Designing Tetraoxa[8]circulenes To Serve as Hosts and Sensors
Petrov, Nino G.; Chartier, Patrick; Maris, Thierry; Wuest, James D.; Journal of the American Chemical Society 144 (2021) 556–572; doi:10.1021/jacs.1c11728

data_4135638
_publ_section_title
;
 Designing Tetraoxa[8]circulenes To Serve as Hosts and Sensors
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              556
_journal_page_last               572
_journal_paper_doi               10.1021/jacs.1c11728
_journal_volume                  144
_journal_year                    2021
_chemical_formula_moiety         'C80 H40 O4, 4(C H Cl3)'
_chemical_formula_sum            'C84 H44 Cl12 O4'
_chemical_formula_weight         1542.59
_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
_atom_sites_solution_primary     dual
_audit_contact_author_name
;
;
_audit_creation_date             2018-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                78.771(2)
_cell_angle_beta                 78.615(2)
_cell_angle_gamma                75.028(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7614(5)
_cell_length_b                   14.9731(6)
_cell_length_c                   17.3086(7)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.706
_cell_measurement_theta_min      2.292
_cell_volume                     3338.5(2)
_computing_cell_refinement
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43606
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.832
_diffrn_reflns_theta_min         2.292
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    3.327
_exptl_absorpt_correction_T_max  0.5163
_exptl_absorpt_correction_T_min  0.3840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1156 before and 0.0749 after correction. The Ratio of minimum to maximum transmission is 0.7438. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       Block
_exptl_crystal_F_000             1568
_exptl_crystal_recrystallization_method 'crystallized from CHCl3/PhNO2'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.850
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         15276
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.254
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0947
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2925
_refine_ls_wR_factor_ref         0.3206
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11067
_reflns_number_total             15276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jw20992_7_4CHCl3.cif
_cod_data_source_block           jw20992
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the built-in table derived from the CIF
Core dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_database_code               4135638
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.635
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-Cl4A \\sim C2-Cl5 \\sim C2-Cl6
 with sigma of 0.02
 C1-Cl1 \\sim C1-Cl2 \\sim C1-Cl3
 with sigma of 0.02
3. Others
 Sof(Cl4B)=1-FVAR(1)
 Sof(Cl4A)=FVAR(1)
 Sof(Cl3B)=1-FVAR(2)
 Sof(Cl3)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C7A(H7A), C7B(H7B), C7C(H7C), C7D(H7D), C8A(H8A), C8B(H8B), C8C(H8C),
 C8D(H8D), C1(H1), C2(H2), C3(H3), C4(H4)
4.b Aromatic/amide H refined with riding coordinates:
 C10B(H10B), C10D(H10D), C10A(H10A), C11C(H11C), C11B(H11B), C11D(H11D),
 C11A(H11A), C12C(H12C), C12B(H12B), C12D(H12D), C12A(H12A), C13A(H13A),
 C13B(H13B), C13D(H13D), C13C(H13C), C14C(H14C), C16A(H16A), C17B(H17B),
 C17A(H17A), C17C(H17C), C17D(H17D), C18B(H18B), C18C(H18C), C18A(H18A),
 C18D(H18D), C19A(H19A), C19C(H19C), C19B(H19B), C19D(H19D), C20C(H20C),
 C20D(H20D), C20B(H20B)
;