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_7247539
_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         '2(C44 H40 N2), 3(C6 H7 N)'
_chemical_formula_sum            'C106 H101 N7'
_chemical_formula_weight         1472.93
_chemical_melting_point          341.35
_chemical_name_systematic
;
N,N'-Bis(5-phenyl-10,11-dihydro-5-dibenzo[a,d]cycloheptenyl)ethylenediamine
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 114.066(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   9.0013(3)
_cell_length_b                   26.7346(9)
_cell_length_c                   9.0416(3)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.48
_cell_volume                     1986.70(12)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0244
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            47566
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_min         2.478
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9478
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelets
_exptl_crystal_F_000             786
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 40methylpyridine'
_exptl_crystal_size_max          0.983
_exptl_crystal_size_mid          0.783
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4910
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0595P)^2^+0.9761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3894
_reflns_number_total             4910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00811h2.cif
_cod_data_source_block           ma222
_cod_depositor_comments
'Adding full bibliography for 7247536--7247540.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7247539
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              37725