New core-expanded calix[4]pyrroles and N-donor-extended dipyrromethanes: syntheses, anion binding and conformational studies.
Mishra, Soumya; Giri, Monalisa; Mishra, Vipin Kumar; Guchhait, Tapas; Organic & biomolecular chemistry 24 (2026) 708–719; doi:10.1039/d5ob01716e

data_7161036
_publ_section_title
;
 New core-expanded calix[4]pyrroles and N-donor-extended dipyrromethanes:
 syntheses, anion binding and conformational studies.
;
_journal_issue                   3
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              708
_journal_page_last               719
_journal_paper_doi               10.1039/d5ob01716e
_journal_volume                  24
_journal_year                    2026
_chemical_formula_moiety         'F6 Si, C38 H44 N6'
_chemical_formula_sum            'C38 H44 F6 N6 Si'
_chemical_formula_weight         726.88
_chemical_name_systematic        'Hexafluorosilicate complex'
_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             2025-09-20
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-09-20 deposited with the CCDC.	2025-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.612(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.435(6)
_cell_length_b                   11.819(2)
_cell_length_c                   23.602(4)
_cell_measurement_reflns_used    96550
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      1.876
_cell_volume                     7645(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1020
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            96550
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         1.876
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1208 before and 0.0858 after correction.
The Ratio of minimum to maximum transmission is 0.8047.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             3056
_exptl_crystal_preparation
'Mixing receptor and H2SiF6 in ethyl acetate and methanol mixture'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         8775
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0473P)^2^+5.9313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5448
_reflns_number_total             8775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob01716e2.cif
_cod_data_source_block           smsilicate
_cod_original_cell_volume        7645(3)
_cod_database_code               7161036
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1-F4 \\sim Si1-F4A
 with sigma of 0.02
 Si1-F3 \\sim Si1-F3A
 with sigma of 0.02
 Si1-F2 \\sim Si1-F2A
 with sigma of 0.02
 Si1-F5 \\sim Si1-F5A
 with sigma of 0.02
3. Others
 Sof(F4A)=Sof(F3A)=Sof(F2A)=Sof(F5A)=1-FVAR(1)
 Sof(F4)=Sof(F3)=Sof(F2)=Sof(F5)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N3(H3), N6(H6)
4.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C17(H17A,H17B), C38(H38A,H38B), C36(H36A,H36B)
4.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N2(H2), N1(H1), N5(H5), C22(H22), C33(H33), C14(H14), C21(H21),
 C34(H34), C15(H15), C27(H27), C12(H12), C8(H8), C28(H28), C2(H2A), C3(H3A),
 C31(H31), C11(H11), C29(H29), C30(H30), C10(H10), C9(H9)
4.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C6(H6A,H6B,H6C), C37(H37A,H37B,H37C), C18(H18A,H18B,H18C)
;
_olex2_submission_original_sample_id SMSiF6
_olex2_submission_special_instructions 'No special instructions were received'