#------------------------------------------------------------------------------
#$Date: 2019-11-24 05:47:18 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236860 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/22/7702238.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_7702238
loop_
_publ_author_name
'Fraser, Hector W. L.'
'Nichol, Gary S.'
'Baldansuren, Amgalanbaatar'
'McInnes, Eric J. L.'
'Brechin, Euan K.'
_publ_section_title
;
 Cages on a plane: a structural matrix for molecular 'sheets'.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15530
_journal_page_last               15537
_journal_paper_doi               10.1039/c8dt03793k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'1(C72 H84 Al6 Cu7 N12 O24), 6(Cl O4), 3(N0.67 O2), 21 (C H4 O)'
_chemical_formula_sum            'C93 H168 Al6 Cl6 Cu7 N14 O75'
_chemical_formula_weight         3501.76
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-11 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   27.8468(6)
_cell_length_b                   27.8468(6)
_cell_length_c                   17.6945(7)
_cell_measurement_reflns_used    16493
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      27.1140
_cell_measurement_theta_min      3.7210
_cell_volume                     11882.8(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  33.00   1.00   20.00    --   -7.39 -99.00-180.00   53
  2  ω    -45.00   3.00   1.00   20.00    --   -7.39  95.00 -16.00   48
  3  ω    -20.00  49.00   1.00   20.00    --    8.80 -99.00   0.00   69
  4  ω    -65.00  40.00   1.00   20.00    --    8.80 -77.00 120.00  105
  5  ω     -5.00  77.00   1.00   20.00    --    8.80  38.00 -30.00   82
  6  ω      2.00  32.00   1.00   20.00    --    8.80 -57.00   0.00   30
  7  ω    -59.00  39.00   1.00   20.00    --    8.80 -19.00 150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0086807000
_diffrn_orient_matrix_UB_12      -0.0039297000
_diffrn_orient_matrix_UB_13      -0.0360400000
_diffrn_orient_matrix_UB_21      -0.0260452000
_diffrn_orient_matrix_UB_22      -0.0243869000
_diffrn_orient_matrix_UB_23      -0.0051867000
_diffrn_orient_matrix_UB_31      -0.0105685000
_diffrn_orient_matrix_UB_32      0.0159508000
_diffrn_orient_matrix_UB_33      -0.0167713000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49850
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         2.856
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0596 before and 0.0518 after correction.
The Ratio of minimum to maximum transmission is 0.8957.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             5421
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.165
_refine_diff_density_max         1.219
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4843
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0561
_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)+(0.0895P)²+80.5735P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4209
_reflns_number_total             4843
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03793k2.cif
_cod_data_source_block           7
_cod_original_cell_volume        11882.8(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7702238
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cu Al'
_chemical_oxdiff_usercomment     '@ 120 K 792o SE'
_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   0.833
_shelx_estimated_absorpt_t_min   0.711
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4 = O3-H3
 0.84 with sigma of 0.02
 O104-N101 = O103-N101
 1.25 with sigma of 0.02
 O6-O7 \\sim O6-O8 \\sim O8A-O6A \\sim O6A-O7A
 with sigma of 0.04
 Cl1-O5 \\sim Cl1-O6 \\sim Cl1-O7 \\sim Cl1-O8 \\sim Cl1-O8A \\sim Cl1-O6A
\\sim Cl1-O7A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl1, O5, O6, O6A, O7, O7A, O8, O8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O103, O104, N101
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O6A)=Sof(O7A)=Sof(O8A)=1-FVAR(1)
 Sof(O6)=Sof(O7)=Sof(O8)=FVAR(1)
 Fixed Sof: O103(0.6666) O104(0.33333) N101(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4A), C7(H7), C8(H8), C9(H9), C10(H10)
;
_olex2_date_sample_data_collection 2017-01-11
_olex2_date_sample_submission    2017-01-11
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id '792o SE'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.211
_oxdiff_exptl_absorpt_empirical_full_min 0.865
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Cu1 Cu 0.68185(2) 0.52394(2) 0.23077(3) 0.03388(19) Uani 1 1 d . . . . .
Cu2 Cu 0.666667 0.333333 0.333333 0.0242(3) Uani 1 6 d S T P . .
Al1 Al 0.61207(4) 0.40221(4) 0.33235(7) 0.0248(3) Uani 1 1 d . . . . .
O1 O 0.74008(11) 0.51203(11) 0.26993(17) 0.0339(7) Uani 1 1 d . . . . .
O2 O 0.61695(11) 0.45656(11) 0.26601(17) 0.0329(6) Uani 1 1 d . . . . .
O3 O 0.67198(10) 0.40042(10) 0.27853(15) 0.0261(6) Uani 1 1 d D . . . .
H3 H 0.6727(18) 0.4039(18) 0.2303(11) 0.031 Uiso 1 1 d DR . . . .
O4 O 0.55626(10) 0.34182(10) 0.27975(16) 0.0279(6) Uani 1 1 d D . . . .
H4 H 0.5544(19) 0.3423(19) 0.2325(11) 0.033 Uiso 1 1 d DR . . . .
N1 N 0.74101(15) 0.57405(15) 0.1595(2) 0.0398(9) Uani 1 1 d . . . . .
N2 N 0.62619(14) 0.54586(14) 0.2058(2) 0.0349(8) Uani 1 1 d . . . . .
C1 C 0.7343(2) 0.5946(2) 0.0951(3) 0.0583(14) Uani 1 1 d . . . . .
H1 H 0.698743 0.589529 0.083656 0.070 Uiso 1 1 calc R . . . .
C2 C 0.7770(3) 0.6231(3) 0.0442(4) 0.0725(18) Uani 1 1 d . . . . .
H2 H 0.771154 0.637495 -0.001414 0.087 Uiso 1 1 calc R . . . .
C3 C 0.8284(3) 0.6300(2) 0.0621(4) 0.0685(17) Uani 1 1 d . . . . .
H3A H 0.858743 0.649425 0.028489 0.082 Uiso 1 1 calc R . . . .
C4 C 0.8355(2) 0.6088(2) 0.1285(3) 0.0574(14) Uani 1 1 d . . . . .
H4A H 0.870687 0.613437 0.141435 0.069 Uiso 1 1 calc R . . . .
C5 C 0.79060(19) 0.58059(18) 0.1760(3) 0.0440(11) Uani 1 1 d . . . . .
C6 C 0.79404(18) 0.55641(18) 0.2502(3) 0.0460(12) Uani 1 1 d . . . . .
H6A H 0.820306 0.542343 0.246209 0.055 Uiso 1 1 calc R . . . .
H6B H 0.807690 0.585343 0.289901 0.055 Uiso 1 1 calc R . . . .
C7 C 0.6354(2) 0.59705(19) 0.1899(3) 0.0424(10) Uani 1 1 d . . . . .
H7 H 0.672402 0.627283 0.190077 0.051 Uiso 1 1 calc R . . . .
C8 C 0.5927(2) 0.6068(2) 0.1732(3) 0.0478(12) Uani 1 1 d . . . . .
H8 H 0.600090 0.643213 0.161653 0.057 Uiso 1 1 calc R . . . .
C9 C 0.5394(2) 0.5631(2) 0.1736(3) 0.0469(12) Uani 1 1 d . . . . .
H9 H 0.509502 0.568940 0.161145 0.056 Uiso 1 1 calc R . . . .
C10 C 0.52910(19) 0.5108(2) 0.1922(2) 0.0397(10) Uani 1 1 d . . . . .
H10 H 0.492297 0.480269 0.193835 0.048 Uiso 1 1 calc R . . . .
C11 C 0.57453(18) 0.50386(17) 0.2085(2) 0.0339(9) Uani 1 1 d . . . . .
C12 C 0.56808(18) 0.44857(18) 0.2291(3) 0.0418(10) Uani 1 1 d . . . . .
H12A H 0.535739 0.428374 0.262959 0.050 Uiso 1 1 calc R . . . .
H12B H 0.561499 0.426054 0.182879 0.050 Uiso 1 1 calc R . . . .
Cl1 Cl 0.69455(5) 0.62993(5) 0.38585(8) 0.0538(3) Uani 1 1 d D U . . .
O5 O 0.71101(15) 0.59917(15) 0.3381(2) 0.0553(9) Uani 1 1 d D U . . .
O6 O 0.6362(3) 0.6039(5) 0.3820(7) 0.076(4) Uani 0.483(15) 1 d D U . A 1
O6A O 0.6566(6) 0.6436(8) 0.3576(7) 0.114(7) Uani 0.517(15) 1 d D U . A 2
O7 O 0.7158(9) 0.6398(11) 0.4565(7) 0.145(10) Uani 0.483(15) 1 d D U . A 1
O7A O 0.6747(9) 0.5990(5) 0.4548(7) 0.144(7) Uani 0.517(15) 1 d D U . A 2
O8 O 0.7146(6) 0.6802(4) 0.3448(9) 0.115(7) Uani 0.483(15) 1 d D U . A 1
O8A O 0.7428(3) 0.6785(4) 0.4147(8) 0.084(5) Uani 0.517(15) 1 d D U . A 2
O103 O 0.5134(7) 0.4661(7) 0.0101(9) 0.201(6) Uiso 0.6666 1 d D U . . .
O104 O 0.5833(9) 0.5517(9) -0.0249(13) 0.139(7) Uiso 0.3333 1 d D U . . .
N101 N 0.5321(8) 0.5149(8) -0.0082(11) 0.094(6) Uiso 0.3333 1 d D U . . .
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'
Al Al 0.0645 0.0514 '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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-29 0 -13 0.1037
-16 38 -5 0.1037
29 1 12 0.1271
16 -38 5 0.1133
-3 -32 -3 0.0924
-30 20 16 0.0919
-9 20 -21 0.0814
13 -23 20 0.0864
-3 -10 23 0.0691
35 -30 -7 0.1717
17 -4 -22 0.1289
-19 -1 -21 0.0914
13 -36 -9 0.1064
25 -13 19 0.1079
17 4 21 0.1100
-20 39 3 0.1060
-10 26 -18 0.0768
18 5 -19 0.1312
-8 7 24 0.0720
12 -11 -23 0.1152
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
O1 Cu1 O2 100.00(11) . .
O1 Cu1 N1 82.89(14) . .
O1 Cu1 N2 169.68(14) . .
O2 Cu1 N1 157.59(15) . .
O2 Cu1 N2 82.87(13) . .
N2 Cu1 N1 98.27(15) . .
Al1 Cu2 Al1 180.0 16_655 .
Al1 Cu2 Al1 60.002(1) 2_655 16_655
Al1 Cu2 Al1 180.0 2_655 17
Al1 Cu2 Al1 119.995(1) 3_665 .
Al1 Cu2 Al1 119.997(1) 3_665 2_655
Al1 Cu2 Al1 119.993(1) 18_545 16_655
Al1 Cu2 Al1 59.997(1) 3_665 17
Al1 Cu2 Al1 119.998(1) 2_655 .
Al1 Cu2 Al1 60.007(1) 18_545 .
Al1 Cu2 Al1 60.005(1) 3_665 16_655
Al1 Cu2 Al1 119.992(1) 17 16_655
Al1 Cu2 Al1 180.0 3_665 18_545
Al1 Cu2 Al1 120.005(1) 18_545 17
Al1 Cu2 Al1 60.008(1) 17 .
Al1 Cu2 Al1 60.001(1) 2_655 18_545
O3 Cu2 Al1 89.60(7) 16_655 18_545
O3 Cu2 Al1 139.72(7) . 16_655
O3 Cu2 Al1 139.73(7) 2_655 17
O3 Cu2 Al1 40.27(7) 16_655 16_655
O3 Cu2 Al1 139.72(7) 18_545 3_665
O3 Cu2 Al1 40.39(7) 3_665 16_655
O3 Cu2 Al1 40.39(7) 17 3_665
O3 Cu2 Al1 40.27(7) 3_665 3_665
O3 Cu2 Al1 89.60(7) . 3_665
O3 Cu2 Al1 90.39(7) 18_545 2_655
O3 Cu2 Al1 40.28(7) 18_545 18_545
O3 Cu2 Al1 139.61(7) 2_655 3_665
O3 Cu2 Al1 40.27(7) . .
O3 Cu2 Al1 40.39(7) 2_655 18_545
O3 Cu2 Al1 40.40(7) 18_545 .
O3 Cu2 Al1 139.61(7) 17 18_545
O3 Cu2 Al1 139.60(7) 18_545 16_655
O3 Cu2 Al1 40.40(7) . 17
O3 Cu2 Al1 90.39(7) 2_655 16_655
O3 Cu2 Al1 139.60(7) . 2_655
O3 Cu2 Al1 90.39(7) 3_665 17
O3 Cu2 Al1 89.61(7) 18_545 17
O3 Cu2 Al1 139.72(7) 3_665 18_545
O3 Cu2 Al1 89.60(7) 17 16_655
O3 Cu2 Al1 40.27(7) 17 17
O3 Cu2 Al1 40.27(7) 2_655 2_655
O3 Cu2 Al1 89.60(7) 3_665 2_655
O3 Cu2 Al1 40.40(7) 16_655 2_655
O3 Cu2 Al1 89.60(7) 2_655 .
O3 Cu2 Al1 90.40(7) . 18_545
O3 Cu2 Al1 90.39(7) 16_655 3_665
O3 Cu2 Al1 90.40(7) 17 .
O3 Cu2 Al1 139.72(7) 17 2_655
O3 Cu2 Al1 139.60(7) 3_665 .
O3 Cu2 Al1 139.60(7) 16_655 17
O3 Cu2 Al1 139.73(7) 16_655 .
O3 Cu2 O3 180.0 2_655 17
O3 Cu2 O3 80.67(9) 17 .
O3 Cu2 O3 99.33(9) 2_655 .
O3 Cu2 O3 80.67(9) . 18_545
O3 Cu2 O3 80.66(9) 3_665 16_655
O3 Cu2 O3 80.67(9) 2_655 18_545
O3 Cu2 O3 99.33(9) 16_655 18_545
O3 Cu2 O3 180.0 16_655 .
O3 Cu2 O3 99.34(9) 17 18_545
O3 Cu2 O3 99.33(9) 3_665 .
O3 Cu2 O3 80.66(9) 3_665 17
O3 Cu2 O3 180.0 3_665 18_545
O3 Cu2 O3 99.34(9) 3_665 2_655
O3 Cu2 O3 99.33(9) 16_655 17
O3 Cu2 O3 80.67(9) 2_655 16_655
Cu2 Al1 Al1 59.995(1) . 17
Cu2 Al1 Al1 60.0 . 18_545
Al1 Al1 Al1 119.979(2) 18_545 17
O1 Al1 Cu2 133.26(10) 18_545 .
O1 Al1 Al1 132.53(11) 18_545 17
O1 Al1 Al1 89.93(9) 18_545 18_545
O1 Al1 O3 90.85(13) 18_545 18_545
O1 Al1 O3 171.41(14) 18_545 .
O1 Al1 O4 95.44(13) 18_545 17
O1 Al1 O4 92.76(13) 18_545 .
O2 Al1 Cu2 132.15(10) . .
O2 Al1 Al1 133.32(11) . 18_545
O2 Al1 Al1 89.77(9) . 17
O2 Al1 O1 94.59(13) . 18_545
O2 Al1 O3 89.84(13) . .
O2 Al1 O3 171.40(14) . 18_545
O2 Al1 O4 96.15(13) . .
O2 Al1 O4 93.46(13) . 17
O3 Al1 Cu2 42.82(8) . .
O3 Al1 Cu2 42.83(8) 18_545 .
O3 Al1 Al1 39.86(8) 18_545 18_545
O3 Al1 Al1 92.38(8) . 18_545
O3 Al1 Al1 39.96(8) . 17
O3 Al1 Al1 91.46(8) 18_545 17
O3 Al1 O3 85.65(16) . 18_545
O4 Al1 Cu2 83.47(8) . .
O4 Al1 Cu2 83.40(8) 17 .
O4 Al1 Al1 37.08(9) 17 17
O4 Al1 Al1 132.36(10) 17 18_545
O4 Al1 Al1 133.76(10) . 17
O4 Al1 Al1 37.18(9) . 18_545
O4 Al1 O3 92.65(12) 17 18_545
O4 Al1 O3 76.92(12) 17 .
O4 Al1 O3 94.08(12) . .
O4 Al1 O3 76.91(12) . 18_545
O4 Al1 O4 166.82(15) . 17
Al1 O1 Cu1 129.89(14) 17 .
C6 O1 Cu1 111.8(2) . .
C6 O1 Al1 118.0(3) . 17
Al1 O2 Cu1 129.77(14) . .
C12 O2 Cu1 111.0(2) . .
C12 O2 Al1 119.1(2) . .
Cu2 O3 H3 124(3) . .
Al1 O3 Cu2 96.76(12) 17 .
Al1 O3 Cu2 96.91(12) . .
Al1 O3 Al1 100.18(12) . 17
Al1 O3 H3 117(3) 17 .
Al1 O3 H3 117(3) . .
Al1 O4 Al1 105.74(14) . 18_545
Al1 O4 H4 123(3) 18_545 .
Al1 O4 H4 121(3) . .
C1 N1 Cu1 126.9(4) . .
C1 N1 C5 119.2(4) . .
C5 N1 Cu1 113.3(3) . .
C7 N2 Cu1 127.5(3) . .
C11 N2 Cu1 113.1(3) . .
C11 N2 C7 119.4(4) . .
N1 C1 H1 118.6 . .
N1 C1 C2 122.8(6) . .
C2 C1 H1 118.6 . .
C1 C2 H2 121.2 . .
C1 C2 C3 117.6(6) . .
C3 C2 H2 121.2 . .
C2 C3 H3A 120.1 . .
C4 C3 C2 119.9(5) . .
C4 C3 H3A 120.1 . .
C3 C4 H4A 120.6 . .
C3 C4 C5 118.8(5) . .
C5 C4 H4A 120.6 . .
N1 C5 C4 121.8(5) . .
N1 C5 C6 115.1(4) . .
C4 C5 C6 123.1(5) . .
O1 C6 C5 109.0(4) . .
O1 C6 H6A 109.9 . .
O1 C6 H6B 109.9 . .
C5 C6 H6A 109.9 . .
C5 C6 H6B 109.9 . .
H6A C6 H6B 108.3 . .
N2 C7 H7 119.1 . .
N2 C7 C8 121.8(5) . .
C8 C7 H7 119.1 . .
C7 C8 H8 120.6 . .
C9 C8 C7 118.8(4) . .
C9 C8 H8 120.6 . .
C8 C9 H9 120.0 . .
C8 C9 C10 120.1(4) . .
C10 C9 H9 120.0 . .
C9 C10 H10 121.0 . .
C9 C10 C11 118.0(4) . .
C11 C10 H10 121.0 . .
N2 C11 C10 121.8(4) . .
N2 C11 C12 115.7(4) . .
C10 C11 C12 122.5(4) . .
O2 C12 C11 109.6(3) . .
O2 C12 H12A 109.7 . .
O2 C12 H12B 109.7 . .
C11 C12 H12A 109.7 . .
C11 C12 H12B 109.7 . .
H12A C12 H12B 108.2 . .
O5 Cl1 O7A 106.6(7) . .
O5 Cl1 O8A 110.1(4) . .
O6 Cl1 O5 107.2(5) . .
O6 Cl1 O8 105.5(8) . .
O6A Cl1 O5 118.0(5) . .
O6A Cl1 O7A 110.7(10) . .
O6A Cl1 O8A 110.6(8) . .
O7 Cl1 O5 115.4(6) . .
O7 Cl1 O6 115.0(10) . .
O7 Cl1 O8 110.9(13) . .
O7A Cl1 O8A 99.2(8) . .
O8 Cl1 O5 101.7(5) . .
N101 O103 N101 66.2(18) . 10_665
O103 N101 O103 113.8(18) . 10_665
O103 N101 O104 128(2) . .
O103 N101 N101 68.2(15) . 10_665
O104 N101 O103 118(2) . 10_665
O104 N101 N101 164(3) . 10_665
N101 N101 O103 45.7(10) 10_665 10_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.938(3) .
Cu1 O2 1.945(3) .
Cu1 N1 1.988(4) .
Cu1 N2 1.979(3) .
Cu2 Al1 2.9848(10) 16_655
Cu2 Al1 2.9844(11) 17
Cu2 Al1 2.9845(11) .
Cu2 Al1 2.9845(10) 3_665
Cu2 Al1 2.9844(11) 18_545
Cu2 Al1 2.9845(11) 2_655
Cu2 O3 2.043(3) 3_665
Cu2 O3 2.043(3) .
Cu2 O3 2.043(3) 17
Cu2 O3 2.043(3) 2_655
Cu2 O3 2.043(3) 16_655
Cu2 O3 2.043(3) 18_545
Al1 Al1 2.9848(10) 17
Al1 Al1 2.9848(11) 18_545
Al1 O1 1.866(3) 18_545
Al1 O2 1.866(3) .
Al1 O3 1.943(3) .
Al1 O3 1.948(3) 18_545
Al1 O4 1.874(3) 17
Al1 O4 1.870(3) .
O1 C6 1.432(5) .
O2 C12 1.423(5) .
O3 H3 0.859(19) .
O4 H4 0.838(19) .
N1 C1 1.330(7) .
N1 C5 1.332(6) .
N2 C7 1.346(5) .
N2 C11 1.326(6) .
C1 H1 0.9500 .
C1 C2 1.381(8) .
C2 H2 0.9500 .
C2 C3 1.383(10) .
C3 H3A 0.9500 .
C3 C4 1.373(9) .
C4 H4A 0.9500 .
C4 C5 1.381(7) .
C5 C6 1.501(7) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 H7 0.9500 .
C7 C8 1.378(7) .
C8 H8 0.9500 .
C8 C9 1.371(7) .
C9 H9 0.9500 .
C9 C10 1.377(7) .
C10 H10 0.9500 .
C10 C11 1.402(6) .
C11 C12 1.503(6) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
Cl1 O5 1.432(3) .
Cl1 O6 1.411(8) .
Cl1 O6A 1.385(8) .
Cl1 O7 1.352(9) .
Cl1 O7A 1.434(9) .
Cl1 O8 1.421(9) .
Cl1 O8A 1.441(8) .
O103 N101 1.231(15) .
O103 N101 1.60(2) 10_665
O104 N101 1.308(17) .
N101 N101 1.57(4) 10_665
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_4
Cu1 O1 C6 C5 -30.4(4) . .
Cu1 O2 C12 C11 -29.7(4) . .
Cu1 N1 C1 C2 -171.1(5) . .
Cu1 N1 C5 C4 172.7(4) . .
Cu1 N1 C5 C6 -8.7(5) . .
Cu1 N2 C7 C8 180.0(4) . .
Cu1 N2 C11 C10 -179.6(3) . .
Cu1 N2 C11 C12 -0.3(5) . .
Cu2 Al1 O2 Cu1 -54.1(3) . .
Cu2 Al1 O2 C12 120.7(3) . .
Cu2 Al1 O4 Al1 47.00(10) . 18_545
Al1 Al1 O2 Cu1 -6.8(2) 17 .
Al1 Al1 O2 Cu1 -139.92(15) 18_545 .
Al1 Al1 O2 C12 34.9(4) 18_545 .
Al1 Al1 O2 C12 168.0(3) 17 .
Al1 Al1 O4 Al1 83.24(16) 17 18_545
Al1 O1 C6 C5 155.2(3) 17 .
Al1 O2 C12 C11 154.5(3) . .
O1 Al1 O2 Cu1 125.8(2) 18_545 .
O1 Al1 O2 C12 -59.3(3) 18_545 .
O1 Al1 O4 Al1 -86.24(16) 18_545 18_545
O2 Al1 O4 Al1 178.84(14) . 18_545
O3 Al1 O2 Cu1 -46.8(2) . .
O3 Al1 O2 C12 128.0(3) . .
O3 Al1 O4 Al1 3.99(13) 18_545 18_545
O3 Al1 O4 Al1 88.56(13) . 18_545
O4 Al1 O2 Cu1 -140.9(2) . .
O4 Al1 O2 Cu1 30.1(2) 17 .
O4 Al1 O2 C12 -155.1(3) 17 .
O4 Al1 O2 C12 33.9(3) . .
O4 Al1 O4 Al1 42.3(4) 17 18_545
N1 C1 C2 C3 0.1(10) . .
N1 C5 C6 O1 25.6(6) . .
N2 C7 C8 C9 0.6(7) . .
N2 C11 C12 O2 19.8(6) . .
C1 N1 C5 C4 0.8(7) . .
C1 N1 C5 C6 179.4(5) . .
C1 C2 C3 C4 0.0(10) . .
C2 C3 C4 C5 0.3(9) . .
C3 C4 C5 N1 -0.7(8) . .
C3 C4 C5 C6 -179.2(5) . .
C4 C5 C6 O1 -155.8(4) . .
C5 N1 C1 C2 -0.5(8) . .
C7 N2 C11 C10 2.6(6) . .
C7 N2 C11 C12 -178.1(4) . .
C7 C8 C9 C10 1.5(7) . .
C8 C9 C10 C11 -1.5(7) . .
C9 C10 C11 N2 -0.6(7) . .
C9 C10 C11 C12 -179.8(4) . .
C10 C11 C12 O2 -160.9(4) . .
C11 N2 C7 C8 -2.6(7) . .
N101 O103 N101 O103 0.000(1) 10_665 10_665
N101 O103 N101 O104 179(3) 10_665 .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-28.9967 0.0014 -13.0155 0.2174 0.8227 0.5248
-15.9988 37.9993 -5.0018 -0.1079 -0.4840 0.8591
28.9974 0.9977 12.0152 -0.1852 -0.8419 -0.4921
15.9988 -37.9993 5.0018 0.1079 0.4840 -0.8591
-2.9992 -31.9985 -3.0072 0.2081 0.8741 -0.4283
-30.0175 20.0241 16.0010 -0.9159 0.2105 0.3683
-8.9862 19.9846 -21.0099 0.6007 -0.1443 0.7661
12.9877 -22.9868 20.0103 -0.5181 0.1185 -0.8395
-3.0176 -9.9788 23.0085 -0.8162 0.2026 -0.5132
35.0118 -30.0179 -6.9966 0.6740 -0.1436 -0.7315
17.0195 -4.0251 -22.0057 0.9566 -0.2310 0.1250
-18.9888 -1.0094 -21.0163 0.5966 0.6282 0.5371
13.0084 -36.0098 -9.0055 0.5790 0.5861 -0.5608
24.9912 -12.9936 19.0152 -0.4173 -0.4327 -0.7903
16.9884 4.0100 21.0161 -0.6257 -0.6493 -0.4680
-20.0055 39.0075 3.0009 -0.4351 -0.4458 0.7833
-9.9884 25.9870 -18.0079 0.4602 -0.2802 0.8221
18.0177 4.9762 -19.0025 0.8217 -0.4921 0.2077
-8.0190 7.0227 24.0100 -0.9625 -0.0869 -0.2059
12.0190 -11.0232 -23.0088 0.9769 0.0751 0.0830
