Selective encapsulation of a chloride anion in a 1<i>H</i>-pyrazole Cu<sup>2+</sup> metallocage.
Pitarch-Jarque, Javier; Jiménez, Hermas R; Kalenius, Elina; Blasco, Salvador; Lopera, Alberto; Clares, M. Paz; Rissanen, Kari; García-España, Enrique; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9010–9015; doi:10.1039/d1dt01302e

data_7707596
_publ_section_title
;
 Selective encapsulation of a chloride anion in a 1<i>H</i>-pyrazole
 Cu<sup>2+</sup> metallocage.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9010
_journal_page_last               9015
_journal_paper_doi               10.1039/d1dt01302e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C40 H68 Cl2 Cu4 N16, 2(Cl), 3(H2 O)'
_chemical_formula_sum            'C40 H74 Cl4 Cu4 N16 O3'
_chemical_formula_weight         1223.11
_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   mixed
_audit_creation_date             2020-03-30
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-02 deposited with the CCDC.	2021-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                108.589(4)
_cell_angle_beta                 90.753(4)
_cell_angle_gamma                99.531(5)
_cell_formula_units_Z            2
_cell_length_a                   12.0598(7)
_cell_length_b                   14.3764(8)
_cell_length_c                   15.6936(6)
_cell_measurement_reflns_used    3716
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      32.3347
_cell_measurement_theta_min      3.0329
_cell_volume                     2537.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27688
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         3.039
_exptl_absorpt_coefficient_mu    1.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       block
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         14775
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0671P)^2^+0.3566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7843
_reflns_number_total             14775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01302e2.cif
_cod_data_source_block           CuBOX_Cl
_cod_depositor_comments
'Adding full bibliography for 7707593--7707596.cif.'
_cod_database_code               7707596
_shelx_shelxl_version_number     2018/3
_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, All N(H) groups,
  All O(H,H) groups
2. Restrained distances
 O3-H3A = O3-H3B
 0.82 with sigma of 0.01
 O1-H1D = O1-H1C
 0.83 with sigma of 0.01
 O2-H2A = O2-H2B
 0.82 with sigma of 0.02
 H3B-H3A
 1.33 with sigma of 0.04
 C30-C29B \\sim C30-C29A
 with sigma of 0.02
 C29B-C28B \\sim C29A-C28A
 with sigma of 0.02
3. Others
 Sof(Cl1)=1-FVAR(1)
 Sof(Cl5)=FVAR(1)
 Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H10C)=Sof(H10D)=Sof(H7BC)=Sof(H7BD)=
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H27C)=Sof(H27D)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H30C)=Sof(H30D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=1-FVAR(2)
 Sof(H10A)=Sof(H10B)=Sof(H7AA)=Sof(H7AB)=Sof(H27A)=Sof(H27B)=Sof(H30A)=
 Sof(H30B)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C29B)=
 Sof(H29C)=Sof(H29D)=Sof(C28B)=Sof(H28A)=Sof(H28B)=FVAR(2)
4.a Rotating group with stretchable bonds:
 O3(H3A,H3B), O2(H2A,H2B), O1(H1C,H1D)
4.b Ternary CH refined with riding coordinates:
 N16(H16), N4(H4), N5(H5), N8(H8), N9(H9), N12(H12), N1(H1), N13(H13A)
4.c Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C29A(H29A,H29B), C10(H10A,H10B), C7(H7BC,H7BD), C7(H7AA,H7AB),
  C37(H37A,H37B), C9A(H9AA,H9AB), C27(H27A,H27B), C27(H27C,H27D), C17(H17A,
 H17B), C8A(H8AA,H8AB), C11(H11A,H11B), C35(H35A,H35B), C20(H20A,H20B),
 C16(H16A,H16B), C6(H6A,H6B), C15(H15A,H15B), C1(H1A,H1B), C19(H19A,H19B),
 C25(H25A,H25B), C30(H30C,H30D), C30(H30A,H30B), C21(H21A,H21B), C31(H31A,H31B),
  C38(H38A,H38B), C39(H39A,H39B), C26(H26A,H26B), C9B(H9BA,H9BB), C8B(H8BA,
 H8BB), C29B(H29C,H29D), C28B(H28A,H28B), C36(H36A,H36B), C40(H40A,H40B),
 C28A(H28C,H28D), C5(H5A,H5B)
4.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C23(H23), C33(H33)
;
_shelx_res_checksum              65861
_olex2_submission_original_sample_id CuBOX_Cl
_olex2_submission_special_instructions 'No special instructions were received'