gamma                66.684(3)
_cell_formula_units_Z            1
_cell_length_a                   8.9716(5)
_cell_length_b                   9.2886(5)
_cell_length_c                   13.8221(8)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.43
_cell_volume                     1009.80(10)
_computing_cell_refinement       'APEX2 v2011.4-1 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2011.4.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material
'PLATON (Spek, 2009) and MERCURY (Macrae, 2008)'
_computing_structure_refinement
'SHELXL-2018/3 (Sheldrick, 2015) and ShelXle (H\"ubschle, 2011)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40261
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.360
_diffrn_reflns_theta_min         2.427
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.745684
_exptl_absorpt_correction_T_min  0.676861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS-2012/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             402
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pyridine'
_exptl_crystal_size_max          0.951
_exptl_crystal_size_mid          0.426
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         5002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0319P)^2^+0.2684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4112
_reflns_number_total             5002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00811h2.cif
_cod_data_source_block           ma171_tw
_cod_depositor_comments
'Adding full bibliography for 7247536--7247540.cif.'
_cod_database_code               7247537
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              23007