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_7247538
_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 H36 N2, 2(C6 H7 N)'
_chemical_formula_sum            'C56 H50 N4'
_chemical_formula_weight         779.00
_chemical_melting_point          336.35
_chemical_name_systematic
;
N,N'-Bis(5-phenyl-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                108.163(3)
_cell_angle_beta                 105.764(2)
_cell_angle_gamma                104.337(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7173(6)
_cell_length_b                   11.2718(8)
_cell_length_c                   12.6826(9)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.55
_cell_volume                     1061.65(13)
_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      200(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.0221
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33628
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.375
_diffrn_reflns_theta_min         1.826
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9594
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             414
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 2-methylpyridine'
_exptl_crystal_size_max          0.780
_exptl_crystal_size_mid          0.745
_exptl_crystal_size_min          0.450
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.034(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   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5285
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0519P)^2^+0.2664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4470
_reflns_number_total             5285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00811h2.cif
_cod_data_source_block           ma049
_cod_depositor_comments
'Adding full bibliography for 7247536--7247540.cif.'
_cod_database_code               7247538
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              77694