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_1566026
_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 H58 Co N20 O14, 2(Cl4 Co)'
_chemical_formula_sum            'C45 H58 Cl8 Co3 N20 O14'
_chemical_formula_weight         1563.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.808(2)
_cell_length_b                   19.9060(17)
_cell_length_c                   13.3851(11)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.52
_cell_volume                     7409.3(10)
_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      273.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            50755
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.974
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7068
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.567
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6708
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0745P)^2^+18.6556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6083
_reflns_number_total             6708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2022-529-120669.cif
_cod_data_source_block           a_b_sq_pl_sq
_cod_database_code               1566026
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.862
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O10) \\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
3. Rigid body (RIGU) restrains
 O8
 with sigma for 1-2 distances of 0.00001 and sigma for 1-3 distances of 0.00001
 O7, O10
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O9, O10
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O10
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Others
 Fixed Sof: O10(0.25) H10(0.5) O9(0.25) H9(0.5)
5.a Rotating group:
 O8(H8C,H8D)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,H9B), C17(H17A,
 H17B), C18(H18A,H18B), C21(H21A,H21B), C23(H23A,H23B), C26(H26A,H26B),
 C27(H27A,H27B), C30(H30A,H30B), C31(H31A,H31B), C46(H46A,H46B)
5.c Tetrahedral OH refined with riding coordinates:
 O7(H7), O10(H10), O9(H9)
;