#------------------------------------------------------------------------------
#$Date: 2021-09-06 14:13:21 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268768 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/75/7707594.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_7707594
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
'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
;
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      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
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   26.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6959 -125.0000    0.0000 71

#__ type_ start__ end____ width___ exp.time_
  2 omega  -27.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6959  -57.0000    0.0000 96

#__ type_ start__ end____ width___ exp.time_
  3 omega -117.00  -19.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -77.0000  150.0000 98

#__ type_ start__ end____ width___ exp.time_
  4 omega  -59.00   27.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   61.0000  -90.0000 86

#__ type_ start__ end____ width___ exp.time_
  5 omega   80.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000  124.0000 35

#__ type_ start__ end____ width___ exp.time_
  6 omega  105.00  169.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   90.0000 64

#__ type_ start__ end____ width___ exp.time_
  7 omega   36.00   81.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -90.0000 45

#__ type_ start__ end____ width___ exp.time_
  8 omega   45.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000  124.0000 26

#__ type_ start__ end____ width___ exp.time_
  9 omega   83.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000  -90.0000 33

#__ type_ start__ end____ width___ exp.time_
 10 omega   40.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000   30.0000 76

#__ type_ start__ end____ width___ exp.time_
 11 omega   36.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000 -180.0000 79

#__ type_ start__ end____ width___ exp.time_
 12 omega   37.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -30.0000 54

#__ type_ start__ end____ width___ exp.time_
 13 omega   36.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  120.0000 55

#__ type_ start__ end____ width___ exp.time_
 14 omega   34.00  163.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000    0.0000 -120.0000 129

#__ type_ start__ end____ width___ exp.time_
 15 omega   37.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000  -30.0000 77

#__ type_ start__ end____ width___ exp.time_
 16 omega   36.00   64.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000  -90.0000 28

#__ type_ start__ end____ width___ exp.time_
 17 omega   42.00  139.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000    0.0000 97

#__ type_ start__ end____ width___ exp.time_
 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       'ω 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/[σ²(Fo²)+(0.0724P)²+31.9845P] where P=(Fo²+2Fc²)/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 > 2σ(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
_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.
;
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'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, -y, -z'
'x, -y, z'
'-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
Br2 Br 0.00723(4) 0.500000 0.39514(3) 0.04094(15) Uani 1 2 d S T P . .
Br1 Br 0.76815(6) 0.500000 0.22554(3) 0.05225(18) Uani 1 2 d S T P . .
Cu2 Cu 0.33671(5) 0.500000 0.30189(4) 0.04579(19) Uani 1 2 d S T P . .
Cu1 Cu 0.19206(5) 0.500000 0.45983(4) 0.04055(18) Uani 1 2 d S T P . .
Cu3 Cu 0.81027(5) 0.67370(3) 0.20206(3) 0.05556(17) Uani 1 1 d . . . . .
N6 N 0.8511(2) 0.7276(2) 0.28191(19) 0.0426(8) Uani 1 1 d . . . . .
N3 N 0.2899(2) 0.57657(17) 0.35460(18) 0.0345(7) Uani 1 1 d . . . . .
N4 N 0.3923(2) 0.5866(2) 0.25381(18) 0.0428(8) Uani 1 1 d . . . . .
H4 H 0.378843 0.577441 0.204103 0.051 Uiso 1 1 calc R . . . .
N5 N 0.5640(3) 0.8762(2) 0.2698(3) 0.0685(14) Uani 1 1 d D U . . .
H5B H 0.583890 0.920651 0.247403 0.082 Uiso 0.561(15) 1 calc R . . A 2
H5A H 0.583356 0.921157 0.247984 0.082 Uiso 0.439(15) 1 calc R . . A 1
N1 N 0.1536(2) 0.58549(17) 0.51703(17) 0.0342(7) Uani 1 1 d . . . . .
H1 H 0.088518 0.574904 0.527918 0.041 Uiso 1 1 calc R . . . .
C10 C 0.6852(2) 0.60427(19) 0.4202(2) 0.0314(7) Uani 1 1 d . . . . .
H10A H 0.670448 0.646111 0.447614 0.038 Uiso 1 1 calc R . . . .
H10B H 0.662801 0.560739 0.441720 0.038 Uiso 1 1 calc R . . . .
N2 N 0.2402(2) 0.57610(16) 0.40822(17) 0.0322(6) Uani 1 1 d . . . . .
N7 N 0.8119(3) 0.7814(2) 0.31244(18) 0.0431(8) Uani 1 1 d . . . . .
C1 C 0.2098(3) 0.5996(2) 0.5830(2) 0.0344(8) Uani 1 1 d . . . . .
H1A H 0.197308 0.561124 0.615005 0.041 Uiso 1 1 calc R . . . .
H1B H 0.188199 0.645076 0.601484 0.041 Uiso 1 1 calc R . . . .
C7 C 0.4948(3) 0.5984(3) 0.2664(2) 0.0409(9) Uani 1 1 d . . . . .
H7A H 0.510694 0.643467 0.244134 0.049 Uiso 1 1 calc R . . . .
H7B H 0.527451 0.559013 0.245384 0.049 Uiso 1 1 calc R . . . .
C8 C 0.5310(3) 0.6025(2) 0.34095(19) 0.0333(8) Uani 1 1 d . . . . .
H8C H 0.514142 0.558342 0.364213 0.040 Uiso 1 1 calc R . . . .
H8D H 0.501647 0.643505 0.362150 0.040 Uiso 1 1 calc R . . . .
N8 N 0.7310(5) 0.8638(2) 0.3925(2) 0.0719(15) Uani 1 1 d D . . . .
H8B H 0.705809 0.913221 0.396637 0.086 Uiso 0.561(15) 1 calc R . . A 2
H8A H 0.703167 0.911784 0.399793 0.086 Uiso 0.439(15) 1 calc R . . A 1
C12 C 0.9382(3) 0.7176(3) 0.3155(3) 0.0538(13) Uani 1 1 d . . . . .
C19B C 0.4504(10) 0.8446(6) 0.3509(8) 0.064(3) Uani 0.561(15) 1 d D . . A 2
H19A H 0.404587 0.819987 0.317912 0.077 Uiso 0.561(15) 1 calc R . . A 2
H19B H 0.414886 0.866874 0.385501 0.077 Uiso 0.561(15) 1 calc R . . A 2
C5 C 0.2919(3) 0.6438(2) 0.3317(2) 0.0375(8) Uani 1 1 d . . . . .
C6 C 0.3383(3) 0.6521(3) 0.2678(2) 0.0476(10) Uani 1 1 d . . . . .
H6A H 0.289906 0.661263 0.229259 0.057 Uiso 1 1 calc R . . . .
H6B H 0.381108 0.693745 0.272222 0.057 Uiso 1 1 calc R . . . .
C17B C 0.5837(9) 0.8140(6) 0.4462(6) 0.048(3) Uani 0.561(15) 1 d D U . A 2
H17A H 0.564836 0.863318 0.456658 0.057 Uiso 0.561(15) 1 calc R . . A 2
H17B H 0.572428 0.784014 0.485538 0.057 Uiso 0.561(15) 1 calc R . . A 2
C20B C 0.4977(8) 0.9033(7) 0.3142(7) 0.059(3) Uani 0.561(15) 1 d D U . A 2
H20A H 0.449034 0.931683 0.287020 0.071 Uiso 0.561(15) 1 calc R . . A 2
H20B H 0.531209 0.935607 0.348127 0.071 Uiso 0.561(15) 1 calc R . . A 2
C4 C 0.2431(3) 0.6882(2) 0.3713(2) 0.0410(9) Uani 1 1 d . . . . .
H4A H 0.233964 0.738366 0.366926 0.049 Uiso 1 1 calc R . . . .
C16B C 0.6868(10) 0.8148(6) 0.4420(6) 0.047(3) Uani 0.561(15) 1 d D . . A 2
H16A H 0.705341 0.765364 0.431821 0.056 Uiso 0.561(15) 1 calc R . . A 2
H16B H 0.717201 0.826212 0.487869 0.056 Uiso 0.561(15) 1 calc R . . A 2
C18B C 0.5174(8) 0.7882(6) 0.3860(6) 0.049(3) Uani 0.561(15) 1 d D U . A 2
H18A H 0.479120 0.748712 0.401487 0.059 Uiso 0.561(15) 1 calc R . . A 2
H18B H 0.555586 0.768313 0.351770 0.059 Uiso 0.561(15) 1 calc R . . A 2
C14 C 0.8710(4) 0.8051(3) 0.3639(3) 0.0577(13) Uani 1 1 d . . . . .
C3 C 0.2109(3) 0.6430(2) 0.4186(2) 0.0349(8) Uani 1 1 d . . . . .
C2 C 0.1457(3) 0.6502(2) 0.4725(2) 0.0404(9) Uani 1 1 d . . . . .
H2A H 0.161989 0.693467 0.499949 0.049 Uiso 1 1 calc R . . . .
H2B H 0.080379 0.655301 0.451188 0.049 Uiso 1 1 calc R . . . .
C9 C 0.6367(3) 0.6115(2) 0.34853(19) 0.0328(7) Uani 1 1 d . . . . .
H9A H 0.651465 0.659297 0.331068 0.039 Uiso 1 1 calc R . . . .
H9B H 0.663588 0.575561 0.319581 0.039 Uiso 1 1 calc R . . . .
C15 C 0.8358(6) 0.8669(3) 0.3999(3) 0.080(2) Uani 1 1 d . . . . .
H15A H 0.856925 0.911984 0.380300 0.096 Uiso 1 1 calc R . . . .
H15B H 0.860319 0.865352 0.448404 0.096 Uiso 1 1 calc R . . . .
C13 C 0.9529(4) 0.7657(3) 0.3679(3) 0.0641(15) Uani 1 1 d . . . . .
H13 H 1.007061 0.770767 0.399565 0.077 Uiso 1 1 calc R . . . .
C11 C 0.5061(4) 0.8391(3) 0.2133(3) 0.0681(16) Uani 1 1 d . U . . .
H11A H 0.449973 0.817820 0.230387 0.082 Uiso 1 1 calc R . . . .
H11B H 0.484674 0.874091 0.177533 0.082 Uiso 1 1 calc R . . . .
C16A C 0.7296(14) 0.8166(11) 0.4548(9) 0.065(5) Uani 0.439(15) 1 d D . . A 1
H16C H 0.747323 0.766797 0.445414 0.078 Uiso 0.439(15) 1 calc R . . A 1
H16D H 0.771758 0.835304 0.493577 0.078 Uiso 0.439(15) 1 calc R . . A 1
C17A C 0.6285(12) 0.8219(7) 0.4675(7) 0.047(3) Uani 0.439(15) 1 d D U . A 1
H17C H 0.613438 0.872950 0.473965 0.056 Uiso 0.439(15) 1 calc R . . A 1
H17D H 0.620694 0.796890 0.510437 0.056 Uiso 0.439(15) 1 calc R . . A 1
C18A C 0.5577(11) 0.7919(7) 0.4128(8) 0.048(3) Uani 0.439(15) 1 d D U . A 1
H18C H 0.522532 0.753291 0.432968 0.058 Uiso 0.439(15) 1 calc R . . A 1
H18D H 0.592364 0.769858 0.377610 0.058 Uiso 0.439(15) 1 calc R . . A 1
C19A C 0.4865(12) 0.8449(9) 0.3779(10) 0.064(3) Uani 0.439(15) 1 d D . . A 1
H19C H 0.453605 0.868548 0.413223 0.077 Uiso 0.439(15) 1 calc R . . A 1
H19D H 0.439071 0.817665 0.348448 0.077 Uiso 0.439(15) 1 calc R . . A 1
C20A C 0.5272(12) 0.9032(9) 0.3349(8) 0.059(3) Uani 0.439(15) 1 d D . . A 1
H20C H 0.477862 0.939350 0.322572 0.071 Uiso 0.439(15) 1 calc R . . A 1
H20D H 0.579122 0.927357 0.362964 0.071 Uiso 0.439(15) 1 calc R . . A 1
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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 '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
N3 Cu2 N3 95.45(19) 6_565 . ?
N3 Cu2 N4 81.01(14) . . ?
N3 Cu2 N4 174.60(15) . 6_565 ?
N3 Cu2 N4 174.60(15) 6_565 . ?
N3 Cu2 N4 81.01(14) 6_565 6_565 ?
N4 Cu2 N4 102.2(2) . 6_565 ?
N1 Cu1 Br2 87.53(9) 6_565 . ?
N1 Cu1 Br2 87.53(9) . . ?
N1 Cu1 N1 101.16(19) 6_565 . ?
N2 Cu1 Br2 97.53(10) 6_565 . ?
N2 Cu1 Br2 97.53(10) . . ?
N2 Cu1 N1 81.51(14) . . ?
N2 Cu1 N1 81.51(14) 6_565 6_565 ?
N2 Cu1 N1 174.41(13) . 6_565 ?
N2 Cu1 N1 174.41(13) 6_565 . ?
N2 Cu1 N2 95.41(19) . 6_565 ?
N6 Cu3 N5 80.4(2) . 7_665 ?
N6 Cu3 N7 94.93(15) . 7_665 ?
N6 Cu3 N8 168.15(17) . 7_665 ?
N7 Cu3 N5 172.50(18) 7_665 7_665 ?
N7 Cu3 N8 81.0(2) 7_665 7_665 ?
N8 Cu3 N5 104.7(2) 7_665 7_665 ?
N7 N6 Cu3 131.9(3) . . ?
N7 N6 C12 106.9(4) . . ?
C12 N6 Cu3 121.0(4) . . ?
N2 N3 Cu2 131.9(2) . . ?
C5 N3 Cu2 119.4(3) . . ?
C5 N3 N2 107.9(3) . . ?
Cu2 N4 H4 106.0 . . ?
C7 N4 Cu2 117.4(3) . . ?
C7 N4 H4 106.0 . . ?
C7 N4 C6 111.8(4) . . ?
C6 N4 Cu2 108.8(3) . . ?
C6 N4 H4 106.0 . . ?
Cu3 N5 H5B 102.4 7_665 . ?
Cu3 N5 H5A 102.9 7_665 . ?
C20B N5 H5B 102.4 . . ?
C20B N5 C11 105.7(7) . . ?
C11 N5 Cu3 113.2(3) . 7_665 ?
C11 N5 H5B 102.4 . . ?
C11 N5 H5A 102.9 . . ?
C11 N5 C20A 124.9(8) . . ?
C20A N5 Cu3 107.0(7) . 7_665 ?
C20A N5 H5A 102.9 . . ?
Cu1 N1 H1 106.0 . . ?
C1 N1 Cu1 118.0(2) . . ?
C1 N1 H1 106.0 . . ?
C1 N1 C2 112.1(3) . . ?
C2 N1 Cu1 108.0(2) . . ?
C2 N1 H1 106.0 . . ?
H10A C10 H10B 108.3 . . ?
C1 C10 H10A 109.9 2_656 . ?
C1 C10 H10B 109.9 2_656 . ?
C1 C10 C9 108.8(3) 2_656 . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
N3 N2 Cu1 132.7(2) . . ?
N3 N2 C3 108.5(3) . . ?
C3 N2 Cu1 118.1(3) . . ?
N6 N7 Cu3 132.9(3) . 7_665 ?
C14 N7 Cu3 117.4(4) . 7_665 ?
C14 N7 N6 109.6(4) . . ?
N1 C1 C10 114.9(3) . 2_656 ?
N1 C1 H1A 108.5 . . ?
N1 C1 H1B 108.5 . . ?
C10 C1 H1A 108.5 2_656 . ?
C10 C1 H1B 108.5 2_656 . ?
H1A C1 H1B 107.5 . . ?
N4 C7 H7A 108.8 . . ?
N4 C7 H7B 108.8 . . ?
N4 C7 C8 113.7(3) . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
C7 C8 H8C 109.8 . . ?
C7 C8 H8D 109.8 . . ?
C7 C8 C9 109.6(3) . . ?
H8C C8 H8D 108.2 . . ?
C9 C8 H8C 109.8 . . ?
C9 C8 H8D 109.8 . . ?
Cu3 N8 H8B 108.9 7_665 . ?
Cu3 N8 H8A 111.3 7_665 . ?
C16B N8 H8B 108.9 . . ?
C15 N8 Cu3 107.1(4) . 7_665 ?
C15 N8 H8B 108.9 . . ?
C15 N8 H8A 111.3 . . ?
C15 N8 C16B 116.2(7) . . ?
C15 N8 C16A 92.6(9) . . ?
C16A N8 Cu3 121.5(10) . 7_665 ?
C16A N8 H8A 111.3 . . ?
N6 C12 C13 109.8(5) . . ?
N6 C12 C11 114.4(5) . 7_665 ?
C13 C12 C11 135.8(5) . 7_665 ?
H19A C19B H19B 107.5 . . ?
C20B C19B H19A 108.5 . . ?
C20B C19B H19B 108.5 . . ?
C20B C19B C18B 115.0(9) . . ?
C18B C19B H19A 108.5 . . ?
C18B C19B H19B 108.5 . . ?
N3 C5 C6 114.3(4) . . ?
N3 C5 C4 109.9(4) . . ?
C4 C5 C6 135.5(4) . . ?
N4 C6 C5 110.9(3) . . ?
N4 C6 H6A 109.5 . . ?
N4 C6 H6B 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.0 . . ?
H17A C17B H17B 106.9 . . ?
C16B C17B H17A 107.3 . . ?
C16B C17B H17B 107.3 . . ?
C16B C17B C18B 119.9(9) . . ?
C18B C17B H17A 107.3 . . ?
C18B C17B H17B 107.3 . . ?
N5 C20B C19B 113.1(10) . . ?
N5 C20B H20A 109.0 . . ?
N5 C20B H20B 109.0 . . ?
C19B C20B H20A 109.0 . . ?
C19B C20B H20B 109.0 . . ?
H20A C20B H20B 107.8 . . ?
C5 C4 H4A 127.9 . . ?
C3 C4 C5 104.1(3) . . ?
C3 C4 H4A 127.9 . . ?
N8 C16B H16A 106.9 . . ?
N8 C16B H16B 106.9 . . ?
C17B C16B N8 121.6(9) . . ?
C17B C16B H16A 106.9 . . ?
C17B C16B H16B 106.9 . . ?
H16A C16B H16B 106.7 . . ?
C19B C18B H18A 108.2 . . ?
C19B C18B H18B 108.2 . . ?
C17B C18B C19B 116.3(9) . . ?
C17B C18B H18A 108.2 . . ?
C17B C18B H18B 108.2 . . ?
H18A C18B H18B 107.4 . . ?
N7 C14 C15 114.1(5) . . ?
N7 C14 C13 109.5(5) . . ?
C13 C14 C15 136.3(5) . . ?
N2 C3 C4 109.5(4) . . ?
N2 C3 C2 115.0(3) . . ?
C4 C3 C2 135.2(4) . . ?
N1 C2 C3 109.6(3) . . ?
N1 C2 H2A 109.8 . . ?
N1 C2 H2B 109.8 . . ?
C3 C2 H2A 109.8 . . ?
C3 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
C10 C9 H9A 108.3 . . ?
C10 C9 H9B 108.3 . . ?
C8 C9 C10 115.8(3) . . ?
C8 C9 H9A 108.3 . . ?
C8 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
N8 C15 H15A 110.0 . . ?
N8 C15 H15B 110.0 . . ?
C14 C15 N8 108.3(5) . . ?
C14 C15 H15A 110.0 . . ?
C14 C15 H15B 110.0 . . ?
H15A C15 H15B 108.4 . . ?
C12 C13 C14 104.2(4) . . ?
C12 C13 H13 127.9 . . ?
C14 C13 H13 127.9 . . ?
N5 C11 H11A 109.6 . . ?
N5 C11 H11B 109.6 . . ?
C12 C11 N5 110.1(4) 7_665 . ?
C12 C11 H11A 109.6 7_665 . ?
C12 C11 H11B 109.6 7_665 . ?
H11A C11 H11B 108.2 . . ?
N8 C16A H16C 111.5 . . ?
N8 C16A H16D 111.5 . . ?
H16C C16A H16D 109.3 . . ?
C17A C16A N8 101.3(10) . . ?
C17A C16A H16C 111.5 . . ?
C17A C16A H16D 111.5 . . ?
C16A C17A H17C 108.3 . . ?
C16A C17A H17D 108.3 . . ?
C16A C17A C18A 116.1(12) . . ?
H17C C17A H17D 107.4 . . ?
C18A C17A H17C 108.3 . . ?
C18A C17A H17D 108.3 . . ?
C17A C18A H18C 108.2 . . ?
C17A C18A H18D 108.2 . . ?
C17A C18A C19A 116.4(12) . . ?
H18C C18A H18D 107.3 . . ?
C19A C18A H18C 108.2 . . ?
C19A C18A H18D 108.2 . . ?
C18A C19A H19C 108.3 . . ?
C18A C19A H19D 108.3 . . ?
C18A C19A C20A 115.8(12) . . ?
H19C C19A H19D 107.4 . . ?
C20A C19A H19C 108.3 . . ?
C20A C19A H19D 108.3 . . ?
N5 C20A C19A 114.8(13) . . ?
N5 C20A H20C 108.6 . . ?
N5 C20A H20D 108.6 . . ?
C19A C20A H20C 108.6 . . ?
C19A C20A H20D 108.6 . . ?
H20C C20A H20D 107.5 . . ?
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
Br2 Cu1 2.8180(9) . ?
Cu2 N3 1.937(3) . ?
Cu2 N3 1.937(3) 6_565 ?
Cu2 N4 2.083(4) . ?
Cu2 N4 2.083(4) 6_565 ?
Cu1 N1 2.071(3) 6_565 ?
Cu1 N1 2.071(3) . ?
Cu1 N2 1.926(3) . ?
Cu1 N2 1.926(3) 6_565 ?
Cu3 N6 1.917(4) . ?
Cu3 N5 2.054(5) 7_665 ?
Cu3 N7 1.936(4) 7_665 ?
Cu3 N8 2.032(5) 7_665 ?
N6 N7 1.332(5) . ?
N6 C12 1.363(6) . ?
N3 N2 1.343(5) . ?
N3 C5 1.339(5) . ?
N4 H4 1.0000 . ?
N4 C7 1.481(5) . ?
N4 C6 1.492(6) . ?
N5 H5B 1.0000 . ?
N5 H5A 1.0000 . ?
N5 C20B 1.456(10) . ?
N5 C11 1.493(9) . ?
N5 C20A 1.534(13) . ?
N1 H1 1.0000 . ?
N1 C1 1.486(5) . ?
N1 C2 1.497(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C1 1.515(5) 2_656 ?
C10 C9 1.521(5) . ?
N2 C3 1.344(5) . ?
N7 C14 1.331(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.516(5) . ?
C8 H8C 0.9900 . ?
C8 H8D 0.9900 . ?
C8 C9 1.517(5) . ?
N8 H8B 1.0000 . ?
N8 H8A 1.0000 . ?
N8 C16B 1.529(10) . ?
N8 C15 1.495(10) . ?
N8 C16A 1.522(13) . ?
C12 C13 1.374(9) . ?
C12 C11 1.480(8) 7_665 ?
C19B H19A 0.9900 . ?
C19B H19B 0.9900 . ?
C19B C20B 1.519(11) . ?
C19B C18B 1.541(12) . ?
C5 C6 1.503(6) . ?
C5 C4 1.385(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C17B H17A 0.9900 . ?
C17B H17B 0.9900 . ?
C17B C16B 1.490(11) . ?
C17B C18B 1.524(11) . ?
C20B H20A 0.9900 . ?
C20B H20B 0.9900 . ?
C4 H4A 0.9500 . ?
C4 C3 1.381(6) . ?
C16B H16A 0.9900 . ?
C16B H16B 0.9900 . ?
C18B H18A 0.9900 . ?
C18B H18B 0.9900 . ?
C14 C15 1.478(9) . ?
C14 C13 1.382(9) . ?
C3 C2 1.500(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C13 H13 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C16A H16C 0.9900 . ?
C16A H16D 0.9900 . ?
C16A C17A 1.501(13) . ?
C17A H17C 0.9900 . ?
C17A H17D 0.9900 . ?
C17A C18A 1.513(12) . ?
C18A H18C 0.9900 . ?
C18A H18D 0.9900 . ?
C18A C19A 1.534(13) . ?
C19A H19C 0.9900 . ?
C19A H19D 0.9900 . ?
C19A C20A 1.539(13) . ?
C20A H20C 0.9900 . ?
C20A H20D 0.9900 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N5 H5A Br1 1.00 2.60 3.336(5) 130.6 4_655 yes
N1 H1 Br2 1.00 2.58 3.433(3) 143.6 2_556 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu2 N3 N2 Cu1 0.7(5) . . . . ?
Cu2 N3 N2 C3 -169.1(3) . . . . ?
Cu2 N3 C5 C6 -4.2(5) . . . . ?
Cu2 N3 C5 C4 171.3(3) . . . . ?
Cu2 N4 C7 C8 -53.4(5) . . . . ?
Cu2 N4 C6 C5 23.8(4) . . . . ?
Cu1 N1 C1 C10 51.4(4) . . . 2_656 ?
Cu1 N1 C2 C3 -28.6(4) . . . . ?
Cu1 N2 C3 C4 -172.3(3) . . . . ?
Cu1 N2 C3 C2 2.3(4) . . . . ?
Cu3 N6 N7 Cu3 7.4(6) . . . 7_665 ?
Cu3 N6 N7 C14 -175.1(3) . . . . ?
Cu3 N6 C12 C13 175.8(3) . . . . ?
Cu3 N6 C12 C11 -2.5(5) . . . 7_665 ?
Cu3 N5 C20B C19B -68.2(12) 7_665 . . . ?
Cu3 N5 C11 C12 -9.5(5) 7_665 . . 7_665 ?
Cu3 N5 C20A C19A -75.2(12) 7_665 . . . ?
Cu3 N7 C14 C15 -4.3(5) 7_665 . . . ?
Cu3 N7 C14 C13 178.1(3) 7_665 . . . ?
Cu3 N8 C16B C17B -68.9(11) 7_665 . . . ?
Cu3 N8 C15 C14 -36.6(5) 7_665 . . . ?
Cu3 N8 C16A C17A -82.1(14) 7_665 . . . ?
N6 N7 C14 C15 177.7(4) . . . . ?
N6 N7 C14 C13 0.2(5) . . . . ?
N6 C12 C13 C14 -0.3(5) . . . . ?
N3 N2 C3 C4 -0.7(4) . . . . ?
N3 N2 C3 C2 173.9(3) . . . . ?
N3 C5 C6 N4 -14.1(5) . . . . ?
N3 C5 C4 C3 -0.8(4) . . . . ?
N4 C7 C8 C9 177.6(3) . . . . ?
N2 N3 C5 C6 -175.1(3) . . . . ?
N2 N3 C5 C4 0.4(4) . . . . ?
N2 C3 C2 N1 18.5(5) . . . . ?
N7 N6 C12 C13 0.4(5) . . . . ?
N7 N6 C12 C11 -178.0(4) . . . 7_665 ?
N7 C14 C15 N8 27.8(6) . . . . ?
N7 C14 C13 C12 0.0(5) . . . . ?
C1 N1 C2 C3 103.0(4) . . . . ?
C1 C10 C9 C8 168.6(3) 2_656 . . . ?
C7 N4 C6 C5 -107.5(4) . . . . ?
C7 C8 C9 C10 -170.3(3) . . . . ?
N8 C16A C17A C18A 63.9(17) . . . . ?
C12 N6 N7 Cu3 -177.9(3) . . . 7_665 ?
C12 N6 N7 C14 -0.3(5) . . . . ?
C5 N3 N2 Cu1 170.0(3) . . . . ?
C5 N3 N2 C3 0.2(4) . . . . ?
C5 C4 C3 N2 0.9(4) . . . . ?
C5 C4 C3 C2 -172.1(4) . . . . ?
C6 N4 C7 C8 73.4(5) . . . . ?
C6 C5 C4 C3 173.3(4) . . . . ?
C20B N5 C11 C12 -153.1(6) . . . 7_665 ?
C20B C19B C18B C17B 67.3(14) . . . . ?
C4 C5 C6 N4 172.0(4) . . . . ?
C4 C3 C2 N1 -168.7(4) . . . . ?
C16B N8 C15 C14 82.5(7) . . . . ?
C16B C17B C18B C19B -114.4(11) . . . . ?
C18B C19B C20B N5 49.0(15) . . . . ?
C18B C17B C16B N8 65.3(14) . . . . ?
C2 N1 C1 C10 -75.0(4) . . . 2_656 ?
C15 N8 C16B C17B 171.8(9) . . . . ?
C15 N8 C16A C17A 166.0(12) . . . . ?
C15 C14 C13 C12 -176.7(6) . . . . ?
C13 C14 C15 N8 -155.6(6) . . . . ?
C11 N5 C20B C19B 68.6(10) . . . . ?
C11 N5 C20A C19A 60.6(13) . . . . ?
C11 C12 C13 C14 177.6(5) 7_665 . . . ?
C16A N8 C15 C14 87.6(10) . . . . ?
C16A C17A C18A C19A -118.1(14) . . . . ?
C17A C18A C19A C20A 66.3(19) . . . . ?
C18A C19A C20A N5 69.3(17) . . . . ?
C20A N5 C11 C12 -142.9(8) . . . 7_665 ?
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 0.000 93.3 0.0 ?
2 0.361 0.000 0.500 394.4 266.6 'CuBr3 13(H2O)'
3 -0.205 0.500 0.000 394.4 266.6 'CuBr3 13(H2O)'
4 0.500 0.500 0.500 93.3 0.0 ?
