#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:27:12 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224262 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/12/7701232.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_7701232
loop_
_publ_author_name
'Stein, Timo'
'Hoffmann, Frank'
'Fröba, Michael'
_publ_section_title
;
 A new set of metal-organic frameworks synthesised from
 diisophthalate-based, 2'-phosphorus-substituted m-terphenyl linker
 molecules.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15127
_journal_page_last               15135
_journal_paper_doi               10.1039/c9dt03044a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'(C156 H114 Cu12 O54 P6), 10(O), O, (Cl -), (C2 H8 N +)'
_chemical_formula_sum            'C158 H122 Cl Cu12 N O65 P6'
_chemical_formula_weight         4058.31
_chemical_name_common            UHM-62
_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'
_symmetry_space_group_name_Hall  '-I 2 2'
_symmetry_space_group_name_H-M   'I m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-07-24 deposited with the CCDC.    2019-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.3318(4)
_cell_length_b                   25.8343(5)
_cell_length_c                   33.4448(6)
_cell_measurement_reflns_used    20450
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.2010
_cell_measurement_theta_min      3.9440
_cell_volume                     15839.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4127
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -58.00 -10.00   1.00   30.00    --  -42.10 -77.00  30.00   48
  2  ω   -115.00 -88.00   1.00   30.00    --  -42.10 -38.00 -30.00   27
  3  ω    -87.00 -18.00   1.00   30.00    --  -42.10 -38.00 -30.00   69
  4  ω   -118.00 -10.00   1.00   30.00    --  -42.10 -77.00-150.00  108
  5  ω   -115.00 -10.00   1.00   30.00    --  -42.10 -77.00 -60.00  105
  6  ω    -67.00 -10.00   1.00   30.00    --  -42.10 -77.00 120.00   57
  7  ω   -100.00  -4.00   1.00   30.00    --  -42.10 -19.00  30.00   96
  8  ω    -70.00  29.00   1.00   30.00    --  -42.10  57.00 -30.00   99
  9  ω    -39.00  29.00   1.00   30.00    --  -42.10  38.00  90.00   68
 10  ω    -30.00  70.00   1.00   30.00    --   42.10 -57.00 150.00  100
 11  ω     30.00  97.00   1.00   30.00    --   42.10-125.00  90.00   67
 12  ω     79.00 176.00   1.00  120.00    --  112.00  77.00-150.00   97
 13  ω     79.00 115.00   1.00  120.00    --  112.00  77.00 120.00   36
 14  ω    116.00 172.00   1.00  120.00    --  112.00  77.00 120.00   56
 15  ω     79.00 155.00   1.00  120.00    --  112.00  77.00 -30.00   76
 16  ω     83.00 108.00   1.00  120.00    --  112.00 -94.00 150.00   25
 17  ω     36.00 116.00   1.00  120.00    --  112.00-111.00-120.00   80
 18  ω     82.00 177.00   1.00  120.00    --  112.00  67.00 154.57   95
 19  ω     79.00 105.00   1.00  120.00    --  112.00  77.00  30.00   26
 20  ω     83.00 177.00   1.00  120.00    --  112.00  61.00  90.00   94
 21  ω     83.00 110.00   1.00  120.00    --  112.00  61.00 -30.00   27
 22  ω     29.00  67.00   1.00  120.00    --  112.00 -94.00 150.00   38
 23  ω    112.00 177.00   1.00  120.00    --  112.00  77.00-120.00   65
 24  ω     79.00 149.00   1.00  120.00    --  112.00  77.00 -90.00   70
 25  ω     83.00 109.00   1.00  120.00    --  112.00  61.00 120.00   26
 26  ω     45.00 145.00   1.00  120.00    --  112.00 -77.00-120.00  100
 27  ω     83.00 109.00   1.00  120.00    --  112.00  61.00 -60.00   26
 28  ω     83.00 109.00   1.00  120.00    --  112.00  61.00  30.00   26
 29  ω     83.00 109.00   1.00  120.00    --  112.00  61.00   0.00   26
 30  ω     83.00 140.00   1.00  120.00    --  112.00  61.00  60.00   57
 31  ω     79.00 105.00   1.00  120.00    --  112.00  77.00-180.00   26
 32  ω     79.00  86.00   1.00  120.00    --  112.00 -94.00 -30.00    7
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0387168000
_diffrn_orient_matrix_UB_12      0.0097672000
_diffrn_orient_matrix_UB_13      -0.0514009000
_diffrn_orient_matrix_UB_21      -0.0650969000
_diffrn_orient_matrix_UB_22      0.0262554000
_diffrn_orient_matrix_UB_23      -0.0163409000
_diffrn_orient_matrix_UB_31      0.0363942000
_diffrn_orient_matrix_UB_32      0.0365650000
_diffrn_orient_matrix_UB_33      0.0254317000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            82547
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.492
_diffrn_reflns_theta_max         67.492
_diffrn_reflns_theta_min         3.421
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.851
_exptl_crystal_description       block
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7657
_refine_ls_number_restraints     494
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0625
_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)+(0.1343P)²+10.7141P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6198
_reflns_number_total             7657
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt03044a2.cif
_cod_data_source_block           UHM-62
_cod_depositor_comments
'Adding full bibliography for 7701221--7701232.cif.'
_cod_database_code               7701232
_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.
;
_cell_oxdiff_length_a            18.3350(4)
_cell_oxdiff_length_b            25.8325(6)
_cell_oxdiff_length_c            33.4452(6)
_cell_oxdiff_angle_alpha         90.0234(17)
_cell_oxdiff_angle_beta          89.9865(18)
_cell_oxdiff_angle_gamma         90.0076(19)
_cell_oxdiff_volume              15841.0(6)
_cell_oxdiff_measurement_reflns_used 20453
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.908
_oxdiff_exptl_absorpt_empirical_full_min 0.682
_oxdiff_exptl_absorpt_empirical_full_max 1.730
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
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
C10A C 0.500000 0.1000(2) 0.29913(18) 0.0663(14) Uani 1 2 d S T P . .
C11A C 0.4349(2) 0.12489(15) 0.29057(13) 0.0670(10) Uani 1 1 d . . . . .
H11A H 0.390089 0.108430 0.296964 0.080 Uiso 1 1 calc R U . . .
C12A C 0.4341(2) 0.17341(15) 0.27284(12) 0.0594(9) Uani 1 1 d . . . . .
C13A C 0.500000 0.1972(2) 0.26336(17) 0.0630(13) Uani 1 2 d S T P . .
H13A H 0.500000 0.229925 0.250353 0.076 Uiso 1 2 calc R U P . .
C14A C 0.3648(2) 0.20016(15) 0.26452(11) 0.0601(9) Uani 1 1 d . . . . .
C20A C 0.500000 0.000000 0.2961(2) 0.0640(18) Uani 1 4 d DS T P . .
C21A C 0.500000 0.0465(2) 0.31728(18) 0.0677(14) Uani 1 2 d DS T P . .
C22A C 0.500000 0.0459(2) 0.3576(2) 0.129(4) Uani 1 2 d DS T P . .
H22A H 0.500000 0.077709 0.371797 0.155 Uiso 1 2 calc R U P . .
C23A C 0.500000 0.000000 0.3786(3) 0.178(9) Uani 1 4 d DS T P . .
H23A H 0.500000 0.000000 0.407054 0.213 Uiso 1 4 calc R U P . .
C40A C 0.5808(9) -0.0343(10) 0.2263(6) 0.363(19) Uani 0.5 1 d D U P . .
H40A H 0.611903 -0.041492 0.249879 0.435 Uiso 0.5 1 calc R U P . .
H40B H 0.567518 -0.067686 0.213742 0.435 Uiso 0.5 1 calc R U P . .
C41A C 0.6224(17) 0.000000 0.1961(11) 0.50(3) Uani 1 2 d DS TU P . .
H41A H 0.666843 -0.017860 0.187461 0.757 Uiso 0.5 1 calc R U P . .
H41B H 0.591278 0.006767 0.172893 0.757 Uiso 0.5 1 calc R U P . .
H41C H 0.635495 0.032862 0.208892 0.757 Uiso 0.5 1 calc R U P . .
P40B P 0.2662(3) 0.11880(18) 0.000000 0.0930(11) Uani 0.5 2 d DS T P A 1
O13B O 0.0593(4) 0.0617(2) 0.07902(18) 0.0545(16) Uani 0.5 1 d . . P A 1
O40B O 0.2103(9) 0.0720(5) 0.000000 0.145(5) Uani 0.5 2 d DS T P A 1
C10B C 0.2016(6) 0.1856(3) 0.0751(2) 0.065(2) Uani 0.5 1 d . . P A 1
C11B C 0.2283(7) 0.2050(5) 0.1109(4) 0.066(3) Uani 0.5 1 d . . P A 1
H11B H 0.259656 0.234255 0.111368 0.079 Uiso 0.5 1 calc R U P A 1
C12B C 0.207(2) 0.180(2) 0.1469(10) 0.064(7) Uani 0.5 1 d . . P A 1
C13B C 0.1585(7) 0.1381(7) 0.1447(5) 0.044(2) Uani 0.5 1 d . . P A 1
H13B H 0.140015 0.123874 0.168854 0.053 Uiso 0.5 1 calc R U P A 1
C14B C 0.1379(6) 0.1181(5) 0.1111(4) 0.048(3) Uani 0.5 1 d . . P A 1
C15B C 0.1541(6) 0.1433(3) 0.0757(2) 0.062(2) Uani 0.5 1 d . . P A 1
H15B H 0.132534 0.131752 0.051499 0.074 Uiso 0.5 1 calc R U P A 1
C17B C 0.0851(6) 0.0744(4) 0.1126(4) 0.040(2) Uani 0.5 1 d . . P A 1
C20B C 0.2228(6) 0.1859(5) 0.000000 0.075(3) Uani 0.5 2 d DS T P A 1
C21B C 0.2169(4) 0.2125(3) 0.0358(2) 0.069(2) Uani 0.5 1 d D . P A 1
C22B C 0.2049(5) 0.2673(3) 0.03560(19) 0.098(4) Uani 0.5 1 d D . P A 1
H22B H 0.200845 0.285709 0.060062 0.118 Uiso 0.5 1 calc R U P A 1
C23B C 0.1994(8) 0.2927(5) 0.000000 0.134(9) Uani 0.5 2 d DS T P A 1
H23B H 0.191455 0.329054 0.000000 0.161 Uiso 0.5 2 calc R U P A 1
C40B C 0.3226(9) 0.1130(6) 0.0417(3) 0.134(5) Uani 0.5 1 d D . P A 1
H40C H 0.292046 0.114666 0.066096 0.161 Uiso 0.5 1 calc R U P A 1
H40D H 0.345997 0.078419 0.041148 0.161 Uiso 0.5 1 calc R U P A 1
C41B C 0.3827(17) 0.1543(15) 0.0449(8) 0.35(3) Uani 0.5 1 d D U P A 1
H41D H 0.411698 0.148212 0.069043 0.531 Uiso 0.5 1 calc R U P A 1
H41E H 0.414319 0.152389 0.021323 0.531 Uiso 0.5 1 calc R U P A 1
H41F H 0.360263 0.188706 0.046319 0.531 Uiso 0.5 1 calc R U P A 1
P40C P 0.1438(3) 0.19166(16) 0.000000 0.0914(11) Uani 0.5 2 d DS T P A 2
O13C O 0.0894(4) 0.0422(3) 0.0797(2) 0.0547(15) Uani 0.5 1 d . . P A 2
O40C O 0.0834(8) 0.1397(5) 0.000000 0.131(4) Uani 0.5 2 d DS T P A 2
C10C C 0.2444(7) 0.1599(5) 0.0754(2) 0.083(3) Uani 0.5 1 d . . P A 2
C11C C 0.2569(7) 0.1877(5) 0.1100(4) 0.070(4) Uani 0.5 1 d . . P A 2
H11C H 0.289742 0.216095 0.108937 0.084 Uiso 0.5 1 calc R U P A 2
C12C C 0.225(2) 0.176(2) 0.1456(10) 0.064(7) Uani 0.5 1 d . . P A 2
C13C C 0.1798(7) 0.1335(7) 0.1487(5) 0.044(2) Uani 0.5 1 d . . P A 2
H13C H 0.160749 0.123017 0.173827 0.053 Uiso 0.5 1 calc R U P A 2
C14C C 0.1627(7) 0.1051(6) 0.1126(4) 0.059(3) Uani 0.5 1 d . . P A 2
C15C C 0.1953(6) 0.1180(4) 0.0766(2) 0.073(2) Uani 0.5 1 d . . P A 2
H15C H 0.184586 0.098850 0.053083 0.087 Uiso 0.5 1 calc R U P A 2
C17C C 0.1071(8) 0.0625(5) 0.1122(4) 0.050(3) Uani 0.5 1 d . . P A 2
C20C C 0.2424(7) 0.1718(5) 0.000000 0.075(3) Uani 0.5 2 d DS T P A 2
C21C C 0.2789(5) 0.1729(3) 0.0358(2) 0.098(4) Uani 0.5 1 d D . P A 2
C22C C 0.3560(7) 0.1753(7) 0.0360(2) 0.177(11) Uani 0.5 1 d D . P A 2
H22C H 0.381827 0.176076 0.060610 0.212 Uiso 0.5 1 calc R U P A 2
C23C C 0.3938(8) 0.1765(10) 0.000000 0.205(16) Uani 0.5 2 d DS T P A 2
H23C H 0.445567 0.178168 0.000000 0.246 Uiso 0.5 2 calc R U P A 2
C40C C 0.1280(9) 0.2271(6) 0.0413(3) 0.137(5) Uani 0.5 1 d D . P A 2
H40E H 0.143766 0.205758 0.064382 0.164 Uiso 0.5 1 calc R U P A 2
H40F H 0.161522 0.257094 0.040174 0.164 Uiso 0.5 1 calc R U P A 2
C41C C 0.0471(13) 0.2499(18) 0.0525(14) 0.61(4) Uani 0.5 1 d D U P A 2
H41G H 0.049844 0.269336 0.077594 0.918 Uiso 0.5 1 calc R U P A 2
H41H H 0.030566 0.272953 0.031009 0.918 Uiso 0.5 1 calc R U P A 2
H41I H 0.012667 0.221204 0.055411 0.918 Uiso 0.5 1 calc R U P A 2
C16B C 0.2344(2) 0.20435(15) 0.18481(11) 0.0596(9) Uani 1 1 d . . . . .
O10A O 0.30729(16) 0.18055(12) 0.27736(9) 0.0715(8) Uani 1 1 d . . . . .
O11A O 0.36911(15) 0.24199(11) 0.24503(9) 0.0705(7) Uani 1 1 d . . . . .
O10B O 0.27070(17) 0.24497(11) 0.18280(8) 0.0711(8) Uani 1 1 d . . . . .
O11B O 0.20875(17) 0.18390(11) 0.21565(8) 0.0685(8) Uani 1 1 d . . . . .
O12B O 0.07498(15) 0.05331(9) 0.14525(6) 0.0569(6) Uani 1 1 d . . . . .
O100 O 0.1491(2) 0.15370(12) 0.30109(10) 0.0888(10) Uani 1 1 d . . . . .
O200 O 0.000000 0.000000 0.22158(15) 0.0684(15) Uani 1 4 d S T P . .
Cl1 Cl 0.000000 0.000000 0.000000 0.0478(5) Uani 1 8 d S T P A .
P40A P 0.500000 0.000000 0.24130(9) 0.1130(12) Uani 1 4 d DS T P . .
O40A O 0.500000 0.0521(4) 0.2220(4) 0.130(6) Uani 0.5 2 d DS T P . .
Cu1 Cu 0.21264(3) 0.21349(2) 0.26913(2) 0.04865(19) Uani 1 1 d . . . . .
Cu2 Cu 0.000000 0.000000 0.15194(2) 0.0444(3) Uani 1 4 d S T P A .
Cu3 Cu 0.000000 0.000000 0.07209(2) 0.0385(2) Uani 1 4 d S T P . .
O50 O 0.000000 0.1479(8) 0.000000 0.116(6) Uani 0.5 4 d S T P B 3
C60 C 0.235(2) 0.000000 0.0368(5) 0.34(3) Uani 0.5 2 d DS TU P C 3
H60A H 0.205396 0.000000 0.061282 0.506 Uiso 0.5 2 calc R U P C 3
H60B H 0.265717 -0.030973 0.036301 0.506 Uiso 0.25 1 calc R U P C 3
H60C H 0.265717 0.030973 0.036301 0.506 Uiso 0.25 1 calc R U P C 3
N60 N 0.1841(19) 0.000000 0.000000 0.183(13) Uani 0.5 4 d DS TU P C 3
H60D H 0.155168 0.028626 0.000000 0.220 Uiso 0.25 2 calc R U P C 3
H60E H 0.155168 -0.028626 0.000000 0.220 Uiso 0.25 2 calc R U P C 3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
C11A C10A C11A 118.9(5) . 12_655
C11A C10A C21A 120.6(3) . .
C11A C10A C21A 120.6(3) 12_655 .
C10A C11A C12A 121.2(4) . .
C10A C11A H11A 119.4 . .
C12A C11A H11A 119.4 . .
C11A C12A C13A 119.1(4) . .
C11A C12A C14A 121.0(4) . .
C13A C12A C14A 119.9(4) . .
C12A C13A C12A 120.4(6) 12_655 .
C12A C13A H13A 119.8 12_655 .
C12A C13A H13A 119.8 . .
O10A C14A O11A 125.4(4) . .
O10A C14A C12A 118.3(4) . .
O11A C14A C12A 116.4(4) . .
C21A C20A C21A 119.0(7) 2_655 .
C21A C20A P40A 120.5(4) 2_655 .
C21A C20A P40A 120.5(4) . .
C22A C21A C20A 119.8(6) . .
C22A C21A C10A 114.5(5) . .
C20A C21A C10A 125.8(5) . .
C21A C22A C23A 121.5(6) . .
C21A C22A H22A 119.3 . .
C23A C22A H22A 119.3 . .
C22A C23A C22A 118.5(9) 11 .
C22A C23A H23A 120.7 11 .
C22A C23A H23A 120.7 . .
C41A C40A P40A 107.8(15) . .
C41A C40A H40A 110.1 . .
P40A C40A H40A 110.1 . .
C41A C40A H40B 110.1 . .
P40A C40A H40B 110.1 . .
H40A C40A H40B 108.5 . .
C41A C40A H41C 39.4(5) . 11
P40A C40A H41C 146.8(18) . 11
H40A C40A H41C 84.8 . 11
H40B C40A H41C 91.6 . 11
C40A C41A H41A 109.5 . .
C40A C41A H41B 109.5 . .
H41A C41A H41B 109.5 . .
C40A C41A H41C 109.5 . .
H41A C41A H41C 109.5 . .
H41B C41A H41C 109.5 . .
C40A C41A H41A 150.9(17) . 11
H41A C41A H41A 56.2 . 11
H41B C41A H41A 99.5 . 11
H41C C41A H41A 61.2 . 11
C40A C41A H41B 97.4(18) . 11
H41A C41A H41B 99.5 . 11
H41B C41A H41B 20.6 . 11
H41C C41A H41B 130.0 . 11
H41A C41A H41B 109.5 11 11
C40A C41A H41C 48.6(11) . 11
H41A C41A H41C 61.2 . 11
H41B C41A H41C 130.0 . 11
H41C C41A H41C 120.1 . 11
H41A C41A H41C 109.5 11 11
H41B C41A H41C 109.5 11 11
O40B P40B C40B 108.5(6) . .
O40B P40B C40B 108.5(6) . 10
C40B P40B C40B 106.3(10) . 10
O40B P40B C20B 115.0(7) . .
C40B P40B C20B 109.0(6) . .
C40B P40B C20B 109.0(6) 10 .
C17B O13B Cu3 121.9(7) . .
C11B C10B C15B 119.3(9) . .
C11B C10B C21B 121.2(9) . .
C15B C10B C21B 119.2(7) . .
C10B C11B C12B 117.9(17) . .
C10B C11B H11B 121.1 . .
C12B C11B H11B 121.1 . .
C13B C12B C11B 119(3) . .
C13B C12B C16B 126(2) . .
C11B C12B C16B 115(2) . .
C14B C13B C12B 123(2) . .
C14B C13B H13B 118.7 . .
C12B C13B H13B 118.7 . .
C13B C14B C15B 119.5(13) . .
C13B C14B C17B 117.6(14) . .
C15B C14B C17B 121.8(10) . .
C14B C15B C10B 121.0(8) . .
C14B C15B H15B 119.5 . .
C10B C15B H15B 119.5 . .
O12B C17B O13B 128.1(11) . .
O12B C17B C14B 117.5(11) . .
O13B C17B C14B 114.2(10) . .
C21B C20B C21B 119.7(10) . 10
C21B C20B P40B 118.9(5) . .
C21B C20B P40B 118.9(5) 10 .
C20B C21B C22B 119.9(7) . .
C20B C21B C10B 122.5(7) . .
C22B C21B C10B 115.4(7) . .
C23B C22B C21B 119.5(6) . .
C23B C22B H22B 120.3 . .
C21B C22B H22B 120.3 . .
C22B C23B C22B 121.6(10) 10 .
C22B C23B H23B 119.2 10 .
C22B C23B H23B 119.2 . .
C41B C40B P40B 114.8(15) . .
C41B C40B H40C 108.6 . .
P40B C40B H40C 108.6 . .
C41B C40B H40D 108.6 . .
P40B C40B H40D 108.6 . .
H40C C40B H40D 107.5 . .
C40B C41B H41D 109.5 . .
C40B C41B H41E 109.5 . .
H41D C41B H41E 109.5 . .
C40B C41B H41F 109.5 . .
H41D C41B H41F 109.5 . .
H41E C41B H41F 109.5 . .
C40C P40C O40C 108.1(6) . .
C40C P40C O40C 108.1(6) 10 .
C40C P40C C20C 108.2(6) . .
C40C P40C C20C 108.2(6) 10 .
O40C P40C C20C 113.7(7) . .
C17C O13C Cu3 123.9(9) . .
C11C C10C C15C 118.7(10) . .
C11C C10C C21C 123.4(10) . .
C15C C10C C21C 117.8(7) . .
C12C C11C C10C 123.3(18) . .
C12C C11C H11C 118.3 . .
C10C C11C H11C 118.3 . .
C11C C12C C13C 120(3) . .
C11C C12C C16B 127(2) . .
C13C C12C C16B 113(2) . .
C12C C13C C14C 118(2) . .
C12C C13C H13C 120.9 . .
C14C C13C H13C 120.9 . .
C15C C14C C13C 120.7(14) . .
C15C C14C C17C 117.5(12) . .
C13C C14C C17C 121.8(14) . .
C14C C15C C10C 119.1(9) . .
C14C C15C H15C 120.4 . .
C10C C15C H15C 120.4 . .
O13C C17C O12B 123.8(14) . .
O13C C17C C14C 119.5(13) . .
O12B C17C C14C 116.2(12) . .
C21C C20C P40C 117.7(5) . .
C21C C20C P40C 117.7(5) 10 .
C20C C21C C22C 119.6(8) . .
C20C C21C C10C 123.9(8) . .
C22C C21C C10C 115.1(8) . .
C23C C22C C21C 119.6(7) . .
C23C C22C H22C 120.2 . .
C21C C22C H22C 120.2 . .
C22C C23C C22C 120.1(12) 10 .
C22C C23C H23C 119.9 10 .
C22C C23C H23C 119.9 . .
C41C C40C P40C 122.5(17) . .
C41C C40C H40E 106.7 . .
P40C C40C H40E 106.7 . .
C41C C40C H40F 106.7 . .
P40C C40C H40F 106.7 . .
H40E C40C H40F 106.6 . .
C40C C41C H41G 109.5 . .
C40C C41C H41H 109.5 . .
H41G C41C H41H 109.5 . .
C40C C41C H41I 109.5 . .
H41G C41C H41I 109.5 . .
H41H C41C H41I 109.5 . .
O10B C16B O11B 127.0(3) . .
O10B C16B C12B 119.3(15) . .
O11B C16B C12B 113.1(13) . .
O10B C16B C12C 114.8(14) . .
O11B C16B C12C 118.1(14) . .
C14A O10A Cu1 121.7(3) . .
C14A O11A Cu1 125.6(3) . 13
C16B O10B Cu1 120.1(3) . 13
C16B O11B Cu1 125.3(2) . .
C17B O12B Cu2 121.1(6) . .
C17C O12B Cu2 123.6(7) . .
Cu3 Cl1 Cu3 180.0 9 .
O40A P40A O40A 128.6(10) 2_655 .
O40A P40A C40A 55.6(9) 2_655 12_655
O40A P40A C40A 108.9(7) . 12_655
O40A P40A C40A 108.9(7) 2_655 11
O40A P40A C40A 55.6(9) . 11
C40A P40A C40A 147.6(13) 12_655 11
O40A P40A C40A 55.6(9) 2_655 .
O40A P40A C40A 108.9(7) . .
C40A P40A C40A 111.0(17) 12_655 .
C40A P40A C40A 59.1(16) 11 .
O40A P40A C40A 108.9(7) 2_655 2_655
O40A P40A C40A 55.6(9) . 2_655
C40A P40A C40A 59.1(16) 12_655 2_655
C40A P40A C40A 111.0(17) 11 2_655
C40A P40A C40A 147.6(13) . 2_655
O40A P40A C20A 115.7(5) 2_655 .
O40A P40A C20A 115.7(5) . .
C40A P40A C20A 106.2(7) 12_655 .
C40A P40A C20A 106.2(7) 11 .
C40A P40A C20A 106.2(7) . .
C40A P40A C20A 106.2(7) 2_655 .
P40A O40A C40A 72.2(9) . 11
P40A O40A C40A 72.2(9) . 2_655
C40A O40A C40A 144.0(19) 11 2_655
O11B Cu1 O11A 88.88(13) . 13
O11B Cu1 O10A 89.48(13) . .
O11A Cu1 O10A 167.34(12) 13 .
O11B Cu1 O10B 167.44(11) . 13
O11A Cu1 O10B 89.77(14) 13 13
O10A Cu1 O10B 89.11(14) . 13
O11B Cu1 O100 98.67(12) . .
O11A Cu1 O100 97.18(13) 13 .
O10A Cu1 O100 95.47(13) . .
O10B Cu1 O100 93.90(12) 13 .
O11B Cu1 Cu1 81.69(8) . 13
O11A Cu1 Cu1 81.98(9) 13 13
O10A Cu1 Cu1 85.36(9) . 13
O10B Cu1 Cu1 85.75(8) 13 13
O100 Cu1 Cu1 179.09(11) . 13
O12B Cu2 O12B 166.88(13) . 2
O12B Cu2 O12B 89.14(16) . 12
O12B Cu2 O12B 89.36(16) 2 12
O12B Cu2 O12B 89.36(16) . 11
O12B Cu2 O12B 89.15(16) 2 11
O12B Cu2 O12B 166.88(13) 12 11
O12B Cu2 O200 96.56(6) . .
O12B Cu2 O200 96.56(6) 2 .
O12B Cu2 O200 96.56(6) 12 .
O12B Cu2 O200 96.56(6) 11 .
O12B Cu2 Cu3 83.44(6) . .
O12B Cu2 Cu3 83.44(6) 2 .
O12B Cu2 Cu3 83.44(6) 12 .
O12B Cu2 Cu3 83.44(6) 11 .
O200 Cu2 Cu3 180.0 . .
O13B Cu3 O13B 166.3(4) . 2
O13B Cu3 O13B 68.0(4) . 12
O13B Cu3 O13B 110.2(4) 2 12
O13B Cu3 O13B 110.2(4) . 11
O13B Cu3 O13B 68.0(4) 2 11
O13B Cu3 O13B 166.3(4) 12 11
O13B Cu3 O13C 153.78(19) . 2
O13B Cu3 O13C 21.9(2) 2 2
O13B Cu3 O13C 88.4(3) 12 2
O13B Cu3 O13C 89.8(3) 11 2
O13B Cu3 O13C 88.4(3) . 11
O13B Cu3 O13C 89.8(3) 2 11
O13B Cu3 O13C 153.78(19) 12 11
O13B Cu3 O13C 21.9(2) 11 11
O13B Cu3 O13C 89.8(3) . 12
O13B Cu3 O13C 88.4(3) 2 12
O13B Cu3 O13C 21.9(2) 12 12
O13B Cu3 O13C 153.78(19) 11 12
O13C Cu3 O13C 165.2(4) 2 .
O13C Cu3 O13C 66.6(4) 11 .
O13C Cu3 O13C 111.3(4) 12 .
O13B Cu3 Cl1 96.85(18) . .
O13B Cu3 Cl1 96.85(18) 2 .
O13B Cu3 Cl1 96.85(18) 12 .
O13B Cu3 Cl1 96.85(18) 11 .
O13C Cu3 Cl1 97.4(2) 2 .
O13C Cu3 Cl1 97.4(2) 11 .
O13C Cu3 Cl1 97.4(2) 12 .
O13C Cu3 Cl1 97.4(2) . .
O13B Cu3 Cu2 83.15(18) . .
O13B Cu3 Cu2 83.15(18) 2 .
O13B Cu3 Cu2 83.15(18) 12 .
O13B Cu3 Cu2 83.15(18) 11 .
O13C Cu3 Cu2 82.6(2) 2 .
O13C Cu3 Cu2 82.6(2) 11 .
O13C Cu3 Cu2 82.6(2) 12 .
O13C Cu3 Cu2 82.6(2) . .
Cl1 Cu3 Cu2 180.0 . .
N60 C60 H60A 109.5 . .
N60 C60 H60B 109.5 . .
H60A C60 H60B 109.5 . .
N60 C60 H60C 109.5 . .
H60A C60 H60C 109.5 . .
H60B C60 H60C 109.5 . .
C60 N60 H60D 110.6 . .
C60 N60 H60D 110.6 4 .
C60 N60 H60E 110.6 . .
C60 N60 H60E 110.6 4 .
H60D N60 H60E 108.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C10A C11A 1.385(5) .
C10A C11A 1.385(5) 12_655
C10A C21A 1.508(8) .
C11A C12A 1.387(6) .
C11A H11A 0.9500 .
C12A C13A 1.393(5) .
C12A C14A 1.473(6) .
C13A H13A 0.9500 .
C14A O10A 1.245(5) .
C14A O11A 1.264(5) .
C20A C21A 1.395(6) 2_655
C20A C21A 1.395(6) .
C20A P40A 1.833(8) .
C21A C22A 1.348(9) .
C22A C23A 1.378(9) .
C22A H22A 0.9500 .
C23A H23A 0.9500 .
C40A C41A 1.544(16) .
C40A P40A 1.798(14) .
C40A H40A 0.9900 .
C40A H40B 0.9900 .
C40A H41C 1.16(2) 11
C41A H41A 0.9800 .
C41A H41B 0.9800 .
C41A H41C 0.9800 .
C41A H41A 0.9800 11
C41A H41B 0.9801 11
C41A H41C 0.9800 11
P40B O40B 1.584(12) .
P40B C40B 1.744(12) .
P40B C40B 1.744(12) 10
P40B C20B 1.907(12) .
O13B C17B 1.262(13) .
O13B Cu3 1.943(6) .
C10B C11B 1.388(14) .
C10B C15B 1.396(11) .
C10B C21B 1.513(11) .
C11B C12B 1.42(4) .
C11B H11B 0.9500 .
C12B C13B 1.40(3) .
C12B C16B 1.50(3) .
C13B C14B 1.294(19) .
C13B H13B 0.9500 .
C14B C15B 1.382(15) .
C14B C17B 1.489(17) .
C15B H15B 0.9500 .
C17B O12B 1.234(12) .
C20B C21B 1.384(9) .
C20B C21B 1.384(9) 10
C21B C22B 1.432(11) .
C22B C23B 1.364(9) .
C22B H22B 0.9500 .
C23B H23B 0.9500 .
C40B C41B 1.537(17) .
C40B H40C 0.9900 .
C40B H40D 0.9900 .
C41B H41D 0.9800 .
C41B H41E 0.9800 .
C41B H41F 0.9800 .
P40C C40C 1.683(9) .
P40C C40C 1.683(9) 10
P40C O40C 1.739(11) .
P40C C20C 1.879(13) .
O13C C17C 1.249(15) .
O13C Cu3 1.984(7) .
C10C C11C 1.383(16) .
C10C C15C 1.409(13) .
C10C C21C 1.506(12) .
C11C C12C 1.36(3) .
C11C H11C 0.9500 .
C12C C13C 1.38(3) .
C12C C16B 1.51(3) .
C13C C14C 1.45(2) .
C13C H13C 0.9500 .
C14C C15C 1.383(17) .
C14C C17C 1.50(2) .
C15C H15C 0.9500 .
C17C O12B 1.276(15) .
C20C C21C 1.371(9) .
C20C C21C 1.371(9) 10
C21C C22C 1.415(14) .
C22C C23C 1.389(12) .
C22C H22C 0.9500 .
C23C H23C 0.9500 .
C40C C41C 1.639(16) .
C40C H40E 0.9900 .
C40C H40F 0.9900 .
C41C H41G 0.9800 .
C41C H41H 0.9800 .
C41C H41I 0.9800 .
C16B O10B 1.245(5) .
C16B O11B 1.251(5) .
O10A Cu1 1.952(3) .
O11A Cu1 1.948(3) 13
O10B Cu1 1.957(3) 13
O11B Cu1 1.946(2) .
O12B Cu2 1.959(2) .
O100 Cu1 2.210(3) .
O200 Cu2 2.329(5) .
Cl1 Cu3 2.4110(7) 9
Cl1 Cu3 2.4111(7) .
P40A O40A 1.492(10) 2_655
P40A O40A 1.492(10) .
Cu1 Cu1 2.6592(10) 13
Cu2 Cu3 2.6707(11) .
C60 N60 1.544(18) .
C60 H60A 0.9800 .
C60 H60B 0.9800 .
C60 H60C 0.9800 .
N60 H60D 0.9100 .
N60 H60E 0.9100 .
