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

data_7244902
_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, 2(C6 H12 N2), C4 H8 O'
_chemical_formula_sum            'C56 H60 I4 N4 O5'
_chemical_formula_weight         1376.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.9348(2)
_cell_length_b                   22.8426(4)
_cell_length_c                   39.6053(6)
_cell_measurement_reflns_used    8639
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.644
_cell_measurement_theta_min      2.378
_cell_volume                     11702.0(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            17013
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.727
_diffrn_reflns_theta_min         2.378
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    2.177
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0896 before and 0.0546 after correction.
The Ratio of minimum to maximum transmission is 0.8570.
The \l/2 correction factor is Not present.
;
_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    1.563
_exptl_crystal_description       prism
_exptl_crystal_F_000             5408
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+56.2392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2362
_reflns_number_total             2779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00193d2.cif
_cod_data_source_block           4-DABCO_aro12dabcothvac_0m
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7244902
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.682
_olex2_refinement_description
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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,H,H,H,H,H) groups
2. Others
 Fixed Sof: H8A(0.5) H8B(0.5) H7A(0.5) H7B(0.5) O2(0.25) C15(0.25) C16(0.25)
 C17(0.25) C18(0.25) H15A(0.25) H15B(0.25) H16A(0.25) H16B(0.25) H17A(0.25)
 H17B(0.25) H18A(0.25) H18B(0.25)
3.a Free rotating group:
 O2(C15,C16,C17,C18,H15A,H15B,H16A,H16B,H17A,H17B,H18A,H18B)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C9(H9A,H9B), C13(H13A,H13B), C14(H14A,H14B),
 C12(H12A,H12B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4)
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_olex2_submission_special_instructions 'No special instructions were received'