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_1566025
_publ_section_title
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 Metal-induced different structures of four
 cyclopentanocucurbit[5]uril-based complexes
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_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 H56 Cr N20 O13, 3(Cl)'
_chemical_formula_sum            'C45 H56 Cl3 Cr N20 O13'
_chemical_formula_weight         1243.44
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.623(3)
_cell_length_b                   20.623(3)
_cell_length_c                   31.896(6)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.21
_cell_volume                     13566(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            434912
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.892
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1259 before and 0.0789 after correction.
The Ratio of minimum to maximum transmission is 0.9482.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             5160
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 4246 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.222(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         11922
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0721
_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^)+(0.1672P)^2^+7.5423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2032
_refine_ls_wR_factor_ref         0.2159
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10611
_reflns_number_total             11922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2022-529-120669.cif
_cod_data_source_block           1_a_sq
_cod_original_cell_volume        13566(5)
_cod_database_code               1566025
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 Cl3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C42) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1AA) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C3AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 Cl3
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C42
 with sigma for 1-2 distances of 0.00001 and sigma for 1-3 distances of 0.00001
5.a Riding coordinates:
 O12W(H12A,H12B)
5.b Rotating group:
 O11W(H11A,H11B), O13W(H13A,H13B)
5.c Secondary CH2 refined with riding coordinates:
 C11(H11C,H11D), C15(H15A,H15B), C19(H19A,H19B), C20(H20A,H20B), C10(H10A,
 H10B), C29(H29A,H29B), C24(H24A,H24B), C28(H28A,H28B), C37(H37A,H37B), C6(H6A,
 H6B), C4(H4A,H4B), C41(H41A,H41B), C2(H2A,H2B), C22(H22A,H22B), C38(H38A,H38B),
  C5(H5A,H5B), C33(H33A,H33B), C31(H31A,H31B), C1(H1A,H1B), C13(H13C,H13D),
 C14(H14A,H14B), C43(H43A,H43B), C42(H42A,H42B), C1AA(H1AA,H1AB), C3AA(H3AA,
 H3AB)
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