Self-assembly of zirconocene-based metal‒organic capsules: the structure, luminescence sensing of Fe3+ and iodine capture
Chen, Siyuan; Cheng, Shuangjing; Zhao, Liang; Sun, Chunyi; Qin, Chao; Su, Zhongmin; New Journal of Chemistry 44 (2020) 21255–21260; doi:10.1039/D0NJ04576D

data_7060105
_publ_section_title
;
 Self-assembly of zirconocene-based metal--organic capsules: the
 structure, luminescence sensing of Fe3+ and iodine capture
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21255
_journal_page_last               21260
_journal_paper_doi               10.1039/D0NJ04576D
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C78 H66 O20 Zr6, 2(Cl), 2.5(C3 H7 N O)'
_chemical_formula_sum            'C85.5 H83.5 Cl2 N2.5 O22.5 Zr6'
_chemical_formula_weight         2124.26
_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             2020-08-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-08-21 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                67.089(3)
_cell_angle_beta                 78.072(3)
_cell_angle_gamma                77.205(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7932(8)
_cell_length_b                   23.6272(15)
_cell_length_c                   25.0116(18)
_cell_measurement_reflns_used    84261
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.953
_cell_volume                     5677.5(7)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      173.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker D8 VENTURE'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  Gromit-Mo-D8
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker D8 VENTURE'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            84261
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.097
_diffrn_reflns_theta_max         25.096
_diffrn_reflns_theta_min         2.272
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.572
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.141
_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     1096
_refine_ls_number_reflns         20012
_refine_ls_number_restraints     296
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0940P)^2^+35.9553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1836
_refine_ls_wR_factor_ref         0.2087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13317
_reflns_number_total             20012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04576d2.cif
_cod_data_source_block           Zr-MC-2
_cod_depositor_comments
'Adding full bibliography for 7060103--7060105.cif.'
_cod_original_formula_sum        'C85.50 H83.50 Cl2 N2.50 O22.50 Zr6'
_cod_database_code               7060105
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C84-N2
 1.5 with sigma of 0.01
 N5-C85 = N5-C86 = N5-C87
 1.5 with sigma of 0.01
 O23-C85
 1.2 with sigma of 0.01
 N2-C82 \\sim N2-C84 \\sim N2-C83
 with sigma of 0.02
 N4-C80 \\sim N4-C79 \\sim N4-C81
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C83 \\sim O22 \\sim C82 \\sim N2 \\sim C84: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.03 within 3.8A
N4 \\sim O21 \\sim C79 \\sim C80 \\sim C81: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.03 within 3.8A
N5 \\sim C86 \\sim C85 \\sim C87 \\sim O23: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.03 within 3.8A
Uanis(C13) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C78) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 C18, C24, C42, C46, C60, C65, C67, C68
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C9, C10, C11, C12, C13, C78
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: N5(0.5) C86(0.5) H86A(0.5) H86B(0.5) H86C(0.5) O23(0.5) C85(0.5)
 H85(0.5) C87(0.5) H87A(0.5) H87B(0.5) H87C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 O3(H3), O4(H4), O5(H5), O7(H7), O8(H8), O16(H16), C7(H7A), C10(H10), C11(H11),
  C13(H13), C14(H14), C15(H15), C16(H16A), C17(H17), C20(H20), C22(H22),
 C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
 C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49),
  C50(H50), C51(H51), C52(H52), C54(H54), C56(H56), C57(H57), 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), C73(H73),
 C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C85(H85), C82(H82)
6.b Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C86(H86A,H86B,H86C), C87(H87A,H87B,
 H87C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C)
;
_shelx_res_checksum              44036
_shelx_fab_checksum              39990
_olex2_submission_special_instructions 'No special instructions were received'