Macrocycle-based charge transfer co-crystals with specific selective vapochromism to benzene
Zeng, Fei; Tang, Lin-Li; Bao, Wen-Hu; New Journal of Chemistry 48 (2024) 14480–14485; doi:10.1039/D4NJ02859G

data_7063361
_publ_section_title
;
 Macrocycle-based charge transfer co-crystals with specific selective
 vapochromism to benzene
;
_journal_issue                   32
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14480
_journal_page_last               14485
_journal_paper_doi               10.1039/D4NJ02859G
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C66 H60 O12, 3(C5 H N2), 2(C2 H3 N)'
_chemical_formula_sum            'C85 H69 N8 O12'
_chemical_formula_weight         1394.48
_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   geom
_audit_creation_date             2024-05-09
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-19 deposited with the CCDC.	2024-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                91.171(8)
_cell_angle_beta                 94.196(8)
_cell_angle_gamma                114.981(7)
_cell_formula_units_Z            2
_cell_length_a                   12.982(7)
_cell_length_b                   13.032(7)
_cell_length_c                   23.658(13)
_cell_measurement_reflns_used    4571
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.02
_cell_measurement_theta_min      2.37
_cell_volume                     3612(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.1036
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            40489
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.603
_diffrn_reflns_theta_min         0.864
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1079 before and 0.0690 after correction.
The Ratio of minimum to maximum transmission is 0.7531.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       prism
_exptl_crystal_F_000             1462
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     960
_refine_ls_number_reflns         15989
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1828
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1548P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2106
_refine_ls_wR_factor_ref         0.2844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6493
_reflns_number_total             15989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02859g2.cif
_cod_data_source_block           11_a
_cod_depositor_comments
'Adding full bibliography for 7063359--7063362.cif.'
_cod_original_cell_volume        3612(4)
_cod_database_code               7063361
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.962
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C67) \\sim Ueq, Uanis(C69) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(N2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N8) \\sim
Ueq, Uanis(C79) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C65(H65A,H65B)
3.b Aromatic/amide H refined with riding coordinates:
 C57(H57), C47(H47), C14(H14), C24(H24), C11(H11), C10(H10), C38(H38), C5(H5),
 C35(H35), C2(H2), C29(H29), C83(H83), C44(H44), C43(H43), C22(H22), C55(H55),
 C21(H21), C60(H60), C66(H66), C26(H26), C73(H73), C54(H54), C68(H68)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C41(H41A,H41B,H41C), C64(H64A,H64B,H64C), C40(H40A,H40B,
 H40C), C19(H19A,H19B,H19C), C53(H53A,H53B,H53C), C31(H31A,H31B,H31C), C20(H20A,
 H20B,H20C), C52(H52A,H52B,H52C), C32(H32A,H32B,H32C), C7(H7A,H7B,H7C),
 C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              96465
_shelx_hkl_checksum              510
_olex2_submission_special_instructions 'No special instructions were received'