#------------------------------------------------------------------------------
#$Date: 2024-09-06 03:57:47 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294583 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/68/7716817.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7716817
loop_
_publ_author_name
'Edwards, Abigail'
'Elkins, Landon J.'
'Slebodnick, Carla'
'Wang, Jinglei'
'Zhang, Qiang'
'Makal, Tegan A.'
_publ_section_title
;
 Structural diversity and solvent-induced transformations of a
 copper-based metal-organic framework with highly aromatic ligands.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14496
_journal_page_last               14504
_journal_paper_doi               10.1039/d4dt02085e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C44 H22 Cu2 O10, 5.5[C3H7NO]'
_chemical_formula_sum            'C60.5 H60.5 Cu2 N5.5 O15.5'
_chemical_formula_weight         1239.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-11 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.262(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1907(3)
_cell_length_b                   14.79129(19)
_cell_length_c                   22.8997(6)
_cell_measurement_reflns_used    35013
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      33.8230
_cell_measurement_theta_min      2.9660
_cell_volume                     6207.4(2)
_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)'
_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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_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_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       prism
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.123
_refine_diff_density_max         2.057
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.125
_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_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.1000
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19494
_reflns_number_total             29748
_reflns_threshold_expression     'I > 2σ(I)'
_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)
;
_cod_data_source_file            d4dt02085e2.cif
_cod_data_source_block           cs2947_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7716813--7716817.cif.'
_cod_original_formula_sum        'C60.50 H60.50 Cu2 N5.50 O15.50'
_cod_database_code               7716817
_chemical_oxdiff_formula         'C60.5 H60.5 Cu2 N5.5 O15.5'
_chemical_oxdiff_usercomment     'Trevor Makal (LJE 01 76 2)'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. 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)
;
_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.
;
_smtbx_masks_void_probe_radius   1.1
_smtbx_masks_void_truncation_radius 1.2
_shelx_shelxl_version_number     2018/3
_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_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
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 . . . . .
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'
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
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_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_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) . . . . ?
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
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
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'
