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_1566027
_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
'C45 H50 Cl2 Hg N20 O10, Cl4 Hg, 3(H2 O), 2(H4 N)'
_chemical_formula_sum            'C45 H64 Cl6 Hg2 N22 O13'
_chemical_formula_weight         1735.06
_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                 93.228(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9075(13)
_cell_length_b                   15.7904(18)
_cell_length_c                   35.312(4)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      2.27
_cell_volume                     6072.3(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1167
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            134820
_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         1.731
_exptl_absorpt_coefficient_mu    5.394
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3258
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_description       block
_exptl_crystal_F_000             3416
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.349
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         10664
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.1426
_refine_ls_R_factor_gt           0.1102
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+198.9035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2012
_refine_ls_wR_factor_ref         0.2141
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8171
_reflns_number_total             10664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2022-529-120669.cif
_cod_data_source_block           jiang3_3hg_0m_sqd_pl_sq
_cod_database_code               1566027
_shelx_estimated_absorpt_t_max   0.564
_shelx_estimated_absorpt_t_min   0.498
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O12) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C39) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
Uanis(C0AA) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C1) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.0002
Uanis(C33) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(O9) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.0002
Uanis(C23) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
Uanis(N8) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.0002
3. Rigid body (RIGU) restrains
 C39
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 Cl3
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C29
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C23
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Others
 Sof(H32C)=Sof(H32D)=Sof(H34C)=Sof(H34D)=Sof(C33)=Sof(H33A)=Sof(H33B)=1-FVAR(1)
 Sof(H32A)=Sof(H32B)=Sof(H34A)=Sof(H34B)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=FVAR(1)
5.a Riding coordinates:
 O11(H11C,H11D), N22(H22C,H22D,H22E,H22F), N21(H21A,H21B,H21C,H21D), O13(H13C,
 H13D)
5.b Free rotating group:
 O12(H12A,H12B)
5.c Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C42(H42A,H42B), C41(H41A,H41B), C1(H1A,H1B), C2(H2A,H2B),
 C6(H6A,H6B), C5(H5A,H5B), C4(H4A,H4B), C10(H10A,H10B), C11(H11A,H11B),
 C15(H15A,H15B), C14(H14A,H14B), C13(H13A,H13B), C19(H19A,H19B), C20(H20A,H20B),
  C22(H22A,H22B), C24(H24A,H24B), C28(H28A,H28B), C29(H29A,H29B), C32(H32A,
 H32B), C32(H32C,H32D), C34(H34A,H34B), C34(H34C,H34D), C38(H38A,H38B),
 C37(H37A,H37B), C0AA(H0AA,H0AB), C33(H33A,H33B), C23(H23A,H23B)
;