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_7707594
_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 Br2 Cu4 N16, 2(Br), 2(C20 H34 Cu2 N8)'
_chemical_formula_sum            'C80 H136 Br4 Cu8 N32'
_chemical_formula_weight         2374.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-07-10
_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                90
_cell_angle_beta                 96.1863(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.34035(14)
_cell_length_b                   18.7171(2)
_cell_length_c                   19.8559(2)
_cell_measurement_reflns_used    12720
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      76.3292
_cell_measurement_theta_min      3.2520
_cell_volume                     5298.48(9)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
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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      123(1)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega   26.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6959 -125.0000    0.0000 71

  2 omega  -27.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6959  -57.0000    0.0000 96

  3 omega -117.00  -19.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -77.0000  150.0000 98

  4 omega  -59.00   27.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   61.0000  -90.0000 86

  5 omega   80.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000  124.0000 35

  6 omega  105.00  169.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   90.0000 64

  7 omega   36.00   81.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -90.0000 45

  8 omega   45.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000  124.0000 26

  9 omega   83.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000  -90.0000 33

 10 omega   40.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000   30.0000 76

 11 omega   36.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000 -180.0000 79

 12 omega   37.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -30.0000 54

 13 omega   36.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  120.0000 55

 14 omega   34.00  163.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000    0.0000 -120.0000 129

 15 omega   37.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000  -30.0000 77

 16 omega   36.00   64.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000  -90.0000 28

 17 omega   42.00  139.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000    0.0000 97

 18 omega   51.00  139.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  150.0000 88
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20584
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.625
_diffrn_reflns_theta_min         1.796
_exptl_absorpt_coefficient_mu    3.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58723
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.2457
_exptl_crystal_size_mid          0.0928
_exptl_crystal_size_min          0.0844
_refine_diff_density_max         1.104
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5669
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0724P)^2^+31.9845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5318
_reflns_number_total             5669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01302e2.cif
_cod_data_source_block           CuBOX_Br
_cod_depositor_comments
'Adding full bibliography for 7707593--7707596.cif.'
_cod_original_cell_volume        5298.49(10)
_cod_database_code               7707594
_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 N(H) groups, All N(H,H) groups
2. Restrained distances
 N5-C20A \\sim N5-C20B
 with sigma of 0.02
 N8-C16A \\sim N8-C16B
 with sigma of 0.02
 C17A-C16A \\sim C17B-C16B \\sim C18A-C17A \\sim C19A-C18A \\sim C18B-C17B
\\sim C19B-C18B \\sim C20A-
 C19A \\sim C20B-C19B
 with sigma of 0.02
3. Rigid bond restraints
 N5, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C20B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C17A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C17B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C19A) = Uanis(C19B)
Uanis(C20A) = Uanis(C20B)
5. Others
 Sof(H5B)=Sof(H8B)=Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(C17B)=Sof(H17A)=Sof(H17B)=
 Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(C16B)=Sof(H16A)=Sof(H16B)=Sof(C18B)=
 Sof(H18A)=Sof(H18B)=1-FVAR(1)
 Sof(H5A)=Sof(H8A)=Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C17A)=Sof(H17C)=Sof(H17D)=
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C20A)=
 Sof(H20C)=Sof(H20D)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 N4(H4), N5(H5B), N5(H5A), N1(H1), N8(H8B), N8(H8A)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C1(H1A,H1B), C7(H7A,H7B), C8(H8C,H8D), C19B(H19A,H19B),
 C6(H6A,H6B), C17B(H17A,H17B), C20B(H20A,H20B), C16B(H16A,H16B), C18B(H18A,
 H18B), C2(H2A,H2B), C9(H9A,H9B), C15(H15A,H15B), C11(H11A,H11B), C16A(H16C,
 H16D), C17A(H17C,H17D), C18A(H18C,H18D), C19A(H19C,H19D), C20A(H20C,H20D)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4A), C13(H13)
;
_shelx_res_checksum              69200
_shelx_fab_checksum              36924
_olex2_submission_special_instructions 'No special instructions were received'