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_7241330
_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         '3(C2 H6 O S), C44 H36 O8'
_chemical_formula_sum            'C50 H54 O11 S3'
_chemical_formula_weight         927.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-06
_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                 108.93(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.713(3)
_cell_length_b                   17.962(4)
_cell_length_c                   16.109(3)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.5
_cell_volume                     4574.4(18)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_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     0.79313
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41425
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        28.417
_diffrn_reflns_theta_max         30.948
_diffrn_reflns_theta_min         1.437
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       prism
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0092(5)
_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   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         10408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0560P)^2^+2.3778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7634
_reflns_number_total             10408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01232g1.cif
_cod_data_source_block           mk2l
_cod_database_code               7241330
_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.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C23(H23A,H23B), C33(H33A,H33B), C34(H34A,H34B), C39(H39A,H39B),
 C41(H41A,H41B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C9(H9), C10(H10), C12(H12), C14(H14), C15(H15), C21(H21),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C32(H32), C35(H35), C36(H36),
  C37(H37), C43(H43), C46(H46), C47(H47)
2.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4), O8(H8), O11(H11)
;
_shelx_res_checksum              16344
_olex2_submission_special_instructions 'No special instructions were received'