# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cs2945
_database_code_depnum_ccdc_archive 'CCDC 2324983'
loop_
_audit_author_name
_audit_author_address
'Carla Slebodnick'
;Virginia Tech
United States of America
;
_audit_update_record             
;
2024-01-11 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_audit_creation_date             2023-03-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
tam9k@uvawise.edu
slebod@vt.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H40 Cu2 N2 O10, 3[C4H9N1O1]'
_chemical_formula_sum            'C64 H67 Cu2 N5 O13'
_chemical_formula_weight         1241.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C61 H62 Cu2 N4 O13'
_chemical_oxdiff_usercomment     'Trevor Makal - UVA Wise  (TM3125-08)'
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'
Cu Cu -1.9646 0.5888 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.7147(2)
_cell_length_b                   37.1847(6)
_cell_length_c                   14.7691(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.982(2)
_cell_angle_gamma                90
_cell_volume                     5876.38(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12078
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9760
_cell_measurement_theta_min      3.7750
_shelx_estimated_absorpt_T_max   0.944
_shelx_estimated_absorpt_T_min   0.879
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.71a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2592
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 1 0.0278
0 -1 -1 0.0278
-3 2 -5 0.0264
3 -2 5 0.0264
0 -5 3 0.0176
0 5 -3 0.0176
2 -5 -1 0.0397
-2 5 1 0.0397
6 13 1 0.0363
-6 -13 -1 0.0363

_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
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
-0.0000 0.9999 1.0000 -0.0536 0.0627 0.0763
0.0000 -0.9999 -1.0000 0.0536 -0.0627 -0.0763
-2.9998 2.0012 -4.9999 -0.0099 -0.0094 -0.6989
2.9998 -2.0012 4.9999 0.0099 0.0094 0.6989
-0.0001 -5.0007 2.9999 -0.2194 -0.1353 0.2731
0.0001 5.0007 -2.9999 0.2194 0.1353 -0.2731
1.9999 -5.0005 -1.0000 0.2437 -0.2384 0.1318
-1.9999 5.0005 1.0000 -0.2437 0.2384 -0.1318
6.0000 12.9998 1.0001 0.6928 0.5055 0.5676
-6.0000 -12.9998 -1.0001 -0.6928 -0.5055 -0.5676

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            47605
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         74.503
_diffrn_reflns_theta_min         3.223
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00 -10.00   0.50    1.00    --  -45.04 119.00 122.00  146
  2  ω   -117.00 -60.00   0.50    1.00    --  -45.04-158.00-117.00  114
  3  ω     40.00  65.00   0.50    1.00    --   45.04-119.00  36.00   50
  4  ω     59.00  84.00   0.50    1.00    --   45.04-158.00-117.00   50
  5  ω   -142.00-117.00   0.50    5.00    --  -88.50-119.00  36.00   50
  6  ω   -121.00 -96.00   0.50    5.00    --  -88.50-158.00-117.00   50
  7  ω    -76.00 -51.00   0.50    5.00    --  -88.50 119.00 122.00   50
  8  ω    -93.00 -68.00   0.50    5.00    --  -88.50 158.00 -83.00   50
  9  ω     93.00 129.00   0.50    5.00    --  110.00-158.00-117.00   72
 10  ω     75.00 108.00   0.50    5.00    --  110.00-119.00  36.00   66
 11  ω    105.00 142.00   0.50    5.00    --  110.00 119.00 122.00   74
 12  ω     88.00 128.00   0.50    5.00    --  110.00 158.00 -83.00   80
 13  ω   -114.00 -85.00   0.50    1.00    --  -45.04 -77.00  90.00   58
 14  ω   -117.00 -88.00   0.50    1.00    --  -45.04 -77.00-150.00   58
 15  ω   -111.00 -86.00   0.50    1.00    --  -45.04 -77.00 -60.00   50
 16  ω   -118.00 -89.00   0.50    1.00    --  -45.04 -77.00  30.00   58
 17  ω   -113.00 -85.00   0.50    1.00    --  -45.04 -77.00 -30.00   56
 18  ω     92.00 118.00   0.50    1.00    --   45.04  77.00 -90.00   52
 19  ω    -67.00 -15.00   0.50    5.00    --  -88.50  61.00 -30.00  104
 20  ω    -48.00 -16.00   0.50    5.00    --  -88.50  45.00 -60.00   64
 21  ω    -51.00 -15.00   0.50    5.00    --  -88.50  45.00 -30.00   72
 22  ω     42.00  69.00   0.50    5.00    --  110.00 -61.00 -90.00   54
 23  ω     38.00 101.00   0.50    5.00    --  110.00 -94.00-150.00  126
 24  ω    114.00 173.00   0.50    5.00    --  110.00  30.00  90.00  118
 25  ω    132.00 178.00   0.50    5.00    --  110.00  30.00 120.00   92
 26  ω     97.00 173.00   0.50    5.00    --  110.00  45.00 -60.00  152
 27  ω     42.00  67.00   0.50    5.00    --  110.00 -61.00  90.00   50
 28  ω     40.00  92.00   0.50    5.00    --  110.00-125.00 -30.00  104
 29  ω     98.00 128.00   0.50    5.00    --  110.00  30.00 120.00   60
 30  ω     45.00 102.00   0.50    5.00    --  110.00 -94.00  90.00  114
 31  ω     61.00 105.00   0.50    5.00    --  110.00 -94.00   0.00   88
 32  ω     38.00 106.00   0.50    5.00    --  110.00 -94.00  30.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku Oxford Diffraction XtaLAB Synergy, Dualflex, HyPix 6000-HE'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1097349000
_diffrn_orient_matrix_UB_12      0.0073307000
_diffrn_orient_matrix_UB_13      -0.0609151000
_diffrn_orient_matrix_UB_21      -0.0070250000
_diffrn_orient_matrix_UB_22      0.0404133000
_diffrn_orient_matrix_UB_23      0.0222805000
_diffrn_orient_matrix_UB_31      0.0929533000
_diffrn_orient_matrix_UB_32      -0.0055353000
_diffrn_orient_matrix_UB_33      0.0818057000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9193
_reflns_number_total             11844
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         11844
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0555
_refine_ls_restrained_S_all      1.048
_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)+(0.0770P)²+3.5511P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1491
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C18(H18), C20(H20), C25(H25), C26(H26), C27(H27), C28(H28), C32(H32),
  C33(H33), C34(H34), C35(H35), C38(H38), C40(H40), C42(H42)
2.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.77975(4) 0.72806(2) 1.00060(3) 0.02346(11) Uani 1 1 d . . . . .
Cu2 Cu 0.60011(4) 0.77745(2) 0.98818(2) 0.02190(11) Uani 1 1 d . . . . .
O1 O 0.6779(2) 0.69771(5) 0.91793(15) 0.0371(5) Uani 1 1 d . . . . .
O2 O 0.53694(19) 0.74184(5) 0.89759(13) 0.0290(4) Uani 1 1 d . . . . .
O3 O 0.3458(2) 0.73450(5) 0.58305(14) 0.0331(5) Uani 1 1 d . . . . .
O4 O 0.1919(2) 0.69328(5) 0.58038(14) 0.0311(4) Uani 1 1 d . . . . .
O5 O 0.79971(19) 0.30042(5) 0.60300(13) 0.0291(4) Uani 1 1 d . . . . .
O6 O 0.6621(2) 0.25462(5) 0.60364(14) 0.0323(4) Uani 1 1 d . . . . .
O7 O 0.4644(2) 0.25248(5) 0.91367(13) 0.0304(4) Uani 1 1 d . . . . .
O8 O 0.3096(2) 0.29308(6) 0.90101(15) 0.0364(5) Uani 1 1 d . . . . .
C1 C 0.4878(3) 0.51472(7) 0.74827(19) 0.0316(6) Uani 1 1 d . . . . .
C2 C 0.5948(3) 0.53635(8) 0.7382(2) 0.0337(7) Uani 1 1 d . . . . .
C3 C 0.7143(3) 0.52088(9) 0.7259(2) 0.0396(7) Uani 1 1 d . . . . .
H3 H 0.723207 0.495459 0.726001 0.048 Uiso 1 1 calc R U . . .
C4 C 0.8156(4) 0.54185(9) 0.7141(2) 0.0450(8) Uani 1 1 d . . . . .
H4 H 0.894644 0.531066 0.706071 0.054 Uiso 1 1 calc R U . . .
C5 C 0.8040(3) 0.57982(9) 0.7136(2) 0.0430(8) Uani 1 1 d . . . . .
H5 H 0.875670 0.594234 0.705048 0.052 Uiso 1 1 calc R U . . .
C6 C 0.6924(3) 0.59589(8) 0.7250(2) 0.0382(7) Uani 1 1 d . . . . .
H6 H 0.687053 0.621393 0.724502 0.046 Uiso 1 1 calc R U . . .
C7 C 0.5826(3) 0.57503(7) 0.73784(19) 0.0303(6) Uani 1 1 d . . . . .
C8 C 0.4651(3) 0.59087(7) 0.74872(19) 0.0299(6) Uani 1 1 d . . . . .
C9 C 0.3592(3) 0.56927(7) 0.7602(2) 0.0328(6) Uani 1 1 d . . . . .
C10 C 0.2385(3) 0.58398(8) 0.7768(2) 0.0412(8) Uani 1 1 d . . . . .
H10 H 0.228220 0.609336 0.778773 0.049 Uiso 1 1 calc R U . . .
C11 C 0.1398(4) 0.56261(9) 0.7896(3) 0.0485(9) Uani 1 1 d . . . . .
H11 H 0.061715 0.573167 0.801755 0.058 Uiso 1 1 calc R U . . .
C12 C 0.1498(4) 0.52471(9) 0.7854(3) 0.0487(9) Uani 1 1 d . . . . .
H12 H 0.078298 0.510104 0.792665 0.058 Uiso 1 1 calc R U . . .
C13 C 0.2619(3) 0.50925(8) 0.7710(2) 0.0421(8) Uani 1 1 d . . . . .
H13 H 0.267685 0.483781 0.768485 0.051 Uiso 1 1 calc R U . . .
C14 C 0.3719(3) 0.53051(7) 0.7594(2) 0.0327(6) Uani 1 1 d . . . . .
C15 C 0.4526(3) 0.63124(7) 0.7485(2) 0.0321(6) Uani 1 1 d . . . . .
C16 C 0.5181(3) 0.65165(7) 0.8136(2) 0.0303(6) Uani 1 1 d . . . . .
H16 H 0.568774 0.640062 0.859509 0.036 Uiso 1 1 calc R U . . .
C17 C 0.5099(3) 0.68913(7) 0.81216(19) 0.0287(6) Uani 1 1 d . . . . .
C18 C 0.4369(3) 0.70608(7) 0.74568(19) 0.0292(6) Uani 1 1 d . . . . .
H18 H 0.431936 0.731582 0.744430 0.035 Uiso 1 1 calc R U . . .
C19 C 0.3703(3) 0.68585(7) 0.68028(19) 0.0285(6) Uani 1 1 d . . . . .
C20 C 0.3772(3) 0.64846(7) 0.6818(2) 0.0308(6) Uani 1 1 d . . . . .
H20 H 0.330793 0.634704 0.637515 0.037 Uiso 1 1 calc R U . . .
C21 C 0.5803(3) 0.71156(7) 0.88132(18) 0.0262(6) Uani 1 1 d . . . . .
C22 C 0.2953(3) 0.70567(7) 0.60831(18) 0.0262(5) Uani 1 1 d . . . . .
C23 C 0.5024(3) 0.47473(8) 0.7494(2) 0.0331(6) Uani 1 1 d . . . . .
C24 C 0.5442(3) 0.45699(7) 0.8284(2) 0.0313(6) Uani 1 1 d . . . . .
C25 C 0.5777(3) 0.47639(8) 0.9102(2) 0.0349(7) Uani 1 1 d . . . . .
H25 H 0.569334 0.501826 0.910623 0.042 Uiso 1 1 calc R U . . .
C26 C 0.6208(4) 0.45952(9) 0.9863(2) 0.0418(8) Uani 1 1 d . . . . .
H26 H 0.640741 0.473070 1.039608 0.050 Uiso 1 1 calc R U . . .
C27 C 0.6365(4) 0.42160(9) 0.9873(2) 0.0411(7) Uani 1 1 d . . . . .
H27 H 0.668294 0.409865 1.040735 0.049 Uiso 1 1 calc R U . . .
C28 C 0.6057(3) 0.40207(8) 0.9112(2) 0.0363(7) Uani 1 1 d . . . . .
H28 H 0.616183 0.376706 0.912679 0.044 Uiso 1 1 calc R U . . .
C29 C 0.5582(3) 0.41862(7) 0.82948(19) 0.0300(6) Uani 1 1 d . . . . .
C30 C 0.5265(3) 0.39889(7) 0.75019(19) 0.0293(6) Uani 1 1 d . . . . .
C31 C 0.4827(3) 0.41624(7) 0.6709(2) 0.0335(6) Uani 1 1 d . . . . .
C32 C 0.4444(4) 0.39715(8) 0.5898(2) 0.0410(8) Uani 1 1 d . . . . .
H32 H 0.450087 0.371656 0.588939 0.049 Uiso 1 1 calc R U . . .
C33 C 0.4003(4) 0.41467(9) 0.5145(2) 0.0501(9) Uani 1 1 d . . . . .
H33 H 0.374549 0.401321 0.461945 0.060 Uiso 1 1 calc R U . . .
C34 C 0.3921(5) 0.45264(10) 0.5131(2) 0.0625(13) Uani 1 1 d . . . . .
H34 H 0.362153 0.464609 0.459419 0.075 Uiso 1 1 calc R U . . .
C35 C 0.4268(4) 0.47202(9) 0.5880(2) 0.0512(10) Uani 1 1 d . . . . .
H35 H 0.421887 0.497521 0.585851 0.061 Uiso 1 1 calc R U . . .
C36 C 0.4705(3) 0.45489(8) 0.6700(2) 0.0364(7) Uani 1 1 d . . . . .
C37 C 0.5392(3) 0.35869(7) 0.75175(19) 0.0291(6) Uani 1 1 d . . . . .
C38 C 0.6203(3) 0.34121(7) 0.69556(19) 0.0285(6) Uani 1 1 d . . . . .
H38 H 0.670404 0.354757 0.656764 0.034 Uiso 1 1 calc R U . . .
C39 C 0.6277(3) 0.30365(7) 0.69643(19) 0.0274(6) Uani 1 1 d . . . . .
C40 C 0.5612(3) 0.28377(7) 0.75659(18) 0.0270(5) Uani 1 1 d . . . . .
H40 H 0.569257 0.258336 0.758532 0.032 Uiso 1 1 calc R U . . .
C41 C 0.4834(3) 0.30104(7) 0.81365(19) 0.0277(6) Uani 1 1 d . . . . .
C42 C 0.4690(3) 0.33840(8) 0.8098(2) 0.0303(6) Uani 1 1 d . . . . .
H42 H 0.411220 0.349940 0.846807 0.036 Uiso 1 1 calc R U . . .
C43 C 0.7042(3) 0.28480(7) 0.62900(18) 0.0255(5) Uani 1 1 d . . . . .
C44 C 0.4131(3) 0.28029(7) 0.88167(18) 0.0259(5) Uani 1 1 d . . . . .
O9 O 0.9484(2) 0.69842(6) 1.01766(15) 0.0348(5) Uani 1 1 d . . . . .
N1 N 1.1507(3) 0.69224(9) 0.9896(2) 0.0497(7) Uani 1 1 d . . . . .
C45 C 1.0287(3) 0.69102(8) 0.9638(2) 0.0395(7) Uani 1 1 d . . . . .
C46 C 0.9940(4) 0.68049(11) 0.8678(3) 0.0552(10) Uani 1 1 d . . . . .
H46A H 1.016635 0.655283 0.858341 0.083 Uiso 1 1 calc R U . . .
H46B H 1.038988 0.695789 0.826349 0.083 Uiso 1 1 calc R U . . .
H46C H 0.903817 0.683528 0.855855 0.083 Uiso 1 1 calc R U . . .
C47 C 1.1883(4) 0.70043(13) 1.0832(3) 0.0631(11) Uani 1 1 d . . . . .
H47A H 1.116299 0.709579 1.114313 0.095 Uiso 1 1 calc R U . . .
H47B H 1.254391 0.718682 1.084792 0.095 Uiso 1 1 calc R U . . .
H47C H 1.219740 0.678551 1.113518 0.095 Uiso 1 1 calc R U . . .
C48 C 1.2478(5) 0.67861(18) 0.9350(4) 0.0885(18) Uani 1 1 d . . . . .
H48A H 1.260911 0.652996 0.947884 0.133 Uiso 1 1 calc R U . . .
H48B H 1.325505 0.691810 0.949262 0.133 Uiso 1 1 calc R U . . .
H48C H 1.223008 0.681752 0.870657 0.133 Uiso 1 1 calc R U . . .
O10 O 0.4322(2) 0.80814(6) 0.97259(15) 0.0349(5) Uani 1 1 d . . . . .
N2 N 0.2308(3) 0.79865(11) 0.9931(3) 0.0723(11) Uani 1 1 d . . . . .
C49 C 0.3401(4) 0.80694(12) 1.0185(3) 0.0635(12) Uani 1 1 d . . . . .
C50 C 0.3526(8) 0.81641(17) 1.1190(3) 0.103(2) Uani 1 1 d . . . . .
H50A H 0.440796 0.815278 1.140020 0.155 Uiso 1 1 calc R U . . .
H50B H 0.304362 0.799259 1.153423 0.155 Uiso 1 1 calc R U . . .
H50C H 0.320743 0.840775 1.128062 0.155 Uiso 1 1 calc R U . . .
C51 C 0.1141(5) 0.79878(19) 1.0328(6) 0.117(3) Uani 1 1 d . . . . .
H51A H 0.126995 0.799323 1.098960 0.176 Uiso 1 1 calc R U . . .
H51B H 0.067540 0.777047 1.014617 0.176 Uiso 1 1 calc R U . . .
H51C H 0.066596 0.820075 1.012440 0.176 Uiso 1 1 calc R U . . .
C52 C 0.2220(8) 0.78701(17) 0.8889(5) 0.114(3) Uani 1 1 d . . . . .
H52A H 0.171344 0.804564 0.853753 0.171 Uiso 1 1 calc R U . . .
H52B H 0.183070 0.763218 0.883045 0.171 Uiso 1 1 calc R U . . .
H52C H 0.306103 0.786110 0.865920 0.171 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Cu1 Cu2 2.6598(5) . ?
Cu1 O1 1.953(2) . ?
Cu1 O3 1.9580(19) 4_676 ?
Cu1 O6 1.958(2) 2_656 ?
Cu1 O8 1.947(2) 3_667 ?
Cu1 O9 2.120(2) . ?
Cu2 O2 1.9765(19) . ?
Cu2 O4 1.9663(19) 4_676 ?
Cu2 O5 1.961(2) 2_656 ?
Cu2 O7 1.9806(19) 3_667 ?
Cu2 O10 2.133(2) . ?
O1 C21 1.262(4) . ?
O2 C21 1.246(3) . ?
O3 C22 1.266(3) . ?
O4 C22 1.250(4) . ?
O5 C43 1.254(3) . ?
O6 C43 1.259(3) . ?
O7 C44 1.252(3) . ?
O8 C44 1.254(4) . ?
C1 C2 1.415(5) . ?
C1 C14 1.391(5) . ?
C1 C23 1.495(4) . ?
C2 C3 1.425(5) . ?
C2 C7 1.444(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.355(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.417(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.355(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.430(5) . ?
C7 C8 1.408(4) . ?
C8 C9 1.407(4) . ?
C8 C15 1.507(4) . ?
C9 C10 1.437(5) . ?
C9 C14 1.448(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.344(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.415(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.358(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.437(5) . ?
C15 C16 1.387(4) . ?
C15 C20 1.397(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.397(4) . ?
C17 C18 1.376(4) . ?
C17 C21 1.493(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.391(4) . ?
C19 C20 1.392(4) . ?
C19 C22 1.493(4) . ?
C20 H20 0.9500 . ?
C23 C24 1.393(4) . ?
C23 C36 1.412(4) . ?
C24 C25 1.436(4) . ?
C24 C29 1.434(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.348(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.420(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.364(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.424(4) . ?
C29 C30 1.409(4) . ?
C30 C31 1.396(4) . ?
C30 C37 1.501(4) . ?
C31 C32 1.434(4) . ?
C31 C36 1.443(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.353(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.415(5) . ?
C34 H34 0.9500 . ?
C34 C35 1.357(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.426(4) . ?
C37 C38 1.394(4) . ?
C37 C42 1.391(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.399(4) . ?
C39 C40 1.382(4) . ?
C39 C43 1.496(4) . ?
C40 H40 0.9500 . ?
C40 C41 1.375(4) . ?
C41 C42 1.398(4) . ?
C41 C44 1.501(4) . ?
C42 H42 0.9500 . ?
O9 C45 1.233(4) . ?
N1 C45 1.343(5) . ?
N1 C47 1.452(6) . ?
N1 C48 1.441(6) . ?
C45 C46 1.499(5) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
O10 C49 1.226(5) . ?
N2 C49 1.250(6) . ?
N2 C51 1.409(7) . ?
N2 C52 1.596(8) . ?
C49 C50 1.525(7) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?

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
O1 Cu1 Cu2 88.70(6) . . ?
O1 Cu1 O3 166.35(9) . 4_676 ?
O1 Cu1 O6 89.44(10) . 2_656 ?
O1 Cu1 O9 102.63(9) . . ?
O3 Cu1 Cu2 77.81(6) 4_676 . ?
O3 Cu1 O6 90.61(9) 4_676 2_656 ?
O3 Cu1 O9 90.99(9) 4_676 . ?
O6 Cu1 Cu2 81.73(6) 2_656 . ?
O6 Cu1 O9 92.96(9) 2_656 . ?
O8 Cu1 Cu2 87.04(6) 3_667 . ?
O8 Cu1 O1 87.31(10) 3_667 . ?
O8 Cu1 O3 89.94(10) 3_667 4_676 ?
O8 Cu1 O6 168.38(9) 3_667 2_656 ?
O8 Cu1 O9 98.65(9) 3_667 . ?
O9 Cu1 Cu2 167.49(6) . . ?
O2 Cu2 Cu1 78.77(6) . . ?
O2 Cu2 O7 89.93(9) . 3_667 ?
O2 Cu2 O10 91.61(8) . . ?
O4 Cu2 Cu1 90.02(6) 4_676 . ?
O4 Cu2 O2 168.76(9) 4_676 . ?
O4 Cu2 O7 89.15(9) 4_676 3_667 ?
O4 Cu2 O10 99.63(9) 4_676 . ?
O5 Cu2 Cu1 85.88(6) 2_656 . ?
O5 Cu2 O2 90.42(9) 2_656 . ?
O5 Cu2 O4 87.85(9) 2_656 4_676 ?
O5 Cu2 O7 166.37(9) 2_656 3_667 ?
O5 Cu2 O10 100.46(8) 2_656 . ?
O7 Cu2 Cu1 80.83(6) 3_667 . ?
O7 Cu2 O10 93.15(9) 3_667 . ?
O10 Cu2 Cu1 168.59(6) . . ?
C21 O1 Cu1 117.09(18) . . ?
C21 O2 Cu2 128.15(18) . . ?
C22 O3 Cu1 129.74(19) . 4_575 ?
C22 O4 Cu2 115.30(17) . 4_575 ?
C43 O5 Cu2 119.54(17) . 2_646 ?
C43 O6 Cu1 124.05(18) . 2_646 ?
C44 O7 Cu2 125.22(19) . 3_667 ?
C44 O8 Cu1 119.46(18) . 3_667 ?
C2 C1 C23 118.8(3) . . ?
C14 C1 C2 120.4(3) . . ?
C14 C1 C23 120.8(3) . . ?
C1 C2 C3 121.5(3) . . ?
C1 C2 C7 119.6(3) . . ?
C3 C2 C7 118.9(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.2(3) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.1(3) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 119.5 . . ?
C5 C6 C7 121.0(3) . . ?
C7 C6 H6 119.5 . . ?
C6 C7 C2 117.8(3) . . ?
C8 C7 C2 119.8(3) . . ?
C8 C7 C6 122.4(3) . . ?
C7 C8 C15 119.7(3) . . ?
C9 C8 C7 120.4(3) . . ?
C9 C8 C15 119.8(3) . . ?
C8 C9 C10 122.8(3) . . ?
C8 C9 C14 119.4(3) . . ?
C10 C9 C14 117.8(3) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 C9 121.4(3) . . ?
C11 C10 H10 119.3 . . ?
C10 C11 H11 119.3 . . ?
C10 C11 C12 121.4(4) . . ?
C12 C11 H11 119.3 . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.9(3) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 119.2 . . ?
C12 C13 C14 121.6(3) . . ?
C14 C13 H13 119.2 . . ?
C1 C14 C9 120.4(3) . . ?
C1 C14 C13 121.7(3) . . ?
C13 C14 C9 118.0(3) . . ?
C16 C15 C8 120.1(2) . . ?
C16 C15 C20 119.4(3) . . ?
C20 C15 C8 120.4(2) . . ?
C15 C16 H16 119.8 . . ?
C15 C16 C17 120.5(3) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C21 121.2(2) . . ?
C18 C17 C16 120.0(3) . . ?
C18 C17 C21 118.7(2) . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.0(3) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 120.3(3) . . ?
C18 C19 C22 117.7(2) . . ?
C20 C19 C22 122.0(2) . . ?
C15 C20 H20 120.1 . . ?
C19 C20 C15 119.8(3) . . ?
C19 C20 H20 120.1 . . ?
O1 C21 C17 116.3(2) . . ?
O2 C21 O1 126.5(2) . . ?
O2 C21 C17 117.2(2) . . ?
O3 C22 C19 113.9(2) . . ?
O4 C22 O3 126.9(2) . . ?
O4 C22 C19 119.2(2) . . ?
C24 C23 C1 120.6(3) . . ?
C24 C23 C36 120.1(3) . . ?
C36 C23 C1 119.3(3) . . ?
C23 C24 C25 121.4(3) . . ?
C23 C24 C29 120.6(3) . . ?
C29 C24 C25 118.0(3) . . ?
C24 C25 H25 119.1 . . ?
C26 C25 C24 121.8(3) . . ?
C26 C25 H25 119.1 . . ?
C25 C26 H26 119.8 . . ?
C25 C26 C27 120.4(3) . . ?
C27 C26 H26 119.8 . . ?
C26 C27 H27 120.1 . . ?
C28 C27 C26 119.8(3) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 119.1 . . ?
C27 C28 C29 121.9(3) . . ?
C29 C28 H28 119.1 . . ?
C28 C29 C24 118.1(3) . . ?
C30 C29 C24 119.2(3) . . ?
C30 C29 C28 122.6(3) . . ?
C29 C30 C37 119.2(2) . . ?
C31 C30 C29 120.8(2) . . ?
C31 C30 C37 120.0(3) . . ?
C30 C31 C32 122.7(3) . . ?
C30 C31 C36 119.6(3) . . ?
C32 C31 C36 117.6(3) . . ?
C31 C32 H32 119.3 . . ?
C33 C32 C31 121.4(3) . . ?
C33 C32 H32 119.3 . . ?
C32 C33 H33 119.6 . . ?
C32 C33 C34 120.8(3) . . ?
C34 C33 H33 119.6 . . ?
C33 C34 H34 119.9 . . ?
C35 C34 C33 120.3(3) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 119.3 . . ?
C34 C35 C36 121.3(3) . . ?
C36 C35 H35 119.3 . . ?
C23 C36 C31 119.6(3) . . ?
C23 C36 C35 121.8(3) . . ?
C35 C36 C31 118.6(3) . . ?
C38 C37 C30 120.9(3) . . ?
C42 C37 C30 119.9(3) . . ?
C42 C37 C38 119.2(3) . . ?
C37 C38 H38 120.1 . . ?
C37 C38 C39 119.8(3) . . ?
C39 C38 H38 120.1 . . ?
C38 C39 C43 119.6(2) . . ?
C40 C39 C38 120.6(3) . . ?
C40 C39 C43 119.7(2) . . ?
C39 C40 H40 120.2 . . ?
C41 C40 C39 119.6(3) . . ?
C41 C40 H40 120.2 . . ?
C40 C41 C42 120.5(3) . . ?
C40 C41 C44 120.8(2) . . ?
C42 C41 C44 118.7(3) . . ?
C37 C42 C41 120.1(3) . . ?
C37 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
O5 C43 O6 127.4(3) . . ?
O5 C43 C39 118.1(2) . . ?
O6 C43 C39 114.6(2) . . ?
O7 C44 O8 127.2(3) . . ?
O7 C44 C41 116.8(3) . . ?
O8 C44 C41 116.0(2) . . ?
C45 O9 Cu1 131.2(2) . . ?
C45 N1 C47 119.7(3) . . ?
C45 N1 C48 123.4(4) . . ?
C48 N1 C47 115.7(4) . . ?
O9 C45 N1 120.7(3) . . ?
O9 C45 C46 121.4(3) . . ?
N1 C45 C46 117.8(3) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N1 C47 H47A 109.5 . . ?
N1 C47 H47B 109.5 . . ?
N1 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N1 C48 H48A 109.5 . . ?
N1 C48 H48B 109.5 . . ?
N1 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C49 O10 Cu2 128.3(2) . . ?
C49 N2 C51 135.4(6) . . ?
C49 N2 C52 111.4(5) . . ?
C51 N2 C52 113.1(6) . . ?
O10 C49 N2 127.7(5) . . ?
O10 C49 C50 119.8(5) . . ?
N2 C49 C50 112.5(5) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N2 C51 H51A 109.5 . . ?
N2 C51 H51B 109.5 . . ?
N2 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N2 C52 H52A 109.5 . . ?
N2 C52 H52B 109.5 . . ?
N2 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

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
Cu1 O1 C21 O2 -5.7(4) . . . . ?
Cu1 O1 C21 C17 174.7(2) . . . . ?
Cu1 O3 C22 O4 5.4(4) 4_575 . . . ?
Cu1 O3 C22 C19 -173.47(19) 4_575 . . . ?
Cu1 O6 C43 O5 -11.6(4) 2_646 . . . ?
Cu1 O6 C43 C39 167.08(18) 2_646 . . . ?
Cu1 O8 C44 O7 6.8(4) 3_667 . . . ?
Cu1 O8 C44 C41 -172.19(18) 3_667 . . . ?
Cu1 O9 C45 N1 139.3(3) . . . . ?
Cu1 O9 C45 C46 -40.6(4) . . . . ?
Cu2 O2 C21 O1 -2.8(4) . . . . ?
Cu2 O2 C21 C17 176.79(19) . . . . ?
Cu2 O4 C22 O3 -0.5(4) 4_575 . . . ?
Cu2 O4 C22 C19 178.30(19) 4_575 . . . ?
Cu2 O5 C43 O6 0.6(4) 2_646 . . . ?
Cu2 O5 C43 C39 -178.07(18) 2_646 . . . ?
Cu2 O7 C44 O8 -4.7(4) 3_667 . . . ?
Cu2 O7 C44 C41 174.35(17) 3_667 . . . ?
Cu2 O10 C49 N2 -118.2(4) . . . . ?
Cu2 O10 C49 C50 62.0(5) . . . . ?
C1 C2 C3 C4 178.3(3) . . . . ?
C1 C2 C7 C6 -178.3(3) . . . . ?
C1 C2 C7 C8 0.9(4) . . . . ?
C1 C23 C24 C25 -1.7(5) . . . . ?
C1 C23 C24 C29 180.0(3) . . . . ?
C1 C23 C36 C31 -179.1(3) . . . . ?
C1 C23 C36 C35 1.2(5) . . . . ?
C2 C1 C14 C9 0.4(4) . . . . ?
C2 C1 C14 C13 -179.1(3) . . . . ?
C2 C1 C23 C24 81.2(4) . . . . ?
C2 C1 C23 C36 -100.3(4) . . . . ?
C2 C3 C4 C5 -0.1(5) . . . . ?
C2 C7 C8 C9 0.1(4) . . . . ?
C2 C7 C8 C15 179.9(2) . . . . ?
C3 C2 C7 C6 0.0(4) . . . . ?
C3 C2 C7 C8 179.2(3) . . . . ?
C3 C4 C5 C6 0.1(5) . . . . ?
C4 C5 C6 C7 -0.1(5) . . . . ?
C5 C6 C7 C2 0.0(5) . . . . ?
C5 C6 C7 C8 -179.1(3) . . . . ?
C6 C7 C8 C9 179.3(3) . . . . ?
C6 C7 C8 C15 -0.9(4) . . . . ?
C7 C2 C3 C4 0.1(5) . . . . ?
C7 C8 C9 C10 176.3(3) . . . . ?
C7 C8 C9 C14 -0.9(4) . . . . ?
C7 C8 C15 C16 -61.0(4) . . . . ?
C7 C8 C15 C20 117.7(3) . . . . ?
C8 C9 C10 C11 -178.4(3) . . . . ?
C8 C9 C14 C1 0.6(4) . . . . ?
C8 C9 C14 C13 -179.8(3) . . . . ?
C8 C15 C16 C17 178.1(3) . . . . ?
C8 C15 C20 C19 -177.6(3) . . . . ?
C9 C8 C15 C16 118.7(3) . . . . ?
C9 C8 C15 C20 -62.5(4) . . . . ?
C9 C10 C11 C12 -1.3(6) . . . . ?
C10 C9 C14 C1 -176.7(3) . . . . ?
C10 C9 C14 C13 2.9(4) . . . . ?
C10 C11 C12 C13 2.1(6) . . . . ?
C11 C12 C13 C14 -0.2(6) . . . . ?
C12 C13 C14 C1 177.4(3) . . . . ?
C12 C13 C14 C9 -2.2(5) . . . . ?
C14 C1 C2 C3 -179.4(3) . . . . ?
C14 C1 C2 C7 -1.2(4) . . . . ?
C14 C1 C23 C24 -97.0(4) . . . . ?
C14 C1 C23 C36 81.5(4) . . . . ?
C14 C9 C10 C11 -1.2(5) . . . . ?
C15 C8 C9 C10 -3.5(4) . . . . ?
C15 C8 C9 C14 179.4(3) . . . . ?
C15 C16 C17 C18 -0.2(5) . . . . ?
C15 C16 C17 C21 -179.6(3) . . . . ?
C16 C15 C20 C19 1.2(5) . . . . ?
C16 C17 C18 C19 0.5(5) . . . . ?
C16 C17 C21 O1 25.3(4) . . . . ?
C16 C17 C21 O2 -154.3(3) . . . . ?
C17 C18 C19 C20 0.0(5) . . . . ?
C17 C18 C19 C22 -178.4(3) . . . . ?
C18 C17 C21 O1 -154.1(3) . . . . ?
C18 C17 C21 O2 26.3(4) . . . . ?
C18 C19 C20 C15 -0.9(5) . . . . ?
C18 C19 C22 O3 36.2(4) . . . . ?
C18 C19 C22 O4 -142.7(3) . . . . ?
C20 C15 C16 C17 -0.7(5) . . . . ?
C20 C19 C22 O3 -142.2(3) . . . . ?
C20 C19 C22 O4 38.9(4) . . . . ?
C21 C17 C18 C19 179.9(3) . . . . ?
C22 C19 C20 C15 177.4(3) . . . . ?
C23 C1 C2 C3 2.4(4) . . . . ?
C23 C1 C2 C7 -179.4(3) . . . . ?
C23 C1 C14 C9 178.6(3) . . . . ?
C23 C1 C14 C13 -1.0(4) . . . . ?
C23 C24 C25 C26 -178.6(3) . . . . ?
C23 C24 C29 C28 177.7(3) . . . . ?
C23 C24 C29 C30 -1.4(5) . . . . ?
C24 C23 C36 C31 -0.6(5) . . . . ?
C24 C23 C36 C35 179.7(4) . . . . ?
C24 C25 C26 C27 1.1(6) . . . . ?
C24 C29 C30 C31 0.5(5) . . . . ?
C24 C29 C30 C37 -179.1(3) . . . . ?
C25 C24 C29 C28 -0.7(5) . . . . ?
C25 C24 C29 C30 -179.8(3) . . . . ?
C25 C26 C27 C28 -1.2(6) . . . . ?
C26 C27 C28 C29 0.3(6) . . . . ?
C27 C28 C29 C24 0.6(5) . . . . ?
C27 C28 C29 C30 179.7(3) . . . . ?
C28 C29 C30 C31 -178.6(3) . . . . ?
C28 C29 C30 C37 1.9(5) . . . . ?
C29 C24 C25 C26 -0.2(5) . . . . ?
C29 C30 C31 C32 -177.3(3) . . . . ?
C29 C30 C31 C36 0.3(5) . . . . ?
C29 C30 C37 C38 -118.4(3) . . . . ?
C29 C30 C37 C42 61.8(4) . . . . ?
C30 C31 C32 C33 178.8(4) . . . . ?
C30 C31 C36 C23 -0.3(5) . . . . ?
C30 C31 C36 C35 179.4(3) . . . . ?
C30 C37 C38 C39 -178.2(3) . . . . ?
C30 C37 C42 C41 -177.9(3) . . . . ?
C31 C30 C37 C38 62.1(4) . . . . ?
C31 C30 C37 C42 -117.8(3) . . . . ?
C31 C32 C33 C34 0.8(7) . . . . ?
C32 C31 C36 C23 177.5(3) . . . . ?
C32 C31 C36 C35 -2.8(5) . . . . ?
C32 C33 C34 C35 -1.0(8) . . . . ?
C33 C34 C35 C36 -0.9(8) . . . . ?
C34 C35 C36 C23 -177.6(4) . . . . ?
C34 C35 C36 C31 2.7(6) . . . . ?
C36 C23 C24 C25 179.8(3) . . . . ?
C36 C23 C24 C29 1.5(5) . . . . ?
C36 C31 C32 C33 1.1(5) . . . . ?
C37 C30 C31 C32 2.2(5) . . . . ?
C37 C30 C31 C36 179.9(3) . . . . ?
C37 C38 C39 C40 -4.1(4) . . . . ?
C37 C38 C39 C43 173.3(3) . . . . ?
C38 C37 C42 C41 2.2(4) . . . . ?
C38 C39 C40 C41 2.5(4) . . . . ?
C38 C39 C43 O5 32.0(4) . . . . ?
C38 C39 C43 O6 -146.9(3) . . . . ?
C39 C40 C41 C42 1.4(4) . . . . ?
C39 C40 C41 C44 -178.1(3) . . . . ?
C40 C39 C43 O5 -150.6(3) . . . . ?
C40 C39 C43 O6 30.6(4) . . . . ?
C40 C41 C42 C37 -3.9(4) . . . . ?
C40 C41 C44 O7 31.5(4) . . . . ?
C40 C41 C44 O8 -149.4(3) . . . . ?
C42 C37 C38 C39 1.7(4) . . . . ?
C42 C41 C44 O7 -148.1(3) . . . . ?
C42 C41 C44 O8 31.1(4) . . . . ?
C43 C39 C40 C41 -174.9(3) . . . . ?
C44 C41 C42 C37 175.7(3) . . . . ?
C47 N1 C45 O9 3.4(5) . . . . ?
C47 N1 C45 C46 -176.7(3) . . . . ?
C48 N1 C45 O9 169.9(4) . . . . ?
C48 N1 C45 C46 -10.2(6) . . . . ?
C51 N2 C49 O10 -173.3(5) . . . . ?
C51 N2 C49 C50 6.5(8) . . . . ?
C52 N2 C49 O10 3.0(6) . . . . ?
C52 N2 C49 C50 -177.2(4) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 558 electrons were 
found in a volume of 1996Å³ in 1 void per unit cell. 
This is consistent with the presence of 
3[C4H9N1O1] per asymmetric Unit 
which account for 576 electrons 
per unit cell.
;
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 -0.500 0.000 -0.245 997.5 279.3 '6 C4H9N1O1'
2 0.000 0.500 -0.384 997.5 279.3 '6 C4H9N1O1'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2022-11-03
_olex2_date_sample_submission    2022-11-03
_olex2_submission_original_sample_id TM3125-08
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.401
_oxdiff_exptl_absorpt_empirical_full_min 0.726
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cs3105
_database_code_depnum_ccdc_archive 'CCDC 2324984'
loop_
_audit_author_name
_audit_author_address
'Carla Slebodnick'
;Virginia Tech
United States of America
;
_audit_update_record             
;
2024-07-18 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_audit_creation_date             2024-07-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
tam9k@uvawise.edu
slebod@vt.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H22 Cu2 O10, 5[C2H6SO]'
_chemical_formula_sum            'C54 H52 Cu2 O15 S5'
_chemical_formula_weight         1228.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cu2 C44 H22 O8 H2 O C3 H7 N O C2 H6 S O'
_chemical_oxdiff_usercomment     'Abigail/Trevor Makal (TM4014 1)'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cu Cu -1.9646 0.5888 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_H-M_alt        'C c c m'
_space_group_name_Hall           '-C 2 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, 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, -y, z-1/2'
'-x, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z-1/2'

_cell_length_a                   10.4087(3)
_cell_length_b                   36.7583(8)
_cell_length_c                   15.4789(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5922.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11748
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      76.6580
_cell_measurement_theta_min      4.3560
_shelx_estimated_absorpt_T_max   0.941
_shelx_estimated_absorpt_T_min   0.657
_exptl_absorpt_coefficient_mu    3.055
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2536
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 0 0.0078
1 1 0 0.0078
-3 13 2 0.0295
3 -13 -2 0.0295
0 8 -5 0.0683
0 -4 5 0.0695

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Crystals grown in DMF and then soaked in DMSO.'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
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
-0.9981 -1.0012 -0.0007 -0.1487 0.0256 0.0286
0.9981 1.0012 0.0007 0.1487 -0.0256 -0.0286
-2.9932 13.0018 1.9901 -0.1008 0.4038 0.5986
2.9932 -13.0018 -1.9901 0.1008 -0.4038 -0.5986
-0.0059 8.0053 -4.9990 0.1488 0.5466 -0.2001
0.0056 -4.0038 4.9974 -0.0644 -0.4329 0.2902

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31846
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.137
_diffrn_reflns_theta_min         4.415
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -120.00 -33.00   0.50    5.00    --  -47.20 -52.00  21.00  174
  2  ω    -61.00  25.00   0.50    5.00    --  -47.20  52.00 166.00  172
  3  ω    -24.00  57.00   0.50    5.00    --   47.20 -52.00  21.00  162
  4  ω     34.00 120.00   0.50    5.00    --   47.20  52.00 166.00  172
  5  ω    -61.00 -14.00   0.50   30.00    --  -86.25  52.00 166.00   94
  6  ω   -159.00 -72.00   0.50   30.00    --  -86.25 -52.00  21.00  174
  7  ω     94.00 178.00   0.50   30.00    --  107.75  52.00 166.00  168
  8  ω    -86.00 -13.00   0.50    5.00    --  -47.20 125.00-120.00  146
  9  ω   -120.00 -85.00   0.50    5.00    --  -47.20 -77.00-120.00   70
 10  ω   -120.00 -85.00   0.50    5.00    --  -47.20 -77.00-150.00   70
 11  ω    -37.00 -11.00   0.50   30.00    --  -86.25  30.00 -60.00   52
 12  ω    -53.00 -14.00   0.50   30.00    --  -86.25  45.00   0.00   78
 13  ω    -37.00 -11.00   0.50   30.00    --  -86.25  30.00 -30.00   52
 14  ω     95.00 178.00   0.50   30.00    --  107.75 125.00  90.00  166
 15  ω     35.00  69.00   0.50   30.00    --  107.75 -61.00-180.00   68
 16  ω     35.00  69.00   0.50   30.00    --  107.75 -61.00  60.00   68
 17  ω     35.00 103.00   0.50   30.00    --  107.75 -77.00   0.00  136
 18  ω     35.00  69.00   0.50   30.00    --  107.75 -61.00 120.00   68
 19  ω     95.00 178.00   0.50   30.00    --  107.75  30.00 -60.00  166
 20  ω     35.00 103.00   0.50   30.00    --  107.75 -77.00-120.00  136
 21  ω     35.00  69.00   0.50   30.00    --  107.75 -61.00-120.00   68
 22  ω     35.00  69.00   0.50   30.00    --  107.75 -61.00 -90.00   68
 23  ω     35.00 103.00   0.50   30.00    --  107.75 -77.00  30.00  136
 24  ω     35.00  69.00   0.50   30.00    --  107.75 -61.00 -30.00   68
 25  ω     35.00 106.00   0.50   30.00    --  107.75 -94.00 120.00  142
 26  ω     95.00 178.00   0.50   30.00    --  107.75  45.00-120.00  166
 27  ω   -120.00 -32.00   0.50    5.00    --  -47.20 -57.00  90.00  176
 28  ω   -120.00 -32.00   0.50    5.00    --  -47.20 -57.00 -30.00  176
 29  ω     32.00  57.00   0.50    5.00    --   47.20  57.00-150.00   50
 30  ω     32.00 120.00   0.50    5.00    --   47.20  57.00 -90.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1278329000
_diffrn_orient_matrix_UB_12      0.0210850000
_diffrn_orient_matrix_UB_13      0.0038526000
_diffrn_orient_matrix_UB_21      -0.0540987000
_diffrn_orient_matrix_UB_22      0.0283757000
_diffrn_orient_matrix_UB_23      -0.0638387000
_diffrn_orient_matrix_UB_31      -0.0513718000
_diffrn_orient_matrix_UB_32      0.0225466000
_diffrn_orient_matrix_UB_33      0.0761994000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2648
_reflns_number_total             3226
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0671
_refine_ls_restrained_S_all      1.077
_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)+(0.0984P)²+19.1137P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2056
_refine_special_details          
;The Laue symmetry and systematic absences were consistent with the 
orthorhombic space group Cccm (#63).  However, based on the structure 
of compound 1-DMF (from the same manuscript, CCDC 2324985), we know that 
this space group occurs from pseudomerohedral twinning of space group 
P2/c. Unfortunately, this sample exhibited both multi-crystal 
(i.e., nonmerohedral) and pseudomerohedral twinning.  As a result, 
we were unable to obtain suitable quality data to refine in P2/c. 
Therefore, our only option was to process as the orthorhombic 
pseudomerohedral twin and refine as disordered in Cccm. The structure 
was solved using SHELXT  and refined using SHELXL  via Olex2.   The 
capping ligands of the paddlewheel complex are modeled as water but 
are likely a combination of water and DMSO. A 2-position disorder model 
was used for the anthracene fragments with relative occupancies 
constrained to 50% by symmetry. The solvent mask feature of OLEX2, 
was used to subtract out a total of 835 e-, equivalent to ~20 DMSO 
molecules (840 e-) from 2698 Å³ total void space per unit cell, 
or ~1.25 DMSO per asymmetric unit. The final refinement model involved 
anisotropic displacement parameters for non-hydrogen atoms and a riding 
model for all hydrogen atoms.,SQUEEZE
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C8A(0.5) C8B(0.5) C9A(0.5) H9A(0.5) C9B(0.5) H9B(0.5) C10A(0.5)
 H10A(0.5) C10B(0.5) H10B(0.5) C11A(0.5) H11A(0.5) C11B(0.5) H11B(0.5)
 C12A(0.5) H12A(0.5) C12B(0.5) H12B(0.5) C13A(0.5) C13B(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9A(H9A), C9B(H9B), C10A(H10A), C10B(H10B), C11A(H11A),
 C11B(H11B), C12A(H12A), C12B(H12B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.15997(7) 0.72415(2) 0.500000 0.0399(2) Uani 1 2 d S T P . .
O1 O 0.0169(4) 0.68320(11) 0.500000 0.0655(11) Uani 1 2 d S T P . .
O2 O 0.2670(3) 0.70057(7) 0.58728(19) 0.0582(7) Uani 1 1 d . . . . .
O3 O 0.4141(3) 0.74499(6) 0.59154(17) 0.0530(7) Uani 1 1 d . . . . .
C1 C 0.3681(4) 0.71549(9) 0.6160(2) 0.0469(8) Uani 1 1 d . . . . .
C2 C 0.4360(4) 0.69554(9) 0.6854(2) 0.0495(9) Uani 1 1 d . . . . .
C3 C 0.500000 0.71414(13) 0.750000 0.0501(12) Uani 1 2 d S T P . .
H3 H 0.500000 0.739980 0.749998 0.060 Uiso 1 2 calc R U P . .
C4 C 0.4320(4) 0.65764(9) 0.6872(2) 0.0501(9) Uani 1 1 d . . . . .
H4 H 0.382636 0.644826 0.645530 0.060 Uiso 1 1 calc R U . . .
C5 C 0.500000 0.63847(13) 0.750000 0.0491(12) Uani 1 2 d S T P A .
C6 C 0.500000 0.59734(12) 0.750000 0.0451(11) Uani 1 2 d S T P . .
C7 C 0.500000 0.52051(12) 0.750000 0.0491(12) Uani 1 2 d S T P . .
C8A C 0.4497(10) 0.58062(19) 0.8205(5) 0.055(2) Uani 0.5 1 d . . P A -1
C8B C 0.3906(7) 0.57695(18) 0.7773(5) 0.0428(15) Uani 0.5 1 d . . P A 2
C9A C 0.3886(11) 0.5981(2) 0.8914(6) 0.069(2) Uani 0.5 1 d . . P A -1
H9A H 0.380477 0.623881 0.890660 0.083 Uiso 0.5 1 calc R U P A -1
C9B C 0.2794(8) 0.5951(2) 0.8089(6) 0.0572(19) Uani 0.5 1 d . . P A 2
H9B H 0.279819 0.620897 0.812818 0.069 Uiso 0.5 1 calc R U P A 2
C10A C 0.3428(13) 0.5799(3) 0.9580(7) 0.090(4) Uani 0.5 1 d . . P A -1
H10A H 0.296366 0.592246 1.002019 0.108 Uiso 0.5 1 calc R U P A -1
C10B C 0.1703(12) 0.5762(3) 0.8340(8) 0.085(3) Uani 0.5 1 d . . P A 2
H10B H 0.096101 0.589000 0.852868 0.102 Uiso 0.5 1 calc R U P A 2
C11A C 0.3630(18) 0.5425(3) 0.9633(7) 0.134(7) Uani 0.5 1 d . . P A -1
H11A H 0.343422 0.530502 1.016047 0.160 Uiso 0.5 1 calc R U P A -1
C11B C 0.1704(9) 0.5376(3) 0.8315(7) 0.070(2) Uani 0.5 1 d . . P A 2
H11B H 0.096259 0.524563 0.849501 0.084 Uiso 0.5 1 calc R U P A 2
C12A C 0.4096(11) 0.52248(19) 0.8965(6) 0.077(3) Uani 0.5 1 d . . P A -1
H12A H 0.413204 0.496700 0.900122 0.093 Uiso 0.5 1 calc R U P A -1
C12B C 0.2736(10) 0.5194(2) 0.8039(6) 0.067(2) Uani 0.5 1 d . . P A 2
H12B H 0.270347 0.493576 0.803018 0.080 Uiso 0.5 1 calc R U P A 2
C13A C 0.4533(9) 0.54112(18) 0.8199(5) 0.0517(19) Uani 0.5 1 d . . P A -1
C13B C 0.3905(8) 0.53726(18) 0.7753(5) 0.0483(18) Uani 0.5 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Cu1 Cu1 2.6691(14) 13_566 ?
Cu1 O1 2.117(4) . ?
Cu1 O2 1.954(3) . ?
Cu1 O2 1.954(3) 10_556 ?
Cu1 O3 1.972(2) 13_566 ?
Cu1 O3 1.972(2) 6_565 ?
O2 C1 1.267(5) . ?
O3 C1 1.245(4) . ?
C1 C2 1.481(5) . ?
C2 C3 1.382(4) . ?
C2 C4 1.394(5) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C4 C5 1.393(4) . ?
C5 C6 1.512(6) . ?
C6 C8A 1.357(8) . ?
C6 C8B 1.427(8) . ?
C6 C8B 1.427(8) 3_656 ?
C7 C7 1.508(9) 2_665 ?
C7 C13A 1.407(8) . ?
C7 C13B 1.353(9) 3_656 ?
C7 C13B 1.353(9) . ?
C8A C9A 1.423(11) . ?
C8A C13A 1.452(9) . ?
C8B C9B 1.423(11) . ?
C8B C13B 1.460(9) . ?
C9A H9A 0.9500 . ?
C9A C10A 1.318(13) . ?
C9B H9B 0.9500 . ?
C9B C10B 1.387(14) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.394(15) . ?
C10B H10B 0.9500 . ?
C10B C11B 1.420(15) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.360(13) . ?
C11B H11B 0.9500 . ?
C11B C12B 1.335(14) . ?
C12A H12A 0.9500 . ?
C12A C13A 1.443(11) . ?
C12B H12B 0.9500 . ?
C12B C13B 1.452(13) . ?

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
O1 Cu1 Cu1 179.91(13) . 13_566 ?
O2 Cu1 Cu1 85.16(9) . 13_566 ?
O2 Cu1 Cu1 85.16(9) 10_556 13_566 ?
O2 Cu1 O1 94.90(12) . . ?
O2 Cu1 O1 94.90(12) 10_556 . ?
O2 Cu1 O2 87.50(18) . 10_556 ?
O2 Cu1 O3 88.92(12) . 6_565 ?
O2 Cu1 O3 88.92(12) 10_556 13_566 ?
O2 Cu1 O3 167.15(13) 10_556 6_565 ?
O2 Cu1 O3 167.15(13) . 13_566 ?
O3 Cu1 Cu1 82.24(8) 6_565 13_566 ?
O3 Cu1 Cu1 82.24(8) 13_566 13_566 ?
O3 Cu1 O1 97.70(12) 6_565 . ?
O3 Cu1 O1 97.70(12) 13_566 . ?
O3 Cu1 O3 91.86(16) 6_565 13_566 ?
C1 O2 Cu1 121.6(2) . . ?
C1 O3 Cu1 124.7(3) . 13_566 ?
O2 C1 C2 115.9(3) . . ?
O3 C1 O2 126.2(3) . . ?
O3 C1 C2 117.9(3) . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 C4 119.6(3) . . ?
C4 C2 C1 119.7(3) . . ?
C2 C3 C2 120.7(5) . 3_656 ?
C2 C3 H3 119.6 . . ?
C2 C3 H3 119.6 3_656 . ?
C2 C4 H4 119.9 . . ?
C5 C4 C2 120.3(3) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C4 119.2(4) . 3_656 ?
C4 C5 C6 120.4(2) 3_656 . ?
C4 C5 C6 120.4(2) . . ?
C8A C6 C5 116.9(3) . . ?
C8A C6 C8B 107.9(5) . 3_656 ?
C8B C6 C5 121.7(3) 3_656 . ?
C8B C6 C5 121.7(3) . . ?
C8B C6 C8B 116.7(7) 3_656 . ?
C13A C7 C7 122.6(3) . 2_665 ?
C13B C7 C13B 125.9(7) . 3_656 ?
C6 C8A C9A 126.0(6) . . ?
C6 C8A C13A 116.0(6) . . ?
C9A C8A C13A 118.0(7) . . ?
C6 C8B C13B 121.2(7) . . ?
C9B C8B C6 120.3(6) . . ?
C9B C8B C13B 118.4(7) . . ?
C8A C9A H9A 118.8 . . ?
C10A C9A C8A 122.4(8) . . ?
C10A C9A H9A 118.8 . . ?
C8B C9B H9B 119.1 . . ?
C10B C9B C8B 121.8(9) . . ?
C10B C9B H9B 119.1 . . ?
C9A C10A H10A 120.2 . . ?
C9A C10A C11A 119.5(9) . . ?
C11A C10A H10A 120.2 . . ?
C9B C10B H10B 120.3 . . ?
C9B C10B C11B 119.5(11) . . ?
C11B C10B H10B 120.3 . . ?
C10A C11A H11A 118.5 . . ?
C12A C11A C10A 122.9(9) . . ?
C12A C11A H11A 118.5 . . ?
C10B C11B H11B 119.7 . . ?
C12B C11B C10B 120.7(10) . . ?
C12B C11B H11B 119.7 . . ?
C11A C12A H12A 120.6 . . ?
C11A C12A C13A 118.7(7) . . ?
C13A C12A H12A 120.6 . . ?
C11B C12B H12B 118.5 . . ?
C11B C12B C13B 123.1(8) . . ?
C13B C12B H12B 118.5 . . ?
C7 C13A C8A 123.5(6) . . ?
C7 C13A C12A 119.0(6) . . ?
C12A C13A C8A 117.5(7) . . ?
C7 C13B C8B 117.4(6) . . ?
C7 C13B C12B 126.1(6) . . ?
C12B C13B C8B 116.5(7) . . ?

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
Cu1 O2 C1 O3 -3.0(6) . . . . ?
Cu1 O2 C1 C2 176.7(2) . . . . ?
Cu1 O3 C1 O2 -0.5(6) 13_566 . . . ?
Cu1 O3 C1 C2 179.7(2) 13_566 . . . ?
O2 C1 C2 C3 -146.5(3) . . . . ?
O2 C1 C2 C4 31.5(6) . . . . ?
O3 C1 C2 C3 33.2(5) . . . . ?
O3 C1 C2 C4 -148.8(4) . . . . ?
C1 C2 C3 C2 -179.7(4) . . . 3_656 ?
C1 C2 C4 C5 177.2(3) . . . . ?
C2 C4 C5 C4 2.4(3) . . . 3_656 ?
C2 C4 C5 C6 -177.6(3) . . . . ?
C3 C2 C4 C5 -4.8(6) . . . . ?
C4 C2 C3 C2 2.4(3) . . . 3_656 ?
C4 C5 C6 C8A -118.3(5) . . . . ?
C4 C5 C6 C8A 61.7(5) 3_656 . . . ?
C4 C5 C6 C8B -74.3(4) 3_656 . . 3_656 ?
C4 C5 C6 C8B -74.3(4) . . . . ?
C4 C5 C6 C8B 105.7(4) 3_656 . . . ?
C4 C5 C6 C8B 105.7(4) . . . 3_656 ?
C5 C6 C8A C9A 5.0(12) . . . . ?
C5 C6 C8A C13A -178.7(6) . . . . ?
C5 C6 C8B C9B -2.6(9) . . . . ?
C5 C6 C8B C13B 178.7(5) . . . . ?
C6 C8A C9A C10A -179.5(11) . . . . ?
C6 C8A C13A C7 -2.8(14) . . . . ?
C6 C8A C13A C12A 175.5(9) . . . . ?
C6 C8B C9B C10B 178.5(8) . . . . ?
C6 C8B C13B C7 2.7(10) . . . . ?
C6 C8B C13B C12B -179.5(6) . . . . ?
C7 C7 C13A C8A -178.6(7) 2_665 . . . ?
C7 C7 C13A C12A 3.2(11) 2_665 . . . ?
C7 C7 C13B C8B 178.7(5) 2_665 . . . ?
C7 C7 C13B C12B 1.2(9) 2_665 . . . ?
C8A C9A C10A C11A 5(2) . . . . ?
C8B C6 C8B C9B 177.4(9) 3_656 . . . ?
C8B C6 C8B C13B -1.3(5) 3_656 . . . ?
C8B C9B C10B C11B 2.4(15) . . . . ?
C9A C8A C13A C7 173.9(8) . . . . ?
C9A C8A C13A C12A -7.9(15) . . . . ?
C9A C10A C11A C12A -11(3) . . . . ?
C9B C8B C13B C7 -176.1(6) . . . . ?
C9B C8B C13B C12B 1.7(11) . . . . ?
C9B C10B C11B C12B -1.0(17) . . . . ?
C10A C11A C12A C13A 7(3) . . . . ?
C10B C11B C12B C13B 0.0(16) . . . . ?
C11A C12A C13A C7 -179.2(12) . . . . ?
C11A C12A C13A C8A 2.5(18) . . . . ?
C11B C12B C13B C7 177.2(8) . . . . ?
C11B C12B C13B C8B -0.4(13) . . . . ?
C13A C8A C9A C10A 4.2(17) . . . . ?
C13B C7 C13B C8B -1.3(5) 3_656 . . . ?
C13B C7 C13B C12B -178.8(9) 3_656 . . . ?
C13B C8B C9B C10B -2.7(13) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 835 electrons were 
found in a volume of 2698Å³ in 1 void per unit cell. 
This is consistent with the presence of 
5 DMSO per formula unit which account for 840 electrons 
per unit cell.
;
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 -0.562 -0.881 -0.526 2697.7 834.8 '20 DMSO'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2023-07-17
_olex2_date_sample_submission    2023-07-17
_olex2_exptl_crystal_mounting_method 
'Mounted on a nylon loop with perfluoroether oil.'
_olex2_submission_original_sample_id 'TM4014 1'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.814
_oxdiff_exptl_absorpt_empirical_full_min 0.515
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cs2947
_database_code_depnum_ccdc_archive 'CCDC 2371664'
loop_
_audit_author_name
_audit_author_address
'Carla Slebodnick'
;Virginia Tech
United States of America
;
_audit_update_record             
;
2024-07-17 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_audit_creation_date             2024-07-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
tam9k@uvawise.edu
slebod@vt.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H20 Cu2 O10, 5[C3H7NO]'
_chemical_formula_sum            'C59 H55 Cu2 N5 O15'
_chemical_formula_weight         1201.16
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cu2 C44 H22 O8 C3 H7 N O H2 O'
_chemical_oxdiff_usercomment     'Trevor Makal UVA Wise LJE-01-68-6'
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'
Cu Cu -1.9646 0.5888 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_H-M_alt        'C c c m'
_space_group_name_Hall           '-C 2 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, 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, -y, z-1/2'
'-x, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z-1/2'

_cell_length_a                   11.3494(3)
_cell_length_b                   36.6729(3)
_cell_length_c                   14.7750(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6149.58(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21903
_cell_measurement_temperature    99.98(16)
_cell_measurement_theta_max      76.5030
_cell_measurement_theta_min      4.0430
_shelx_estimated_absorpt_T_max   0.849
_shelx_estimated_absorpt_T_min   0.710
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2488
_exptl_crystal_recrystallization_method 'crystallized from DMF'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58535
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.420
_diffrn_reflns_theta_min         2.410
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  32.00   0.50    2.00    --  -45.04  13.00 108.00  114
  2  ω   -122.00 -21.00   0.50    2.00    --  -45.04 -13.00 -63.00  202
  3  ω     55.00  95.00   0.50    2.00    --   45.04  13.00 108.00   80
  4  ω    -32.00  21.00   0.50    2.00    --   45.04 -13.00 -63.00  106
  5  ω   -138.00-113.00   0.50   10.00    --  -88.50 -13.00 -63.00   50
  6  ω     81.00 126.00   0.50   10.00    --  110.00  13.00 108.00   90
  7  ω     -1.00  28.00   0.50    2.00    --  -45.04  77.00 150.00   58
  8  ω    -78.00 -15.00   0.50    2.00    --  -45.04 125.00-180.00  126
  9  ω   -117.00 -85.00   0.50    2.00    --  -45.04 -77.00 -30.00   64
 10  ω    -28.00  33.00   0.50    2.00    --  -45.04  19.00 -90.00  122
 11  ω    -69.00 -30.00   0.50    2.00    --  -45.04  77.00 150.00   78
 12  ω     38.00  92.00   0.50    2.00    --   45.04-125.00 120.00  108
 13  ω    -48.00 -22.00   0.50   10.00    --  -88.50  45.00   0.00   52
 14  ω     45.00  85.00   0.50   10.00    --  110.00 -94.00   0.00   80
 15  ω     55.00  96.00   0.50   10.00    --  110.00 -94.00-150.00   82
 16  ω     81.00 106.00   0.50   10.00    --  110.00-104.00 -29.67   50
 17  ω     79.00 106.00   0.50   10.00    --  110.00-105.00  88.48   54
 18  ω     39.00  68.00   0.50   10.00    --  110.00 -61.00 150.00   58
 19  ω     41.00  69.00   0.50   10.00    --  110.00 -61.00 -60.00   56
 20  ω     94.00 120.00   0.50   10.00    --  110.00  45.00-120.00   52
 21  ω     41.00  74.00   0.50   10.00    --  110.00-105.00  88.48   66
 22  ω     84.00 138.00   0.50   10.00    --  110.00  15.00  30.00  108
 23  ω     38.00  69.00   0.50   10.00    --  110.00 -61.00  30.00   62
 24  ω     50.00  75.00   0.50   10.00    --  110.00-125.00-120.00   50
 25  ω     87.00 112.00   0.50   10.00    --  110.00-125.00-120.00   50
 26  ω     43.00  80.00   0.50   10.00    --  110.00-125.00 120.00   74
 27  ω     41.00  68.00   0.50   10.00    --  110.00 -88.00 118.14   54
 28  ω     51.00  77.00   0.50   10.00    --  110.00-125.00 -60.00   52
 29  ω     84.00 112.00   0.50   10.00    --  110.00-125.00 -60.00   56
 30  ω     92.00 163.00   0.50   10.00    --  110.00  45.00 -60.00  142
 31  ω     43.00  69.00   0.50   10.00    --  110.00-125.00  30.00   52
 32  ω     81.00 111.00   0.50   10.00    --  110.00-125.00  30.00   60
 33  ω     96.00 178.00   0.50   10.00    --  110.00  15.00 -90.00  164
 34  ω     39.00  87.00   0.50   10.00    --  110.00 -77.00 -60.00   96
 35  ω     96.00 121.00   0.50   10.00    --  110.00  30.00 150.00   50
 36  ω    134.00 160.00   0.50   10.00    --  110.00  30.00 150.00   52
 37  ω    104.00 163.00   0.50   10.00    --  110.00 125.00 120.00  118
 38  ω    116.00 172.00   0.50   10.00    --  110.00  15.00 -30.00  112
 39  ω     84.00 109.00   0.50   10.00    --  110.00 -85.00 -76.77   50
 40  ω     41.00  74.00   0.50   10.00    --  110.00 -85.00 -76.77   66
 41  ω    105.00 142.00   0.50   10.00    --  110.00  69.00 127.66   74
 42  ω     41.00  67.00   0.50   10.00    --  110.00 -61.00-180.00   52
 43  ω     39.00  64.00   0.50   10.00    --  110.00 -77.00-150.00   50
 44  ω     88.00 113.00   0.50   10.00    --  110.00  15.00 -30.00   50
 45  ω     41.00  92.00   0.50   10.00    --  110.00-125.00-150.00  102
 46  ω     96.00 175.00   0.50   10.00    --  110.00 125.00 150.00  158
 47  ω     81.00 112.00   0.50   10.00    --  110.00-125.00 150.00   62
 48  ω     86.00 112.00   0.50   10.00    --  110.00-125.00 120.00   52
 49  ω     38.00  93.00   0.50   10.00    --  110.00 -94.00 120.00  110
 50  ω     94.00 141.00   0.50   10.00    --  110.00 -88.00 118.14   94
 51  ω    128.00 154.00   0.50   10.00    --  110.00 125.00  90.00   52
 52  ω    111.00 136.00   0.50   10.00    --  110.00  45.00 120.00   50
 53  ω     93.00 123.00   0.50   10.00    --  110.00  30.00-180.00   60
 54  ω    135.00 160.00   0.50   10.00    --  110.00  30.00-180.00   50
 55  ω     39.00  65.00   0.50   10.00    --  110.00 -94.00 -90.00   52
 56  ω     80.00 106.00   0.50   10.00    --  110.00 -94.00 -90.00   52
 57  ω     42.00  67.00   0.50   10.00    --  110.00-125.00   0.00   50
 58  ω     82.00 107.00   0.50   10.00    --  110.00-125.00   0.00   50
 59  ω     48.00  73.00   0.50   10.00    --  110.00 -64.00-146.55   50
 60  ω     96.00 174.00   0.50   10.00    --  110.00  45.00-150.00  156
 61  ω    113.00 153.00   0.50   10.00    --  110.00  61.00   0.00   80
 62  ω     78.00 103.00   0.50   10.00    --  110.00 -77.00-120.00   50
 63  ω     52.00  77.00   0.50   10.00    --  110.00 -77.00   0.00   50
 64  ω     67.00  92.00   0.50   10.00    --  110.00 -77.00 -30.00   50
 65  ω     78.00 104.00   0.50   10.00    --  110.00 -94.00-120.00   52
 66  ω     54.00 106.00   0.50   10.00    --  110.00 -78.00  22.12  104
 67  ω     50.00  75.00   0.50   10.00    --  110.00-125.00  60.00   50
 68  ω     85.00 110.00   0.50   10.00    --  110.00-125.00  90.00   50
 69  ω     38.00  63.00   0.50   10.00    --  110.00 -61.00 120.00   50
 70  ω     98.00 171.00   0.50   10.00    --  110.00  45.00-180.00  146
 71  ω    134.00 159.00   0.50   10.00    --  110.00 125.00  30.00   50
 72  ω    110.00 135.00   0.50   10.00    --  110.00-159.00 142.98   50
 73  ω    104.00 152.00   0.50   10.00    --  110.00  45.00  90.00   96
 74  ω     95.00 120.00   0.50   10.00    --  110.00  30.00-150.00   50
 75  ω    113.00 139.00   0.50   10.00    --  110.00  61.00-180.00   52
 76  ω    117.00 142.00   0.50   10.00    --  110.00  61.00 120.00   50
 77  ω     46.00  73.00   0.50   10.00    --  110.00-104.00 -29.67   54
 78  ω     60.00 108.00   0.50   10.00    --  110.00 -83.00 134.79   96
 79  ω     89.00 114.00   0.50   10.00    --  110.00 -84.00 -32.79   50
 80  ω     44.00  69.00   0.50   10.00    --  110.00 -85.00  89.44   50
 81  ω    111.00 136.00   0.50   10.00    --  110.00 -85.00  89.44   50
 82  ω     52.00 106.00   0.50   10.00    --  110.00-107.00 154.58  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku Oxford Diffraction XtaLAB Synergy, Dualflex, HyPix 6000-HE'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1020457000
_diffrn_orient_matrix_UB_12      0.0067615000
_diffrn_orient_matrix_UB_13      0.0667110000
_diffrn_orient_matrix_UB_21      -0.0888665000
_diffrn_orient_matrix_UB_22      0.0027221000
_diffrn_orient_matrix_UB_23      0.0785055000
_diffrn_orient_matrix_UB_31      0.0106697000
_diffrn_orient_matrix_UB_32      -0.0413781000
_diffrn_orient_matrix_UB_33      0.0159743000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2919
_reflns_number_total             3398
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.948
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.370
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3398
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0910
_refine_ls_restrained_S_all      1.370
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2891
_refine_ls_wR_factor_ref         0.2989
_refine_special_details          
;The Laue symmetry and systematic absences were consistent with the 
orthorhombic space group Cccm (#63).  However, in this space group, 
there were systematically weak reflection suggesting a superlattice 
and the preliminary structure model showed significant disorder 
with unreasonable steric interactions.   Upon more careful analysis  
of the diffraction data, a monoclinic P2/c (#13) pseudomerohedral twin was 
identified (twin law 180 deg rotation about [001]) that accounted for 
the majority of the systematically weak reflection. During structure 
refinement on the HLKF 5 twin data, the twin ratios refined to 
approximately 50/50 (0.517(2) and 0.483(2)) accounting for the pseudo- 
orthorhombic symmetry. In the P2/c structure model, the the diphenyl-
bianthracene ligand is ordered and corresponds to CSD 2324985.

In this CIF, the structure is refined as disordered in Cccm to 
allow for direct comparison between this DMF analog and the DMSO analog 
(CSD 2324984). The DMSO analog has multiple twinning issues that resulted in 
the failure to obtain a structure model in P2/c. In this Cccm model, the 
capping ligands of the paddlewheel complex are modeled as water but are 
likely a combination of water and DMF and a2-position disorder model was 
used for the anthracene fragments with relative occupancies constrained 
to 50% by symmetry. In addition, the solvent mask feature of OLEX2 was 
used to subtract a total of 782 e-, equivalent to ~20 DMF molecules 
(800 e-) from 2969Å³ total void space per unit cell. The final 
refinement model involved anisotropic displacement parameters for 
non-hydrogen atoms and a riding model for all hydrogen atoms.,SQUEEZE
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C13B(0.5) C8A(0.5) C13A(0.5) C12A(0.5) H12A(0.5) C11A(0.5)
 H11A(0.5) C10A(0.5) H10A(0.5) C9A(0.5) H9A(0.5) C8B(0.5) C10B(0.5) H10B(0.5)
 C9B(0.5) H9B(0.5) C11B(0.5) H11B(0.5) C12B(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C12A(H12A), C11A(H11A), C10A(H10A), C9A(H9A), C10B(H10B),
 C9B(H9B), C11B(H11B)
3.b Fitted hexagon refined as free rotating group:
 C8A(C13A,C12A,C11A,C10A,C9A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.82852(6) 0.27677(2) 0.500000 0.0538(3) Uani 1 2 d S T P . .
O2 O 0.7295(2) 0.29978(6) 0.40926(15) 0.0695(6) Uani 1 1 d . . . . .
O3 O 0.5987(3) 0.25337(6) 0.40557(17) 0.0739(7) Uani 1 1 d . . . . .
C7 C 0.500000 0.47942(9) 0.250000 0.0543(9) Uani 1 2 d S T P . .
O1 O 0.9606(4) 0.31761(11) 0.500000 0.1118(18) Uani 1 2 d S T P . .
C5 C 0.500000 0.36146(11) 0.250000 0.0674(11) Uani 1 2 d S T P . .
C4 C 0.5701(4) 0.34257(8) 0.3102(2) 0.0696(9) Uani 1 1 d . . . . .
H4 H 0.619692 0.355559 0.350741 0.084 Uiso 1 1 calc R U . . .
C6 C 0.500000 0.40256(10) 0.250000 0.0604(10) Uani 1 2 d S T P . .
C2 C 0.5687(4) 0.30447(8) 0.3120(2) 0.0707(9) Uani 1 1 d . . . . .
C1 C 0.6385(4) 0.28426(9) 0.3813(2) 0.0669(8) Uani 1 1 d . . . . .
C3 C 0.500000 0.28494(12) 0.250000 0.0726(13) Uani 1 2 d S T P . .
H3 H 0.499997 0.259031 0.249998 0.087 Uiso 1 2 calc R U P . .
C13B C 0.3949(6) 0.46257(16) 0.2628(4) 0.0591(14) Uani 0.5 1 d . . P A 2
C8A C 0.4601(4) 0.42052(9) 0.3288(2) 0.0574(12) Uani 0.5 1 d G . P A -1
C13A C 0.4622(4) 0.45842(9) 0.3293(2) 0.0583(13) Uani 0.5 1 d G . P A -1
C12A C 0.4251(4) 0.47743(7) 0.4055(3) 0.0623(14) Uani 0.5 1 d G . P A -1
H12A H 0.426553 0.503328 0.405784 0.075 Uiso 0.5 1 calc R U P A -1
C11A C 0.3858(5) 0.45854(10) 0.4813(2) 0.075(2) Uani 0.5 1 d G . P A -1
H11A H 0.360396 0.471536 0.533350 0.091 Uiso 0.5 1 calc R U P A -1
C10A C 0.3836(5) 0.42065(10) 0.4808(2) 0.076(2) Uani 0.5 1 d G . P A -1
H10A H 0.356785 0.407739 0.532606 0.091 Uiso 0.5 1 calc R U P A -1
C9A C 0.4208(5) 0.40163(7) 0.4046(3) 0.0662(15) Uani 0.5 1 d G . P A -1
H9A H 0.419330 0.375734 0.404294 0.079 Uiso 0.5 1 calc R U P A -1
C8B C 0.3953(6) 0.42287(15) 0.2642(4) 0.0603(14) Uani 0.5 1 d . . P A 2
C10B C 0.1831(9) 0.4248(3) 0.2978(6) 0.086(2) Uani 0.5 1 d . . P A 2
H10B H 0.111783 0.412301 0.311340 0.104 Uiso 0.5 1 calc R U P A 2
C9B C 0.2880(8) 0.4047(2) 0.2837(5) 0.077(2) Uani 0.5 1 d . . P A 2
H9B H 0.286549 0.378848 0.287389 0.092 Uiso 0.5 1 calc R U P A 2
C11B C 0.1838(7) 0.4622(3) 0.2921(7) 0.081(2) Uani 0.5 1 d . . P A 2
H11B H 0.112244 0.475363 0.298490 0.097 Uiso 0.5 1 calc R U P A 2
C12B C 0.2852(7) 0.48026(17) 0.2774(5) 0.0670(15) Uani 0.5 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Cu1 Cu1 2.6520(11) 13_656 ?
Cu1 O2 1.942(2) 10_556 ?
Cu1 O2 1.942(2) . ?
Cu1 O3 1.962(2) 13_656 ?
Cu1 O3 1.962(2) 6_655 ?
Cu1 O1 2.119(4) . ?
O2 C1 1.250(5) . ?
O3 C1 1.271(4) . ?
C7 C7 1.509(7) 2_665 ?
C7 C13B 1.357(7) . ?
C7 C13B 1.357(7) 3_655 ?
C7 C13A 1.466(3) . ?
C5 C4 1.380(4) 3_655 ?
C5 C4 1.380(4) . ?
C5 C6 1.507(5) . ?
C4 H4 0.9500 . ?
C4 C2 1.397(4) . ?
C6 C8A 1.413(3) . ?
C6 C8B 1.418(7) 3_655 ?
C6 C8B 1.418(7) . ?
C2 C1 1.491(5) . ?
C2 C3 1.400(4) . ?
C3 H3 0.9500 . ?
C13B C8B 1.456(8) . ?
C13B C12B 1.420(10) . ?
C8A C13A 1.3900 . ?
C8A C9A 1.3900 . ?
C13A C12A 1.3900 . ?
C12A H12A 0.9500 . ?
C12A C11A 1.3900 . ?
C11A H11A 0.9500 . ?
C11A C10A 1.3900 . ?
C10A H10A 0.9500 . ?
C10A C9A 1.3900 . ?
C9A H9A 0.9500 . ?
C8B C9B 1.418(10) . ?
C10B H10B 0.9500 . ?
C10B C9B 1.415(15) . ?
C10B C11B 1.375(14) . ?
C9B H9B 0.9500 . ?
C11B H11B 0.9500 . ?
C11B C12B 1.346(11) . ?
C12B C12B 1.658(14) 4_565 ?

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
O2 Cu1 Cu1 86.14(8) 10_556 13_656 ?
O2 Cu1 Cu1 86.14(8) . 13_656 ?
O2 Cu1 O2 87.29(16) . 10_556 ?
O2 Cu1 O3 89.86(12) . 6_655 ?
O2 Cu1 O3 89.86(12) 10_556 13_656 ?
O2 Cu1 O3 168.24(11) 10_556 6_655 ?
O2 Cu1 O3 168.24(11) . 13_656 ?
O2 Cu1 O1 95.89(12) 10_556 . ?
O2 Cu1 O1 95.89(12) . . ?
O3 Cu1 Cu1 82.28(7) 13_656 13_656 ?
O3 Cu1 Cu1 82.28(7) 6_655 13_656 ?
O3 Cu1 O3 90.63(17) 6_655 13_656 ?
O3 Cu1 O1 95.76(12) 13_656 . ?
O3 Cu1 O1 95.76(12) 6_655 . ?
O1 Cu1 Cu1 177.19(14) . 13_656 ?
C1 O2 Cu1 120.6(2) . . ?
C1 O3 Cu1 123.6(2) . 13_656 ?
C13A C7 C7 121.71(18) . 2_665 ?
C4 C5 C4 119.7(4) . 3_655 ?
C4 C5 C6 120.1(2) . . ?
C4 C5 C6 120.1(2) 3_655 . ?
C5 C4 H4 119.8 . . ?
C5 C4 C2 120.5(3) . . ?
C2 C4 H4 119.8 . . ?
C8A C6 C5 117.80(19) . . ?
C8A C6 C8B 98.4(3) . 3_655 ?
C8B C6 C5 121.7(3) . . ?
C8B C6 C5 121.7(3) 3_655 . ?
C8B C6 C8B 116.6(5) 3_655 . ?
C4 C2 C1 120.3(3) . . ?
C4 C2 C3 120.4(3) . . ?
C3 C2 C1 119.4(3) . . ?
O2 C1 O3 127.3(3) . . ?
O2 C1 C2 116.1(3) . . ?
O3 C1 C2 116.6(3) . . ?
C2 C3 C2 118.4(4) . 3_655 ?
C2 C3 H3 120.8 . . ?
C2 C3 H3 120.8 3_655 . ?
C7 C13B C8B 117.0(5) . . ?
C7 C13B C12B 125.7(5) . . ?
C12B C13B C8B 117.3(6) . . ?
C13A C8A C6 117.7(3) . . ?
C13A C8A C9A 120.0 . . ?
C9A C8A C6 122.3(3) . . ?
C8A C13A C7 121.8(2) . . ?
C8A C13A C12A 120.0 . . ?
C12A C13A C7 118.2(2) . . ?
C13A C12A H12A 120.0 . . ?
C13A C12A C11A 120.0 . . ?
C11A C12A H12A 120.0 . . ?
C12A C11A H11A 120.0 . . ?
C10A C11A C12A 120.0 . . ?
C10A C11A H11A 120.0 . . ?
C11A C10A H10A 120.0 . . ?
C11A C10A C9A 120.0 . . ?
C9A C10A H10A 120.0 . . ?
C8A C9A H9A 120.0 . . ?
C10A C9A C8A 120.0 . . ?
C10A C9A H9A 120.0 . . ?
C6 C8B C13B 121.8(5) . . ?
C6 C8B C9B 120.2(6) . . ?
C9B C8B C13B 118.0(6) . . ?
C9B C10B H10B 119.9 . . ?
C11B C10B H10B 119.9 . . ?
C11B C10B C9B 120.3(7) . . ?
C8B C9B H9B 119.7 . . ?
C10B C9B C8B 120.6(7) . . ?
C10B C9B H9B 119.7 . . ?
C10B C11B H11B 119.8 . . ?
C12B C11B C10B 120.5(8) . . ?
C12B C11B H11B 119.8 . . ?
C13B C12B C12B 109.0(4) . 4_565 ?
C11B C12B C13B 123.3(7) . . ?
C11B C12B C12B 120.6(5) . 4_565 ?

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
Cu1 O2 C1 O3 0.0(6) . . . . ?
Cu1 O2 C1 C2 179.7(2) . . . . ?
Cu1 O3 C1 O2 2.9(6) 13_656 . . . ?
Cu1 O3 C1 C2 -176.8(2) 13_656 . . . ?
C7 C7 C13B C8B -179.0(3) 2_665 . . . ?
C7 C7 C13B C12B -0.9(7) 2_665 . . . ?
C7 C7 C13A C8A 178.8(2) 2_665 . . . ?
C7 C7 C13A C12A 0.4(3) 2_665 . . . ?
C7 C13B C8B C6 -2.0(7) . . . . ?
C7 C13B C8B C9B 175.7(5) . . . . ?
C7 C13B C12B C11B -178.2(7) . . . . ?
C7 C13B C12B C12B 31.5(9) . . . 4_565 ?
C7 C13A C12A C11A 178.4(4) . . . . ?
C5 C4 C2 C1 -175.9(3) . . . . ?
C5 C4 C2 C3 2.9(6) . . . . ?
C5 C6 C8A C13A 178.83(19) . . . . ?
C5 C6 C8A C9A -0.5(3) . . . . ?
C5 C6 C8B C13B -179.0(4) . . . . ?
C5 C6 C8B C9B 3.4(6) . . . . ?
C4 C5 C4 C2 -1.4(3) 3_655 . . . ?
C4 C5 C6 C8A -63.1(3) . . . . ?
C4 C5 C6 C8A 116.9(3) 3_655 . . . ?
C4 C5 C6 C8B 58.2(3) 3_655 . . . ?
C4 C5 C6 C8B -121.8(3) . . . . ?
C4 C5 C6 C8B -121.8(3) 3_655 . . 3_655 ?
C4 C5 C6 C8B 58.2(3) . . . 3_655 ?
C4 C2 C1 O2 -28.8(6) . . . . ?
C4 C2 C1 O3 150.9(4) . . . . ?
C4 C2 C3 C2 -1.4(3) . . . 3_655 ?
C6 C5 C4 C2 178.6(3) . . . . ?
C6 C8A C13A C7 2.3(4) . . . . ?
C6 C8A C13A C12A -179.3(4) . . . . ?
C6 C8A C9A C10A 179.3(4) . . . . ?
C6 C8B C9B C10B -179.9(6) . . . . ?
C1 C2 C3 C2 177.4(4) . . . 3_655 ?
C3 C2 C1 O2 152.4(3) . . . . ?
C3 C2 C1 O3 -27.9(5) . . . . ?
C13B C7 C13B C8B 1.0(3) 3_655 . . . ?
C13B C7 C13B C12B 179.1(6) 3_655 . . . ?
C13B C8B C9B C10B 2.4(10) . . . . ?
C8A C13A C12A C11A 0.0 . . . . ?
C13A C8A C9A C10A 0.0 . . . . ?
C13A C12A C11A C10A 0.0 . . . . ?
C12A C11A C10A C9A 0.0 . . . . ?
C11A C10A C9A C8A 0.0 . . . . ?
C9A C8A C13A C7 -178.3(4) . . . . ?
C9A C8A C13A C12A 0.0 . . . . ?
C8B C6 C8B C13B 1.0(4) 3_655 . . . ?
C8B C6 C8B C9B -176.6(6) 3_655 . . . ?
C8B C13B C12B C11B -0.1(10) . . . . ?
C8B C13B C12B C12B -150.4(6) . . . 4_565 ?
C10B C11B C12B C13B 3.1(14) . . . . ?
C10B C11B C12B C12B 150.1(9) . . . 4_565 ?
C9B C10B C11B C12B -3.3(15) . . . . ?
C11B C10B C9B C8B 0.5(13) . . . . ?
C12B C13B C8B C6 179.7(5) . . . . ?
C12B C13B C8B C9B -2.6(8) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 782 electrons were 
found in a volume of 2969Å³ in 1 void per unit cell. 
This is consistent with the presence of 
5[C3H7NO] per formula unit which account for 800 electrons 
per unit cell.
;
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 -0.265 -0.003 -0.869 2969.2 782.0 '20 DMF'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2022-11-30
_olex2_date_sample_submission    2022-11-30
_olex2_exptl_crystal_mounting_method 
'mounted on a nylon loop with perfluoroether oil'
_olex2_submission_original_sample_id LJE-01-68-6
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.785
_oxdiff_exptl_absorpt_empirical_full_min 0.422
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cs2957
_database_code_depnum_ccdc_archive 'CCDC 2324986'
loop_
_audit_author_name
_audit_author_address
'Carla Slebodnick'
;Virginia Tech
United States of America
;
_audit_update_record             
;
2024-01-11 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
tam9k@uvawise.edu
slebod@vt.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H25 N2 O6 Zn, 2(C3 H7 N O)'
_chemical_formula_sum            'C34 H39 N4 O8 Zn'
_chemical_formula_weight         697.06
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C34 H39 N4 O8 Zn'
_chemical_oxdiff_usercomment     'Trevor Makal (UVA Wise) TM3125 10'
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'
N N 0.0311 0.0180 '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'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   38.9726(6)
_cell_length_b                   24.8157(5)
_cell_length_c                   13.8024(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13348.7(4)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    12826
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      76.9250
_cell_measurement_theta_min      3.7770
_shelx_estimated_absorpt_T_max   0.916
_shelx_estimated_absorpt_T_min   0.796
_exptl_absorpt_coefficient_mu    1.498
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.71a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             5840
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 -2 -1 0.0473
5 2 1 0.0473
4 -5 3 0.0573
-4 5 -3 0.0573
-3 -5 1 0.0715
3 5 -1 0.0715
5 -1 0 0.0505
-5 1 0 0.0505
2 -5 -3 0.0577
-2 5 3 0.0577
5 1 -1 0.0410
-5 -1 1 0.0410
-4 -3 -5 0.0464
4 3 5 0.0464
1 3 -5 0.0390
-1 -3 5 0.0390
5 -1 2 0.0404
-5 1 -2 0.0471
-5 1 2 0.0299
5 -1 -2 0.0299

_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
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
-4.9990 -1.9999 -1.0001 0.0243 0.0149 -0.2570
4.9990 1.9999 1.0001 -0.0243 -0.0149 0.2570
4.0009 -4.9997 3.0000 0.4153 0.1819 0.1672
-4.0009 4.9997 -3.0000 -0.4153 -0.1819 -0.1672
-2.9986 -4.9997 0.9999 0.2941 0.1060 -0.1582
2.9986 4.9997 -0.9999 -0.2941 -0.1060 0.1582
5.0009 -0.9999 0.0000 -0.0014 0.1604 0.1312
-5.0009 0.9999 -0.0000 0.0014 -0.1604 -0.1312
2.0039 -4.9997 -3.0001 -0.0936 0.3970 -0.2198
-2.0039 4.9997 3.0001 0.0936 -0.3970 0.2198
5.0005 1.0000 -1.0000 -0.1623 0.1162 0.1248
-5.0005 -1.0000 1.0000 0.1623 -0.1162 -0.1248
-3.9964 -2.9998 -5.0001 -0.2961 0.2566 -0.4665
3.9964 2.9998 5.0001 0.2961 -0.2566 0.4665
1.0014 2.9998 -5.0000 -0.5548 0.1097 -0.1682
-1.0014 -2.9998 5.0000 0.5548 -0.1097 0.1682
4.9998 -0.9999 2.0000 0.1733 0.0732 0.2395
-4.9998 0.9999 -2.0000 -0.1733 -0.0732 -0.2395
-5.0019 0.9999 2.0000 0.1762 -0.2476 -0.0229
5.0019 -0.9999 -2.0000 -0.1762 0.2476 0.0229

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30940
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.352
_diffrn_reflns_theta_min         3.836
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -117.00 -27.00   0.50    4.00    --  -44.79 -51.00-145.00  180
  2  ω    -60.00  29.00   0.50    4.00    --  -44.79  51.00   0.00  178
  3  ω    -60.00 -15.00   0.50   20.00    --  -88.50  51.00   0.00   90
  4  ω   -161.00 -70.00   0.50   20.00    --  -88.50 -51.00-145.00  182
  5  ω     92.00 178.00   0.50   20.00    --  110.00  51.00   0.00  172
  6  ω    -85.00 -13.00   0.50    4.00    --  -44.79 125.00  60.00  144
  7  ω    -28.00  56.00   0.50    4.00    --   44.79 -51.00-145.00  168
  8  ω    -53.00 -28.00   0.50   20.00    --  -88.50  45.00-180.00   50
  9  ω     59.00  85.00   0.50   20.00    --  110.00-113.00-136.18   52
 10  ω     39.00  64.00   0.50   20.00    --  110.00 -61.00-120.00   50
 11  ω     44.00  70.00   0.50   20.00    --  110.00-125.00  60.00   52
 12  ω    153.00 178.00   0.50   20.00    --  110.00  95.00-110.84   50
 13  ω     43.00  68.00   0.50   20.00    --  110.00 -61.00 150.00   50
 14  ω     47.00  72.00   0.50   20.00    --  110.00-125.00  30.00   50
 15  ω     85.00 112.00   0.50   20.00    --  110.00-125.00  30.00   54
 16  ω     55.00  81.00   0.50   20.00    --  110.00 -94.00-150.00   52
 17  ω     38.00  63.00   0.50   20.00    --  110.00 -61.00   0.00   50
 18  ω     47.00  93.00   0.50   20.00    --  110.00 -77.00 -90.00   92
 19  ω     76.00 102.00   0.50   20.00    --  110.00 -94.00  60.00   52
 20  ω    105.00 131.00   0.50   20.00    --  110.00  95.00-110.84   52
 21  ω     39.00  64.00   0.50   20.00    --  110.00 -94.00  60.00   50
 22  ω     39.00 102.00   0.50   20.00    --  110.00 -77.00 -30.00  126
 23  ω     39.00  66.00   0.50   20.00    --  110.00 -77.00  90.00   54
 24  ω     71.00  96.00   0.50   20.00    --  110.00 -77.00  90.00   50
 25  ω     97.00 122.00   0.50   20.00    --  110.00  45.00-120.00   50
 26  ω     40.00  77.00   0.50   20.00    --  110.00 -77.00 150.00   74
 27  ω     38.00  66.00   0.50   20.00    --  110.00 -61.00 -90.00   56
 28  ω     39.00  64.00   0.50   20.00    --  110.00 -61.00 -60.00   50
 29  ω    112.00 169.00   0.50   20.00    --  110.00  15.00 -90.00  114
 30  ω     51.00 102.00   0.50   20.00    --  110.00 -77.00 120.00  102
 31  ω    152.00 177.00   0.50   20.00    --  110.00 126.00  93.87   50
 32  ω     85.00 135.00   0.50   20.00    --  110.00  77.00-120.00  100
 33  ω    142.00 171.00   0.50   20.00    --  110.00  77.00-120.00   58
 34  ω     41.00  67.00   0.50   20.00    --  110.00 -77.00   0.00   52
 35  ω     38.00  69.00   0.50   20.00    --  110.00 -61.00-180.00   62
 36  ω     40.00  68.00   0.50   20.00    --  110.00 -61.00-150.00   56
 37  ω    116.00 142.00   0.50   20.00    --  110.00  30.00 120.00   52
 38  ω    146.00 177.00   0.50   20.00    --  110.00  59.00 -93.41   62
 39  ω     74.00 105.00   0.50   20.00    --  110.00-125.00  60.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku Oxford Diffraction XtaLAB Synergy, Dualflex, HyPix 6000-HE'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0076380000
_diffrn_orient_matrix_UB_12      -0.0367617000
_diffrn_orient_matrix_UB_13      0.0873702000
_diffrn_orient_matrix_UB_21      0.0232994000
_diffrn_orient_matrix_UB_22      -0.0438982000
_diffrn_orient_matrix_UB_23      -0.0436031000
_diffrn_orient_matrix_UB_31      0.0310103000
_diffrn_orient_matrix_UB_32      0.0238885000
_diffrn_orient_matrix_UB_33      0.0541787000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.826
_reflns_Friedel_fraction_max     0.792
_reflns_number_gt                5764
_reflns_number_total             6325
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.30(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6325
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0762
_refine_ls_restrained_S_all      1.048
_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)+(0.1899P)²+2.7196P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2121
_refine_ls_wR_factor_ref         0.2194
_refine_special_details          
;
A DMF solvate was modeled with 2-position disorder with relative 
occupancies that refined to 0.715(17) and 0.285(17).  For the 
minor component, DFIX restraints and isotropic refinement with 
an EADP command were necessary to keep the refinement stable.  
For the final refinement model, the remainder of the non-H 
atoms were refine anisotropically. A riding model was used 
for all hydrogen atoms.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.70(5)
 0.30(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O8-C32B
 1.25 with sigma of 0.02
 C32B-N4
 1.31 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(C32B) = Uiso(C33B) = Uiso(C34B)
5. Others
 Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C32B)=Sof(H32B)=Sof(C33B)=
 Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(1)
 Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=FVAR(1)
6.a Me refined with riding coordinates:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C34B(H34D,H34E,H34F), C33B(H33D,
 H33E,H33F)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C26(H26), C29(H29), C32(H32),
 C32B(H32B)
6.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Zn1 Zn 0.75039(2) 0.60708(3) 0.25797(8) 0.0410(3) Uani 1 1 d . . . . .
O1 O 0.73287(11) 0.56403(18) 0.3642(3) 0.0440(9) Uani 1 1 d . . . . .
O2 O 0.68904(10) 0.55124(19) 0.2627(4) 0.0468(9) Uani 1 1 d . . . . .
O3 O 0.73240(10) 0.42880(17) 0.6419(3) 0.0442(9) Uani 1 1 d . . . . .
O4 O 0.68784(11) 0.44152(18) 0.7411(3) 0.0451(10) Uani 1 1 d . . . . .
O5 O 0.77919(12) 0.66289(19) 0.3242(4) 0.0524(11) Uani 1 1 d . . . . .
O6 O 0.71960(13) 0.6642(2) 0.2041(4) 0.0567(12) Uani 1 1 d . . . . .
N1 N 0.82496(16) 0.7133(3) 0.3592(5) 0.0609(16) Uani 1 1 d . . . . .
N2 N 0.67295(18) 0.7016(3) 0.1354(5) 0.0648(16) Uani 1 1 d . . . . .
C1 C 0.63016(11) 0.4951(2) 0.4989(4) 0.0320(9) Uani 1 1 d . . . . .
C2 C 0.64831(14) 0.5175(2) 0.4228(4) 0.0358(10) Uani 1 1 d . . . . .
H2 H 0.636205 0.532370 0.369330 0.043 Uiso 1 1 calc R U . . .
C3 C 0.68393(13) 0.5187(2) 0.4233(4) 0.0353(10) Uani 1 1 d . . . . .
C4 C 0.70194(11) 0.4954(2) 0.5014(5) 0.0353(10) Uani 1 1 d . . . . .
H4 H 0.726318 0.495448 0.501933 0.042 Uiso 1 1 calc R U . . .
C5 C 0.68382(13) 0.4722(2) 0.5778(4) 0.0349(10) Uani 1 1 d . . . . .
C6 C 0.64777(13) 0.4731(2) 0.5771(4) 0.0349(10) Uani 1 1 d . . . . .
H6 H 0.635362 0.458626 0.630321 0.042 Uiso 1 1 calc R U . . .
C7 C 0.70281(14) 0.5462(2) 0.3431(4) 0.0390(11) Uani 1 1 d . . . . .
C8 C 0.70216(15) 0.4455(2) 0.6605(4) 0.0396(11) Uani 1 1 d . . . . .
C9 C 0.59186(11) 0.4961(2) 0.5012(5) 0.0332(9) Uani 1 1 d . . . . .
C10 C 0.57467(13) 0.5311(2) 0.5627(4) 0.0320(10) Uani 1 1 d . . . . .
C11 C 0.59236(13) 0.5667(2) 0.6280(4) 0.0369(11) Uani 1 1 d . . . . .
H11 H 0.616739 0.566618 0.628927 0.044 Uiso 1 1 calc R U . . .
C12 C 0.57518(15) 0.6001(3) 0.6880(5) 0.0437(13) Uani 1 1 d . . . . .
H12 H 0.587630 0.623505 0.729647 0.052 Uiso 1 1 calc R U . . .
C13 C 0.53855(16) 0.6008(2) 0.6896(5) 0.0410(12) Uani 1 1 d . . . . .
H13 H 0.526745 0.624635 0.731976 0.049 Uiso 1 1 calc R U . . .
C14 C 0.52073(13) 0.5676(2) 0.6307(4) 0.0345(10) Uani 1 1 d . . . . .
H14 H 0.496384 0.567625 0.633970 0.041 Uiso 1 1 calc R U . . .
C15 C 0.53747(13) 0.5322(2) 0.5632(4) 0.0318(10) Uani 1 1 d . . . . .
C16 C 0.51919(10) 0.4992(2) 0.5004(5) 0.0308(9) Uani 1 1 d . . . . .
C17 C 0.53629(12) 0.4635(2) 0.4377(4) 0.0313(10) Uani 1 1 d . . . . .
C18 C 0.51856(14) 0.4284(2) 0.3743(4) 0.0361(11) Uani 1 1 d . . . . .
H18 H 0.494191 0.429171 0.373104 0.043 Uiso 1 1 calc R U . . .
C19 C 0.53549(15) 0.3933(2) 0.3148(5) 0.0414(12) Uani 1 1 d . . . . .
H19 H 0.522875 0.371119 0.271427 0.050 Uiso 1 1 calc R U . . .
C20 C 0.57201(16) 0.3899(2) 0.3174(5) 0.0433(13) Uani 1 1 d . . . . .
H20 H 0.583671 0.364433 0.277895 0.052 Uiso 1 1 calc R U . . .
C21 C 0.59005(14) 0.4231(2) 0.3766(4) 0.0398(11) Uani 1 1 d . . . . .
H21 H 0.614378 0.420857 0.377179 0.048 Uiso 1 1 calc R U . . .
C22 C 0.57345(13) 0.4616(2) 0.4385(4) 0.0326(10) Uani 1 1 d . . . . .
C23 C 0.81034(17) 0.6723(3) 0.3158(5) 0.0484(14) Uani 1 1 d . . . . .
H23 H 0.823971 0.649055 0.276815 0.058 Uiso 1 1 calc R U . . .
C24 C 0.8616(2) 0.7244(4) 0.3536(8) 0.072(2) Uani 1 1 d . . . . .
H24A H 0.872590 0.714350 0.414910 0.107 Uiso 1 1 calc R U . . .
H24B H 0.865261 0.762864 0.341377 0.107 Uiso 1 1 calc R U . . .
H24C H 0.871740 0.703339 0.300692 0.107 Uiso 1 1 calc R U . . .
C25 C 0.8043(4) 0.7503(4) 0.4183(11) 0.089(4) Uani 1 1 d . . . . .
H25A H 0.809964 0.787583 0.401462 0.133 Uiso 1 1 calc R U . . .
H25B H 0.809131 0.744088 0.487035 0.133 Uiso 1 1 calc R U . . .
H25C H 0.779847 0.743810 0.405756 0.133 Uiso 1 1 calc R U . . .
C26 C 0.68794(18) 0.6635(3) 0.1853(5) 0.0503(14) Uani 1 1 d . . . . .
H26 H 0.674491 0.634200 0.208196 0.060 Uiso 1 1 calc R U . . .
C27 C 0.6917(3) 0.7473(4) 0.0980(10) 0.079(3) Uani 1 1 d . . . . .
H27A H 0.712726 0.752425 0.135852 0.119 Uiso 1 1 calc R U . . .
H27B H 0.677416 0.779739 0.102822 0.119 Uiso 1 1 calc R U . . .
H27C H 0.697662 0.740919 0.029993 0.119 Uiso 1 1 calc R U . . .
C28 C 0.6369(2) 0.6962(5) 0.1095(10) 0.093(3) Uani 1 1 d . . . . .
H28A H 0.625108 0.730592 0.120812 0.139 Uiso 1 1 calc R U . . .
H28B H 0.626265 0.668124 0.149427 0.139 Uiso 1 1 calc R U . . .
H28C H 0.634907 0.686437 0.040965 0.139 Uiso 1 1 calc R U . . .
O7 O 0.63198(16) 0.5971(4) -0.1017(6) 0.089(2) Uani 1 1 d . . . . .
N3 N 0.68838(16) 0.5784(2) -0.1226(5) 0.0549(13) Uani 1 1 d . . . . .
C29 C 0.6569(2) 0.5840(4) -0.1505(7) 0.077(2) Uani 1 1 d . . . . .
H29 H 0.652485 0.576979 -0.217062 0.092 Uiso 1 1 calc R U . . .
C30 C 0.6975(3) 0.5926(5) -0.0257(8) 0.087(3) Uani 1 1 d . . . . .
H30A H 0.722378 0.598374 -0.021927 0.130 Uiso 1 1 calc R U . . .
H30B H 0.690992 0.563310 0.018261 0.130 Uiso 1 1 calc R U . . .
H30C H 0.685550 0.625665 -0.007012 0.130 Uiso 1 1 calc R U . . .
C31 C 0.7158(2) 0.5621(4) -0.1866(8) 0.073(2) Uani 1 1 d . . . . .
H31A H 0.725655 0.528077 -0.163674 0.109 Uiso 1 1 calc R U . . .
H31B H 0.733679 0.589955 -0.187191 0.109 Uiso 1 1 calc R U . . .
H31C H 0.706803 0.557294 -0.252277 0.109 Uiso 1 1 calc R U . . .
O8 O 0.6467(3) 0.3661(6) 0.0338(9) 0.159(6) Uani 1 1 d D . . . .
N4 N 0.68582(17) 0.4199(3) 0.1067(5) 0.0574(14) Uani 1 1 d D . . . .
C32 C 0.6739(5) 0.3944(7) 0.0331(12) 0.102(7) Uani 0.715(17) 1 d . . P A 1
H32 H 0.686307 0.396782 -0.026058 0.122 Uiso 0.715(17) 1 calc R U P A 1
C33 C 0.6713(3) 0.4144(4) 0.2021(8) 0.061(3) Uani 0.715(17) 1 d . . P A 1
H33A H 0.684040 0.437175 0.247673 0.092 Uiso 0.715(17) 1 calc R U P A 1
H33B H 0.647191 0.425710 0.200841 0.092 Uiso 0.715(17) 1 calc R U P A 1
H33C H 0.672749 0.376735 0.222798 0.092 Uiso 0.715(17) 1 calc R U P A 1
C34 C 0.7158(3) 0.4553(5) 0.0983(11) 0.071(3) Uani 0.715(17) 1 d . . P A 1
H34A H 0.720991 0.471097 0.161702 0.107 Uiso 0.715(17) 1 calc R U P A 1
H34B H 0.735576 0.434337 0.075799 0.107 Uiso 0.715(17) 1 calc R U P A 1
H34C H 0.710909 0.484131 0.051776 0.107 Uiso 0.715(17) 1 calc R U P A 1
C34B C 0.6956(11) 0.4401(16) 0.009(4) 0.090(7) Uiso 0.285(17) 1 d . . P A 2
H34D H 0.713486 0.467544 0.015234 0.135 Uiso 0.285(17) 1 calc R U P A 2
H34E H 0.704182 0.410102 -0.030451 0.135 Uiso 0.285(17) 1 calc R U P A 2
H34F H 0.675403 0.455902 -0.022744 0.135 Uiso 0.285(17) 1 calc R U P A 2
C32B C 0.6615(8) 0.3821(13) 0.110(2) 0.090(7) Uiso 0.285(17) 1 d D . P A 2
H32B H 0.655271 0.366896 0.170200 0.108 Uiso 0.285(17) 1 calc R U P A 2
C33B C 0.7077(11) 0.4299(16) 0.181(4) 0.090(7) Uiso 0.285(17) 1 d . . P A 2
H33D H 0.723300 0.459227 0.163481 0.135 Uiso 0.285(17) 1 calc R U P A 2
H33E H 0.694478 0.440420 0.238828 0.135 Uiso 0.285(17) 1 calc R U P A 2
H33F H 0.720979 0.397388 0.195718 0.135 Uiso 0.285(17) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Zn1 O1 1.938(5) . ?
Zn1 O3 1.952(5) 10_664 ?
Zn1 O5 2.003(5) . ?
Zn1 O6 2.000(5) . ?
O1 C7 1.286(7) . ?
O2 C7 1.239(8) . ?
O3 C8 1.275(7) . ?
O4 C8 1.249(8) . ?
O5 C23 1.242(8) . ?
O6 C26 1.261(9) . ?
N1 C23 1.313(9) . ?
N1 C24 1.458(10) . ?
N1 C25 1.468(13) . ?
N2 C26 1.307(10) . ?
N2 C27 1.446(13) . ?
N2 C28 1.457(12) . ?
C1 C2 1.384(8) . ?
C1 C6 1.390(8) . ?
C1 C9 1.493(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.388(8) . ?
C3 C4 1.411(8) . ?
C3 C7 1.494(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.393(9) . ?
C5 C6 1.405(7) . ?
C5 C8 1.501(8) . ?
C6 H6 0.9500 . ?
C9 C10 1.387(8) . ?
C9 C22 1.413(8) . ?
C10 C11 1.437(7) . ?
C10 C15 1.450(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.351(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.428(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.350(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.437(7) . ?
C15 C16 1.389(8) . ?
C16 C16 1.496(8) 2_665 ?
C16 C17 1.407(7) . ?
C17 C18 1.416(7) . ?
C17 C22 1.449(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.366(8) . ?
C19 H19 0.9500 . ?
C19 C20 1.427(8) . ?
C20 H20 0.9500 . ?
C20 C21 1.358(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.435(7) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
O7 C29 1.225(12) . ?
N3 C29 1.295(11) . ?
N3 C30 1.428(13) . ?
N3 C31 1.445(11) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
O8 C32 1.273(15) . ?
O8 C32B 1.26(2) . ?
N4 C32 1.284(16) . ?
N4 C33 1.441(12) . ?
N4 C34 1.467(13) . ?
N4 C34B 1.49(5) . ?
N4 C32B 1.33(2) . ?
N4 C33B 1.36(5) . ?
C32 H32 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C34B H34D 0.9800 . ?
C34B H34E 0.9800 . ?
C34B H34F 0.9800 . ?
C32B H32B 0.9500 . ?
C33B H33D 0.9800 . ?
C33B H33E 0.9800 . ?
C33B H33F 0.9800 . ?

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
O1 Zn1 O3 119.36(17) . 10_664 ?
O1 Zn1 O5 103.5(2) . . ?
O1 Zn1 O6 117.4(2) . . ?
O3 Zn1 O5 119.83(19) 10_664 . ?
O3 Zn1 O6 103.0(2) 10_664 . ?
O6 Zn1 O5 90.9(2) . . ?
C7 O1 Zn1 109.8(4) . . ?
C8 O3 Zn1 107.5(4) . 10_665 ?
C23 O5 Zn1 129.4(5) . . ?
C26 O6 Zn1 130.8(5) . . ?
C23 N1 C24 123.2(7) . . ?
C23 N1 C25 120.0(7) . . ?
C24 N1 C25 116.8(8) . . ?
C26 N2 C27 122.0(8) . . ?
C26 N2 C28 119.7(8) . . ?
C27 N2 C28 118.1(8) . . ?
C2 C1 C6 119.7(4) . . ?
C2 C1 C9 121.3(5) . . ?
C6 C1 C9 118.9(5) . . ?
C1 C2 H2 119.5 . . ?
C1 C2 C3 121.0(5) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 C4 119.5(5) . . ?
C2 C3 C7 119.9(5) . . ?
C4 C3 C7 120.6(5) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.7(4) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 119.7(5) . . ?
C4 C5 C8 121.1(5) . . ?
C6 C5 C8 119.3(5) . . ?
C1 C6 C5 120.3(5) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
O1 C7 C3 116.0(5) . . ?
O2 C7 O1 124.2(6) . . ?
O2 C7 C3 119.8(5) . . ?
O3 C8 C5 115.5(5) . . ?
O4 C8 O3 124.5(5) . . ?
O4 C8 C5 119.9(5) . . ?
C10 C9 C1 120.4(5) . . ?
C10 C9 C22 120.6(4) . . ?
C22 C9 C1 118.9(5) . . ?
C9 C10 C11 122.4(5) . . ?
C9 C10 C15 119.8(5) . . ?
C11 C10 C15 117.7(5) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 C10 121.6(5) . . ?
C12 C11 H11 119.2 . . ?
C11 C12 H12 119.6 . . ?
C11 C12 C13 120.9(5) . . ?
C13 C12 H12 119.6 . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.8(5) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 H14 119.0 . . ?
C13 C14 C15 122.0(5) . . ?
C15 C14 H14 119.0 . . ?
C14 C15 C10 117.9(5) . . ?
C16 C15 C10 119.9(5) . . ?
C16 C15 C14 122.1(4) . . ?
C15 C16 C16 119.8(4) . 2_665 ?
C15 C16 C17 120.8(4) . . ?
C17 C16 C16 119.3(4) . 2_665 ?
C16 C17 C18 122.5(5) . . ?
C16 C17 C22 119.3(4) . . ?
C18 C17 C22 118.2(5) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 C17 121.9(5) . . ?
C19 C18 H18 119.1 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.3(5) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.7(5) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 119.0 . . ?
C20 C21 C22 122.0(5) . . ?
C22 C21 H21 119.0 . . ?
C9 C22 C17 119.5(5) . . ?
C9 C22 C21 122.6(5) . . ?
C21 C22 C17 117.9(5) . . ?
O5 C23 N1 121.8(7) . . ?
O5 C23 H23 119.1 . . ?
N1 C23 H23 119.1 . . ?
N1 C24 H24A 109.5 . . ?
N1 C24 H24B 109.5 . . ?
N1 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N1 C25 H25A 109.5 . . ?
N1 C25 H25B 109.5 . . ?
N1 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O6 C26 N2 122.4(7) . . ?
O6 C26 H26 118.8 . . ?
N2 C26 H26 118.8 . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N2 C28 H28A 109.5 . . ?
N2 C28 H28B 109.5 . . ?
N2 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C29 N3 C30 119.3(8) . . ?
C29 N3 C31 123.4(8) . . ?
C30 N3 C31 117.1(7) . . ?
O7 C29 N3 128.0(10) . . ?
O7 C29 H29 116.0 . . ?
N3 C29 H29 116.0 . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
N3 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C32 N4 C33 122.4(8) . . ?
C32 N4 C34 121.4(9) . . ?
C33 N4 C34 116.2(8) . . ?
C32B N4 C34B 116(2) . . ?
C32B N4 C33B 123(2) . . ?
C33B N4 C34B 118(2) . . ?
O8 C32 N4 124.5(12) . . ?
O8 C32 H32 117.7 . . ?
N4 C32 H32 117.7 . . ?
N4 C33 H33A 109.5 . . ?
N4 C33 H33B 109.5 . . ?
N4 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N4 C34 H34A 109.5 . . ?
N4 C34 H34B 109.5 . . ?
N4 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N4 C34B H34D 109.5 . . ?
N4 C34B H34E 109.5 . . ?
N4 C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
O8 C32B N4 122(3) . . ?
O8 C32B H32B 119.2 . . ?
N4 C32B H32B 119.2 . . ?
N4 C33B H33D 109.5 . . ?
N4 C33B H33E 109.5 . . ?
N4 C33B H33F 109.5 . . ?
H33D C33B H33E 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?

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
Zn1 O1 C7 O2 7.2(7) . . . . ?
Zn1 O1 C7 C3 -171.8(4) . . . . ?
Zn1 O3 C8 O4 3.8(7) 10_665 . . . ?
Zn1 O3 C8 C5 -177.3(4) 10_665 . . . ?
Zn1 O5 C23 N1 174.6(6) . . . . ?
Zn1 O6 C26 N2 -168.4(6) . . . . ?
C1 C2 C3 C4 1.7(8) . . . . ?
C1 C2 C3 C7 -176.2(5) . . . . ?
C1 C9 C10 C11 -1.5(9) . . . . ?
C1 C9 C10 C15 179.1(5) . . . . ?
C1 C9 C22 C17 -178.0(5) . . . . ?
C1 C9 C22 C21 4.0(9) . . . . ?
C2 C1 C6 C5 -1.8(8) . . . . ?
C2 C1 C9 C10 -105.4(7) . . . . ?
C2 C1 C9 C22 73.4(7) . . . . ?
C2 C3 C4 C5 -1.0(8) . . . . ?
C2 C3 C7 O1 154.1(5) . . . . ?
C2 C3 C7 O2 -25.0(8) . . . . ?
C3 C4 C5 C6 -1.0(8) . . . . ?
C3 C4 C5 C8 178.0(5) . . . . ?
C4 C3 C7 O1 -23.8(8) . . . . ?
C4 C3 C7 O2 157.1(6) . . . . ?
C4 C5 C6 C1 2.5(8) . . . . ?
C4 C5 C8 O3 -23.4(8) . . . . ?
C4 C5 C8 O4 155.6(6) . . . . ?
C6 C1 C2 C3 -0.3(8) . . . . ?
C6 C1 C9 C10 71.8(7) . . . . ?
C6 C1 C9 C22 -109.4(6) . . . . ?
C6 C5 C8 O3 155.7(5) . . . . ?
C6 C5 C8 O4 -25.4(8) . . . . ?
C7 C3 C4 C5 176.9(5) . . . . ?
C8 C5 C6 C1 -176.5(5) . . . . ?
C9 C1 C2 C3 176.9(5) . . . . ?
C9 C1 C6 C5 -179.1(5) . . . . ?
C9 C10 C11 C12 -179.4(6) . . . . ?
C9 C10 C15 C14 177.7(5) . . . . ?
C9 C10 C15 C16 -1.6(8) . . . . ?
C10 C9 C22 C17 0.8(9) . . . . ?
C10 C9 C22 C21 -177.2(5) . . . . ?
C10 C11 C12 C13 0.9(10) . . . . ?
C10 C15 C16 C16 -179.4(5) . . . 2_665 ?
C10 C15 C16 C17 1.7(9) . . . . ?
C11 C10 C15 C14 -1.7(8) . . . . ?
C11 C10 C15 C16 179.0(5) . . . . ?
C11 C12 C13 C14 0.2(10) . . . . ?
C12 C13 C14 C15 -2.0(9) . . . . ?
C13 C14 C15 C10 2.8(8) . . . . ?
C13 C14 C15 C16 -177.9(6) . . . . ?
C14 C15 C16 C16 1.3(8) . . . 2_665 ?
C14 C15 C16 C17 -177.6(5) . . . . ?
C15 C10 C11 C12 0.0(9) . . . . ?
C15 C16 C17 C18 178.5(5) . . . . ?
C15 C16 C17 C22 -0.5(9) . . . . ?
C16 C16 C17 C18 -0.4(8) 2_665 . . . ?
C16 C16 C17 C22 -179.4(5) 2_665 . . . ?
C16 C17 C18 C19 -179.0(6) . . . . ?
C16 C17 C22 C9 -0.7(8) . . . . ?
C16 C17 C22 C21 177.4(5) . . . . ?
C17 C18 C19 C20 2.2(9) . . . . ?
C18 C17 C22 C9 -179.8(5) . . . . ?
C18 C17 C22 C21 -1.7(8) . . . . ?
C18 C19 C20 C21 -2.6(10) . . . . ?
C19 C20 C21 C22 0.9(10) . . . . ?
C20 C21 C22 C9 179.3(6) . . . . ?
C20 C21 C22 C17 1.3(9) . . . . ?
C22 C9 C10 C11 179.7(5) . . . . ?
C22 C9 C10 C15 0.4(9) . . . . ?
C22 C17 C18 C19 0.0(8) . . . . ?
C24 N1 C23 O5 177.8(8) . . . . ?
C25 N1 C23 O5 -1.1(13) . . . . ?
C27 N2 C26 O6 0.0(13) . . . . ?
C28 N2 C26 O6 175.2(9) . . . . ?
C30 N3 C29 O7 -5.2(16) . . . . ?
C31 N3 C29 O7 179.3(10) . . . . ?
C33 N4 C32 O8 7(3) . . . . ?
C34 N4 C32 O8 -174.9(18) . . . . ?
C34B N4 C32B O8 -3(5) . . . . ?
C33B N4 C32B O8 -165(3) . . . . ?

_olex2_date_sample_data_collection 2022-11-16
_olex2_date_sample_submission    2022-11-03
_olex2_exptl_crystal_mounting_method 
'Mounted on nylon loop with perfluoroether oil'
_olex2_submission_original_sample_id 'TM3125 10'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.649
_oxdiff_exptl_absorpt_empirical_full_min 0.598
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.70(5)
2 0.30(5)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cs2947_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2324985'
loop_
_audit_author_name
_audit_author_address
'Carla Slebodnick'
;Virginia Tech
United States of America
;
_audit_update_record             
;
2024-01-11 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_audit_creation_date             2023-03-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H22 Cu2 O10, 5.5[C3H7NO]'
_chemical_formula_sum            'C60.50 H60.50 Cu2 N5.50 O15.50'
_chemical_formula_weight         1239.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60.5 H60.5 Cu2 N5.5 O15.5'
_chemical_oxdiff_usercomment     'Trevor Makal (LJE 01 76 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'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   19.1907(3)
_cell_length_b                   14.79129(19)
_cell_length_c                   22.8997(6)
_cell_angle_alpha                90
_cell_angle_beta                 107.262(2)
_cell_angle_gamma                90
_cell_volume                     6207.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    35013
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      33.8230
_cell_measurement_theta_min      2.9660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.399
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.71a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2576
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 0 -5 0.0770
-3 0 5 0.0460
4 3 3 0.0811
-4 -3 -3 0.0811
6 -3 -3 0.1079
-6 3 3 0.1079
-1 3 -5 0.1232
-4 -1 -2 0.0886
-2 -5 -3 0.1046
0 0 -5 0.0702
-5 -5 4 0.0849
0 -1 5 0.0847
-1 -3 -5 0.0810
5 -2 1 0.1013
-5 2 -1 0.1013
-4 -15 22 0.0996
-1 5 0 0.1451
3 -3 5 0.0872

_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.123
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
3.4461 0.0011 -4.9921 -0.1189 -0.1261 -0.0362
-3.4461 -0.0011 4.9921 0.1189 0.1261 0.0362
3.5265 2.9994 3.0170 -0.1130 0.0496 0.2034
-3.5265 -2.9994 -3.0170 0.1130 -0.0496 -0.2034
6.4633 -2.9990 -2.9805 -0.2575 0.0094 -0.1093
-6.4633 2.9990 2.9805 0.2575 -0.0094 0.1093
-0.5500 3.0007 -5.0055 0.0525 -0.2089 0.0552
-4.0160 -0.9997 -2.0170 0.1448 -0.0626 -0.1083
-1.5284 -4.9992 -3.0105 0.0234 0.0016 -0.2705
0.4491 0.0009 -5.0031 -0.0077 -0.1439 -0.0644
-4.9544 -5.0006 3.9836 0.1380 0.1865 -0.2067
-0.4491 -1.0009 5.0027 -0.0000 0.1636 0.0214
-0.5497 -2.9989 -5.0080 0.0061 -0.0906 -0.2028
4.5056 -1.9999 1.0166 -0.1844 0.0954 -0.0298
-4.5056 1.9999 -1.0166 0.1844 -0.0954 0.0298
-3.7737 -15.0032 22.0008 -0.0153 0.9181 -0.3784
-0.9992 4.9996 -0.0016 0.0757 -0.1045 0.2055
2.5480 -3.0006 5.0128 -0.1266 0.2207 -0.0363

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29748
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        30.629
_diffrn_reflns_theta_max         30.629
_diffrn_reflns_theta_min         2.545
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -1.00  60.00   0.50   40.00    --   17.84-107.00 -58.00  122
  2  ω     42.00  96.00   0.50   40.00    --   17.84 178.00 -30.00  108
  3  ω    -62.00   3.00   0.50   40.00    --   17.84 -19.00 150.00  130
  4  ω    -95.00 -51.00   0.50   40.00    --  -18.23 -38.00 120.00   88
  5  ω    -11.00  41.00   0.50   40.00    --   17.84  77.00-180.00  104
  6  ω    -11.00  41.00   0.50   40.00    --   17.84  77.00  60.00  104
  7  ω    -59.00  20.00   0.50   40.00    --   17.84 -38.00  60.00  158
  8  ω    -95.00   5.00   0.50   40.00    --  -18.23 -38.00  90.00  200
  9  ω    -95.00   4.00   0.50   40.00    --  -18.23 -38.00 120.00  198
 10  ω    -26.00   4.00   0.50   40.00    --  -18.23 -38.00 120.00   60
 11  ω    -44.00 -17.00   0.50   40.00    --  -18.23  77.00 -90.00   54
 12  ω    -35.00   4.00   0.50   40.00    --  -18.23  81.00 -50.57   78
 13  ω    -34.00   5.00   0.50   40.00    --  -18.23 -77.00  30.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0370834000
_diffrn_orient_matrix_UB_12      0.0077293000
_diffrn_orient_matrix_UB_13      -0.0017858000
_diffrn_orient_matrix_UB_21      0.0058070000
_diffrn_orient_matrix_UB_22      -0.0197258000
_diffrn_orient_matrix_UB_23      0.0292740000
_diffrn_orient_matrix_UB_31      0.0093687000
_diffrn_orient_matrix_UB_32      0.0429862000
_diffrn_orient_matrix_UB_33      0.0137209000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                19494
_reflns_number_total             29748
_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         2.057
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         29748
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.1000
_refine_ls_restrained_S_all      1.076
_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)+(0.1421P)²+11.6678P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2859
_refine_ls_wR_factor_ref         0.3179
_refine_special_details          
;
The Laue symmetry and systematic absences were consistent with the 
orthorhombic space group Cccm (#63).  However, in this space group, 
there were systematically weak reflection suggesting a superlattice 
and the preliminary structure model showed significant disorder 
with unreasonable steric interactions and the preliminarly 
structure model showed significant disorder with unreasonable 
steric interactions.   Upon more careful analysis of the 
diffraction data, a monoclinic nonmerohedral twin was identified
(twin law 180 deg rotation about [001]) that accounted for the 
majority of the systematically weak reflection. During structure 
refinement on the HLKF 5 twin data, the twin ratios refined to 
approximately 50/50 (0.517(2) and 0.483(2)) accounting for the 
pseudo-orthorhombic symmetry.
The structure was solved in space group P2/c (#13) using SHELXT 
and refined using SHELXL  via Olex2.   Unlike the Cccm model, 
the diphenyl-bianthracene ligand is fully ordered in P2/c. The 
capping ligands of the paddlewheel complex are modeled as water 
but are likely a combination of water and DMF based on the presence
 of multiple difference electron density peaks near the coordinated 
oxygen. Attempts to model partial DMF occupancy at this site were 
unsuccessful--presumably the DMF is in dynamic motion. There is also 
evidence of multiple disordered DMF molecules in the solvent 
cavities. Using the solvent mask feature of OLEX2, a total of 
893 e-, equivalent to ~22 DMF molecules (880 e-) was subtracted 
from 3665 Å³ total void space per unit cell, or 
~5.5 DMF per asymmetric unit (223 e- subtracted/916 Å³). The final 
refinement model involved anisotropic displacement parameters for 
non-hydrogen atoms and a riding model for all hydrogen atoms.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.516(2)
 0.484(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C18(H18), C20(H20), C25(H25), C26(H26), C27(H27), C28(H28), C32(H32),
  C33(H33), C34(H34), C35(H35), C38(H38), C40(H40), C42(H42)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 -0.05336(4) 0.49433(3) 0.27548(5) 0.02410(19) Uani 1 1 d . . . . .
Cu2 Cu -0.05360(4) 0.00019(3) 0.44795(5) 0.0270(2) Uani 1 1 d . . . . .
O1 O 0.1038(2) 0.4084(3) 0.2874(3) 0.0369(11) Uani 1 1 d . . . . .
O2 O 0.0066(2) 0.3936(2) 0.3226(2) 0.0344(9) Uani 1 1 d . . . . .
O3 O 0.0097(2) 0.0866(3) 0.4231(3) 0.0432(12) Uani 1 1 d . . . . .
O4 O 0.1019(2) 0.0837(3) 0.5115(3) 0.0396(12) Uani 1 1 d . . . . .
O5 O 0.9047(2) 0.4092(3) 0.7159(3) 0.0381(11) Uani 1 1 d . . . . .
O6 O 0.9930(3) 0.4170(2) 0.6700(3) 0.0391(10) Uani 1 1 d . . . . .
O7 O 0.9975(3) 0.1019(3) 0.5709(3) 0.0408(11) Uani 1 1 d . . . . .
O8 O 0.9049(2) 0.0983(3) 0.4839(3) 0.0352(10) Uani 1 1 d . . . . .
O9 O -0.1378(4) -0.0023(2) 0.3625(3) 0.0529(16) Uani 1 1 d . . . . .
O12 O -0.1356(3) 0.4821(4) 0.3211(4) 0.0647(17) Uani 1 1 d . . . . .
C1 C 0.4635(2) 0.2466(4) 0.4893(5) 0.0313(9) Uani 1 1 d . . . . .
C2 C 0.4274(2) 0.2337(3) 0.4267(2) 0.0317(10) Uani 1 1 d . . . . .
C3 C 0.4661(3) 0.2202(4) 0.3827(3) 0.0408(12) Uani 1 1 d . . . . .
H3 H 0.517916 0.221345 0.395613 0.049 Uiso 1 1 calc R U . . .
C4 C 0.4310(3) 0.2064(4) 0.3249(3) 0.0516(15) Uani 1 1 d . . . . .
H4 H 0.457986 0.198294 0.296546 0.062 Uiso 1 1 calc R U . . .
C5 C 0.3528(4) 0.2031(4) 0.3034(3) 0.0552(16) Uani 1 1 d . . . . .
H5 H 0.328393 0.192049 0.261420 0.066 Uiso 1 1 calc R U . . .
C6 C 0.3135(3) 0.2162(4) 0.3438(3) 0.0430(13) Uani 1 1 d . . . . .
H6 H 0.261701 0.213940 0.329693 0.052 Uiso 1 1 calc R U . . .
C7 C 0.3482(2) 0.2324(3) 0.4045(3) 0.0388(12) Uani 1 1 d . . . . .
C8 C 0.3080(2) 0.2459(4) 0.4499(5) 0.0363(11) Uani 1 1 d . . . . .
C9 C 0.3452(3) 0.2602(3) 0.5104(3) 0.0348(11) Uani 1 1 d . . . . .
C10 C 0.3095(3) 0.2793(3) 0.5559(3) 0.0469(14) Uani 1 1 d . . . . .
H10 H 0.257727 0.283366 0.543264 0.056 Uiso 1 1 calc R U . . .
C11 C 0.3458(3) 0.2921(4) 0.6165(3) 0.0479(14) Uani 1 1 d . . . . .
H11 H 0.319308 0.302934 0.644881 0.058 Uiso 1 1 calc R U . . .
C12 C 0.4220(3) 0.2891(4) 0.6364(3) 0.0480(14) Uani 1 1 d . . . . .
H12 H 0.447896 0.298122 0.678247 0.058 Uiso 1 1 calc R U . . .
C13 C 0.4585(3) 0.2729(4) 0.5946(3) 0.0467(14) Uani 1 1 d . . . . .
H13 H 0.510268 0.270569 0.608683 0.056 Uiso 1 1 calc R U . . .
C14 C 0.4234(3) 0.2594(3) 0.5308(3) 0.0379(12) Uani 1 1 d . . . . .
C15 C 0.2272(2) 0.2430(4) 0.4279(5) 0.0387(14) Uani 1 1 d . . . . .
C16 C 0.1871(3) 0.3061(4) 0.3826(4) 0.0457(18) Uani 1 1 d . . . . .
H16 H 0.211717 0.347185 0.363630 0.055 Uiso 1 1 calc R U . . .
C17 C 0.1121(3) 0.3054(4) 0.3672(4) 0.0404(16) Uani 1 1 d . . . . .
C18 C 0.0730(2) 0.2412(4) 0.3878(4) 0.0344(13) Uani 1 1 d . . . . .
H18 H 0.021362 0.238652 0.371868 0.041 Uiso 1 1 calc R U . . .
C19 C 0.1114(3) 0.1784(4) 0.4336(4) 0.0351(14) Uani 1 1 d . . . . .
C20 C 0.1888(3) 0.1811(4) 0.4523(3) 0.0326(13) Uani 1 1 d . . . . .
H20 H 0.215131 0.139417 0.482326 0.039 Uiso 1 1 calc R U . . .
C21 C 0.0713(3) 0.3758(4) 0.3220(4) 0.0389(16) Uani 1 1 d . . . . .
C22 C 0.0718(3) 0.1123(4) 0.4588(3) 0.0347(14) Uani 1 1 d . . . . .
C23 C 0.5448(2) 0.2492(4) 0.5081(4) 0.0276(9) Uani 1 1 d . . . . .
C24 C 0.5851(2) 0.1735(3) 0.5374(2) 0.0335(10) Uani 1 1 d . . . . .
C25 C 0.5483(3) 0.0924(3) 0.5483(3) 0.0429(13) Uani 1 1 d . . . . .
H25 H 0.496463 0.090795 0.536014 0.051 Uiso 1 1 calc R U . . .
C26 C 0.5866(4) 0.0180(4) 0.5760(4) 0.0441(15) Uani 1 1 d . . . . .
H26 H 0.561354 -0.035095 0.581273 0.053 Uiso 1 1 calc R U . . .
C27 C 0.6628(3) 0.0202(4) 0.5965(3) 0.0422(14) Uani 1 1 d . . . . .
H27 H 0.689117 -0.031605 0.615600 0.051 Uiso 1 1 calc R U . . .
C28 C 0.6999(3) 0.0971(3) 0.5890(3) 0.0391(12) Uani 1 1 d . . . . .
H28 H 0.751574 0.098355 0.604849 0.047 Uiso 1 1 calc R U . . .
C29 C 0.6628(2) 0.1746(3) 0.5583(2) 0.0299(10) Uani 1 1 d . . . . .
C30 C 0.6995(2) 0.2533(4) 0.5488(5) 0.0309(9) Uani 1 1 d . . . . .
C31 C 0.6611(2) 0.3298(3) 0.5200(2) 0.0341(11) Uani 1 1 d . . . . .
C32 C 0.6969(3) 0.4098(3) 0.5098(3) 0.0366(11) Uani 1 1 d . . . . .
H32 H 0.748669 0.411888 0.522359 0.044 Uiso 1 1 calc R U . . .
C33 C 0.6589(4) 0.4826(4) 0.4829(4) 0.0446(16) Uani 1 1 d . . . . .
H33 H 0.684237 0.534819 0.476145 0.053 Uiso 1 1 calc R U . . .
C34 C 0.5815(4) 0.4827(4) 0.4643(4) 0.0475(18) Uani 1 1 d . . . . .
H34 H 0.555424 0.535162 0.446117 0.057 Uiso 1 1 calc R U . . .
C35 C 0.5440(3) 0.4066(3) 0.4727(3) 0.0400(12) Uani 1 1 d . . . . .
H35 H 0.492135 0.406702 0.459394 0.048 Uiso 1 1 calc R U . . .
C36 C 0.5824(2) 0.3272(3) 0.5012(2) 0.0321(10) Uani 1 1 d . . . . .
C37 C 0.7809(2) 0.2547(4) 0.5683(5) 0.0335(10) Uani 1 1 d . . . . .
C38 C 0.8194(3) 0.3155(4) 0.6140(4) 0.0375(15) Uani 1 1 d . . . . .
H38 H 0.793964 0.354723 0.633479 0.045 Uiso 1 1 calc R U . . .
C39 C 0.8943(3) 0.3170(4) 0.6298(4) 0.0367(15) Uani 1 1 d . . . . .
C40 C 0.9337(2) 0.2586(4) 0.6067(4) 0.0355(11) Uani 1 1 d . . . . .
H40 H 0.985522 0.260402 0.620419 0.043 Uiso 1 1 calc R U . . .
C41 C 0.8970(3) 0.1951(4) 0.5622(4) 0.0329(13) Uani 1 1 d . . . . .
C42 C 0.8186(3) 0.1962(3) 0.5429(3) 0.0288(12) Uani 1 1 d . . . . .
H42 H 0.792668 0.155546 0.511876 0.035 Uiso 1 1 calc R U . . .
C43 C 0.9337(3) 0.3880(4) 0.6757(3) 0.0332(14) Uani 1 1 d . . . . .
C44 C 0.9364(3) 0.1272(3) 0.5372(3) 0.0295(12) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Cu1 Cu1 2.6412(19) 2 ?
Cu1 O1 1.949(5) 2 ?
Cu1 O2 1.992(4) . ?
Cu1 O5 1.973(5) 4_465 ?
Cu1 O6 1.940(5) 3_666 ?
Cu1 O12 2.143(7) . ?
Cu2 Cu2 2.6464(19) 3_556 ?
Cu2 O3 1.961(5) . ?
Cu2 O4 1.942(5) 3_556 ?
Cu2 O7 1.974(4) 3_656 ?
Cu2 O8 1.951(5) 1_455 ?
Cu2 O9 2.137(7) . ?
O1 C21 1.241(9) . ?
O2 C21 1.274(8) . ?
O3 C22 1.286(7) . ?
O4 C22 1.247(9) . ?
O5 C43 1.249(9) . ?
O6 C43 1.259(8) . ?
O7 C44 1.255(7) . ?
O8 C44 1.265(8) . ?
C1 C2 1.409(11) . ?
C1 C14 1.401(11) . ?
C1 C23 1.491(6) . ?
C2 C3 1.432(8) . ?
C2 C7 1.453(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.312(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.435(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.370(9) . ?
C6 H6 0.9500 . ?
C6 C7 1.372(8) . ?
C7 C8 1.481(12) . ?
C8 C9 1.374(12) . ?
C8 C15 1.481(6) . ?
C9 C10 1.435(8) . ?
C9 C14 1.435(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.368(9) . ?
C11 H11 0.9500 . ?
C11 C12 1.397(9) . ?
C12 H12 0.9500 . ?
C12 C13 1.365(9) . ?
C13 H13 0.9500 . ?
C13 C14 1.429(9) . ?
C15 C16 1.438(10) . ?
C15 C20 1.393(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.376(8) . ?
C17 C18 1.378(9) . ?
C17 C21 1.513(8) . ?
C18 H18 0.9500 . ?
C18 C19 1.430(9) . ?
C19 C20 1.419(7) . ?
C19 C22 1.457(9) . ?
C20 H20 0.9500 . ?
C23 C24 1.412(7) . ?
C23 C36 1.394(7) . ?
C24 C25 1.453(6) . ?
C24 C29 1.423(6) . ?
C25 H25 0.9500 . ?
C25 C26 1.369(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.396(9) . ?
C27 H27 0.9500 . ?
C27 C28 1.380(8) . ?
C28 H28 0.9500 . ?
C28 C29 1.420(6) . ?
C29 C30 1.411(7) . ?
C30 C31 1.403(8) . ?
C30 C37 1.490(5) . ?
C31 C32 1.422(6) . ?
C31 C36 1.444(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.343(8) . ?
C33 H33 0.9500 . ?
C33 C34 1.419(9) . ?
C34 H34 0.9500 . ?
C34 C35 1.379(8) . ?
C35 H35 0.9500 . ?
C35 C36 1.436(6) . ?
C37 C38 1.411(10) . ?
C37 C42 1.365(10) . ?
C38 H38 0.9500 . ?
C38 C39 1.375(8) . ?
C39 C40 1.353(9) . ?
C39 C43 1.521(8) . ?
C40 H40 0.9500 . ?
C40 C41 1.411(9) . ?
C41 C42 1.437(7) . ?
C41 C44 1.471(8) . ?
C42 H42 0.9500 . ?

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
O1 Cu1 Cu1 87.34(16) 2 2 ?
O1 Cu1 O2 89.61(19) 2 . ?
O1 Cu1 O5 87.1(3) 2 4_465 ?
O1 Cu1 O12 91.7(2) 2 . ?
O2 Cu1 Cu1 80.83(15) . 2 ?
O2 Cu1 O12 93.6(2) . . ?
O5 Cu1 Cu1 84.56(15) 4_465 2 ?
O5 Cu1 O2 165.2(2) 4_465 . ?
O5 Cu1 O12 100.9(2) 4_465 . ?
O6 Cu1 Cu1 83.77(15) 3_666 2 ?
O6 Cu1 O1 170.9(2) 3_666 2 ?
O6 Cu1 O2 91.0(2) 3_666 . ?
O6 Cu1 O5 90.0(2) 3_666 4_465 ?
O6 Cu1 O12 97.4(2) 3_666 . ?
O12 Cu1 Cu1 174.38(18) . 2 ?
O3 Cu2 Cu2 83.08(17) . 3_556 ?
O3 Cu2 O7 90.6(2) . 3_656 ?
O3 Cu2 O9 96.4(2) . . ?
O4 Cu2 Cu2 85.48(15) 3_556 3_556 ?
O4 Cu2 O3 168.5(2) 3_556 . ?
O4 Cu2 O7 89.1(2) 3_556 3_656 ?
O4 Cu2 O8 87.7(2) 3_556 1_455 ?
O4 Cu2 O9 95.1(2) 3_556 . ?
O7 Cu2 Cu2 82.34(16) 3_656 3_556 ?
O7 Cu2 O9 95.7(2) 3_656 . ?
O8 Cu2 Cu2 85.81(15) 1_455 3_556 ?
O8 Cu2 O3 90.2(2) 1_455 . ?
O8 Cu2 O7 167.9(2) 1_455 3_656 ?
O8 Cu2 O9 96.2(2) 1_455 . ?
O9 Cu2 Cu2 177.96(19) . 3_556 ?
C21 O1 Cu1 119.4(4) . 2 ?
C21 O2 Cu1 123.8(4) . . ?
C22 O3 Cu2 123.1(5) . . ?
C22 O4 Cu2 122.1(4) . 3_556 ?
C43 O5 Cu1 120.7(4) . 4_666 ?
C43 O6 Cu1 123.2(5) . 3_666 ?
C44 O7 Cu2 124.4(4) . 3_656 ?
C44 O8 Cu2 121.4(4) . 1_655 ?
C2 C1 C23 117.0(10) . . ?
C14 C1 C2 120.3(4) . . ?
C14 C1 C23 122.7(10) . . ?
C1 C2 C3 122.2(5) . . ?
C1 C2 C7 120.4(5) . . ?
C3 C2 C7 117.4(5) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 120.9(5) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 119.2 . . ?
C3 C4 C5 121.5(6) . . ?
C5 C4 H4 119.2 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.5(6) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.7(5) . . ?
C7 C6 H6 119.7 . . ?
C2 C7 C8 117.5(5) . . ?
C6 C7 C2 120.0(5) . . ?
C6 C7 C8 122.5(5) . . ?
C7 C8 C15 117.9(8) . . ?
C9 C8 C7 120.4(4) . . ?
C9 C8 C15 121.7(8) . . ?
C8 C9 C10 123.1(5) . . ?
C8 C9 C14 120.5(5) . . ?
C14 C9 C10 116.4(5) . . ?
C9 C10 H10 118.2 . . ?
C11 C10 C9 123.6(5) . . ?
C11 C10 H10 118.2 . . ?
C10 C11 H11 120.2 . . ?
C10 C11 C12 119.7(5) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 H12 120.6 . . ?
C13 C12 C11 118.9(6) . . ?
C13 C12 H12 120.6 . . ?
C12 C13 H13 118.1 . . ?
C12 C13 C14 123.9(5) . . ?
C14 C13 H13 118.1 . . ?
C1 C14 C9 120.9(5) . . ?
C1 C14 C13 121.7(5) . . ?
C13 C14 C9 117.4(5) . . ?
C16 C15 C8 120.6(7) . . ?
C20 C15 C8 120.6(7) . . ?
C20 C15 C16 118.8(4) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 C15 118.4(7) . . ?
C17 C16 H16 120.8 . . ?
C16 C17 C18 123.5(6) . . ?
C16 C17 C21 117.4(6) . . ?
C18 C17 C21 119.0(5) . . ?
C17 C18 H18 120.5 . . ?
C17 C18 C19 119.0(4) . . ?
C19 C18 H18 120.5 . . ?
C18 C19 C22 120.7(5) . . ?
C20 C19 C18 117.9(6) . . ?
C20 C19 C22 121.3(5) . . ?
C15 C20 C19 121.9(5) . . ?
C15 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
O1 C21 O2 127.1(6) . . ?
O1 C21 C17 116.6(6) . . ?
O2 C21 C17 116.3(6) . . ?
O3 C22 C19 116.1(6) . . ?
O4 C22 O3 126.1(6) . . ?
O4 C22 C19 117.8(5) . . ?
C24 C23 C1 119.7(5) . . ?
C36 C23 C1 121.4(4) . . ?
C36 C23 C24 118.8(4) . . ?
C23 C24 C25 120.7(4) . . ?
C23 C24 C29 121.5(4) . . ?
C29 C24 C25 117.7(4) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 C24 121.4(5) . . ?
C26 C25 H25 119.3 . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.2(6) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 H27 119.9 . . ?
C28 C27 C26 120.3(5) . . ?
C28 C27 H27 119.9 . . ?
C27 C28 H28 119.2 . . ?
C27 C28 C29 121.7(5) . . ?
C29 C28 H28 119.2 . . ?
C28 C29 C24 118.6(4) . . ?
C30 C29 C24 118.6(4) . . ?
C30 C29 C28 122.8(4) . . ?
C29 C30 C37 119.5(5) . . ?
C31 C30 C29 121.4(3) . . ?
C31 C30 C37 119.1(5) . . ?
C30 C31 C32 122.5(4) . . ?
C30 C31 C36 118.5(4) . . ?
C32 C31 C36 119.1(4) . . ?
C31 C32 H32 119.3 . . ?
C33 C32 C31 121.4(5) . . ?
C33 C32 H32 119.3 . . ?
C32 C33 H33 119.5 . . ?
C32 C33 C34 121.1(6) . . ?
C34 C33 H33 119.5 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 C33 120.0(5) . . ?
C35 C34 H34 120.0 . . ?
C34 C35 H35 119.6 . . ?
C34 C35 C36 120.8(5) . . ?
C36 C35 H35 119.6 . . ?
C23 C36 C31 121.2(4) . . ?
C23 C36 C35 121.0(4) . . ?
C35 C36 C31 117.7(4) . . ?
C38 C37 C30 120.2(7) . . ?
C42 C37 C30 120.3(7) . . ?
C42 C37 C38 119.5(4) . . ?
C37 C38 H38 120.6 . . ?
C39 C38 C37 118.8(7) . . ?
C39 C38 H38 120.6 . . ?
C38 C39 C43 117.4(6) . . ?
C40 C39 C38 123.3(6) . . ?
C40 C39 C43 119.3(5) . . ?
C39 C40 H40 120.4 . . ?
C39 C40 C41 119.3(4) . . ?
C41 C40 H40 120.4 . . ?
C40 C41 C42 117.9(6) . . ?
C40 C41 C44 122.1(5) . . ?
C42 C41 C44 119.9(5) . . ?
C37 C42 C41 121.0(6) . . ?
C37 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
O5 C43 O6 127.4(6) . . ?
O5 C43 C39 116.4(5) . . ?
O6 C43 C39 116.2(6) . . ?
O7 C44 O8 125.7(6) . . ?
O7 C44 C41 117.3(6) . . ?
O8 C44 C41 116.9(5) . . ?

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
Cu1 O1 C21 O2 -1.8(10) 2 . . . ?
Cu1 O1 C21 C17 176.4(5) 2 . . . ?
Cu1 O2 C21 O1 -10.0(10) . . . . ?
Cu1 O2 C21 C17 171.8(5) . . . . ?
Cu1 O5 C43 O6 5.9(9) 4_666 . . . ?
Cu1 O5 C43 C39 -176.3(4) 4_666 . . . ?
Cu1 O6 C43 O5 -0.8(9) 3_666 . . . ?
Cu1 O6 C43 C39 -178.6(4) 3_666 . . . ?
Cu2 O3 C22 O4 3.9(9) . . . . ?
Cu2 O3 C22 C19 -178.7(4) . . . . ?
Cu2 O4 C22 O3 -5.6(9) 3_556 . . . ?
Cu2 O4 C22 C19 177.1(4) 3_556 . . . ?
Cu2 O7 C44 O8 -7.8(9) 3_656 . . . ?
Cu2 O7 C44 C41 170.8(4) 3_656 . . . ?
Cu2 O8 C44 O7 4.5(9) 1_655 . . . ?
Cu2 O8 C44 C41 -174.2(4) 1_655 . . . ?
C1 C2 C3 C4 178.5(6) . . . . ?
C1 C2 C7 C6 -177.4(5) . . . . ?
C1 C2 C7 C8 0.6(7) . . . . ?
C1 C23 C24 C25 1.3(14) . . . . ?
C1 C23 C24 C29 -177.3(9) . . . . ?
C1 C23 C36 C31 179.3(9) . . . . ?
C1 C23 C36 C35 -3.4(14) . . . . ?
C2 C1 C14 C9 -0.5(8) . . . . ?
C2 C1 C14 C13 -179.8(5) . . . . ?
C2 C1 C23 C24 -103.9(11) . . . . ?
C2 C1 C23 C36 80.6(9) . . . . ?
C2 C3 C4 C5 -0.7(9) . . . . ?
C2 C7 C8 C9 0.8(8) . . . . ?
C2 C7 C8 C15 -178.9(5) . . . . ?
C3 C2 C7 C6 1.8(7) . . . . ?
C3 C2 C7 C8 179.8(5) . . . . ?
C3 C4 C5 C6 1.0(10) . . . . ?
C4 C5 C6 C7 0.1(9) . . . . ?
C5 C6 C7 C2 -1.5(8) . . . . ?
C5 C6 C7 C8 -179.4(5) . . . . ?
C6 C7 C8 C9 178.7(5) . . . . ?
C6 C7 C8 C15 -0.9(8) . . . . ?
C7 C2 C3 C4 -0.7(8) . . . . ?
C7 C8 C9 C10 176.0(5) . . . . ?
C7 C8 C9 C14 -2.0(8) . . . . ?
C7 C8 C15 C16 -60.2(10) . . . . ?
C7 C8 C15 C20 122.0(9) . . . . ?
C8 C9 C10 C11 178.8(5) . . . . ?
C8 C9 C14 C1 1.8(8) . . . . ?
C8 C9 C14 C13 -178.8(5) . . . . ?
C8 C15 C16 C17 -174.8(9) . . . . ?
C8 C15 C20 C19 178.0(8) . . . . ?
C9 C8 C15 C16 120.2(9) . . . . ?
C9 C8 C15 C20 -57.7(10) . . . . ?
C9 C10 C11 C12 1.7(8) . . . . ?
C10 C9 C14 C1 -176.3(5) . . . . ?
C10 C9 C14 C13 3.1(6) . . . . ?
C10 C11 C12 C13 -0.3(8) . . . . ?
C11 C12 C13 C14 0.5(9) . . . . ?
C12 C13 C14 C1 177.4(6) . . . . ?
C12 C13 C14 C9 -2.0(8) . . . . ?
C14 C1 C2 C3 -179.9(5) . . . . ?
C14 C1 C2 C7 -0.7(8) . . . . ?
C14 C1 C23 C24 78.3(8) . . . . ?
C14 C1 C23 C36 -97.2(12) . . . . ?
C14 C9 C10 C11 -3.1(7) . . . . ?
C15 C8 C9 C10 -4.4(9) . . . . ?
C15 C8 C9 C14 177.7(5) . . . . ?
C15 C16 C17 C18 -7.5(14) . . . . ?
C15 C16 C17 C21 176.7(8) . . . . ?
C16 C15 C20 C19 0.1(13) . . . . ?
C16 C17 C18 C19 8.4(14) . . . . ?
C16 C17 C21 O1 23.0(11) . . . . ?
C16 C17 C21 O2 -158.6(8) . . . . ?
C17 C18 C19 C20 -4.7(12) . . . . ?
C17 C18 C19 C22 177.0(6) . . . . ?
C18 C17 C21 O1 -153.0(7) . . . . ?
C18 C17 C21 O2 25.4(11) . . . . ?
C18 C19 C20 C15 0.7(11) . . . . ?
C18 C19 C22 O3 28.8(9) . . . . ?
C18 C19 C22 O4 -153.6(6) . . . . ?
C20 C15 C16 C17 3.1(14) . . . . ?
C20 C19 C22 O3 -149.5(7) . . . . ?
C20 C19 C22 O4 28.1(10) . . . . ?
C21 C17 C18 C19 -175.9(6) . . . . ?
C22 C19 C20 C15 179.0(7) . . . . ?
C23 C1 C2 C3 2.3(7) . . . . ?
C23 C1 C2 C7 -178.6(4) . . . . ?
C23 C1 C14 C9 177.3(4) . . . . ?
C23 C1 C14 C13 -2.0(7) . . . . ?
C23 C24 C25 C26 179.2(7) . . . . ?
C23 C24 C29 C28 178.2(6) . . . . ?
C23 C24 C29 C30 -0.6(10) . . . . ?
C24 C23 C36 C31 3.7(11) . . . . ?
C24 C23 C36 C35 -178.9(6) . . . . ?
C24 C25 C26 C27 2.4(11) . . . . ?
C24 C29 C30 C31 0.8(12) . . . . ?
C24 C29 C30 C37 -177.8(7) . . . . ?
C25 C24 C29 C28 -0.5(8) . . . . ?
C25 C24 C29 C30 -179.2(6) . . . . ?
C25 C26 C27 C28 0.1(12) . . . . ?
C26 C27 C28 C29 -2.8(11) . . . . ?
C27 C28 C29 C24 2.9(8) . . . . ?
C27 C28 C29 C30 -178.4(7) . . . . ?
C28 C29 C30 C31 -177.9(6) . . . . ?
C28 C29 C30 C37 3.5(12) . . . . ?
C29 C24 C25 C26 -2.2(9) . . . . ?
C29 C30 C31 C32 -180.0(6) . . . . ?
C29 C30 C31 C36 1.2(12) . . . . ?
C29 C30 C37 C38 -116.8(9) . . . . ?
C29 C30 C37 C42 62.1(12) . . . . ?
C30 C31 C32 C33 -179.2(8) . . . . ?
C30 C31 C36 C23 -3.5(10) . . . . ?
C30 C31 C36 C35 179.1(7) . . . . ?
C30 C37 C38 C39 -178.2(8) . . . . ?
C30 C37 C42 C41 -178.4(7) . . . . ?
C31 C30 C37 C38 64.6(12) . . . . ?
C31 C30 C37 C42 -116.5(9) . . . . ?
C31 C32 C33 C34 0.9(11) . . . . ?
C32 C31 C36 C23 177.6(6) . . . . ?
C32 C31 C36 C35 0.2(8) . . . . ?
C32 C33 C34 C35 -1.4(13) . . . . ?
C33 C34 C35 C36 1.2(12) . . . . ?
C34 C35 C36 C23 -178.1(7) . . . . ?
C34 C35 C36 C31 -0.6(9) . . . . ?
C36 C23 C24 C25 176.9(6) . . . . ?
C36 C23 C24 C29 -1.7(11) . . . . ?
C36 C31 C32 C33 -0.3(9) . . . . ?
C37 C30 C31 C32 -1.4(12) . . . . ?
C37 C30 C31 C36 179.8(7) . . . . ?
C37 C38 C39 C40 -4.7(13) . . . . ?
C37 C38 C39 C43 175.6(7) . . . . ?
C38 C37 C42 C41 0.5(12) . . . . ?
C38 C39 C40 C41 2.9(14) . . . . ?
C38 C39 C43 O5 33.0(10) . . . . ?
C38 C39 C43 O6 -148.9(7) . . . . ?
C39 C40 C41 C42 0.6(12) . . . . ?
C39 C40 C41 C44 -177.3(6) . . . . ?
C40 C39 C43 O5 -146.6(7) . . . . ?
C40 C39 C43 O6 31.5(10) . . . . ?
C40 C41 C42 C37 -2.3(10) . . . . ?
C40 C41 C44 O7 27.9(9) . . . . ?
C40 C41 C44 O8 -153.3(7) . . . . ?
C42 C37 C38 C39 2.9(13) . . . . ?
C42 C41 C44 O7 -150.0(6) . . . . ?
C42 C41 C44 O8 28.8(9) . . . . ?
C43 C39 C40 C41 -177.4(6) . . . . ?
C44 C41 C42 C37 175.7(7) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 893 electrons were 
found in a volume of 3665Å³ in 1 void per unit cell. 
This is consistent with the presence of 
5.5[C3H7NO] per unit cell 
which account for 880 electrons 
per unit cell.
;
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 -0.761 -0.386 -0.452 3665.1 893.1 '22 DMF'

_smtbx_masks_void_probe_radius   1.1
_smtbx_masks_void_truncation_radius 1.2
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
tam9k@uvawise.edu
slebod@vt.edu
_olex2_date_sample_data_collection 2022-11-30
_olex2_date_sample_submission    2022-11-03
_olex2_submission_original_sample_id 'LJE 01 76 2'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.745
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.516(2) 37317 93622 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.484(2) 37382 93622 nmt 0.9991 0.0000 0.4895 -0.0000 -1.0000 0.0002 0.0036
-0.0004 -0.9992

_twin_special_details            
;
Component 2 rotated by -179.9841° 
around [1.00 -0.00 0.00] (reciprocal) or [0.97 0.00 0.24] (direct)
;
