#------------------------------------------------------------------------------
#$Date: 2021-09-06 14:13:21 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268768 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/75/7707595.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7707595
loop_
_publ_author_name
'Pitarch-Jarque, Javier'
'Jiménez, Hermas R'
'Kalenius, Elina'
'Blasco, Salvador'
'Lopera, Alberto'
'Clares, M. Paz'
'Rissanen, Kari'
'García-España, Enrique'
_publ_section_title
;
 Selective encapsulation of a chloride anion in a 1H-pyrazole
 Cu²⁺ 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
'5.33(I0.75), C40 H60 Cu4 N16, 4(Cu0.25 I0.75), 2(Cl0.5 O2)'
_chemical_formula_sum            'C40 H60 Cl Cu5 I7 N16 O4'
_chemical_formula_weight         2070.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-24
_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            2
_cell_length_a                   20.5739(9)
_cell_length_b                   14.4716(5)
_cell_length_c                   11.8083(4)
_cell_measurement_reflns_used    2409
_cell_measurement_temperature    291.0(2)
_cell_measurement_theta_max      23.6490
_cell_measurement_theta_min      3.8390
_cell_volume                     3515.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      291.0(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device       'four-circle diffractometer'
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9900
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.004
_diffrn_reflns_theta_min         3.287
_exptl_absorpt_coefficient_mu    4.644
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    1.956
_exptl_crystal_description       block
_exptl_crystal_F_000             1954
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.826
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0553
_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/[σ²(Fo²)+(0.0985P)²+2.9250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1536
_reflns_number_total             2586
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01302e2.cif
_cod_data_source_block           CuBOX_I
_cod_depositor_comments
'Adding full bibliography for 7707593--7707596.cif.'
_cod_database_code               7707595
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.654
_shelx_estimated_absorpt_t_min   0.457
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 Cu1
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Others
 Fixed Sof: I2(0.25) I3(0.125) Cu2(0.125) I1(0.125) Cl1(0.125) O2(0.25) O1(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B), C3(H3A,H3B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I5 I 0.500000 0.000000 0.000000 0.0804(4) Uani 1 8 d S T P . .
Cu1 Cu 0.40457(4) 0.23756(6) 0.500000 0.0530(3) Uani 1 2 d S TU P . .
I2 I 0.31392(7) 0.34879(11) 0.000000 0.0684(4) Uani 0.5 2 d S T P A 1
I3 I 0.13195(12) 0.500000 0.000000 0.0819(7) Uani 0.5 4 d S T P A 1
I4 I 0.35998(8) 0.000000 0.000000 0.1608(7) Uani 1 4 d S T P . .
Cu2 Cu 0.25508(16) 0.500000 0.000000 0.0713(8) Uani 0.5 4 d S T P A 1
N2 N 0.3412(3) 0.2392(3) 0.3652(5) 0.0740(14) Uani 1 1 d . . . . .
C2 C 0.4455(3) 0.2186(3) 0.2742(4) 0.0599(14) Uani 1 1 d . . . . .
C5 C 0.3522(3) 0.4105(4) 0.3351(5) 0.0632(14) Uani 1 1 d . . . . .
H5A H 0.379173 0.402989 0.268339 0.076 Uiso 1 1 calc R . . . .
H5B H 0.380335 0.413780 0.400821 0.076 Uiso 1 1 calc R . . . .
C1 C 0.500000 0.2093(6) 0.2033(6) 0.080(3) Uani 1 2 d S T P . .
H1 H 0.500000 0.199106 0.125586 0.096 Uiso 1 2 calc RS T P . .
C6 C 0.3119(4) 0.500000 0.3252(7) 0.068(2) Uani 1 2 d S T P . .
H6A H 0.289642 0.500000 0.252768 0.082 Uiso 1 2 calc RS T P . .
H6B H 0.279030 0.500000 0.384058 0.082 Uiso 1 2 calc RS T P . .
C4 C 0.3068(3) 0.3296(4) 0.3462(6) 0.0752(17) Uani 1 1 d . . . . .
H4A H 0.280782 0.324918 0.277856 0.090 Uiso 1 1 calc R . . . .
H4B H 0.277416 0.340723 0.408986 0.090 Uiso 1 1 calc R . . . .
C3 C 0.3765(4) 0.2074(5) 0.2609(6) 0.089(2) Uani 1 1 d . . . . .
H3A H 0.366652 0.142861 0.246789 0.107 Uiso 1 1 calc R . . . .
H3B H 0.361840 0.242934 0.196072 0.107 Uiso 1 1 calc R . . . .
N1 N 0.4675(2) 0.2350(2) 0.3805(3) 0.0475(9) Uani 1 1 d . . . . .
I1 I 0.28570(17) 0.3776(2) 0.000000 0.0813(9) Uani 0.25 2 d S T P B 2
Cl1 Cl 0.4006(6) 0.000000 0.500000 0.115(4) Uani 0.5 4 d S T P C 2
O2 O 0.4567(10) 0.000000 0.382(3) 0.163(8) Uani 0.5 2 d S T P C 2
O1 O 0.3571(12) 0.0813(19) 0.500000 0.210(13) Uani 0.5 2 d S T P C 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I4 I5 I4 180.0 . 9_655 ?
N2 Cu1 N2 101.4(3) 10_556 . ?
N1 Cu1 N2 176.7(2) . 10_556 ?
N1 Cu1 N2 176.7(2) 10_556 . ?
N1 Cu1 N2 81.9(2) 10_556 10_556 ?
N1 Cu1 N2 81.9(2) . . ?
N1 Cu1 N1 94.9(2) . 10_556 ?
I2 Cu2 I2 122.10(15) 3_565 . ?
I2 Cu2 I3 118.95(8) 3_565 . ?
I2 Cu2 I3 118.95(8) . . ?
C4 N2 Cu1 115.1(4) . . ?
C3 N2 Cu1 109.0(4) . . ?
C3 N2 C4 111.8(5) . . ?
C1 C2 C3 135.4(5) . . ?
N1 C2 C1 107.6(5) . . ?
N1 C2 C3 116.8(5) . . ?
C4 C5 C6 109.1(5) . . ?
C2 C1 C2 105.8(6) . 11_655 ?
C5 C6 C5 114.3(6) 12_565 . ?
C5 C4 N2 113.4(5) . . ?
C2 C3 N2 110.7(5) . . ?
C2 N1 Cu1 117.3(4) . . ?
N1 N1 Cu1 132.54(11) 11_655 . ?
N1 N1 C2 109.5(3) 11_655 . ?
O1 Cl1 O2 112.7(6) 3_556 . ?
O1 Cl1 O2 112.7(6) . . ?
O1 Cl1 O1 105.5(18) . 3_556 ?
O2 O2 Cl1 129.6(9) 2_655 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I5 I4 2.8808(16) . ?
I5 I4 2.8809(16) 9_655 ?
Cu1 N2 2.057(5) 10_556 ?
Cu1 N2 2.057(5) . ?
Cu1 N1 1.916(4) . ?
Cu1 N1 1.916(4) 10_556 ?
I2 Cu2 2.501(2) . ?
I3 Cu2 2.533(4) . ?
N2 C4 1.505(7) . ?
N2 C3 1.502(9) . ?
C2 C1 1.405(7) . ?
C2 C3 1.438(10) . ?
C2 N1 1.355(6) . ?
C5 C6 1.542(7) . ?
C5 C4 1.504(7) . ?
N1 N1 1.335(8) 11_655 ?
Cl1 O2 1.81(3) 10_556 ?
Cl1 O2 1.81(3) . ?
Cl1 O1 1.48(3) 3_556 ?
Cl1 O1 1.48(3) . ?
O2 O2 1.78(4) 2_655 ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.503 221.7 31.5 ?
2 0.500 0.500 -0.438 221.7 31.5 ?
