Metal-induced different structures of four cyclopentanocucurbit[5]uril-based complexes
Zheng, Jun; Meng, Ye; Zhang, Lin; Yang, Xinan; Ma, Peihua; Inorganica Chimica Acta 529 (2022) 120669–; doi:10.1016/j.ica.2021.120669

data_1566028
_publ_section_title
;
 Metal-induced different structures of four
 cyclopentanocucurbit[5]uril-based complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120669
_journal_paper_doi               10.1016/j.ica.2021.120669
_journal_volume                  529
_journal_year                    2022
_chemical_formula_moiety         'C90 H106 N40 O24 Pb4, Cl, 7(Cl O4), 3(H2 O)'
_chemical_formula_sum            'C90 H112 Cl8 N40 O55 Pb4'
_chemical_formula_weight         3746.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 102.518(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.305(4)
_cell_length_b                   14.774(2)
_cell_length_c                   33.700(5)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.973
_cell_measurement_theta_min      2.224
_cell_volume                     13272(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1827
_diffrn_reflns_av_unetI/netI     0.1287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            203022
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.576
_diffrn_source_current           35.0
_diffrn_source_power             1.4
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    5.326
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4111
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       block
_exptl_crystal_F_000             7344
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.214
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1985
_refine_ls_number_reflns         23383
_refine_ls_number_restraints     849
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0803
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1231P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1947
_refine_ls_wR_factor_ref         0.2213
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12504
_reflns_number_total             23383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2022-529-120669.cif
_cod_data_source_block           p_sq
_cod_original_cell_volume        13272(4)
_cod_database_code               1566028
_shelx_estimated_absorpt_t_max   0.416
_shelx_estimated_absorpt_t_min   0.361
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Cl2-O24 = Cl2-O22 = Cl2-O23 = Cl2-O21
 1.35 with sigma of 0.02
 O43-O44 \\sim O43-O45 \\sim O44-O45
 with sigma of 0.02
 Cl5-O39 \\sim Cl5-O41 \\sim Cl5-O40 \\sim Cl5-O38
 with sigma of 0.01
 Cl2-O22 \\sim Cl2-O23 \\sim Cl2-O24 \\sim Cl2-O21
 with sigma of 0.01
 Cl6-O39 \\sim Cl6-O41 \\sim Cl6-O40 \\sim Cl6-O42
 with sigma of 0.01
 O22-O23 \\sim O22-O21 \\sim O22-O24 \\sim O23-O21 \\sim O23-O24 \\sim O21-O24
 with sigma of 0.01
 O39-O41 \\sim O39-O40 \\sim O41-O40 \\sim O41-O38 \\sim O40-O38 \\sim O39-O38
 with sigma of 0.01
 O39-O41 \\sim O39-O40 \\sim O41-O40 \\sim O41-O42 \\sim O40-O42 \\sim O39-O42
 with sigma of 0.01
 Cl1-O22 \\sim Cl1-O23 \\sim Cl1-O21 \\sim Cl1-O25
 with sigma of 0.01
 O22-O23 \\sim O22-O21 \\sim O23-O21 \\sim O22-O25 \\sim O23-O25 \\sim O21-O25
 with sigma of 0.01
 O37-O36 \\sim O37-O35 \\sim O36-O35 \\sim O37-O34 \\sim O35-O34 \\sim O36-O34
 with sigma of 0.01
 Cl4-O37 \\sim Cl4-O36 \\sim Cl4-O35 \\sim Cl4-O34
 with sigma of 0.01
 Cl9-O30 \\sim Cl9-O27 \\sim Cl9-O32 \\sim Cl9-O29
 with sigma of 0.01
 O33-O26 \\sim O33-O28 \\sim O33-O31 \\sim O26-O28 \\sim O26-O31 \\sim O28-O31
 with sigma of 0.01
 O30-O27 \\sim O30-O32 \\sim O30-O29 \\sim O27-O32 \\sim O27-O29 \\sim O32-O29
 with sigma of 0.01
 Cl12-O63 \\sim Cl12-O60 \\sim Cl12-O57 \\sim Cl12-O59
 with sigma of 0.01
 Cl9-O33 \\sim Cl9-O26 \\sim Cl9-O28 \\sim Cl9-O31
 with sigma of 0.01
 O63-O60 \\sim O63-O57 \\sim O60-O59 \\sim O57-O59 \\sim O59-O63 \\sim O57-O60
 with sigma of 0.01
 Cl12-O58 \\sim Cl12-O56 \\sim Cl12-O61 \\sim Cl12-O62
 with sigma of 0.01
 O58-O56 \\sim O58-O61 \\sim O58-O62 \\sim O62-O61 \\sim O62-O56 \\sim O61-O56
 with sigma of 0.01
 Cl11-O50 \\sim Cl11-O54 \\sim Cl11-O49 \\sim Cl11-O52
 with sigma of 0.01
 O50-O54 \\sim O50-O49 \\sim O54-O49 \\sim O54-O52 \\sim O49-O52
 with sigma of 0.01
 Cl10-O48 \\sim Cl10-O53 \\sim Cl10-O55 \\sim Cl10-O51
 with sigma of 0.01
 O48-O53 \\sim O48-O55 \\sim O48-O51 \\sim O53-O55 \\sim O53-O51 \\sim O55-O51
 with sigma of 0.02
 O43-O44 \\sim O44-O45
 with sigma of 0.02
 Cl8-O43 \\sim Cl8-O44 \\sim Cl8-O45 \\sim Cl8-O47
 with sigma of 0.01
 Cl7-O43 \\sim Cl7-O44 \\sim Cl7-O45 \\sim Cl7-O46
 with sigma of 0.01
 O47-O43 \\sim O47-O45 \\sim O47-O44 \\sim O43-O45 \\sim O43-O44 \\sim O45-O44
 with sigma of 0.01
 O46-O43 \\sim O46-O45 \\sim O46-O44 \\sim O43-O45 \\sim O43-O44 \\sim O45-O44
 with sigma of 0.01
 C84-C94 \\sim C86-C94 \\sim C85-C86 \\sim C85-C84
 with sigma of 0.02
 C91-C39 \\sim C91-C41 \\sim C40-C41 \\sim C40-C39
 with sigma of 0.02
 C93-C12 \\sim C93-C14 \\sim C13-C12 \\sim C13-C14
 with sigma of 0.02
 C92-C30 \\sim C31-C30 \\sim C31-C32 \\sim C92-C32
 with sigma of 0.02
3. Rigid bond restraints
 O39, O40, O41, Cl5, O38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O39, O40, O41, Cl6, O42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O21, O22, O23, Cl1, O25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl4, O34, O35, O36, O37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O21, O22, O23, Cl2, O24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O21, O22, O23, Cl2, O24, Cl1, O25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl11, O49, O50, O52, O54
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl9, O26, O28, O31, O33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O39 \\sim O40 \\sim O41 \\sim Cl5 \\sim O38: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O39 \\sim O40 \\sim O41 \\sim Cl6 \\sim O42: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Cl4 \\sim O34 \\sim O35 \\sim O36 \\sim O37: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Cl9 \\sim O27 \\sim O29 \\sim O30 \\sim O32 \\sim O26 \\sim O28 \\sim O31 \\sim
O33: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Cl12 \\sim O57 \\sim O59 \\sim O60 \\sim O63 \\sim O56 \\sim O58 \\sim O61
\\sim O62: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C11 \\sim C12 \\sim C14 \\sim C15 \\sim C13 \\sim C93: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(O24) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl2)
\\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O59) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O48) \\sim Ueq, Uanis(O55) \\sim Ueq, Uanis(O53) \\sim Ueq, Uanis(O51)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O61) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C94) \\sim Ueq, Uanis(C85) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O5W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl11) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C93) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl3) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C31) \\sim Ueq, Uanis(C92) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(H12C)=Sof(H12D)=Sof(H14C)=Sof(H14D)=Sof(H30C)=Sof(H30D)=Sof(H32C)=
 Sof(H32D)=Sof(H39C)=Sof(H39D)=Sof(H41C)=Sof(H41D)=Sof(H84C)=Sof(H84D)=
 Sof(H86C)=Sof(H86D)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(C92)=Sof(H92A)=Sof(H92B)=
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(O56)=Sof(O58)=
 Sof(O61)=Sof(O62)=Sof(Cl1)=Sof(O25)=Sof(Cl5)=Sof(O38)=Sof(Cl8)=Sof(O47)=
 Sof(Cl10)=Sof(O48)=Sof(O51)=Sof(O53)=Sof(O55)=1-FVAR(1)
 Sof(H12A)=Sof(H12B)=Sof(H14A)=Sof(H14B)=Sof(H30A)=Sof(H30B)=Sof(H32A)=
 Sof(H32B)=Sof(H39A)=Sof(H39B)=Sof(H41A)=Sof(H41B)=Sof(H84A)=Sof(H84B)=
 Sof(H86A)=Sof(H86B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C31)=Sof(H31A)=Sof(H31B)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(O57)=Sof(O59)=
 Sof(O60)=Sof(O63)=Sof(Cl2)=Sof(O24)=Sof(Cl6)=Sof(O42)=Sof(Cl7)=Sof(O46)=
 Sof(Cl11)=Sof(O49)=Sof(O50)=Sof(O52)=Sof(O54)=FVAR(1)
 Sof(O26)=Sof(O28)=Sof(O31)=Sof(O33)=1-FVAR(2)
 Sof(O27)=Sof(O29)=Sof(O30)=Sof(O32)=FVAR(2)
6.a Riding coordinates:
 O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
6.b Rotating group:
 O6W(H6WA,H6WB), O7W(H7WA,H7WB)
6.c Secondary CH2 refined with riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C8(H8A,
 H8B), C9(H9A,H9B), C12(H12C,H12D), C12(H12A,H12B), C14(H14C,H14D), C14(H14A,
 H14B), C17(H17A,H17B), C18(H18A,H18B), C21(H21A,H21B), C22(H22A,H22B),
 C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B), C30(H30C,H30D), C30(H30A,H30B),
  C32(H32C,H32D), C32(H32A,H32B), C35(H35A,H35B), C36(H36A,H36B), C39(H39C,
 H39D), C39(H39A,H39B), C41(H41C,H41D), C41(H41A,H41B), C44(H44A,H44B),
 C45(H45A,H45B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C53(H53A,H53B),
  C54(H54A,H54B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C62(H62A,
 H62B), C63(H63A,H63B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B),
 C71(H71A,H71B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C80(H80A,H80B),
  C81(H81A,H81B), C84(H84C,H84D), C84(H84A,H84B), C86(H86C,H86D), C86(H86A,
 H86B), C89(H89A,H89B), C13(H13A,H13B), C31(H31A,H31B), C40(H40A,H40B),
 C85(H85A,H85B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B)
6.d Aromatic/amide H refined with riding coordinates:
 C72(H72), C90(H90)
;