Design, synthesis, and characterization of pyridine-containing organic crystals with different substitution positions using solvothermal method
Wu, Jiasheng; Zou, Jiacheng; Zhuge, Xiangxue; Jia, Zhitai; Lin, Na; Yuan, Chunxue; CrystEngComm 23 (2021) 3152–3159; doi:10.1039/D1CE00165E

data_7242563
_publ_section_title
;
 Design, synthesis, and characterization of pyridine-containing organic
 crystals with different substitution positions using solvothermal method
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              3152
_journal_page_last               3159
_journal_paper_doi               10.1039/D1CE00165E
_journal_volume                  23
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H24 N4'
_chemical_formula_sum            'C29 H24 N4'
_chemical_formula_weight         428.52
_chemical_name_common            TBOP
_chemical_name_systematic
2,8-bis((E)-2-(pyridin-2-yl)vinyl)-6H,12H-5,11-methanodibenzo[b,f][1,5]diazocine
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-07-13 deposited with the CCDC.	2021-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.6255(10)
_cell_length_b                   6.0517(4)
_cell_length_c                   47.672(4)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      67.80
_cell_measurement_theta_min      2.78
_cell_volume                     4507.9(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            64635
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.474
_diffrn_reflns_theta_min         3.709
_exptl_absorpt_coefficient_mu    0.588
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Solvothermal Method'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   0.7531
_exptl_transmission_factor_min   0.6333
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 2699 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.5(2)
_refine_ls_extinction_coef       0.0027(4)
_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   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         8195
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0637
_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^)+(0.1312P)^2^+0.3926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1920
_reflns_Friedel_coverage         0.954
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                6568
_reflns_number_total             8195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00165e2.cif
_cod_data_source_block           ba_a
_cod_depositor_comments
'Adding full bibliography for 7242563--7242566.cif.'
_cod_original_cell_volume        4507.9(5)
_cod_database_code               7242563
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.917
_shelx_res_checksum              93312
_shelx_hkl_checksum              73449