Nuclearity control in calix[4]arene based zinc (II) coordination complexes
KNIAZEVA, Mariia; Ovsyannikov, Alexander; Islamov, Daut; Samigullina, Aida I.; Gubaidullin, Aidar Timergalievich; Dorovatovskii, Pavel; Solovieva, Svetlana; Igor, Antipin S.; Ferlay, Sylvie; CrystEngComm  (2020) –; doi:10.1039/D0CE01232G

data_7241332
_publ_section_title
;
 Nuclearity control in calix[4]arene based zinc (II) coordination
 complexes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01232G
_journal_year                    2020
_chemical_formula_moiety         'C90 H92 N2 O23 S4 Zn3, 4(C3 H7 N O)'
_chemical_formula_sum            'C102 H120 N6 O27 S4 Zn3'
_chemical_formula_weight         2186.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-07-14 deposited with the CCDC.	2020-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.971(5)
_cell_length_b                   23.006(5)
_cell_length_c                   35.506(7)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.5
_cell_volume                     22031(8)
_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(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79312
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            179407
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        28.416
_diffrn_reflns_theta_max         30.975
_diffrn_reflns_theta_min         1.447
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       prism
_exptl_crystal_F_000             9152
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.500
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00093(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1317
_refine_ls_number_reflns         25092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0625
_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^)+(0.1159P)^2^+5.8736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.1947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16513
_reflns_number_total             25092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01232g1.cif
_cod_data_source_block           1
_cod_database_code               7241332
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2. Others
 Sof(H92)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(O27)=1-FVAR(1)
 Sof(H92A)=Sof(H92B)=Sof(H92C)=Sof(H101)=Sof(O28)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C66(H66A,H66B), C67(H67A,H67B), C70(H70A,H70B), C82(H82A,
 H82B), C86(H86A,H86B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C19(H19), C24(H24), C25(H25), C27(H27),
 C29(H29), C31(H31), C32(H32), C37(H37), C40(H40), C43(H43), C45(H45), C47(H47),
  C49(H49), C51(H51), C55(H55), C56(H56), C57(H57), C59(H59), C61(H61),
 C64(H64), C69(H69), C72(H72), C73(H73), C76(H76), C79(H79), C84(H84), C85(H85),
  C92(H92), C94(H94), C100(H100), C101(H101)
3.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C58(H58A,H58B,
 H58C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C71(H71A,H71B,H71C), C74(H74A,
 H74B,H74C), C77(H77A,H77B,H77C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C),
 C83(H83A,H83B,H83C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C), C90(H90A,H90B,
 H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C95(H95A,
 H95B,H95C), C96(H96A,H96B,H96C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C),
 C99(H99A,H99B,H99C), C101(H10D,H10E,H10F), C102(H10A,H10B,H10C)
3.d Idealised tetrahedral OH refined as rotating group:
 O17(H17), O23(H23)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              238
_shelx_fab_checksum              35360
_olex2_submission_special_instructions 'No special instructions were received'