Impact of flexible succinate connectors on the formation of tetrasulfonylcalix[4]arene based nano-sized polynuclear cages: structural diversity and induced chirality study
Kniazeva, Mariia V.; Ovsyannikov, Alexander S.; Samigullina, Aida I.; Islamov, Daut R.; Gubaidullin, Aidar T.; Dorovatovskii, Pavel V.; Lazarenko, Vladimir A.; Solovieva, Svetlana E.; Antipin, Igor S.; Ferlay, Sylvie; CrystEngComm 24 (2022) 628–638; doi:10.1039/D1CE01482J

data_7244096
_publ_section_title
;
 Impact of flexible succinate connectors on the formation of
 tetrasulfonylcalix[4]arene based nano-sized polynuclear cages: structural
 diversity and induced chirality study
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              628
_journal_page_last               638
_journal_paper_doi               10.1039/D1CE01482J
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C100 H124 N4 O38 S8 Zn6, 10(C3 H7 N O)'
_chemical_formula_sum            'C130 H194 N14 O48 S8 Zn6'
_chemical_formula_weight         3369.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2911t7
_audit_creation_date             2021-10-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-10-17 deposited with the CCDC.	2021-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.887(6)
_cell_length_b                   23.216(5)
_cell_length_c                   23.261(5)
_cell_measurement_reflns_used    10103
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      28.141
_cell_measurement_theta_min      1.211
_cell_volume                     17220(6)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7931
_diffrn_reflns_av_R_equivalents  0.1427
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            105374
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        28.141
_diffrn_reflns_theta_max         28.141
_diffrn_reflns_theta_min         1.211
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsh, 2010)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       plate
_exptl_crystal_F_000             7056
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         14774
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0713
_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^)+(0.1291P)^2^+14.7811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.2170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9717
_reflns_number_total             14774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01482j2.cif
_cod_data_source_block           kmv270drombfin
_cod_depositor_comments
'Adding full bibliography for 7244095--7244098.cif.'
_cod_database_code               7244096
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.936
_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. Restrained distances
 C0AA-C41 \\sim C41-C44
 with sigma of 0.02
 C44-C41 \\sim C41-C9
 with sigma of 0.02
 C9-C41 \\sim C41-C42
 with sigma of 0.02
 C42-C41 \\sim C41-C2
 with sigma of 0.02
 C2-C41 \\sim C41-C43
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O77) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(N77) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C79) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.1
Uanis(C1A) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(N71) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(O71)
\\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C43) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O62) = Uanis(C62)
Uanis(C65) = Uanis(O65)
4. Others
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=1-FVAR(1)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
5.a Free rotating group:
 O3(C17,N4,C1A,C1B)
5.b Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C57(H57A,H57B)
5.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C14(H14), C4(H4), C12(H12), C6(H6), C22(H22), C28(H28), C20(H20),
 C62(H62), C65(H65), C74(H74), C68(H68), C77(H77), C17(H17), C71(H71)
5.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C46(H46A,H46B,H46C), C34(H34A,H34B,H34C), C70(H70A,H70B,H70C), C48(H48A,
 H48B,H48C), C39(H39A,H39B,H39C), C47(H47A,H47B,H47C), C66(H66A,H66B,H66C),
 C69(H69A,H69B,H69C), C64(H64A,H64B,H64C), C75(H75A,H75B,H75C), C78(H78A,H78B,
 H78C), C67(H67A,H67B,H67C), C63(H63A,H63B,H63C), C76(H76A,H76B,H76C), C79(H79A,
 H79B,H79C), C44(H44A,H44B,H44C), C43(H43A,H43B,H43C), C2(H2A,H2B,H2C),
 C0AA(H0AA,H0AB,H0AC), C9(H9A,H9B,H9C), C42(H42A,H42B,H42C), C1A(H1AA,H1AB,
 H1AC), C1B(H1BA,H1BB,H1BC), C73(H73A,H73B,H73C), C72(H72A,H72B,H72C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49139
_shelx_hkl_checksum              8971
_shelx_fab_checksum              7242
_olex2_submission_special_instructions 'No special instructions were received'