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_7707593
_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 H76 Cu4 N16 O4, 2(F6 P), 2(F), 1.33(H2 O)'
_chemical_formula_sum            'C40 H78.67 Cu4 F14 N16 O5.33 P2'
_chemical_formula_weight         1451.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-12-10
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.861(3)
_cell_length_b                   20.5434(17)
_cell_length_c                   23.7890(18)
_cell_measurement_reflns_used    1333
_cell_measurement_temperature    291.0(2)
_cell_measurement_theta_max      32.3967
_cell_measurement_theta_min      3.2117
_cell_volume                     6774.0(17)
_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      291.0(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.1500
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            12959
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         32.468
_diffrn_reflns_theta_min         3.218
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03514
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             2981
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         5683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.2068
_refine_ls_R_factor_gt           0.0835
_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^)+(0.1154P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2034
_refine_ls_wR_factor_ref         0.2520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2350
_reflns_number_total             5683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01302e2.cif
_cod_data_source_block           CuBOX_F
_cod_depositor_comments
'Adding full bibliography for 7707593--7707596.cif.'
_cod_database_code               7707593
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.683
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(F3)=0.25*(1-FVAR(2))
 Sof(F2)=0.25*FVAR(2)
 Fixed Sof: F1(0.25) O2(0.3333) H2A(0.3333) H2B(0.3333)
 Fixed X: H2A(0.441449) H2B(0.34577)
 Fixed Y: H2A(0.60311) H2B(0.611271)
 Fixed Z: H2A(0.175429) H2B(0.16951)
3.a Rotating group:
 O1(H1A,H1B)
3.b Ternary CH refined with riding coordinates:
 N2(H2), N3(H3)
3.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C4(H4A,H4B), C7(H7A,H7B), C9(H9A,H9B), C6(H6A,H6B), C3(H3A,H3B),
 C5(H5A,H5B)
3.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C1(H1)
;
_shelx_res_checksum              74189
_olex2_submission_special_instructions 'No special instructions were received'