Alternative separation strategy for o-/p-dichlorobenzene mixtures through supramolecular chemistry protocols
Barnardo, Brandon; Barton, Benita; Hosten, Eric C.; CrystEngComm 26 (2024) 4876–4885; doi:10.1039/D4CE00684D

data_7249209
_publ_section_title
;
 Alternative separation strategy for o-/p-dichlorobenzene mixtures through
 supramolecular chemistry protocols
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              4876
_journal_page_last               4885
_journal_paper_doi               10.1039/D4CE00684D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C42 H36 N2 O2, 1.5(C6 H4 Cl2)'
_chemical_formula_sum            'C51 H42 Cl3 N2 O2'
_chemical_formula_weight         821.21
_chemical_name_common
N,N-bis(9-phenyl-9H-xanthen-9-yl)butane-1,4-diamine
_chemical_temperature_decomposition 329.75
_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-2019/3
_audit_update_record
;
2024-08-02 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                85.3830(15)
_cell_angle_beta                 83.1590(16)
_cell_angle_gamma                77.5052(14)
_cell_formula_units_Z            2
_cell_length_a                   8.8318(4)
_cell_length_b                   14.6939(6)
_cell_length_c                   16.5191(7)
_cell_measurement_reflns_used    9480
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.50
_cell_volume                     2074.75(15)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service V6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material
'PLATON (Spek, 2009) and MERCURY (Macrae, 2008)'
_computing_structure_refinement
'SHELXL-2019/2 (Sheldrick, 2015b)  and ShelXle (H\"ubschle, 2011)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'Bruker PHOTON II 7 detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0274
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            170208
_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         28.295
_diffrn_reflns_theta_min         1.941
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             70
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9153
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2016/2 (Krause, 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.355
_exptl_crystal_size_min          0.328
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0102(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         10290
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0646P)^2^+1.7610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7352
_reflns_number_total             10290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00684d2.cif
_cod_data_source_block           bq057
_cod_depositor_comments          'Adding full bibliography for 7249209.cif.'
_cod_original_cell_volume        2074.76(15)
_cod_database_code               7249209
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.918
_shelx_res_checksum              73697