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_7241329
_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         'C108 H88 N4 O16 Zn2, 4(C5 H5 N), C5 H7 N'
_chemical_formula_sum            'C133 H115 N9 O16 Zn2'
_chemical_formula_weight         2226.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                66.56(3)
_cell_angle_beta                 67.55(3)
_cell_angle_gamma                76.46(3)
_cell_formula_units_Z            1
_cell_length_a                   14.070(3)
_cell_length_b                   14.720(3)
_cell_length_c                   15.430(3)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.7
_cell_volume                     2697.0(12)
_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 0.993
_diffrn_measured_fraction_theta_max 0.989
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            56420
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        28.417
_diffrn_reflns_theta_max         30.955
_diffrn_reflns_theta_min         1.691
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       prism
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         12169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0623P)^2^+1.4712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10727
_reflns_number_total             12169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01232g1.cif
_cod_data_source_block           mk24fin
_cod_original_cell_volume        2697.1(13)
_cod_database_code               7241329
_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 O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C72) = Uanis(C69) = Uanis(C71) = Uanis(C70) = Uanis(C68) = Uanis(N5)
Uanis(C50) = Uanis(N6)
3. Others
 Fixed Sof: N3(0.5) C50(0.5) H50(0.5) H56A(0.5) H57A(0.5) C58(0.5) H58(0.5)
 C61(0.5) H61(0.5) C62(0.5) H62(0.5) C65(0.5) H65(0.5) C67(0.5) H67(0.5)
 C68(0.5) H68(0.5) C69(0.5) H69(0.5) C70(0.5) H70(0.5) N5(0.5) C71(0.5)
 H71(0.5) C72(0.5) H72(0.5) N6(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C30(H30A,H30B), C42(H42A,H42B), C43(H43A,H43B), C46(H46A,H46B),
 C49(H49A,H49B)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21),
 C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C31(H31), C32(H32),
  C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C44(H44),
 C45(H45), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
  C55(H55), C56(H56), C56(H56A), C57(H57), C57(H57A), C58(H58), C59(H59),
 C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67),
  C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
4.c Idealised tetrahedral OH refined as rotating group:
 O4(H4), O6(H6)
;
_shelx_res_checksum              73360
_olex2_submission_special_instructions 'No special instructions were received'