Halogen-bonded architectures of multivalent calix[4]arenes
Gullo, Maria Chiara; Marchiò, Luciano; Casnati, Alessandro; Baldini, Laura; CrystEngComm  (2022) –; doi:10.1039/D2CE00193D

data_7244901
_publ_section_title
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 Halogen-bonded architectures of multivalent calix[4]arenes
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00193D
_journal_year                    2022
_chemical_formula_moiety         'C40 H28 I4 O4'
_chemical_formula_sum            'C40 H28 I4 O4'
_chemical_formula_weight         1080.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
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2022-01-20 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 98.548(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8824(8)
_cell_length_b                   19.0447(11)
_cell_length_c                   15.1918(11)
_cell_measurement_reflns_used    1262
_cell_measurement_temperature    200
_cell_measurement_theta_max      43.709
_cell_measurement_theta_min      4.178
_cell_volume                     3685.8(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker D8 venture PhotonII area detector'
_diffrn_measurement_method       'omega and theta scans'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.1719
_diffrn_reflns_Laue_measured_fraction_full 0.919
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2999
_diffrn_reflns_point_group_measured_fraction_full 0.919
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        66.580
_diffrn_reflns_theta_max         66.580
_diffrn_reflns_theta_min         4.175
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    26.874
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 42251 reflections, Rint = 0.2163
 (8267 with I > 3sig(I), Rint = 0.1373)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2999
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1554
_refine_ls_R_factor_gt           0.0990
_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^)+(0.0789P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2093
_refine_ls_wR_factor_ref         0.2351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1541
_reflns_number_total             2999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00193d2.cif
_cod_data_source_block           cu_aro12_0m_4
_cod_database_code               7244901
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.347
_shelx_estimated_absorpt_t_min   0.196
_olex2_refinement_description
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1. Restrained distances
 C17-C16
 1.35 with sigma of 0.02
 C18-C17 = C21-C20
 1.18 with sigma of 0.02
 C17-C16 = C20-C19
 1.46 with sigma of 0.02
 O2-C19 = O1-C16
 1.43 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C10 \\sim C8 \\sim C9 \\sim C13 \\sim C12 \\sim C11: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 1.7A
C17 \\sim C18: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C17 \\sim C18 \\sim C16: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
C19 \\sim C20 \\sim C21: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
3. Others
 Fixed Sof: H15A(0.5) H15B(0.5) H14A(0.5) H14B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C7(H7A,H7B), C15(H15A,H15B), C16(H16A,H16B), C14(H14A,H14B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C9(H9)
4.c Fitted hexagon refined as free rotating group:
 C10(C11,C12,C13,C8,C9)
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_olex2_submission_special_instructions 'No special instructions were received'