# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_BUT-103
_database_code_depnum_ccdc_archive 'CCDC 1888829'
loop_
_audit_author_name
_audit_author_address
'Xiang-Jing Kong'
;Beijing University of Technology
China
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2019-01-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C74 H78 Mn4 N10 O22, 3(C3 H7 N O)'
_chemical_formula_sum            'C83 H99 Mn4 N13 O25'
_chemical_formula_weight         1898.51
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mn C N O'
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'
Mn Mn -0.5299 2.8052 '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           4
_space_group_name_H-M_alt        'P 21 '
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.08670(10)
_cell_length_b                   15.6900(2)
_cell_length_c                   15.2941(2)
_cell_angle_alpha                90
_cell_angle_beta                 105.4640(10)
_cell_angle_gamma                90
_cell_volume                     2332.82(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    24042
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.2600
_cell_measurement_theta_min      2.8490
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.963
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             988
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40263
_diffrn_reflns_point_group_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         2.998
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -126.00  -2.00   0.50    0.50    --  -36.20 -39.00  55.00  248
  2  ω   -140.00 -16.00   0.50    0.50    -- -105.40  39.00-149.00  248
  3  ω   -195.00 -71.00   0.50    0.50    -- -105.40 -39.00  55.00  248
  4  ω    -84.00  39.00   0.50    0.50    --    5.00 -39.00  55.00  246
  5  ω    -71.00  53.00   0.50    0.50    --  -36.20  38.00 120.00  248
  6  ω    -71.00  53.00   0.50    0.50    --  -36.20  69.00 150.84  248
  7  ω    -71.00  53.00   0.50    0.50    --  -36.20  39.00-149.00  248
  8  ω    -71.00  53.00   0.50    0.50    --  -36.20  41.00 -44.73  248
  9  ω    -71.00  53.00   0.50    0.50    --  -36.20  72.00   6.45  248
 10  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00 150.00  248
 11  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00-120.00  248
 12  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00  30.00  248
 13  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00  90.00  248
 14  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00 -60.00  248
 15  ω   -195.00 -71.00   0.50    0.50    -- -105.40 -19.00-180.00  248
 16  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00-180.00  248
 17  ω   -195.00 -71.00   0.50    0.50    -- -105.40 -47.00   5.31  248
 18  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00   0.00  248
 19  ω   -140.00 -16.00   0.50    0.50    -- -105.40  19.00  60.00  248
 20  ω   -140.00 -16.00   0.50    0.50    -- -105.40  19.00 120.00  248
 21  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00 -90.00  248
 22  ω   -195.00 -16.00   0.50    0.50    -- -105.40   0.00-150.00  358
 23  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00   0.00  248
 24  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00  60.00  248
 25  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00 120.00  248
 26  ω   -140.00 -16.00   0.50    0.50    -- -105.40  38.00 -60.00  248
 27  ω   -140.00 -16.00   0.50    0.50    -- -105.40  57.00 120.00  248
 28  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00-150.00  248
 29  ω   -140.00 -16.00   0.50    0.50    -- -105.40  72.00 -30.00  248
 30  ω    -29.00  94.00   0.50    0.50    --    5.00  57.00-180.00  246
 31  ω   -126.00  -2.00   0.50    0.50    --  -36.20 -69.00 114.24  248
 32  ω   -126.00  -2.00   0.50    0.50    --  -36.20 -58.00 -79.83  248
 33  ω   -126.00  -2.00   0.50    0.50    --  -36.20 -52.00 -46.50  248
 34  ω   -126.00  -2.00   0.50    0.50    --  -36.20 -38.00 -30.00  248
 35  ω   -126.00  -2.00   0.50    0.50    --  -36.20 -58.00-160.23  248
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0356752000
_diffrn_orient_matrix_UB_12      0.0326757000
_diffrn_orient_matrix_UB_13      0.0859313000
_diffrn_orient_matrix_UB_21      0.1370768000
_diffrn_orient_matrix_UB_22      -0.0355587000
_diffrn_orient_matrix_UB_23      0.0587981000
_diffrn_orient_matrix_UB_31      0.0709561000
_diffrn_orient_matrix_UB_32      0.0855742000
_diffrn_orient_matrix_UB_33      -0.0083085000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    0.759
_reflns_Friedel_fraction_max     0.759
_reflns_number_gt                7208
_reflns_number_total             7367
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 
;
 Flack x determined using 2814 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         7367
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0464
_refine_ls_restrained_S_all      1.062
_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)+(0.1029P)²+1.0512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1321
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N7-C41
 1.5 with sigma of 0.01
 C13-O13
 1.25 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N7)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: C13(0.5) H13(0.5) N7(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
 C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) O13(0.5)
5.a Rotating group:
 N2(H2A,H2B), N1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C22(H22), C6(H6), C20(H20), C8(H8), C10(H10), C11(H11), C17(H17),
 C33(H33), C23(H23), C26(H26), C14(H14), C0AA(H0AA), C28(H28), C25(H25),
 C40(H40), C35(H35), C31(H31), C13(H13)
5.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C38(H38A,H38B,H38C), C32(H32A,H32B,H32C), C29(H29A,H29B,
 H29C), C37(H37A,H37B,H37C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C30(H30A,
 H30B,H30C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C)
;
_atom_sites_solution_hydrogens   mixed
_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
Mn2 Mn 0.02257(6) 0.49569(5) 0.64235(4) 0.01826(18) Uani 1 1 d . . . . .
Mn1 Mn 0.20148(7) 0.35978(5) 0.53075(5) 0.0245(2) Uani 1 1 d . . . . .
O1 O 0.0243(4) 0.5603(2) 0.5229(2) 0.0344(8) Uani 1 1 d . . . . .
O9 O 0.9371(3) 0.5798(2) 0.7353(2) 0.0268(7) Uani 1 1 d . . . . .
O10 O -0.0328(3) 0.8585(2) 0.4027(2) 0.0234(6) Uani 1 1 d . . . . .
O11 O -0.0209(4) 0.8812(2) 0.2631(2) 0.0317(8) Uani 1 1 d . . . . .
O4 O 0.2253(3) 0.5284(3) 0.7092(2) 0.0328(9) Uani 1 1 d . . . . .
O8 O 0.8002(3) 0.5067(3) 0.6237(2) 0.0340(8) Uani 1 1 d . . . . .
O7 O 0.3047(4) 0.2527(3) 0.6137(3) 0.0429(10) Uani 1 1 d . . . . .
O3 O 0.3275(4) 0.4445(3) 0.6291(3) 0.0443(10) Uani 1 1 d . . . . .
O2 O 0.1068(5) 0.4619(3) 0.4467(3) 0.0454(11) Uani 1 1 d . . . . .
O6 O 0.0931(5) 0.2654(3) 0.4343(3) 0.0462(10) Uani 1 1 d . . . . .
C3 C 0.5739(5) 0.5327(3) 0.6920(3) 0.0255(10) Uani 1 1 d . . . . .
H3 H 0.564782 0.496715 0.642427 0.031 Uiso 1 1 calc R . . . .
O5 O 0.3577(5) 0.3495(4) 0.4584(4) 0.0600(13) Uani 1 1 d . . . . .
N5 N -0.0443(6) 0.2719(3) 0.2917(3) 0.0409(11) Uani 1 1 d . . . . .
C22 C 0.0918(5) 0.5717(3) 0.3022(3) 0.0280(10) Uani 1 1 d . . . . .
H22 H 0.120790 0.515936 0.298167 0.034 Uiso 1 1 calc R . . . .
C15 C 0.0647(5) 0.5352(3) 0.4563(3) 0.0268(10) Uani 1 1 d . . . . .
C16 C 0.0588(5) 0.5977(3) 0.3807(3) 0.0255(10) Uani 1 1 d . . . . .
C2 C 0.4630(5) 0.5462(3) 0.7274(3) 0.0248(10) Uani 1 1 d . . . . .
C6 C 0.7125(4) 0.6252(3) 0.8054(3) 0.0258(10) Uani 1 1 d . . . . .
H6 H 0.796558 0.651443 0.830933 0.031 Uiso 1 1 calc R . . . .
C4 C 0.6984(5) 0.5724(3) 0.7302(3) 0.0245(9) Uani 1 1 d . . . . .
C21 C 0.0826(5) 0.6266(3) 0.2297(3) 0.0285(10) Uani 1 1 d . . . . .
C7 C 0.6024(5) 0.6395(3) 0.8434(3) 0.0267(10) Uani 1 1 d . . . . .
C20 C 0.0430(5) 0.7109(4) 0.2385(3) 0.0285(10) Uani 1 1 d . . . . .
H20 H 0.036812 0.748898 0.190848 0.034 Uiso 1 1 calc R . . . .
C8 C 0.4763(4) 0.5990(3) 0.8021(3) 0.0248(10) Uani 1 1 d . . . . .
H8 H 0.401036 0.607803 0.825238 0.030 Uiso 1 1 calc R . . . .
C10 C 0.7216(5) 0.7537(4) 0.9514(4) 0.0345(12) Uani 1 1 d . . . . .
H10 H 0.778019 0.764798 0.913528 0.041 Uiso 1 1 calc R . . . .
C19 C -0.0176(4) 0.8302(3) 0.3274(3) 0.0238(9) Uani 1 1 d . . . . .
C1 C 0.3280(4) 0.5033(4) 0.6847(3) 0.0262(9) Uani 1 1 d . . . . .
C5 C 0.8192(5) 0.5528(3) 0.6939(3) 0.0244(10) Uani 1 1 d . . . . .
C11 C 0.7397(6) 0.7987(4) 1.0317(4) 0.0410(13) Uani 1 1 d . . . . .
H11 H 0.809682 0.839061 1.047038 0.049 Uiso 1 1 calc R . . . .
N2 N 0.6765(6) 0.8338(5) 1.1698(4) 0.0635(18) Uani 1 1 d . . . . .
H2A H 0.651999 0.885701 1.155565 0.076 Uiso 1 1 d GR . . . .
H2B H 0.626196 0.813044 1.202149 0.076 Uiso 1 1 d GR . . . .
N3 N 0.5656(5) 0.3233(4) 0.4362(4) 0.0551(15) Uani 1 1 d . . . . .
C9 C 0.6188(5) 0.6918(4) 0.9270(3) 0.0308(11) Uani 1 1 d . . . . .
C17 C 0.0191(5) 0.6824(3) 0.3886(3) 0.0236(9) Uani 1 1 d . . . . .
H17 H -0.002558 0.700477 0.441003 0.028 Uiso 1 1 calc R . . . .
C18 C 0.0124(5) 0.7391(3) 0.3180(3) 0.0236(10) Uani 1 1 d . . . . .
C24 C 0.1185(6) 0.5984(4) 0.1461(3) 0.0338(12) Uani 1 1 d . . . . .
C12 C 0.6580(6) 0.7859(5) 1.0895(4) 0.0480(16) Uani 1 1 d . . . . .
N4 N 0.4523(6) 0.1486(4) 0.5996(4) 0.0581(16) Uani 1 1 d . . . . .
C33 C -0.0071(7) 0.2424(4) 0.3747(4) 0.0409(13) Uani 1 1 d . . . . .
H33 H -0.061859 0.200166 0.389663 0.049 Uiso 1 1 calc R . . . .
N1 N 0.2294(7) 0.5287(5) -0.0907(4) 0.0652(19) Uani 1 1 d . . . . .
H1A H 0.293533 0.490391 -0.077700 0.078 Uiso 1 1 d GR . . . .
H1B H 0.160029 0.508431 -0.131738 0.078 Uiso 1 1 d GR . . . .
C23 C 0.2246(6) 0.5412(4) 0.1489(4) 0.0386(13) Uani 1 1 d . . . . .
H23 H 0.272238 0.517870 0.204313 0.046 Uiso 1 1 calc R . . . .
C26 C 0.0828(8) 0.6049(6) -0.0159(4) 0.060(2) Uani 1 1 d . . . . .
H26 H 0.033467 0.626775 -0.071545 0.072 Uiso 1 1 calc R . . . .
C34 C -0.1633(8) 0.2384(5) 0.2273(5) 0.0611(19) Uani 1 1 d . . . . .
H34A H -0.197356 0.190016 0.253116 0.092 Uiso 1 1 calc GR . . . .
H34B H -0.138893 0.221220 0.173392 0.092 Uiso 1 1 calc GR . . . .
H34C H -0.233362 0.281433 0.212324 0.092 Uiso 1 1 calc GR . . . .
C14 C 0.5364(6) 0.6778(5) 0.9860(4) 0.0453(15) Uani 1 1 d . . . . .
H14 H 0.466877 0.637181 0.971305 0.054 Uiso 1 1 calc R . . . .
C27 C 0.1899(7) 0.5492(4) -0.0133(4) 0.0455(15) Uani 1 1 d . . . . .
C0AA C 0.5562(7) 0.7231(6) 1.0651(5) 0.061(2) Uani 1 1 d . . . . .
H0AA H 0.500637 0.711888 1.103473 0.073 Uiso 1 1 calc R . . . .
C28 C 0.2612(7) 0.5182(4) 0.0709(4) 0.0428(14) Uani 1 1 d . . . . .
H28 H 0.334741 0.481259 0.075158 0.051 Uiso 1 1 calc R . . . .
C25 C 0.0467(7) 0.6287(5) 0.0604(4) 0.0499(16) Uani 1 1 d . . . . .
H25 H -0.026803 0.665845 0.055461 0.060 Uiso 1 1 calc R . . . .
C40 C 0.3293(6) 0.1844(4) 0.5800(4) 0.0446(14) Uani 1 1 d . . . . .
H40 H 0.257285 0.157115 0.538766 0.054 Uiso 1 1 calc R . . . .
N6 N 0.1832(9) 0.8640(6) 0.0888(6) 0.086(2) Uani 1 1 d . . . . .
C35 C 0.4779(8) 0.3556(5) 0.4803(5) 0.0552(17) Uani 1 1 d . . . . .
H35 H 0.516399 0.385838 0.533283 0.066 Uiso 1 1 calc R . . . .
C38 C 0.4741(12) 0.0666(7) 0.5613(6) 0.091(4) Uani 1 1 d . . . . .
H38A H 0.503626 0.025709 0.609265 0.137 Uiso 1 1 calc GR . . . .
H38B H 0.543293 0.072278 0.529129 0.137 Uiso 1 1 calc GR . . . .
H38C H 0.389637 0.047698 0.520315 0.137 Uiso 1 1 calc GR . . . .
C32 C 0.0448(15) 0.3285(8) 0.2615(6) 0.109(5) Uani 1 1 d . . . . .
H32A H 0.013567 0.386100 0.263636 0.164 Uiso 1 1 calc GR . . . .
H32B H 0.044286 0.314492 0.200272 0.164 Uiso 1 1 calc GR . . . .
H32C H 0.136595 0.323140 0.300081 0.164 Uiso 1 1 calc GR . . . .
O12 O 0.0631(11) 0.8116(7) -0.0488(5) 0.119(3) Uani 1 1 d . . . . .
C29 C 0.2831(12) 0.8519(10) 0.1689(8) 0.103(4) Uani 1 1 d . . . . .
H29A H 0.315899 0.794250 0.171872 0.155 Uiso 1 1 calc GR . . . .
H29B H 0.244992 0.862582 0.219079 0.155 Uiso 1 1 calc GR . . . .
H29C H 0.358057 0.890405 0.171679 0.155 Uiso 1 1 calc GR . . . .
C37 C 0.7115(9) 0.3423(9) 0.4694(9) 0.096(4) Uani 1 1 d . . . . .
H37A H 0.741701 0.372266 0.423474 0.143 Uiso 1 1 calc GR . . . .
H37B H 0.762307 0.290123 0.483964 0.143 Uiso 1 1 calc GR . . . .
H37C H 0.726913 0.377135 0.522821 0.143 Uiso 1 1 calc GR . . . .
C36 C 0.5142(12) 0.2785(10) 0.3521(8) 0.117(5) Uani 1 1 d . . . . .
H36A H 0.425688 0.254586 0.349847 0.176 Uiso 1 1 calc GR . . . .
H36B H 0.576771 0.233543 0.347814 0.176 Uiso 1 1 calc GR . . . .
H36C H 0.505661 0.317276 0.302377 0.176 Uiso 1 1 calc GR . . . .
C39 C 0.5689(9) 0.1879(7) 0.6631(8) 0.090(3) Uani 1 1 d . . . . .
H39A H 0.626842 0.214402 0.630383 0.135 Uiso 1 1 calc GR . . . .
H39B H 0.620301 0.145157 0.703009 0.135 Uiso 1 1 calc GR . . . .
H39C H 0.536826 0.230116 0.698058 0.135 Uiso 1 1 calc GR . . . .
C31 C 0.1560(12) 0.8053(9) 0.0217(7) 0.095(4) Uani 1 1 d . . . . .
H31 H 0.211220 0.756925 0.029363 0.115 Uiso 1 1 calc R . . . .
C30 C 0.1007(13) 0.9388(8) 0.0786(10) 0.102(4) Uani 1 1 d . . . . .
H30A H 0.057913 0.942349 0.127543 0.153 Uiso 1 1 calc GR . . . .
H30B H 0.031030 0.936498 0.021926 0.153 Uiso 1 1 calc GR . . . .
H30C H 0.157460 0.988092 0.079469 0.153 Uiso 1 1 calc GR . . . .
C13 C 0.647(2) 0.493(2) 1.2121(15) 0.123(9) Uani 0.5 1 d D U P . .
H13 H 0.698692 0.535638 1.247174 0.148 Uiso 0.5 1 calc R . P . .
N7 N 0.6692(12) 0.4771(9) 1.1426(9) 0.063(3) Uani 0.5 1 d D U P . .
C42 C 0.782(2) 0.5195(18) 1.1124(17) 0.100(7) Uani 0.5 1 d . U P . .
H42A H 0.764670 0.579630 1.106051 0.150 Uiso 0.5 1 calc GR . P . .
H42B H 0.786249 0.496195 1.055146 0.150 Uiso 0.5 1 calc GR . P . .
H42C H 0.868292 0.509900 1.156690 0.150 Uiso 0.5 1 calc GR . P . .
C41 C 0.597(2) 0.4354(18) 1.0529(18) 0.178(16) Uani 0.5 1 d D U P . .
H41A H 0.580055 0.376560 1.062968 0.266 Uiso 0.5 1 calc GR . P . .
H41B H 0.654978 0.439347 1.012194 0.266 Uiso 0.5 1 calc GR . P . .
H41C H 0.511817 0.463984 1.026857 0.266 Uiso 0.5 1 calc GR . P . .
O13 O 0.5563(19) 0.4556(17) 1.2437(11) 0.138(8) Uani 0.5 1 d D . P . .


_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
Mn2 O1 2.094(3) . ?
Mn2 O9 2.271(3) 1_455 ?
Mn2 O10 2.270(4) 2_546 ?
Mn2 O11 2.309(4) 2_546 ?
Mn2 O4 2.091(3) . ?
Mn2 O8 2.191(3) 1_455 ?
Mn2 C5 2.549(4) 1_455 ?
Mn1 O10 2.204(3) 2_546 ?
Mn1 O7 2.194(4) . ?
Mn1 O3 2.150(4) . ?
Mn1 O2 2.115(4) . ?
Mn1 O6 2.169(4) . ?
Mn1 O5 2.160(4) . ?
O1 C15 1.256(6) . ?
O9 C5 1.263(6) . ?
O10 C19 1.281(6) . ?
O11 C19 1.261(6) . ?
O4 C1 1.255(6) . ?
O8 C5 1.266(6) . ?
O7 C40 1.241(8) . ?
O3 C1 1.255(7) . ?
O2 C15 1.249(6) . ?
O6 C33 1.221(8) . ?
C3 C2 1.382(6) . ?
C3 C4 1.384(7) . ?
O5 C35 1.172(9) . ?
N5 C33 1.309(8) . ?
N5 C34 1.435(9) . ?
N5 C32 1.426(10) . ?
C22 C16 1.390(7) . ?
C22 C21 1.388(7) . ?
C15 C16 1.504(7) . ?
C16 C17 1.402(7) . ?
C2 C8 1.388(7) . ?
C2 C1 1.503(6) . ?
C6 C4 1.394(7) . ?
C6 C7 1.401(7) . ?
C4 C5 1.499(6) . ?
C21 C20 1.398(8) . ?
C21 C24 1.486(6) . ?
C7 C8 1.411(7) . ?
C7 C9 1.491(7) . ?
C20 C18 1.404(7) . ?
C10 C11 1.386(8) . ?
C10 C9 1.397(8) . ?
C19 C18 1.476(7) . ?
C11 C12 1.375(9) . ?
N2 C12 1.410(8) . ?
N3 C35 1.347(9) . ?
N3 C37 1.455(10) . ?
N3 C36 1.436(11) . ?
C9 C14 1.397(8) . ?
C17 C18 1.386(7) . ?
C24 C23 1.389(8) . ?
C24 C25 1.400(8) . ?
C12 C0AA 1.399(10) . ?
N4 C40 1.322(9) . ?
N4 C38 1.454(11) . ?
N4 C39 1.449(11) . ?
N1 C27 1.384(7) . ?
C23 C28 1.388(7) . ?
C26 C27 1.382(11) . ?
C26 C25 1.364(8) . ?
C14 C0AA 1.371(9) . ?
C27 C28 1.385(9) . ?
N6 C29 1.376(13) . ?
N6 C31 1.351(13) . ?
N6 C30 1.423(15) . ?
O12 C31 1.229(13) . ?
C13 N7 1.17(3) . ?
C13 O13 1.28(2) . ?
N7 C42 1.50(3) . ?
N7 C41 1.517(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 Mn2 O9 110.98(14) . 1_455 ?
O1 Mn2 O10 100.51(13) . 2_546 ?
O1 Mn2 O11 157.86(14) . 2_546 ?
O1 Mn2 O8 95.43(15) . 1_455 ?
O1 Mn2 C5 107.14(15) . 1_455 ?
O9 Mn2 O11 89.59(13) 1_455 2_546 ?
O9 Mn2 C5 29.66(14) 1_455 1_455 ?
O10 Mn2 O9 142.76(12) 2_546 1_455 ?
O10 Mn2 O11 57.38(11) 2_546 2_546 ?
O10 Mn2 C5 122.17(14) 2_546 1_455 ?
O11 Mn2 C5 86.49(15) 2_546 1_455 ?
O4 Mn2 O1 94.19(15) . . ?
O4 Mn2 O9 92.10(13) . 1_455 ?
O4 Mn2 O10 105.24(13) . 2_546 ?
O4 Mn2 O11 93.10(15) . 2_546 ?
O4 Mn2 O8 151.39(14) . 1_455 ?
O4 Mn2 C5 121.71(15) . 1_455 ?
O8 Mn2 O9 59.31(12) 1_455 1_455 ?
O8 Mn2 O10 99.38(14) 1_455 2_546 ?
O8 Mn2 O11 87.98(15) 1_455 2_546 ?
O8 Mn2 C5 29.78(14) 1_455 1_455 ?
O7 Mn1 O10 91.82(15) . 2_546 ?
O3 Mn1 O10 93.87(14) . 2_546 ?
O3 Mn1 O7 88.17(18) . . ?
O3 Mn1 O6 173.91(18) . . ?
O3 Mn1 O5 91.64(19) . . ?
O2 Mn1 O10 90.49(15) . 2_546 ?
O2 Mn1 O7 177.55(17) . . ?
O2 Mn1 O3 92.51(19) . . ?
O2 Mn1 O6 92.27(17) . . ?
O2 Mn1 O5 91.0(2) . . ?
O6 Mn1 O10 89.85(16) . 2_546 ?
O6 Mn1 O7 86.90(17) . . ?
O5 Mn1 O10 174.22(18) . 2_546 ?
O5 Mn1 O7 86.6(2) . . ?
O5 Mn1 O6 84.5(2) . . ?
C15 O1 Mn2 129.5(3) . . ?
C5 O9 Mn2 87.5(3) . 1_655 ?
Mn1 O10 Mn2 103.60(13) 2_556 2_556 ?
C19 O10 Mn2 91.7(3) . 2_556 ?
C19 O10 Mn1 135.3(3) . 2_556 ?
C19 O11 Mn2 90.5(3) . 2_556 ?
C1 O4 Mn2 123.7(3) . . ?
C5 O8 Mn2 91.0(3) . 1_655 ?
C40 O7 Mn1 122.5(4) . . ?
C1 O3 Mn1 145.5(3) . . ?
C15 O2 Mn1 137.6(3) . . ?
C33 O6 Mn1 151.2(4) . . ?
C2 C3 C4 120.2(4) . . ?
C35 O5 Mn1 133.4(5) . . ?
C33 N5 C34 120.5(6) . . ?
C33 N5 C32 119.5(6) . . ?
C32 N5 C34 119.4(6) . . ?
C21 C22 C16 121.9(5) . . ?
O1 C15 C16 117.6(4) . . ?
O2 C15 O1 125.3(5) . . ?
O2 C15 C16 117.1(4) . . ?
C22 C16 C15 120.2(5) . . ?
C22 C16 C17 119.4(4) . . ?
C17 C16 C15 120.3(4) . . ?
C3 C2 C8 120.2(4) . . ?
C3 C2 C1 119.7(4) . . ?
C8 C2 C1 120.2(4) . . ?
C4 C6 C7 121.3(4) . . ?
C3 C4 C6 119.8(4) . . ?
C3 C4 C5 119.1(4) . . ?
C6 C4 C5 120.9(4) . . ?
C22 C21 C20 118.1(4) . . ?
C22 C21 C24 121.6(5) . . ?
C20 C21 C24 120.3(5) . . ?
C6 C7 C8 117.5(4) . . ?
C6 C7 C9 121.6(4) . . ?
C8 C7 C9 120.8(4) . . ?
C21 C20 C18 121.0(4) . . ?
C2 C8 C7 121.0(4) . . ?
C11 C10 C9 120.3(5) . . ?
O10 C19 C18 120.0(4) . . ?
O11 C19 O10 119.7(5) . . ?
O11 C19 C18 120.1(4) . . ?
O4 C1 C2 117.0(4) . . ?
O3 C1 O4 125.3(4) . . ?
O3 C1 C2 117.6(4) . . ?
O9 C5 Mn2 62.9(2) . 1_655 ?
O9 C5 O8 121.7(4) . . ?
O9 C5 C4 119.7(4) . . ?
O8 C5 Mn2 59.2(2) . 1_655 ?
O8 C5 C4 118.5(4) . . ?
C4 C5 Mn2 170.9(4) . 1_655 ?
C12 C11 C10 122.3(6) . . ?
C35 N3 C37 119.1(7) . . ?
C35 N3 C36 120.3(7) . . ?
C36 N3 C37 120.3(7) . . ?
C10 C9 C7 121.1(5) . . ?
C10 C9 C14 117.6(5) . . ?
C14 C9 C7 121.3(5) . . ?
C18 C17 C16 119.8(4) . . ?
C20 C18 C19 119.2(4) . . ?
C17 C18 C20 119.8(5) . . ?
C17 C18 C19 121.0(4) . . ?
C23 C24 C21 121.9(5) . . ?
C23 C24 C25 116.8(5) . . ?
C25 C24 C21 121.4(5) . . ?
C11 C12 N2 121.2(6) . . ?
C11 C12 C0AA 117.1(5) . . ?
C0AA C12 N2 121.7(6) . . ?
C40 N4 C38 121.3(7) . . ?
C40 N4 C39 121.0(7) . . ?
C39 N4 C38 117.6(7) . . ?
O6 C33 N5 125.9(6) . . ?
C28 C23 C24 121.3(5) . . ?
C25 C26 C27 122.3(6) . . ?
C0AA C14 C9 121.1(6) . . ?
N1 C27 C28 121.1(7) . . ?
C26 C27 N1 121.6(6) . . ?
C26 C27 C28 117.1(5) . . ?
C14 C0AA C12 121.6(6) . . ?
C27 C28 C23 121.2(6) . . ?
C26 C25 C24 121.2(6) . . ?
O7 C40 N4 123.5(6) . . ?
C29 N6 C30 118.6(11) . . ?
C31 N6 C29 122.3(10) . . ?
C31 N6 C30 119.0(10) . . ?
O5 C35 N3 126.4(7) . . ?
O12 C31 N6 124.3(12) . . ?
N7 C13 O13 125(3) . . ?
C13 N7 C42 122(2) . . ?
C13 N7 C41 139(2) . . ?
C42 N7 C41 97.6(17) . . ?

_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 1.184
_oxdiff_exptl_absorpt_empirical_full_min 0.898
####################################################################### 
# 
# 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_BUT-101(Cu)
_database_code_depnum_ccdc_archive 'CCDC 1888831'
loop_
_audit_author_name
_audit_author_address
'Xiang-Jing Kong'
;Beijing University of Technology
China
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2017-11-14
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.06(C252 H162 Cu18 N18 O72)'
_chemical_formula_sum            'C14 H9 Cu N O4'
_chemical_formula_weight         318.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Cu'
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      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m'
_space_group_name_Hall           '-R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   18.6355(7)
_cell_length_b                   18.6355(7)
_cell_length_c                   34.4019(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10346.5(9)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    3995
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      74.2420
_cell_measurement_theta_min      3.7200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.413
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    0.921
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2898
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            7625
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.756
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  20.00   1.00    3.00    --  -41.94  57.00 -90.00   90
  2  ω      6.00  36.00   1.00    3.00    --   41.94 -38.00 -60.00   30
  3  ω    145.00 175.00   1.00   10.00    --  107.13 125.00 -60.00   30
  4  ω     84.00 177.00   1.00   10.00    --  107.13  45.00 120.00   93
  5  ω     95.00 157.00   1.00   10.00    --  107.13 125.00 120.00   62
  6  ω     36.00 104.00   1.00   10.00    --  107.13 -61.00  60.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0066536000
_diffrn_orient_matrix_UB_12      0.0013675000
_diffrn_orient_matrix_UB_13      -0.0446060000
_diffrn_orient_matrix_UB_21      -0.0942962000
_diffrn_orient_matrix_UB_22      -0.0355188000
_diffrn_orient_matrix_UB_23      -0.0032414000
_diffrn_orient_matrix_UB_31      0.0134318000
_diffrn_orient_matrix_UB_32      0.0886175000
_diffrn_orient_matrix_UB_33      -0.0006567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2064
_reflns_number_total             2276
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2276
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0381
_refine_ls_restrained_S_all      1.086
_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)+(0.0750P)²+16.2290P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1244
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Others
 Fixed Sof: H00A(0.5) H00B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 N004(H00A,H00B)
3.b Aromatic/amide H refined with riding coordinates:
 C007(H007), C00A(H00C), C00C(H00D), C00D(H00E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cu01 Cu 1.14330(2) 0.85670(2) 0.30179(2) 0.02064(18) Uani 1 2 d S T P . .
O002 O 1.07712(10) 0.77466(11) 0.38306(4) 0.0379(4) Uani 1 1 d . . . . .
O003 O 1.03815(10) 0.81507(11) 0.32974(4) 0.0390(4) Uani 1 1 d . . . . .
N004 N 0.76862(8) 0.53723(16) 0.58431(6) 0.0348(6) Uani 1 2 d S T P . .
H00A H 0.7909 0.5047 0.5857 0.042 Uiso 0.5 1 calc R . . . .
H00B H 0.7139 0.5047 0.5857 0.042 Uiso 0.5 1 calc R . . . .
C005 C 0.83015(11) 0.6603(2) 0.47556(8) 0.0335(7) Uani 1 2 d S T P . .
C006 C 1.02690(14) 0.78571(14) 0.36374(6) 0.0308(5) Uani 1 1 d . . . . .
C007 C 0.89028(11) 0.7806(2) 0.36387(8) 0.0344(7) Uani 1 2 d S T P . .
H007 H 0.9026 0.8052 0.3394 0.041 Uiso 1 2 calc RS T P . .
C008 C 0.94554(14) 0.76209(15) 0.38220(6) 0.0347(5) Uani 1 1 d . . . . .
C009 C 0.78875(9) 0.57750(19) 0.54751(8) 0.0325(7) Uani 1 2 d S T P . .
C00A C 0.92613(15) 0.72405(16) 0.41853(6) 0.0379(5) Uani 1 1 d . . . . .
H00C H 0.9639 0.7126 0.4307 0.045 Uiso 1 1 calc R . . . .
C00B C 0.85130(11) 0.7026(2) 0.43733(9) 0.0356(7) Uani 1 2 d S T P . .
C00C C 0.7363(2) 0.5979(3) 0.52972(8) 0.0688(10) Uani 1 1 d . . . . .
H00D H 0.6859 0.5842 0.5413 0.083 Uiso 1 1 calc R . . . .
C00D C 0.7579(2) 0.6393(3) 0.49419(9) 0.0725(11) Uani 1 1 d . . . . .
H00E H 0.7213 0.6531 0.4827 0.087 Uiso 1 1 calc R . . . .


_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
Cu01 Cu01 2.6433(7) 31_765 ?
Cu01 O002 1.9665(15) 31_765 ?
Cu01 O002 1.9665(15) 16_545 ?
Cu01 O003 1.9612(15) 22_775 ?
Cu01 O003 1.9611(15) . ?
Cu01 N004 2.199(2) 15_664 ?
O002 Cu01 1.9665(15) 31_765 ?
O002 C006 1.246(3) . ?
O003 C006 1.264(3) . ?
N004 Cu01 2.199(2) 8_655 ?
N004 H00A 0.8900 . ?
N004 H00B 0.8900 . ?
N004 C009 1.423(4) . ?
C005 C00B 1.482(4) . ?
C005 C00D 1.360(3) . ?
C005 C00D 1.360(3) 23_655 ?
C006 C008 1.493(3) . ?
C007 H007 0.9300 . ?
C007 C008 1.390(3) . ?
C007 C008 1.390(3) 23_655 ?
C008 C00A 1.392(3) . ?
C009 C00C 1.359(3) . ?
C009 C00C 1.359(3) 23_655 ?
C00A H00C 0.9300 . ?
C00A C00B 1.402(3) . ?
C00B C00A 1.402(3) 23_655 ?
C00C H00D 0.9300 . ?
C00C C00D 1.393(4) . ?
C00D H00E 0.9300 . ?

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
O002 Cu01 Cu01 84.12(4) 31_765 31_765 ?
O002 Cu01 Cu01 84.12(4) 16_545 31_765 ?
O002 Cu01 O002 89.22(11) 16_545 31_765 ?
O002 Cu01 N004 97.69(6) 16_545 15_664 ?
O002 Cu01 N004 97.69(6) 31_765 15_664 ?
O003 Cu01 Cu01 84.01(4) . 31_765 ?
O003 Cu01 Cu01 84.01(4) 22_775 31_765 ?
O003 Cu01 O002 89.95(8) . 16_545 ?
O003 Cu01 O002 168.13(6) . 31_765 ?
O003 Cu01 O002 89.95(8) 22_775 31_765 ?
O003 Cu01 O002 168.13(6) 22_775 16_545 ?
O003 Cu01 O003 88.43(11) . 22_775 ?
O003 Cu01 N004 94.16(6) . 15_664 ?
O003 Cu01 N004 94.16(6) 22_775 15_664 ?
N004 Cu01 Cu01 177.44(7) 15_664 31_765 ?
C006 O002 Cu01 122.79(13) . 31_765 ?
C006 O003 Cu01 122.81(14) . . ?
Cu01 N004 H00A 108.4 8_655 . ?
Cu01 N004 H00B 108.4 8_655 . ?
H00A N004 H00B 107.5 . . ?
C009 N004 Cu01 115.46(19) . 8_655 ?
C009 N004 H00A 108.4 . . ?
C009 N004 H00B 108.4 . . ?
C00D C005 C00B 122.21(15) 23_655 . ?
C00D C005 C00B 122.21(15) . . ?
C00D C005 C00D 115.6(3) . 23_655 ?
O002 C006 O003 126.1(2) . . ?
O002 C006 C008 117.42(17) . . ?
O003 C006 C008 116.46(18) . . ?
C008 C007 H007 120.1 23_655 . ?
C008 C007 H007 120.1 . . ?
C008 C007 C008 119.8(3) . 23_655 ?
C007 C008 C006 120.21(19) . . ?
C007 C008 C00A 119.8(2) . . ?
C00A C008 C006 119.93(19) . . ?
C00C C009 N004 120.76(15) . . ?
C00C C009 N004 120.76(15) 23_655 . ?
C00C C009 C00C 118.5(3) . 23_655 ?
C008 C00A H00C 119.1 . . ?
C008 C00A C00B 121.8(2) . . ?
C00B C00A H00C 119.1 . . ?
C00A C00B C005 121.55(14) 23_655 . ?
C00A C00B C005 121.56(14) . . ?
C00A C00B C00A 116.9(3) 23_655 . ?
C009 C00C H00D 120.0 . . ?
C009 C00C C00D 120.1(3) . . ?
C00D C00C H00D 120.0 . . ?
C005 C00D C00C 122.9(3) . . ?
C005 C00D H00E 118.6 . . ?
C00C C00D H00E 118.6 . . ?

_smtbx_masks_special_details     ?
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 -0.146 -0.289 -0.021 5998.0 1835.2 ?


_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.799
####################################################################### 
# 
# 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_BUT-104
_database_code_depnum_ccdc_archive 'CCDC 1888833'
loop_
_audit_author_name
_audit_author_address
'Xiang-Jing Kong'
;Beijing University of Technology
China
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-07-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C160 H88 N8 O64 Zr12)'
_chemical_formula_sum            'C40 H22 N2 O16 Zr3'
_chemical_formula_weight         1060.25
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Zr'
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'
Zr Zr -0.1862 2.2449 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   35.346(2)
_cell_length_b                   18.477(4)
_cell_length_c                   18.0998(12)
_cell_angle_alpha                90
_cell_angle_beta                 92.956(7)
_cell_angle_gamma                90
_cell_volume                     11805(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1568
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      68.4800
_cell_measurement_theta_min      4.4380
_shelx_estimated_absorpt_T_max   0.871
_shelx_estimated_absorpt_T_min   0.749
_exptl_absorpt_coefficient_mu    2.362
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    0.597
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1807
_diffrn_reflns_av_unetI/netI     0.2013
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22058
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        62.991
_diffrn_reflns_theta_max         62.991
_diffrn_reflns_theta_min         3.408
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -45.00    0.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5605   38.0000  -90.0000 45

#__ type_ start__ end____ width___ exp.time_
  2 omega -114.00  -23.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5605  -57.0000  150.0000 91

#__ type_ start__ end____ width___ exp.time_
  3 omega  -84.00   -2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5605  125.0000  -90.0000 82

#__ type_ start__ end____ width___ exp.time_
  4 omega   92.00  151.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759   45.0000  150.0000 59

#__ type_ start__ end____ width___ exp.time_
  5 omega   33.00  117.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759 -125.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
  6 omega   53.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759   15.0000  -90.0000 123

#__ type_ start__ end____ width___ exp.time_
  7 omega   23.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -94.0000  150.0000 86

#__ type_ start__ end____ width___ exp.time_
  8 omega  132.00  160.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  125.0000  -30.0000 28

#__ type_ start__ end____ width___ exp.time_
  9 omega   39.00  125.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -61.0000  -30.0000 86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0093288000
_diffrn_orient_matrix_UB_12      -0.0740417000
_diffrn_orient_matrix_UB_13      -0.0337216000
_diffrn_orient_matrix_UB_21      -0.0058862000
_diffrn_orient_matrix_UB_22      -0.0366931000
_diffrn_orient_matrix_UB_23      0.0749797000
_diffrn_orient_matrix_UB_31      -0.0422270000
_diffrn_orient_matrix_UB_32      -0.0112508000
_diffrn_orient_matrix_UB_33      -0.0223300000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3861
_reflns_number_total             9846
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.506
_refine_diff_density_min         -1.576
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         9846
_refine_ls_number_restraints     265
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.1305
_refine_ls_restrained_S_all      0.936
_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)+(0.1802P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3114
_refine_ls_wR_factor_ref         0.3681
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Zr1-O2_$1
 2.02 with sigma of 0.002
 Zr2-O2
 2.02 with sigma of 0.002
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(Zr1) \\sim Ueq, Uanis(Zr2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0
Uanis(O5) = Uanis(O6)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C19(H19), C18(H18), C4(H4), C13(H13), C11(H11), C7(H7), C16(H16),
 C9(H9), C6(H6), C15(H15)
;
_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
Zr1 Zr 0.56897(3) 1.000000 0.50067(6) 0.0742(6) Uani 1 2 d DS TU P . .
Zr2 Zr 1.00232(2) 0.59591(7) 0.59822(4) 0.0783(5) Uani 1 1 d D U . . .
O4 O 0.90064(16) 0.5737(5) 0.5735(4) 0.070(2) Uani 1 1 d . U . . .
O6 O 0.60270(18) 0.9285(5) 0.5750(4) 0.0863(17) Uani 1 1 d . U . . .
O2 O 0.96712(19) 0.5855(3) 0.5065(3) 0.124(3) Uani 1 1 d D U . . .
O7 O 0.56071(19) 0.8708(5) 0.6357(5) 0.103(3) Uani 1 1 d . U . . .
O8 O 1.0043(2) 0.5913(5) 0.7197(4) 0.091(3) Uani 1 1 d . U . . .
O9 O 1.0026(2) 0.7154(5) 0.5981(4) 0.096(2) Uani 1 1 d . U . . .
O3 O 0.9714(3) 0.500000 0.5983(7) 0.106(3) Uani 1 2 d S TU P . .
C20 C 0.5940(3) 0.8840(8) 0.6222(6) 0.081(3) Uani 1 1 d . U . . .
C3 C 0.8876(3) 0.6831(8) 0.7328(6) 0.104(4) Uani 1 1 d . U . . .
H3 H 0.912350 0.692021 0.750644 0.124 Uiso 1 1 calc R . . . .
C2 C 0.8809(3) 0.6433(9) 0.6650(6) 0.100(4) Uani 1 1 d . U . . .
C1 C 0.9105(3) 0.6144(8) 0.6213(6) 0.084(4) Uani 1 1 d . U . . .
C5 C 0.8215(3) 0.6996(10) 0.7483(6) 0.110(5) Uani 1 1 d . U . . .
C17 C 0.6268(3) 0.8561(9) 0.6673(6) 0.103(4) Uani 1 1 d . U . . .
C19 C 0.6542(3) 0.7839(9) 0.7703(6) 0.106(5) Uani 1 1 d . U . . .
H19 H 0.650628 0.754536 0.811111 0.127 Uiso 1 1 calc R . . . .
N1 N 0.7642(3) 0.7388(10) 0.9835(5) 0.153(6) Uani 1 1 d . U . . .
C18 C 0.6232(3) 0.8118(9) 0.7325(6) 0.108(5) Uani 1 1 d . U . . .
H18 H 0.599201 0.802253 0.748959 0.130 Uiso 1 1 calc R . . . .
C4 C 0.8592(3) 0.7067(9) 0.7694(6) 0.112(5) Uani 1 1 d . U . . .
H4 H 0.865074 0.730420 0.813850 0.135 Uiso 1 1 calc R . . . .
C13 C 0.7561(3) 0.7506(10) 0.7537(6) 0.131(6) Uani 1 1 d . U . . .
H13 H 0.755497 0.755077 0.702519 0.157 Uiso 1 1 calc R . . . .
C11 C 0.7259(3) 0.7678(10) 0.8672(6) 0.132(6) Uani 1 1 d . U . . .
H11 H 0.704642 0.779203 0.893190 0.158 Uiso 1 1 calc R . . . .
C7 C 0.8435(3) 0.6327(9) 0.6414(7) 0.115(5) Uani 1 1 d . U . . .
H7 H 0.837657 0.606940 0.598184 0.138 Uiso 1 1 calc R . . . .
C8 C 0.7881(3) 0.7215(11) 0.7883(6) 0.131(5) Uani 1 1 d . U . . .
C16 C 0.6634(3) 0.8668(10) 0.6450(7) 0.125(5) Uani 1 1 d . U . . .
H16 H 0.666782 0.892330 0.601530 0.150 Uiso 1 1 calc R . . . .
C12 C 0.7257(3) 0.7732(10) 0.7889(6) 0.126(5) Uani 1 1 d . U . . .
C9 C 0.7906(3) 0.7224(10) 0.8661(6) 0.138(6) Uani 1 1 d . U . . .
H9 H 0.812728 0.708189 0.892031 0.166 Uiso 1 1 calc R . . . .
C10 C 0.7595(3) 0.7447(10) 0.9031(5) 0.134(6) Uani 1 1 d . U . . .
C6 C 0.8142(3) 0.6608(10) 0.6828(7) 0.132(6) Uani 1 1 d . U . . .
H6 H 0.789245 0.653363 0.666001 0.158 Uiso 1 1 calc R . . . .
C14 C 0.6907(3) 0.7978(10) 0.7502(6) 0.115(5) Uani 1 1 d . U . . .
C15 C 0.6956(3) 0.8404(10) 0.6858(7) 0.139(6) Uani 1 1 d . U . . .
H15 H 0.719766 0.850778 0.670802 0.167 Uiso 1 1 calc R . . . .
O5 O 0.94622(18) 0.6308(5) 0.6369(4) 0.0863(17) Uani 1 1 d . U . . .
O1 O 1.0348(3) 0.500000 0.6004(7) 0.105(3) Uani 1 2 d S TU P . .


_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
Zr1 Zr2 3.4968(14) 7_666 ?
Zr1 Zr2 3.4968(14) 4_656 ?
Zr1 Zr2 3.4982(14) 3_455 ?
Zr1 Zr2 3.4982(14) 8_465 ?
Zr1 O4 2.228(8) 7_666 ?
Zr1 O4 2.228(8) 4_656 ?
Zr1 O6 2.194(8) 6_575 ?
Zr1 O6 2.194(8) . ?
Zr1 O2 2.030(2) 7_666 ?
Zr1 O2 2.030(2) 4_656 ?
Zr1 O3 2.231(11) 7_666 ?
Zr1 O1 2.222(10) 3_455 ?
Zr2 Zr2 3.544(3) 6_565 ?
Zr2 Zr2 3.5508(16) 2_756 ?
Zr2 O2 2.238(7) 2_756 ?
Zr2 O2 2.032(2) . ?
Zr2 O7 2.226(8) 8_565 ?
Zr2 O8 2.198(7) . ?
Zr2 O9 2.208(10) . ?
Zr2 O3 2.082(6) . ?
Zr2 O5 2.232(7) . ?
Zr2 O1 2.112(7) . ?
O4 C1 1.184(14) . ?
O6 C20 1.235(14) . ?
O7 C20 1.240(13) . ?
C20 C17 1.475(15) . ?
C3 C2 1.440(16) . ?
C3 C4 1.306(15) . ?
C2 C1 1.447(15) . ?
C2 C7 1.383(15) . ?
C1 O5 1.314(13) . ?
C5 C4 1.374(15) . ?
C5 C8 1.473(15) . ?
C5 C6 1.398(18) . ?
C17 C18 1.447(17) . ?
C17 C16 1.388(16) . ?
C19 C18 1.362(15) . ?
C19 C14 1.383(15) . ?
N1 N1 1.27(2) 7_667 ?
N1 C10 1.459(12) . ?
C13 C8 1.372(15) . ?
C13 C12 1.346(15) . ?
C11 C12 1.420(14) . ?
C11 C10 1.391(15) . ?
C7 C6 1.407(16) . ?
C8 C9 1.407(14) . ?
C16 C15 1.411(16) . ?
C12 C14 1.462(15) . ?
C9 C10 1.380(14) . ?
C14 C15 1.425(18) . ?

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
Zr2 Zr1 Zr2 60.88(5) 8_465 3_455 ?
Zr2 Zr1 Zr2 91.65(4) 4_656 8_465 ?
Zr2 Zr1 Zr2 91.65(4) 7_666 3_455 ?
Zr2 Zr1 Zr2 61.01(3) 7_666 8_465 ?
Zr2 Zr1 Zr2 61.01(3) 4_656 3_455 ?
Zr2 Zr1 Zr2 60.90(5) 7_666 4_656 ?
O4 Zr1 Zr2 74.85(17) 4_656 4_656 ?
O4 Zr1 Zr2 74.85(17) 7_666 7_666 ?
O4 Zr1 Zr2 166.50(18) 4_656 8_465 ?
O4 Zr1 Zr2 166.50(18) 7_666 3_455 ?
O4 Zr1 Zr2 111.00(17) 4_656 7_666 ?
O4 Zr1 Zr2 111.00(17) 7_666 4_656 ?
O4 Zr1 Zr2 110.7(2) 7_666 8_465 ?
O4 Zr1 Zr2 110.7(2) 4_656 3_455 ?
O4 Zr1 O4 75.4(4) 7_666 4_656 ?
O4 Zr1 O3 79.9(3) 4_656 7_666 ?
O4 Zr1 O3 79.9(3) 7_666 7_666 ?
O6 Zr1 Zr2 166.8(2) . 4_656 ?
O6 Zr1 Zr2 110.8(2) . 3_455 ?
O6 Zr1 Zr2 75.18(19) . 8_465 ?
O6 Zr1 Zr2 111.3(2) . 7_666 ?
O6 Zr1 Zr2 110.8(2) 6_575 8_465 ?
O6 Zr1 Zr2 75.18(19) 6_575 3_455 ?
O6 Zr1 Zr2 111.3(2) 6_575 4_656 ?
O6 Zr1 Zr2 166.8(2) 6_575 7_666 ?
O6 Zr1 O4 74.8(3) 6_575 4_656 ?
O6 Zr1 O4 118.3(3) . 4_656 ?
O6 Zr1 O4 118.3(3) 6_575 7_666 ?
O6 Zr1 O4 74.8(3) . 7_666 ?
O6 Zr1 O6 74.1(5) . 6_575 ?
O6 Zr1 O3 142.9(2) . 7_666 ?
O6 Zr1 O3 142.9(2) 6_575 7_666 ?
O6 Zr1 O1 78.6(3) . 3_455 ?
O6 Zr1 O1 78.6(3) 6_575 3_455 ?
O2 Zr1 Zr2 30.60(8) 4_656 4_656 ?
O2 Zr1 Zr2 37.0(2) 4_656 3_455 ?
O2 Zr1 Zr2 85.86(18) 7_666 4_656 ?
O2 Zr1 Zr2 89.4(3) 4_656 8_465 ?
O2 Zr1 Zr2 85.86(18) 4_656 7_666 ?
O2 Zr1 Zr2 89.4(3) 7_666 3_455 ?
O2 Zr1 Zr2 37.0(2) 7_666 8_465 ?
O2 Zr1 Zr2 30.60(8) 7_666 7_666 ?
O2 Zr1 O4 139.3(2) 7_666 4_656 ?
O2 Zr1 O4 139.3(2) 4_656 7_666 ?
O2 Zr1 O4 78.9(3) 4_656 4_656 ?
O2 Zr1 O4 78.9(3) 7_666 7_666 ?
O2 Zr1 O6 83.7(3) 7_666 . ?
O2 Zr1 O6 145.9(2) 7_666 6_575 ?
O2 Zr1 O6 83.7(3) 4_656 6_575 ?
O2 Zr1 O6 145.9(2) 4_656 . ?
O2 Zr1 O2 102.2(5) 7_666 4_656 ?
O2 Zr1 O3 64.9(2) 4_656 7_666 ?
O2 Zr1 O3 64.9(2) 7_666 7_666 ?
O2 Zr1 O1 71.7(3) 4_656 3_455 ?
O2 Zr1 O1 71.7(3) 7_666 3_455 ?
O3 Zr1 Zr2 34.43(16) 7_666 4_656 ?
O3 Zr1 Zr2 89.2(3) 7_666 3_455 ?
O3 Zr1 Zr2 89.2(3) 7_666 8_465 ?
O3 Zr1 Zr2 34.43(17) 7_666 7_666 ?
O1 Zr1 Zr2 35.12(17) 3_455 3_455 ?
O1 Zr1 Zr2 90.5(3) 3_455 7_666 ?
O1 Zr1 Zr2 90.5(3) 3_455 4_656 ?
O1 Zr1 Zr2 35.12(17) 3_455 8_465 ?
O1 Zr1 O4 142.1(2) 3_455 7_666 ?
O1 Zr1 O4 142.1(2) 3_455 4_656 ?
O1 Zr1 O3 107.5(5) 3_455 7_666 ?
Zr1 Zr2 Zr1 88.35(4) 7_666 3_545 ?
Zr1 Zr2 Zr2 59.56(2) 3_545 6_565 ?
Zr1 Zr2 Zr2 59.51(3) 7_666 2_756 ?
Zr1 Zr2 Zr2 59.48(3) 3_545 2_756 ?
Zr1 Zr2 Zr2 59.55(2) 7_666 6_565 ?
Zr2 Zr2 Zr2 90.0 6_565 2_756 ?
O2 Zr2 Zr1 83.65(18) 2_756 7_666 ?
O2 Zr2 Zr1 33.05(8) 2_756 3_545 ?
O2 Zr2 Zr1 30.57(8) . 7_666 ?
O2 Zr2 Zr1 86.5(3) . 3_545 ?
O2 Zr2 Zr2 31.92(9) 2_756 2_756 ?
O2 Zr2 Zr2 84.56(17) . 6_565 ?
O2 Zr2 Zr2 85.06(17) 2_756 6_565 ?
O2 Zr2 Zr2 35.6(2) . 2_756 ?
O2 Zr2 O2 66.5(3) . 2_756 ?
O2 Zr2 O7 142.6(3) . 8_565 ?
O2 Zr2 O8 143.1(3) . . ?
O2 Zr2 O9 95.6(3) . . ?
O2 Zr2 O3 67.7(3) . . ?
O2 Zr2 O5 76.5(3) . . ?
O2 Zr2 O1 104.2(4) . . ?
O7 Zr2 Zr1 158.2(3) 8_565 7_666 ?
O7 Zr2 Zr1 69.9(2) 8_565 3_545 ?
O7 Zr2 Zr2 106.0(2) 8_565 6_565 ?
O7 Zr2 Zr2 107.4(2) 8_565 2_756 ?
O7 Zr2 O2 78.6(3) 8_565 2_756 ?
O7 Zr2 O5 130.5(3) 8_565 . ?
O8 Zr2 Zr1 119.9(2) . 3_545 ?
O8 Zr2 Zr1 118.5(2) . 7_666 ?
O8 Zr2 Zr2 177.6(2) . 2_756 ?
O8 Zr2 Zr2 87.8(2) . 6_565 ?
O8 Zr2 O2 148.5(2) . 2_756 ?
O8 Zr2 O7 74.0(3) . 8_565 ?
O8 Zr2 O9 92.3(3) . . ?
O8 Zr2 O5 71.3(3) . . ?
O9 Zr2 Zr1 120.2(2) . 3_545 ?
O9 Zr2 Zr1 120.6(2) . 7_666 ?
O9 Zr2 Zr2 89.95(19) . 2_756 ?
O9 Zr2 Zr2 179.7(2) . 6_565 ?
O9 Zr2 O2 94.7(3) . 2_756 ?
O9 Zr2 O7 73.7(3) . 8_565 ?
O9 Zr2 O5 73.5(3) . . ?
O3 Zr2 Zr1 86.3(4) . 3_545 ?
O3 Zr2 Zr1 37.3(3) . 7_666 ?
O3 Zr2 Zr2 31.7(3) . 6_565 ?
O3 Zr2 Zr2 90.2(4) . 2_756 ?
O3 Zr2 O2 101.7(4) . 2_756 ?
O3 Zr2 O7 135.5(4) . 8_565 ?
O3 Zr2 O8 87.5(4) . . ?
O3 Zr2 O9 148.6(3) . . ?
O3 Zr2 O5 76.7(4) . . ?
O3 Zr2 O1 64.6(4) . . ?
O5 Zr2 Zr1 159.6(2) . 3_545 ?
O5 Zr2 Zr1 71.2(2) . 7_666 ?
O5 Zr2 Zr2 106.8(2) . 6_565 ?
O5 Zr2 Zr2 108.56(18) . 2_756 ?
O5 Zr2 O2 140.0(2) . 2_756 ?
O1 Zr2 Zr1 87.8(3) . 7_666 ?
O1 Zr2 Zr1 37.3(3) . 3_545 ?
O1 Zr2 Zr2 32.9(3) . 6_565 ?
O1 Zr2 Zr2 90.9(3) . 2_756 ?
O1 Zr2 O2 70.0(3) . 2_756 ?
O1 Zr2 O7 74.4(4) . 8_565 ?
O1 Zr2 O8 87.7(4) . . ?
O1 Zr2 O9 146.8(3) . . ?
O1 Zr2 O5 136.7(4) . . ?
C1 O4 Zr1 134.0(7) . 7_666 ?
C20 O6 Zr1 132.7(7) . . ?
Zr1 O2 Zr2 118.83(15) 7_666 . ?
Zr1 O2 Zr2 110.0(3) 7_666 2_756 ?
Zr2 O2 Zr2 112.5(3) . 2_756 ?
C20 O7 Zr2 139.5(10) . 8_465 ?
Zr2 O3 Zr1 108.3(4) 6_565 7_666 ?
Zr2 O3 Zr1 108.3(4) . 7_666 ?
Zr2 O3 Zr2 116.7(6) 6_565 . ?
O6 C20 O7 122.7(11) . . ?
O6 C20 C17 113.6(11) . . ?
O7 C20 C17 123.2(12) . . ?
C4 C3 C2 120.4(11) . . ?
C3 C2 C1 124.2(11) . . ?
C7 C2 C3 116.7(11) . . ?
C7 C2 C1 119.1(12) . . ?
O4 C1 C2 116.0(11) . . ?
O4 C1 O5 123.2(10) . . ?
O5 C1 C2 120.7(12) . . ?
C4 C5 C8 129.0(12) . . ?
C4 C5 C6 114.7(11) . . ?
C6 C5 C8 116.1(12) . . ?
C18 C17 C20 123.3(11) . . ?
C16 C17 C20 120.3(12) . . ?
C16 C17 C18 116.1(11) . . ?
C18 C19 C14 122.3(13) . . ?
N1 N1 C10 113.1(13) 7_667 . ?
C19 C18 C17 121.4(11) . . ?
C3 C4 C5 126.0(12) . . ?
C12 C13 C8 124.5(11) . . ?
C10 C11 C12 116.6(10) . . ?
C2 C7 C6 120.0(12) . . ?
C13 C8 C5 123.1(10) . . ?
C13 C8 C9 117.3(11) . . ?
C9 C8 C5 119.0(10) . . ?
C17 C16 C15 122.4(13) . . ?
C13 C12 C11 119.1(11) . . ?
C13 C12 C14 123.2(10) . . ?
C11 C12 C14 117.5(10) . . ?
C10 C9 C8 118.7(10) . . ?
C11 C10 N1 122.7(10) . . ?
C9 C10 N1 114.1(11) . . ?
C9 C10 C11 123.2(10) . . ?
C5 C6 C7 122.2(12) . . ?
C19 C14 C12 126.4(13) . . ?
C19 C14 C15 118.3(11) . . ?
C15 C14 C12 115.3(11) . . ?
C16 C15 C14 119.3(12) . . ?
C1 O5 Zr2 136.4(8) . . ?
Zr2 O1 Zr1 107.6(4) . 3_545 ?
Zr2 O1 Zr1 107.6(4) 6_565 3_545 ?
Zr2 O1 Zr2 114.1(5) 6_565 . ?

_smtbx_masks_special_details     ?
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 -0.980 -0.991 -0.753 8903.2 1858.8 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_BUT-108(Hf)
_database_code_depnum_ccdc_archive 'CCDC 1888835'
loop_
_audit_author_name
_audit_author_address
'Xiang-Jing Kong'
;Beijing University of Technology
China
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-07-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.06(C384 H208 B48 Hf48 O320)'
_chemical_formula_sum            'C24 H13 B3 Hf3 O20'
_chemical_formula_weight         1189.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O B Hf'
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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -6.1794 4.9776 '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      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'

_cell_length_a                   40.4997(4)
_cell_length_b                   40.4997(4)
_cell_length_c                   16.9534(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     27807.4(9)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    15582
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.6800
_cell_measurement_theta_min      4.1700
_shelx_estimated_absorpt_T_max   0.729
_shelx_estimated_absorpt_T_min   0.486
_exptl_absorpt_coefficient_mu    8.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             8768
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42600
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         3.571
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  49.00   0.50    2.00    --  -38.80  68.00 -86.00  130
  2  ω    -62.00 -25.00   0.50    2.00    --  -38.80  68.00 -86.00   74
  3  ω   -102.00 -70.00   0.50    2.00    --  -38.80 -52.00 -49.00   64
  4  ω   -161.00-136.00   0.50   12.00    -- -104.00 -52.00 -49.00   50
  5  ω    -75.00 -15.00   0.50   12.00    -- -104.00  68.00 -86.00  120
  6  ω   -160.00-135.00   0.50   12.00    -- -104.00 -68.00 140.00   50
  7  ω     13.00  38.00   0.50    2.00    --    5.00  68.00 -86.00   50
  8  ω      2.00  51.00   0.50    2.00    --    5.00  38.00-180.00   98
  9  ω   -125.00 -15.00   0.50   12.00    -- -104.00  72.00  30.00  220
 10  ω   -109.00 -84.00   0.50   12.00    -- -104.00 -38.00-180.00   50
 11  ω   -119.00 -86.00   0.50   12.00    -- -104.00  19.00  60.00   66
 12  ω    -79.00 -34.00   0.50   12.00    -- -104.00  19.00  60.00   90
 13  ω   -142.00-116.00   0.50   12.00    -- -104.00 -38.00-180.00   52
 14  ω   -180.00-154.00   0.50   12.00    -- -104.00 -38.00-180.00   52
 15  ω   -125.00 -28.00   0.50   12.00    -- -104.00  72.00 -30.00  194
 16  ω    -76.00 -51.00   0.50   12.00    -- -104.00  57.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0263720000
_diffrn_orient_matrix_UB_12      -0.0163452000
_diffrn_orient_matrix_UB_13      0.0524548000
_diffrn_orient_matrix_UB_21      -0.0133771000
_diffrn_orient_matrix_UB_22      0.0343323000
_diffrn_orient_matrix_UB_23      0.0225405000
_diffrn_orient_matrix_UB_31      -0.0239121000
_diffrn_orient_matrix_UB_32      -0.0011437000
_diffrn_orient_matrix_UB_33      -0.0707023000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5212
_reflns_number_total             6304
_reflns_odcompleteness_completeness 97.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.832
_refine_diff_density_min         -1.555
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         6304
_refine_ls_number_restraints     241
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0593
_refine_ls_restrained_S_all      1.088
_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)+(0.1071P)²+124.6450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1842
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C13-O4 = C13-O5
 1.4 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C15) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
5. Others
 Fixed Sof: C13(0.5) O11(0.5) C14(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C8(H8), C3(H3), C7(H7), C4(H4), C15(H15)
;
_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
Hf2 Hf 0.54295(2) 0.52075(2) 0.09065(2) 0.0780(2) Uani 1 1 d . U . . .
Hf1 Hf 0.500000 0.44631(2) 0.06768(3) 0.0850(2) Uani 1 2 d S TU P . .
O10 O 0.500000 0.64344(17) 0.6858(4) 0.0606(15) Uani 1 2 d S TU P . .
O9 O 0.65697(11) 0.71732(19) 0.7765(3) 0.0889(18) Uani 1 1 d . U . . .
O8 O 0.67864(12) 0.68944(18) 0.6734(3) 0.0816(16) Uani 1 1 d . U . . .
O1 O 0.5282(2) 0.54557(14) 0.1995(3) 0.103(2) Uani 1 1 d . U . . .
O5 O 0.56563(18) 0.4922(2) 0.1889(4) 0.1042(19) Uani 1 1 d D U . . .
O2 O 0.500000 0.49335(19) 0.1246(7) 0.103(3) Uani 1 2 d S TU P . .
O3 O 0.5426(2) 0.47354(14) 0.0366(4) 0.117(2) Uani 1 1 d . U . . .
O4 O 0.5313(3) 0.43346(16) 0.1682(4) 0.127(3) Uani 1 1 d D U . . .
O6 O 0.5959(2) 0.51770(18) 0.0688(6) 0.133(3) Uani 1 1 d . U . . .
O12 O 0.52869(18) 0.6153(3) 0.5826(4) 0.133(3) Uani 1 1 d . U . . .
O7 O 0.500000 0.5446(3) 0.0537(7) 0.125(3) Uani 1 2 d S TU P . .
C12 C 0.56577(18) 0.6730(2) 0.7362(5) 0.078(2) Uani 1 1 d . U . . .
H12 H 0.547669 0.678300 0.767444 0.093 Uiso 1 1 calc R . . . .
C11 C 0.59590(19) 0.6869(2) 0.7514(5) 0.080(2) Uani 1 1 d . U . . .
H11 H 0.598190 0.700655 0.795062 0.096 Uiso 1 1 calc R . . . .
C9 C 0.62273(18) 0.6812(2) 0.7043(5) 0.078(2) Uani 1 1 d . U . . .
C10 C 0.65537(18) 0.6973(3) 0.7198(5) 0.080(2) Uani 1 1 d . U . . .
C1 C 0.500000 0.5518(3) 0.2301(7) 0.093(3) Uani 1 2 d S TU P . .
C2 C 0.500000 0.5667(3) 0.3109(8) 0.102(4) Uani 1 2 d S TU P . .
C6 C 0.5622(2) 0.6510(3) 0.6743(5) 0.099(3) Uani 1 1 d . U . . .
C8 C 0.6195(2) 0.6601(4) 0.6410(7) 0.129(5) Uani 1 1 d . U . . .
H8 H 0.637464 0.655770 0.608547 0.155 Uiso 1 1 calc R . . . .
C5 C 0.500000 0.5945(4) 0.4587(9) 0.116(5) Uani 1 2 d S TU P . .
C3 C 0.5299(4) 0.5727(4) 0.3490(6) 0.138(5) Uani 1 1 d . U . . .
H3 H 0.549867 0.567610 0.324613 0.165 Uiso 1 1 calc R . . . .
C7 C 0.5897(2) 0.6455(4) 0.6260(7) 0.141(5) Uani 1 1 d . U . . .
H7 H 0.587593 0.631571 0.582665 0.170 Uiso 1 1 calc R . . . .
C4 C 0.5293(4) 0.5863(4) 0.4246(7) 0.134(5) Uani 1 1 d . U . . .
H4 H 0.548953 0.589851 0.451784 0.161 Uiso 1 1 calc R . . . .
B1 B 0.500000 0.6111(6) 0.5421(9) 0.113(5) Uani 1 2 d S TU P . .
B2 B 0.5290(3) 0.6319(4) 0.6550(7) 0.104(3) Uani 1 1 d . U . . .
C15 C 0.6067(6) 0.500000 0.000000 0.148(6) Uani 1 2 d S TU P . .
H15 H 0.629704 0.500003 -0.000001 0.178 Uiso 1 2 calc RS T P . .
C13 C 0.5582(5) 0.4562(4) 0.1987(12) 0.114(5) Uani 0.5 1 d D U . . .
O11 O 0.5342(3) 0.5956(3) 0.7235(8) 0.091(3) Uani 0.5 1 d . U . . .
C14 C 0.5183(4) 0.4062(4) 0.2125(8) 0.074(3) Uani 0.5 1 d . 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
Hf2 Hf2 3.4794(11) 22_655 ?
Hf2 Hf2 3.5030(7) 6_565 ?
Hf2 Hf1 3.5021(5) . ?
Hf2 Hf1 3.4657(6) 17_665 ?
Hf2 O8 2.183(5) 8_665 ?
Hf2 O1 2.185(6) . ?
Hf2 O5 2.226(7) . ?
Hf2 O2 2.142(6) . ?
Hf2 O3 2.120(5) . ?
Hf2 O3 2.170(7) 6_565 ?
Hf2 O6 2.179(9) . ?
Hf2 O7 2.087(5) . ?
Hf1 O9 2.186(6) 24 ?
Hf1 O9 2.186(6) 3_644 ?
Hf1 O2 2.136(7) . ?
Hf1 O3 2.112(8) 22_655 ?
Hf1 O3 2.113(8) . ?
Hf1 O4 2.186(7) 22_655 ?
Hf1 O4 2.186(7) . ?
Hf1 O7 2.091(10) 17_665 ?
O10 B2 1.367(12) 22_655 ?
O10 B2 1.367(12) . ?
O9 C10 1.259(11) . ?
O8 C10 1.269(9) . ?
O1 C1 1.279(9) . ?
O5 C13 1.501(14) . ?
O4 C13 1.516(16) . ?
O4 C14 1.436(19) . ?
O6 C15 1.437(10) . ?
O12 B1 1.361(11) . ?
O12 B2 1.400(12) . ?
C12 C11 1.369(11) . ?
C12 C6 1.383(12) . ?
C11 C9 1.368(11) . ?
C9 C10 1.497(11) . ?
C9 C8 1.379(13) . ?
C1 C2 1.498(16) . ?
C2 C3 1.394(15) . ?
C2 C3 1.394(15) 22_655 ?
C6 C7 1.399(12) . ?
C6 B2 1.584(14) . ?
C8 C7 1.367(14) . ?
C5 C4 1.361(15) . ?
C5 C4 1.361(15) 22_655 ?
C5 B1 1.566(19) . ?
C3 C4 1.397(13) . ?
B2 O11 1.89(2) . ?
O11 C14 1.264(19) 6_566 ?
C14 C14 1.48(3) 22_655 ?

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
Hf2 Hf2 Hf2 90.0 22_655 6_565 ?
Hf2 Hf2 Hf1 60.217(9) 22_655 . ?
Hf1 Hf2 Hf2 59.871(9) 17_665 22_655 ?
Hf1 Hf2 Hf2 60.338(12) 17_665 6_565 ?
Hf1 Hf2 Hf2 59.306(12) . 6_565 ?
Hf1 Hf2 Hf1 89.765(16) 17_665 . ?
O8 Hf2 Hf2 109.06(18) 8_665 22_655 ?
O8 Hf2 Hf2 110.79(14) 8_665 6_565 ?
O8 Hf2 Hf1 73.63(16) 8_665 17_665 ?
O8 Hf2 Hf1 163.39(16) 8_665 . ?
O8 Hf2 O1 75.5(2) 8_665 . ?
O8 Hf2 O5 115.7(3) 8_665 . ?
O1 Hf2 Hf2 164.1(2) . 6_565 ?
O1 Hf2 Hf2 74.1(2) . 22_655 ?
O1 Hf2 Hf1 109.9(2) . 17_665 ?
O1 Hf2 Hf1 110.74(18) . . ?
O1 Hf2 O5 73.7(3) . . ?
O5 Hf2 Hf2 114.38(19) . 22_655 ?
O5 Hf2 Hf2 114.1(2) . 6_565 ?
O5 Hf2 Hf1 80.9(2) . . ?
O5 Hf2 Hf1 170.7(2) . 17_665 ?
O2 Hf2 Hf2 89.3(3) . 6_565 ?
O2 Hf2 Hf2 35.7(2) . 22_655 ?
O2 Hf2 Hf1 35.0(2) . . ?
O2 Hf2 Hf1 90.0(3) . 17_665 ?
O2 Hf2 O8 141.3(3) . 8_665 ?
O2 Hf2 O1 77.8(3) . . ?
O2 Hf2 O5 82.2(3) . . ?
O2 Hf2 O3 108.5(4) . 6_565 ?
O2 Hf2 O6 144.6(3) . . ?
O3 Hf2 Hf2 89.6(3) . 22_655 ?
O3 Hf2 Hf2 89.6(3) 6_565 22_655 ?
O3 Hf2 Hf2 34.80(15) 6_565 6_565 ?
O3 Hf2 Hf2 35.75(19) . 6_565 ?
O3 Hf2 Hf1 90.5(2) . 17_665 ?
O3 Hf2 Hf1 35.4(2) 6_565 17_665 ?
O3 Hf2 Hf1 34.1(2) . . ?
O3 Hf2 Hf1 88.7(2) 6_565 . ?
O3 Hf2 O8 78.1(2) 6_565 8_665 ?
O3 Hf2 O8 143.3(2) . 8_665 ?
O3 Hf2 O1 142.1(2) 6_565 . ?
O3 Hf2 O1 141.1(2) . . ?
O3 Hf2 O5 81.9(3) . . ?
O3 Hf2 O5 143.4(3) 6_565 . ?
O3 Hf2 O2 69.1(3) . . ?
O3 Hf2 O3 70.5(3) . 6_565 ?
O3 Hf2 O6 83.3(4) . . ?
O3 Hf2 O6 81.0(4) 6_565 . ?
O6 Hf2 Hf2 79.8(3) . 6_565 ?
O6 Hf2 Hf2 169.7(3) . 22_655 ?
O6 Hf2 Hf1 114.9(2) . . ?
O6 Hf2 Hf1 112.6(2) . 17_665 ?
O6 Hf2 O8 73.3(3) . 8_665 ?
O6 Hf2 O1 116.0(4) . . ?
O6 Hf2 O5 72.1(3) . . ?
O7 Hf2 Hf2 33.5(2) . 22_655 ?
O7 Hf2 Hf2 87.7(4) . 6_565 ?
O7 Hf2 Hf1 87.2(3) . . ?
O7 Hf2 Hf1 34.0(3) . 17_665 ?
O7 Hf2 O8 78.7(3) . 8_665 ?
O7 Hf2 O1 79.1(4) . . ?
O7 Hf2 O5 144.0(3) . . ?
O7 Hf2 O2 69.1(3) . . ?
O7 Hf2 O3 69.3(4) . 6_565 ?
O7 Hf2 O3 106.4(5) . . ?
O7 Hf2 O6 142.7(3) . . ?
Hf2 Hf1 Hf2 59.570(18) . 22_655 ?
Hf2 Hf1 Hf2 60.359(13) 6_565 . ?
Hf2 Hf1 Hf2 90.238(16) 17_665 . ?
Hf2 Hf1 Hf2 60.359(13) 17_665 22_655 ?
Hf2 Hf1 Hf2 60.263(19) 17_665 6_565 ?
Hf2 Hf1 Hf2 90.239(16) 6_565 22_655 ?
O9 Hf1 Hf2 111.24(17) 3_644 . ?
O9 Hf1 Hf2 74.29(14) 3_644 6_565 ?
O9 Hf1 Hf2 109.70(16) 3_644 17_665 ?
O9 Hf1 Hf2 164.52(14) 24 . ?
O9 Hf1 Hf2 109.70(16) 24 6_565 ?
O9 Hf1 Hf2 164.52(14) 3_644 22_655 ?
O9 Hf1 Hf2 74.29(14) 24 17_665 ?
O9 Hf1 Hf2 111.24(17) 24 22_655 ?
O9 Hf1 O9 74.5(4) 24 3_644 ?
O9 Hf1 O4 115.2(3) 3_644 22_655 ?
O9 Hf1 O4 74.0(3) 24 22_655 ?
O9 Hf1 O4 115.2(3) 24 . ?
O9 Hf1 O4 74.0(2) 3_644 . ?
O2 Hf1 Hf2 35.12(16) . 22_655 ?
O2 Hf1 Hf2 90.4(3) . 17_665 ?
O2 Hf1 Hf2 90.4(3) . 6_565 ?
O2 Hf1 Hf2 35.11(16) . . ?
O2 Hf1 O9 142.62(18) . 24 ?
O2 Hf1 O9 142.62(18) . 3_644 ?
O2 Hf1 O4 82.0(3) . 22_655 ?
O2 Hf1 O4 82.0(3) . . ?
O3 Hf1 Hf2 90.9(2) . 17_665 ?
O3 Hf1 Hf2 34.23(17) . . ?
O3 Hf1 Hf2 36.5(2) 22_655 17_665 ?
O3 Hf1 Hf2 34.24(17) 22_655 22_655 ?
O3 Hf1 Hf2 90.9(2) 22_655 6_565 ?
O3 Hf1 Hf2 89.1(2) 22_655 . ?
O3 Hf1 Hf2 36.6(2) . 6_565 ?
O3 Hf1 Hf2 89.1(2) . 22_655 ?
O3 Hf1 O9 78.9(2) . 3_644 ?
O3 Hf1 O9 142.6(2) 22_655 3_644 ?
O3 Hf1 O9 78.9(2) 22_655 24 ?
O3 Hf1 O9 142.6(2) . 24 ?
O3 Hf1 O2 69.3(2) 22_655 . ?
O3 Hf1 O2 69.3(2) . . ?
O3 Hf1 O3 109.3(5) 22_655 . ?
O3 Hf1 O4 81.1(4) 22_655 22_655 ?
O3 Hf1 O4 142.3(3) . 22_655 ?
O3 Hf1 O4 81.1(4) . . ?
O3 Hf1 O4 142.3(3) 22_655 . ?
O4 Hf1 Hf2 170.5(2) 22_655 6_565 ?
O4 Hf1 Hf2 113.98(17) 22_655 . ?
O4 Hf1 Hf2 80.2(2) 22_655 22_655 ?
O4 Hf1 Hf2 80.2(2) . . ?
O4 Hf1 Hf2 113.8(3) . 6_565 ?
O4 Hf1 Hf2 113.8(3) 22_655 17_665 ?
O4 Hf1 Hf2 170.5(2) . 17_665 ?
O4 Hf1 Hf2 113.98(17) . 22_655 ?
O4 Hf1 O4 70.8(5) . 22_655 ?
O7 Hf1 Hf2 87.6(3) 17_665 22_655 ?
O7 Hf1 Hf2 33.91(16) 17_665 17_665 ?
O7 Hf1 Hf2 87.6(3) 17_665 . ?
O7 Hf1 Hf2 33.91(16) 17_665 6_565 ?
O7 Hf1 O9 79.2(3) 17_665 3_644 ?
O7 Hf1 O9 79.2(3) 17_665 24 ?
O7 Hf1 O2 106.8(5) 17_665 . ?
O7 Hf1 O3 70.3(3) 17_665 22_655 ?
O7 Hf1 O3 70.3(3) 17_665 . ?
O7 Hf1 O4 144.0(3) 17_665 . ?
O7 Hf1 O4 144.0(3) 17_665 22_655 ?
B2 O10 B2 118.5(10) 22_655 . ?
C10 O9 Hf1 132.2(5) . 4_565 ?
C10 O8 Hf2 133.1(6) . 8_665 ?
C1 O1 Hf2 132.6(7) . . ?
C13 O5 Hf2 120.3(8) . . ?
Hf2 O2 Hf2 108.6(4) . 22_655 ?
Hf1 O2 Hf2 109.9(3) . . ?
Hf1 O2 Hf2 109.9(3) . 22_655 ?
Hf2 O3 Hf2 109.5(3) . 6_565 ?
Hf1 O3 Hf2 111.7(4) . . ?
Hf1 O3 Hf2 108.0(4) . 6_565 ?
C13 O4 Hf1 122.5(7) . . ?
C14 O4 Hf1 112.3(9) . . ?
C14 O4 C13 123.4(10) . . ?
C15 O6 Hf2 117.9(12) . . ?
B1 O12 B2 120.7(10) . . ?
Hf2 O7 Hf2 113.0(5) . 22_655 ?
Hf2 O7 Hf1 112.1(4) . 17_665 ?
Hf2 O7 Hf1 112.1(4) 22_655 17_665 ?
C11 C12 C6 120.1(7) . . ?
C9 C11 C12 121.8(8) . . ?
C11 C9 C10 121.7(8) . . ?
C11 C9 C8 118.9(8) . . ?
C8 C9 C10 119.4(7) . . ?
O9 C10 O8 126.7(8) . . ?
O9 C10 C9 117.4(7) . . ?
O8 C10 C9 115.9(8) . . ?
O1 C1 O1 126.4(11) . 22_655 ?
O1 C1 C2 116.8(6) . . ?
O1 C1 C2 116.8(6) 22_655 . ?
C3 C2 C1 119.5(6) 22_655 . ?
C3 C2 C1 119.5(6) . . ?
C3 C2 C3 120.8(13) . 22_655 ?
C12 C6 C7 117.6(8) . . ?
C12 C6 B2 124.0(8) . . ?
C7 C6 B2 118.4(8) . . ?
C7 C8 C9 119.8(9) . . ?
C4 C5 C4 121.4(15) . 22_655 ?
C4 C5 B1 119.2(7) . . ?
C4 C5 B1 119.2(7) 22_655 . ?
C2 C3 C4 118.5(13) . . ?
C8 C7 C6 121.6(9) . . ?
C5 C4 C3 120.1(14) . . ?
O12 B1 O12 117.3(12) 22_655 . ?
O12 B1 C5 120.7(7) . . ?
O12 B1 C5 120.7(7) 22_655 . ?
O10 B2 O12 119.3(10) . . ?
O10 B2 C6 119.0(9) . . ?
O10 B2 O11 97.3(8) . . ?
O12 B2 C6 115.0(8) . . ?
O12 B2 O11 99.5(10) . . ?
C6 B2 O11 99.2(10) . . ?
O6 C15 O6 144(2) 6_565 . ?
O5 C13 O4 134.2(13) . . ?
C14 O11 B2 121.1(12) 6_566 . ?
O4 C14 C14 111.5(8) . 22_655 ?
O11 C14 O4 107.9(15) 6_566 . ?
O11 C14 C14 120.6(10) 6_566 22_655 ?

_smtbx_masks_special_details     ?
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 -0.779 -0.848 -0.222 17729.5 2617.1 ?

_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 2.785
_oxdiff_exptl_absorpt_empirical_full_min 0.446
####################################################################### 
# 
# 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_BUT-109(Zr)
_database_code_depnum_ccdc_archive 'CCDC 1888834'
loop_
_audit_author_name
_audit_author_address
'Xiang-Jing Kong'
;Beijing University of Technology
China
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-09-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C28.5 H6 N3 O19 Zr3)'
_chemical_formula_sum            'C57 H12 N6 O38 Zr6'
_chemical_formula_weight         1936.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Zr'
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'
Zr Zr -0.1862 2.2449 '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      cubic
_space_group_IT_number           229
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'

_cell_length_a                   19.225(2)
_cell_length_b                   19.225(2)
_cell_length_c                   19.225(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7105(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    359
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      56.5890
_cell_measurement_theta_min      4.5520
_shelx_estimated_absorpt_T_max   0.798
_shelx_estimated_absorpt_T_min   0.798
_exptl_absorpt_coefficient_mu    3.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark grey'
_exptl_crystal_density_diffrn    0.905
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2912
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        63.488
_diffrn_reflns_theta_max         63.488
_diffrn_reflns_theta_min         4.600
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00 -27.00   1.00   15.00    --  -41.69 125.00-180.00   57
  2  ω    153.00 178.00   1.00   25.00    --  107.13  78.00 137.00   25
  3  ω     34.00 107.00   1.00   25.00    --  107.13 -94.00-120.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0724163000
_diffrn_orient_matrix_UB_12      -0.0065587000
_diffrn_orient_matrix_UB_13      -0.0350022000
_diffrn_orient_matrix_UB_21      0.0350348000
_diffrn_orient_matrix_UB_22      0.0064072000
_diffrn_orient_matrix_UB_23      0.0711961000
_diffrn_orient_matrix_UB_31      -0.0029213000
_diffrn_orient_matrix_UB_32      -0.0796022000
_diffrn_orient_matrix_UB_33      0.0086312000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                377
_reflns_number_total             612
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     63.60
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         612
_refine_ls_number_restraints     104
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_gt           0.1155
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.3000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3515
_refine_ls_wR_factor_ref         0.4127
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-C3
 1.35 with sigma of 0.01
 C3-C4
 1.45 with sigma of 0.02
 C4-C5
 1.34 with sigma of 0.01
 C5-N1
 1.48 with sigma of 0.02
 N1-C6
 1.4 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: C2(0.1875) C3(0.125) H3(0.125) C4(0.125) H4(0.125) N1(0.125)
 C5(0.0625) O3(0.125) C6(0.125) C8(0.0625) C7(0.125) C9(0.125)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_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
Zr1 Zr 0.500000 0.500000 0.37097(7) 0.0757(4) Uani 1 8 d S TU P . .
O1 O 0.4352(3) 0.5648(3) 0.4352(3) 0.088(2) Uani 1 6 d S TU P . .
O2 O 0.3993(4) 0.500000 0.3144(4) 0.1035(18) Uani 1 2 d S TU P . .
C1 C 0.3330(5) 0.500000 0.3330(5) 0.108(3) Uani 1 4 d S TU P . .
C2 C 0.2827(3) 0.500000 0.2827(3) 0.115(4) Uani 0.75 4 d DS TU P . .
C3 C 0.3011(6) 0.500000 0.2150(3) 0.101(5) Uani 0.25 2 d DS TU P . .
H3 H 0.348067 0.500000 0.203259 0.121 Uiso 0.25 2 calc RS T P . .
C4 C 0.2498(3) 0.500000 0.1604(5) 0.106(5) Uani 0.25 2 d DS TU P . .
H4 H 0.261023 0.500000 0.113362 0.127 Uiso 0.25 2 calc RS T P . .
N1 N 0.1299(3) 0.500000 0.1299(3) 0.099(2) Uani 0.5 4 d DS TU P . .
C5 C 0.1843(3) 0.500000 0.1843(3) 0.087(4) Uani 0.25 4 d DS TU P . .
O3 O 0.1297(6) 0.3836(13) 0.1297(6) 0.113(3) Uani 0.25 2 d S TU P . .
C6 C 0.1069(6) 0.4352(6) 0.1069(6) 0.095(2) Uani 0.25 2 d DS TU P . .
C8 C 0.0272(10) 0.500000 0.0272(10) 0.078(4) Uani 0.25 4 d S TU P . .
C7 C 0.0519(8) 0.4402(16) 0.0519(8) 0.080(2) Uani 0.25 2 d S TU P . .
C9 C 0.000000 0.3701(13) 0.0411(11) 0.064(4) Uani 0.25 2 d S TU P . .


_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
Zr1 Zr1 3.5079(19) 57_666 ?
Zr1 Zr1 3.5079(19) 9 ?
Zr1 Zr1 3.5079(19) 5 ?
Zr1 Zr1 3.5079(19) 53_666 ?
Zr1 O1 2.151(4) . ?
Zr1 O1 2.151(4) 2_665 ?
Zr1 O1 2.151(4) 52_655 ?
Zr1 O1 2.151(4) 51_565 ?
Zr1 O2 2.220(7) . ?
Zr1 O2 2.220(7) 61_665 ?
Zr1 O2 2.220(7) 62 ?
Zr1 O2 2.220(7) 2_665 ?
O2 C1 1.324(10) . ?
C1 C2 1.369(17) . ?
C2 C3 1.349(7) . ?
C2 C3 1.349(7) 22_565 ?
C3 C4 1.439(11) . ?
C4 C5 1.341(6) . ?
N1 C5 1.478(11) . ?
N1 C6 1.395(12) . ?
N1 C6 1.395(12) 51_565 ?
O3 C6 1.17(3) . ?
C6 C7 1.50(3) . ?
C8 C8 1.05(4) 50 ?
C8 C8 1.05(4) 2_565 ?
C8 C8 1.48(5) 49_565 ?
C8 C7 1.33(3) . ?
C8 C7 1.96(3) 52 ?
C8 C7 1.33(3) 51_565 ?
C8 C7 1.96(3) 4_565 ?
C8 C7 1.96(3) 2_565 ?
C8 C7 1.96(3) 50 ?
C7 C7 1.99(3) 50 ?
C7 C7 1.99(3) 52 ?
C7 C9 1.69(3) . ?
C7 C9 1.69(3) 21 ?
C9 C9 1.12(3) 21 ?
C9 C9 1.12(3) 70 ?
C9 C9 1.58(4) 50 ?

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
Zr1 Zr1 Zr1 60.0 57_666 53_666 ?
Zr1 Zr1 Zr1 60.0 57_666 5 ?
Zr1 Zr1 Zr1 60.0 9 5 ?
Zr1 Zr1 Zr1 90.0 57_666 9 ?
Zr1 Zr1 Zr1 60.0 53_666 9 ?
Zr1 Zr1 Zr1 90.0 53_666 5 ?
O1 Zr1 Zr1 35.39(14) 2_665 53_666 ?
O1 Zr1 Zr1 90.2(2) . 9 ?
O1 Zr1 Zr1 35.39(14) . 57_666 ?
O1 Zr1 Zr1 35.39(14) . 5 ?
O1 Zr1 Zr1 35.38(14) 51_565 9 ?
O1 Zr1 Zr1 35.39(14) 52_655 53_666 ?
O1 Zr1 Zr1 90.2(2) . 53_666 ?
O1 Zr1 Zr1 35.38(14) 52_655 57_666 ?
O1 Zr1 Zr1 35.38(14) 2_665 9 ?
O1 Zr1 Zr1 90.2(2) 2_665 5 ?
O1 Zr1 Zr1 90.2(2) 51_565 57_666 ?
O1 Zr1 Zr1 90.2(2) 52_655 9 ?
O1 Zr1 Zr1 90.2(2) 52_655 5 ?
O1 Zr1 Zr1 90.2(2) 2_665 57_666 ?
O1 Zr1 Zr1 35.39(14) 51_565 5 ?
O1 Zr1 Zr1 90.2(2) 51_565 53_666 ?
O1 Zr1 O1 70.8(3) . 52_655 ?
O1 Zr1 O1 110.0(6) . 2_665 ?
O1 Zr1 O1 70.8(3) 52_655 2_665 ?
O1 Zr1 O1 70.8(3) . 51_565 ?
O1 Zr1 O1 110.0(6) 52_655 51_565 ?
O1 Zr1 O1 70.8(3) 2_665 51_565 ?
O1 Zr1 O2 77.1(3) 52_655 2_665 ?
O1 Zr1 O2 77.1(3) 51_565 . ?
O1 Zr1 O2 141.81(7) . 2_665 ?
O1 Zr1 O2 141.81(7) 52_655 62 ?
O1 Zr1 O2 77.1(3) 52_655 61_665 ?
O1 Zr1 O2 141.81(7) 51_565 61_665 ?
O1 Zr1 O2 141.81(7) . 62 ?
O1 Zr1 O2 77.1(3) . 61_665 ?
O1 Zr1 O2 141.81(7) 52_655 . ?
O1 Zr1 O2 141.81(7) 2_665 . ?
O1 Zr1 O2 77.1(3) 2_665 62 ?
O1 Zr1 O2 77.1(3) 2_665 2_665 ?
O1 Zr1 O2 77.1(3) 51_565 62 ?
O1 Zr1 O2 141.81(7) 2_665 61_665 ?
O1 Zr1 O2 141.81(7) 51_565 2_665 ?
O1 Zr1 O2 77.1(3) . . ?
O2 Zr1 Zr1 164.33(19) . 53_666 ?
O2 Zr1 Zr1 74.33(19) . 5 ?
O2 Zr1 Zr1 74.33(19) 62 9 ?
O2 Zr1 Zr1 110.27(12) 2_665 9 ?
O2 Zr1 Zr1 110.27(12) 61_665 5 ?
O2 Zr1 Zr1 74.33(19) 61_665 57_666 ?
O2 Zr1 Zr1 164.33(19) 2_665 5 ?
O2 Zr1 Zr1 164.33(19) 62 57_666 ?
O2 Zr1 Zr1 110.27(12) 61_665 53_666 ?
O2 Zr1 Zr1 110.27(12) 62 53_666 ?
O2 Zr1 Zr1 164.33(19) 61_665 9 ?
O2 Zr1 Zr1 74.33(19) 2_665 53_666 ?
O2 Zr1 Zr1 110.27(12) . 9 ?
O2 Zr1 Zr1 110.27(12) 62 5 ?
O2 Zr1 Zr1 110.27(12) . 57_666 ?
O2 Zr1 Zr1 110.27(12) 2_665 57_666 ?
O2 Zr1 O2 76.12(16) . 62 ?
O2 Zr1 O2 121.3(4) 62 61_665 ?
O2 Zr1 O2 76.12(16) . 61_665 ?
O2 Zr1 O2 76.12(16) 61_665 2_665 ?
O2 Zr1 O2 121.3(4) . 2_665 ?
O2 Zr1 O2 76.12(16) 62 2_665 ?
Zr1 O1 Zr1 109.2(3) 57_666 . ?
Zr1 O1 Zr1 109.2(3) 57_666 5 ?
Zr1 O1 Zr1 109.2(3) 5 . ?
C1 O2 Zr1 135.0(7) . . ?
O2 C1 O2 121.3(12) 22_565 . ?
O2 C1 C2 119.3(6) . . ?
O2 C1 C2 119.3(6) 22_565 . ?
C3 C2 C1 119.7(6) 22_565 . ?
C3 C2 C1 119.7(6) . . ?
C3 C2 C3 120.5(12) . 22_565 ?
C2 C3 C4 121.5(10) . . ?
C5 C4 C3 113.2(9) . . ?
C6 N1 C5 116.7(7) . . ?
C6 N1 C5 116.7(7) 51_565 . ?
C6 N1 C6 126.6(14) 51_565 . ?
C4 C5 C4 130.1(11) 22_565 . ?
C4 C5 N1 115.0(6) . . ?
C4 C5 N1 115.0(6) 22_565 . ?
N1 C6 C7 113.0(15) . . ?
O3 C6 N1 121.3(16) . . ?
O3 C6 C7 125.7(18) . . ?
C8 C8 C8 44.997(1) 50 49_565 ?
C8 C8 C8 89.994(8) 50 2_565 ?
C8 C8 C8 44.997(4) 2_565 49_565 ?
C8 C8 C7 110.8(9) 2_565 . ?
C8 C8 C7 110.8(9) 2_565 51_565 ?
C8 C8 C7 110.8(9) 50 51_565 ?
C8 C8 C7 103.9(7) 2_565 4_565 ?
C8 C8 C7 39.3(8) 2_565 2_565 ?
C8 C8 C7 110.8(9) 50 . ?
C8 C8 C7 67.9(8) 49_565 2_565 ?
C8 C8 C7 39.3(8) 50 4_565 ?
C8 C8 C7 67.9(8) 49_565 50 ?
C8 C8 C7 39.3(8) 2_565 52 ?
C8 C8 C7 103.9(7) 50 2_565 ?
C8 C8 C7 39.3(8) 50 50 ?
C8 C8 C7 67.9(8) 49_565 4_565 ?
C8 C8 C7 103.9(7) 2_565 50 ?
C8 C8 C7 103.9(7) 50 52 ?
C8 C8 C7 67.9(8) 49_565 52 ?
C7 C8 C8 120.2(14) . 49_565 ?
C7 C8 C8 120.2(14) 51_565 49_565 ?
C7 C8 C7 71.5(13) 51_565 2_565 ?
C7 C8 C7 91.7(15) 52 50 ?
C7 C8 C7 134.1(7) 51_565 50 ?
C7 C8 C7 135.7(15) 50 2_565 ?
C7 C8 C7 134.1(7) 51_565 52 ?
C7 C8 C7 135.7(15) 52 4_565 ?
C7 C8 C7 134.1(7) . 2_565 ?
C7 C8 C7 91.7(15) 4_565 2_565 ?
C7 C8 C7 71.5(13) . 52 ?
C7 C8 C7 120(3) 51_565 . ?
C7 C8 C7 71.7(16) 50 4_565 ?
C7 C8 C7 71.5(13) 51_565 4_565 ?
C7 C8 C7 71.7(16) 52 2_565 ?
C7 C8 C7 71.5(13) . 50 ?
C7 C8 C7 134.1(7) . 4_565 ?
C6 C7 C8 138.9(16) . 2_565 ?
C6 C7 C8 138.9(16) . 50 ?
C6 C7 C7 134.88(8) . 52 ?
C6 C7 C7 134.88(8) . 50 ?
C6 C7 C9 116.9(18) . . ?
C6 C7 C9 116.9(18) . 21 ?
C8 C7 C6 124(2) . . ?
C8 C7 C8 29.9(12) . 2_565 ?
C8 C7 C8 29.9(12) . 50 ?
C8 C7 C8 44.3(15) 2_565 50 ?
C8 C7 C7 69.2(9) . 50 ?
C8 C7 C7 76.1(7) 50 52 ?
C8 C7 C7 76.1(7) 2_565 50 ?
C8 C7 C7 69.2(9) . 52 ?
C8 C7 C7 39.3(8) 50 50 ?
C8 C7 C7 39.3(8) 2_565 52 ?
C8 C7 C9 115.9(17) . 21 ?
C8 C7 C9 115.9(17) . . ?
C7 C7 C7 89.999(1) 50 52 ?
C9 C7 C8 88.9(10) . 2_565 ?
C9 C7 C8 103.3(13) . 50 ?
C9 C7 C8 103.3(13) 21 2_565 ?
C9 C7 C8 88.9(10) 21 50 ?
C9 C7 C7 83.0(9) . 50 ?
C9 C7 C7 83.0(9) 21 52 ?
C9 C7 C7 53.8(9) . 52 ?
C9 C7 C7 53.8(9) 21 50 ?
C9 C7 C9 38.7(13) . 21 ?
C7 C9 C7 72.4(17) . 52 ?
C9 C9 C7 97.0(9) 50 52 ?
C9 C9 C7 120.3(10) 21 52 ?
C9 C9 C7 70.7(7) 21 . ?
C9 C9 C7 97.0(9) 50 . ?
C9 C9 C7 70.7(7) 70 52 ?
C9 C9 C7 120.3(10) 70 . ?
C9 C9 C9 45.000(2) 70 50 ?
C9 C9 C9 45.000(4) 21 50 ?
C9 C9 C9 90.000(7) 70 21 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.250 0.500 21.6 1.5 ?
2 0.000 0.500 0.250 21.6 1.5 ?
3 0.000 0.500 0.750 21.6 1.5 ?
4 0.000 0.750 0.500 21.6 1.6 ?
5 0.250 0.250 0.250 165.3 12.1 ?
6 0.250 0.250 0.750 165.3 12.1 ?
7 0.250 0.750 0.250 165.3 12.1 ?
8 0.250 0.750 0.750 165.3 12.1 ?
9 0.250 0.000 0.500 21.6 1.5 ?
10 0.250 0.500 0.000 21.6 1.8 ?
11 0.500 0.000 0.250 21.6 1.5 ?
12 0.500 0.000 0.750 21.6 1.5 ?
13 0.500 0.250 0.000 21.6 1.6 ?
14 0.500 0.750 0.000 21.6 1.5 ?
15 0.750 0.250 0.250 165.3 12.1 ?
16 0.750 0.250 0.750 165.3 12.1 ?
17 0.750 0.750 0.250 165.3 12.1 ?
18 0.750 0.750 0.750 165.3 12.1 ?
19 0.750 0.000 0.500 21.6 1.8 ?
20 0.750 0.500 0.000 21.6 1.5 ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.845
_oxdiff_exptl_absorpt_empirical_full_min 0.347
####################################################################### 
# 
# 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_BUT-102
_database_code_depnum_ccdc_archive 'CCDC 1888832'
loop_
_audit_author_name
_audit_author_address
'Xiang-Jing Kong'
;Beijing University of Technology
China
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-07-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H11 Cd N O5'
_chemical_formula_sum            'C14 H11 Cd N O5'
_chemical_formula_weight         385.64
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
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'
Cd Cd 0.1185 4.6533 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.6897(3)
_cell_length_b                   8.7992(3)
_cell_length_c                   12.7198(4)
_cell_angle_alpha                87.203(3)
_cell_angle_beta                 74.302(3)
_cell_angle_gamma                76.159(3)
_cell_volume                     804.39(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6264
_cell_measurement_temperature    292.5(4)
_cell_measurement_theta_max      73.8780
_cell_measurement_theta_min      5.1480
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.054
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8628
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.052
_diffrn_reflns_theta_max         67.052
_diffrn_reflns_theta_min         3.610
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.5(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1688
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  32.00   1.00    1.00    --  -41.94  38.00 120.00   98
  2  ω   -116.00 -17.00   1.00    1.00    --  -41.94 -38.00  60.00   99
  3  ω    -75.00  34.00   1.00    1.00    --  -41.94  77.00 -30.00  109
  4  ω    -70.00  31.00   1.00    1.00    --  -41.94  57.00-150.00  101
  5  ω     24.00  99.00   1.00    1.00    --   41.94-126.00-121.00   75
  6  ω     35.00 136.00   1.00    1.00    --  107.13 -61.00 -30.00  101
  7  ω     31.00 140.00   1.00    1.00    --  107.13 -77.00 150.00  109
  8  ω     34.00 121.00   1.00    1.00    --  107.13-125.00  30.00   87
  9  ω     34.00 121.00   1.00    1.00    --  107.13-125.00 150.00   87
 10  ω     81.00 178.00   1.00    1.00    --  107.13  45.00 -30.00   97
 11  ω     78.00 178.00   1.00    1.00    --  107.13  61.00  30.00  100
 12  ω     31.00 140.00   1.00    1.00    --  107.13 -77.00-150.00  109
 13  ω     94.00 178.00   1.00    1.00    --  107.13 125.00-150.00   84
 14  ω     75.00 178.00   1.00    1.00    --  107.13  77.00 -90.00  103
 15  ω     81.00 178.00   1.00    1.00    --  107.13  45.00-150.00   97
 16  ω   -114.00 -14.00   1.00    1.00    --  -41.94 -57.00 -30.00  100
 17  ω   -114.00 -14.00   1.00    1.00    --  -41.94 -57.00 -90.00  100
 18  ω   -118.00  -9.00   1.00    1.00    --  -41.94 -77.00 120.00  109
 19  ω   -118.00  -9.00   1.00    1.00    --  -41.94 -77.00-150.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1469301000
_diffrn_orient_matrix_UB_12      -0.0837034000
_diffrn_orient_matrix_UB_13      -0.0142093000
_diffrn_orient_matrix_UB_21      -0.0652665000
_diffrn_orient_matrix_UB_22      -0.0166689000
_diffrn_orient_matrix_UB_23      0.1247618000
_diffrn_orient_matrix_UB_31      -0.1413901000
_diffrn_orient_matrix_UB_32      0.1588671000
_diffrn_orient_matrix_UB_33      0.0080372000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2643
_reflns_number_total             2871
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2871
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0327
_refine_ls_restrained_S_all      1.046
_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)+(0.0515P)²+0.0521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0860
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1C,H1D)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C3(H3), C11(H11), C14(H14), C10(H10), C13(H13)
;
_atom_sites_solution_hydrogens   mixed
_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
Cd1 Cd 0.98428(3) 0.29030(3) 0.57298(2) 0.03178(12) Uani 1 1 d . . . . .
O3 O 0.7875(4) 0.5990(3) 0.5323(2) 0.0370(6) Uani 1 1 d . . . . .
O4 O 0.1951(4) 1.0359(3) 0.5707(2) 0.0413(6) Uani 1 1 d . . . . .
O2 O 0.8260(4) 0.4910(3) 0.6872(2) 0.0437(7) Uani 1 1 d . . . . .
O5 O 0.1653(4) 1.2099(3) 0.6964(2) 0.0455(7) Uani 1 1 d . . . . .
O1 O 0.9303(5) 0.2302(4) 0.4143(2) 0.0570(8) Uani 1 1 d . . . . .
H1A H 0.854258 0.319010 0.377659 0.086 Uiso 1 1 d GR . . . .
H1B H 0.845757 0.154956 0.419842 0.086 Uiso 1 1 d GR . . . .
N1 N 0.2601(5) 0.8371(5) 1.3454(2) 0.0455(9) Uani 1 1 d . . . . .
H1C H 0.227592 0.934741 1.371709 0.055 Uiso 1 1 calc R . . . .
H1D H 0.361583 0.787963 1.365058 0.055 Uiso 1 1 calc R . . . .
C1 C 0.7464(5) 0.5977(4) 0.6357(3) 0.0321(8) Uani 1 1 d . . . . .
C2 C 0.5960(5) 0.7271(4) 0.7000(3) 0.0296(8) Uani 1 1 d . . . . .
C4 C 0.3500(5) 0.9550(4) 0.7098(3) 0.0316(8) Uani 1 1 d . . . . .
C7 C 0.5583(5) 0.7300(4) 0.8130(3) 0.0343(8) Uani 1 1 d . . . . .
H7 H 0.628767 0.652244 0.846706 0.041 Uiso 1 1 calc R . . . .
C5 C 0.2300(5) 1.0752(4) 0.6561(3) 0.0359(8) Uani 1 1 d . . . . .
C8 C 0.4187(5) 0.8451(4) 0.8780(3) 0.0303(8) Uani 1 1 d . . . . .
C9 C 0.3785(5) 0.8454(4) 0.9989(3) 0.0317(8) Uani 1 1 d . . . . .
C6 C 0.3168(5) 0.9591(4) 0.8227(3) 0.0322(8) Uani 1 1 d . . . . .
H6 H 0.224444 1.039633 0.862791 0.039 Uiso 1 1 calc R . . . .
C3 C 0.4894(5) 0.8378(4) 0.6480(3) 0.0311(8) Uani 1 1 d . . . . .
H3 H 0.510746 0.833874 0.572540 0.037 Uiso 1 1 calc R . . . .
C12 C 0.3046(5) 0.8419(5) 1.2283(3) 0.0373(9) Uani 1 1 d . . . . .
C11 C 0.2076(6) 0.9604(5) 1.1766(3) 0.0469(11) Uani 1 1 d . . . . .
H11 H 0.115832 1.040118 1.217914 0.056 Uiso 1 1 calc R . . . .
C14 C 0.4737(6) 0.7271(5) 1.0528(3) 0.0492(11) Uani 1 1 d . . . . .
H14 H 0.564810 0.646547 1.011915 0.059 Uiso 1 1 calc R . . . .
C10 C 0.2451(6) 0.9618(5) 1.0646(3) 0.0441(10) Uani 1 1 d . . . . .
H10 H 0.178664 1.043821 1.031848 0.053 Uiso 1 1 calc R . . . .
C13 C 0.4371(6) 0.7254(6) 1.1651(3) 0.0531(12) Uani 1 1 d . . . . .
H13 H 0.503441 0.644010 1.198385 0.064 Uiso 1 1 calc R . . . .


_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
Cd1 O3 2.290(3) 2_766 ?
Cd1 O4 2.426(3) 1_645 ?
Cd1 O2 2.230(3) . ?
Cd1 O5 2.346(3) 1_645 ?
Cd1 O1 2.278(3) . ?
Cd1 N1 2.388(4) 2_667 ?
Cd1 C5 2.729(4) 1_645 ?
O3 C1 1.266(4) . ?
O4 C5 1.270(5) . ?
O2 C1 1.252(4) . ?
O5 C5 1.247(5) . ?
N1 C12 1.437(5) . ?
C1 C2 1.501(5) . ?
C2 C7 1.388(5) . ?
C2 C3 1.382(5) . ?
C4 C5 1.496(5) . ?
C4 C6 1.391(5) . ?
C4 C3 1.387(5) . ?
C7 C8 1.393(5) . ?
C8 C9 1.485(5) . ?
C8 C6 1.402(5) . ?
C9 C14 1.388(5) . ?
C9 C10 1.384(5) . ?
C12 C11 1.379(6) . ?
C12 C13 1.368(6) . ?
C11 C10 1.375(6) . ?
C14 C13 1.380(6) . ?

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
O3 Cd1 O4 93.26(10) 2_766 1_645 ?
O3 Cd1 O5 89.59(10) 2_766 1_645 ?
O3 Cd1 N1 170.44(10) 2_766 2_667 ?
O3 Cd1 C5 92.82(10) 2_766 1_645 ?
O4 Cd1 C5 27.73(10) 1_645 1_645 ?
O2 Cd1 O3 99.24(10) . 2_766 ?
O2 Cd1 O4 140.04(9) . 1_645 ?
O2 Cd1 O5 87.31(10) . 1_645 ?
O2 Cd1 O1 127.48(12) . . ?
O2 Cd1 N1 87.02(12) . 2_667 ?
O2 Cd1 C5 113.29(11) . 1_645 ?
O5 Cd1 O4 54.80(9) 1_645 1_645 ?
O5 Cd1 N1 97.96(11) 1_645 2_667 ?
O5 Cd1 C5 27.12(10) 1_645 1_645 ?
O1 Cd1 O3 87.01(10) . 2_766 ?
O1 Cd1 O4 90.75(11) . 1_645 ?
O1 Cd1 O5 145.14(11) . 1_645 ?
O1 Cd1 N1 83.45(11) . 2_667 ?
O1 Cd1 C5 118.44(12) . 1_645 ?
N1 Cd1 O4 86.39(12) 2_667 1_645 ?
N1 Cd1 C5 91.29(12) 2_667 1_645 ?
C1 O3 Cd1 123.6(2) . 2_766 ?
C5 O4 Cd1 89.5(2) . 1_465 ?
C1 O2 Cd1 108.9(2) . . ?
C5 O5 Cd1 93.8(2) . 1_465 ?
C12 N1 Cd1 114.3(3) . 2_667 ?
O3 C1 C2 119.5(3) . . ?
O2 C1 O3 122.4(3) . . ?
O2 C1 C2 118.1(3) . . ?
C7 C2 C1 119.4(3) . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 C7 120.1(3) . . ?
C6 C4 C5 119.3(3) . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 C6 120.2(3) . . ?
C2 C7 C8 122.5(3) . . ?
O4 C5 Cd1 62.75(19) . 1_465 ?
O4 C5 C4 118.6(3) . . ?
O5 C5 Cd1 59.09(19) . 1_465 ?
O5 C5 O4 121.7(3) . . ?
O5 C5 C4 119.8(3) . . ?
C4 C5 Cd1 174.8(3) . 1_465 ?
C7 C8 C9 121.8(3) . . ?
C7 C8 C6 116.2(3) . . ?
C6 C8 C9 122.0(3) . . ?
C14 C9 C8 121.3(3) . . ?
C10 C9 C8 122.7(3) . . ?
C10 C9 C14 116.0(3) . . ?
C4 C6 C8 121.8(3) . . ?
C2 C3 C4 119.2(3) . . ?
C11 C12 N1 120.6(4) . . ?
C13 C12 N1 121.2(4) . . ?
C13 C12 C11 118.2(4) . . ?
C10 C11 C12 120.7(4) . . ?
C13 C14 C9 122.0(4) . . ?
C11 C10 C9 122.3(4) . . ?
C12 C13 C14 120.9(4) . . ?

_smtbx_masks_special_details     ?
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 0.126 0.500 -0.126 192.5 58.7 ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.898
_oxdiff_exptl_absorpt_empirical_full_min 0.690
####################################################################### 
# 
# 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_BUT-108(Zr)
_database_code_depnum_ccdc_archive 'CCDC 1888836'
loop_
_audit_author_name
_audit_author_address
'Xiang-Jing Kong'
;Beijing University of Technology
China
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-07-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.06(C384 H208 B48 O320 Zr48)'
_chemical_formula_sum            'C24 H13 B3 O20 Zr3'
_chemical_formula_weight         927.43
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
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'
B B 0.0090 0.0039 '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'
Zr Zr -0.1862 2.2449 '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      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'

_cell_length_a                   40.5746(8)
_cell_length_b                   40.5746(8)
_cell_length_c                   17.0198(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     28019.7(13)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    3288
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      62.6430
_cell_measurement_theta_min      4.1440
_shelx_estimated_absorpt_T_max   0.858
_shelx_estimated_absorpt_T_min   0.797
_exptl_absorpt_coefficient_mu    3.956
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark colourless'
_exptl_crystal_density_diffrn    0.879
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             7232
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26464
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.581
_diffrn_reflns_theta_max         66.581
_diffrn_reflns_theta_min         3.560
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -108.00 -82.00   1.00   30.00    --  -42.06-138.00-103.00   26
  2  ω    -96.00  -2.00   1.00   30.00    --  -42.06 125.00 -90.00   94
  3  ω    102.00 128.00   1.00   60.00    --  107.13 125.00 150.00   26
  4  ω    113.00 178.00   1.00   60.00    --  107.13 125.00 -90.00   65
  5  ω     97.00 140.00   1.00   60.00    --  107.13 125.00-120.00   43
  6  ω     87.00 167.00   1.00   60.00    --  107.13  45.00 -30.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0139905000
_diffrn_orient_matrix_UB_12      -0.0115258000
_diffrn_orient_matrix_UB_13      0.0795330000
_diffrn_orient_matrix_UB_21      0.0035827000
_diffrn_orient_matrix_UB_22      0.0361623000
_diffrn_orient_matrix_UB_23      0.0262934000
_diffrn_orient_matrix_UB_31      -0.0351138000
_diffrn_orient_matrix_UB_32      -0.0009519000
_diffrn_orient_matrix_UB_33      0.0343121000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3714
_reflns_number_total             6381
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.153
_refine_diff_density_min         -2.398
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         6381
_refine_ls_number_restraints     226
_refine_ls_R_factor_all          0.1378
_refine_ls_R_factor_gt           0.1028
_refine_ls_restrained_S_all      1.166
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2872
_refine_ls_wR_factor_ref         0.3466
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Fixed Sof: O9(0.5) C8(0.5) C10(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C3(H3), C13(H13), C4(H4), C12(H12), C9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Zr2 Zr 0.72925(2) 0.29308(3) 0.84091(5) 0.0900(4) Uani 1 1 d . U . . .
Zr1 Zr 0.69608(2) 0.250000 0.68242(8) 0.0974(6) Uani 1 2 d S TU P . .
O2 O 0.67834(14) 0.3106(2) 0.8264(4) 0.094(2) Uani 1 1 d . U . . .
O1 O 0.65639(14) 0.2833(2) 0.7238(5) 0.100(2) Uani 1 1 d . U . . .
O7 O 0.7429(2) 0.250000 0.6229(8) 0.115(3) Uani 1 2 d S TU P . .
O3 O 0.72380(16) 0.2925(3) 0.7152(5) 0.128(3) Uani 1 1 d . U . . .
O12 O 0.5265(3) 0.45427(16) 1.3022(4) 0.117(3) Uani 1 1 d . U . . .
O11 O 0.5290(2) 0.3855(3) 0.9150(6) 0.155(4) Uani 1 1 d . U . . .
O5 O 0.7330(2) 0.3456(3) 0.8208(6) 0.133(3) Uani 1 1 d . U . . .
C2 C 0.6231(2) 0.3192(3) 0.7963(7) 0.092(3) Uani 1 1 d . U . . .
C7 C 0.5959(2) 0.3130(3) 0.7495(6) 0.085(3) Uani 1 1 d . U . . .
H7 H 0.597697 0.298228 0.707925 0.102 Uiso 1 1 calc R . . . .
C6 C 0.5659(2) 0.3285(3) 0.7639(6) 0.086(3) Uani 1 1 d . U . . .
H6 H 0.547911 0.323780 0.731963 0.103 Uiso 1 1 calc R . . . .
C1 C 0.6550(2) 0.3038(3) 0.7808(7) 0.093(3) Uani 1 1 d . U . . .
C15 C 0.500000 0.4483(4) 1.2651(9) 0.113(5) Uani 1 2 d S TU P . .
O4 O 0.7034(4) 0.250000 0.8051(8) 0.132(3) Uani 1 2 d S TU P . .
C5 C 0.5622(3) 0.3511(3) 0.8253(6) 0.096(3) Uani 1 1 d . U . . .
C14 C 0.500000 0.4337(4) 1.1901(10) 0.119(5) Uani 1 2 d S TU P . .
C3 C 0.6196(3) 0.3409(4) 0.8562(8) 0.129(5) Uani 1 1 d . U . . .
H3 H 0.637551 0.344777 0.889012 0.154 Uiso 1 1 calc R . . . .
C13 C 0.5284(5) 0.4260(4) 1.1521(8) 0.151(6) Uani 1 1 d . U . . .
H13 H 0.548302 0.429540 1.177795 0.181 Uiso 1 1 calc R . . . .
C11 C 0.500000 0.4042(5) 1.0450(10) 0.119(5) Uani 1 2 d S TU P . .
C4 C 0.5904(3) 0.3575(4) 0.8703(8) 0.141(5) Uani 1 1 d . U . . .
H4 H 0.589522 0.373087 0.910229 0.169 Uiso 1 1 calc R . . . .
C12 C 0.5292(4) 0.4130(4) 1.0774(9) 0.146(6) Uani 1 1 d . U . . .
H12 H 0.548878 0.410465 1.050214 0.175 Uiso 1 1 calc R . . . .
O6 O 0.7573(2) 0.3163(2) 0.9378(4) 0.107(2) Uani 1 1 d . U . . .
O8 O 0.6833(2) 0.2810(4) 0.5824(5) 0.150(4) Uani 1 1 d . U . . .
B2 B 0.500000 0.3905(7) 0.9500(13) 0.126(7) Uani 1 2 d S TU P . .
O10 O 0.500000 0.35720(18) 0.8148(4) 0.0592(17) Uani 1 2 d S TU P . .
O9 O 0.6553(3) 0.2852(3) 0.4724(8) 0.079(3) Uani 0.5 1 d . U . . .
C8 C 0.6577(5) 0.2690(6) 0.5364(10) 0.085(5) Uani 0.5 1 d . U . . .
B1 B 0.5292(4) 0.3693(5) 0.8414(9) 0.127(5) Uani 1 1 d . U . . .
C9 C 0.750000 0.3550(6) 0.750000 0.131(5) Uani 1 2 d S TU P . .
H9 H 0.750001 0.377922 0.750000 0.157 Uiso 1 2 calc RS T P . .
C10 C 0.7938(8) 0.3131(8) 0.9550(18) 0.132(9) Uani 0.5 1 d . 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
Zr2 Zr2 3.496(2) 29 ?
Zr2 Zr2 3.5231(17) 5_656 ?
Zr2 Zr1 3.4847(15) . ?
Zr2 Zr1 3.5203(12) 25_656 ?
Zr2 O2 2.198(6) . ?
Zr2 O7 2.171(7) 25_656 ?
Zr2 O3 2.151(9) . ?
Zr2 O3 2.131(6) 5_656 ?
Zr2 O12 2.188(8) 7_547 ?
Zr2 O5 2.163(11) . ?
Zr2 O4 2.127(8) . ?
Zr2 O6 2.215(8) . ?
Zr1 O1 2.217(7) 29 ?
Zr1 O1 2.217(7) . ?
Zr1 O7 2.152(9) . ?
Zr1 O3 2.132(10) 29 ?
Zr1 O3 2.132(10) . ?
Zr1 O4 2.109(13) . ?
Zr1 O8 2.179(10) 29 ?
Zr1 O8 2.179(10) . ?
O2 C1 1.253(12) . ?
O1 C1 1.280(13) . ?
O12 C15 1.270(12) . ?
O11 B2 1.335(13) . ?
O11 B1 1.414(14) . ?
O5 C9 1.441(10) . ?
C2 C7 1.382(14) . ?
C2 C1 1.462(14) . ?
C2 C3 1.355(16) . ?
C7 C6 1.394(13) . ?
C6 C5 1.398(13) . ?
C15 C14 1.41(2) . ?
C5 C4 1.401(15) . ?
C5 B1 1.555(16) . ?
C14 C13 1.359(17) 22_655 ?
C14 C13 1.359(17) . ?
C3 C4 1.384(16) . ?
C13 C12 1.376(17) . ?
C11 C12 1.353(17) . ?
C11 C12 1.353(17) 22_655 ?
C11 B2 1.71(3) . ?
O6 C10 1.51(3) . ?
O8 C8 1.39(2) . ?
O8 C10 1.72(4) 5_656 ?
O10 B1 1.359(15) 22_655 ?
O10 B1 1.359(15) . ?
O9 C8 1.28(2) . ?
O9 B1 1.84(2) 7_546 ?
C8 C8 1.54(5) 29 ?

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
Zr2 Zr2 Zr2 90.0 29 5_656 ?
Zr2 Zr2 Zr1 60.23(2) 29 25_656 ?
Zr1 Zr2 Zr2 60.31(3) . 5_656 ?
Zr1 Zr2 Zr2 59.31(3) 25_656 5_656 ?
Zr1 Zr2 Zr2 59.89(2) . 29 ?
Zr1 Zr2 Zr1 89.77(4) . 25_656 ?
O2 Zr2 Zr2 108.8(2) . 29 ?
O2 Zr2 Zr2 110.50(18) . 5_656 ?
O2 Zr2 Zr1 73.2(2) . . ?
O2 Zr2 Zr1 163.0(2) . 25_656 ?
O2 Zr2 O6 115.4(3) . . ?
O7 Zr2 Zr2 36.4(3) 25_656 29 ?
O7 Zr2 Zr2 90.0(3) 25_656 5_656 ?
O7 Zr2 Zr1 35.3(2) 25_656 25_656 ?
O7 Zr2 Zr1 91.0(3) 25_656 . ?
O7 Zr2 O2 141.4(3) 25_656 . ?
O7 Zr2 O12 76.0(4) 25_656 7_547 ?
O7 Zr2 O6 82.2(4) 25_656 . ?
O3 Zr2 Zr2 34.46(17) . 5_656 ?
O3 Zr2 Zr2 89.3(3) 5_656 29 ?
O3 Zr2 Zr2 34.8(2) 5_656 5_656 ?
O3 Zr2 Zr2 89.3(3) . 29 ?
O3 Zr2 Zr1 35.4(3) . . ?
O3 Zr2 Zr1 89.6(3) 5_656 . ?
O3 Zr2 Zr1 34.3(3) 5_656 25_656 ?
O3 Zr2 Zr1 88.3(2) . 25_656 ?
O3 Zr2 O2 78.2(3) . . ?
O3 Zr2 O2 142.5(3) 5_656 . ?
O3 Zr2 O7 69.6(4) 5_656 25_656 ?
O3 Zr2 O7 109.0(4) . 25_656 ?
O3 Zr2 O3 69.3(4) 5_656 . ?
O3 Zr2 O12 140.9(3) . 7_547 ?
O3 Zr2 O12 141.5(3) 5_656 7_547 ?
O3 Zr2 O5 83.0(4) 5_656 . ?
O3 Zr2 O5 82.0(4) . . ?
O3 Zr2 O6 143.0(3) . . ?
O3 Zr2 O6 83.0(4) 5_656 . ?
O12 Zr2 Zr2 72.1(3) 7_547 29 ?
O12 Zr2 Zr2 162.1(3) 7_547 5_656 ?
O12 Zr2 Zr1 109.8(2) 7_547 25_656 ?
O12 Zr2 Zr1 108.1(3) 7_547 . ?
O12 Zr2 O2 76.0(3) 7_547 . ?
O12 Zr2 O6 75.6(3) 7_547 . ?
O5 Zr2 Zr2 80.1(3) . 5_656 ?
O5 Zr2 Zr2 170.1(3) . 29 ?
O5 Zr2 Zr1 114.3(2) . 25_656 ?
O5 Zr2 Zr1 113.5(2) . . ?
O5 Zr2 O2 74.3(3) . . ?
O5 Zr2 O7 143.2(3) . 25_656 ?
O5 Zr2 O12 117.8(4) . 7_547 ?
O5 Zr2 O6 70.2(3) . . ?
O4 Zr2 Zr2 34.7(3) . 29 ?
O4 Zr2 Zr2 89.1(4) . 5_656 ?
O4 Zr2 Zr1 89.1(4) . 25_656 ?
O4 Zr2 Zr1 34.5(4) . . ?
O4 Zr2 O2 76.7(4) . . ?
O4 Zr2 O7 71.1(4) . 25_656 ?
O4 Zr2 O3 69.8(4) . . ?
O4 Zr2 O3 107.6(5) . 5_656 ?
O4 Zr2 O12 75.9(5) . 7_547 ?
O4 Zr2 O5 143.0(4) . . ?
O4 Zr2 O6 144.7(4) . . ?
O6 Zr2 Zr2 115.2(2) . 29 ?
O6 Zr2 Zr2 114.1(2) . 5_656 ?
O6 Zr2 Zr1 171.3(2) . . ?
O6 Zr2 Zr1 81.5(2) . 25_656 ?
Zr2 Zr1 Zr2 60.38(3) 29 25_656 ?
Zr2 Zr1 Zr2 90.23(4) 29 5_656 ?
Zr2 Zr1 Zr2 60.39(3) . 5_656 ?
Zr2 Zr1 Zr2 60.22(4) . 29 ?
Zr2 Zr1 Zr2 90.23(4) . 25_656 ?
Zr2 Zr1 Zr2 59.55(4) 5_656 25_656 ?
O1 Zr1 Zr2 109.9(2) 29 . ?
O1 Zr1 Zr2 164.5(2) . 25_656 ?
O1 Zr1 Zr2 111.0(2) . 5_656 ?
O1 Zr1 Zr2 164.5(2) 29 5_656 ?
O1 Zr1 Zr2 111.0(2) 29 25_656 ?
O1 Zr1 Zr2 74.3(2) . . ?
O1 Zr1 Zr2 74.3(2) 29 29 ?
O1 Zr1 Zr2 109.9(2) . 29 ?
O1 Zr1 O1 75.1(4) . 29 ?
O7 Zr1 Zr2 91.4(3) . . ?
O7 Zr1 Zr2 35.7(2) . 25_656 ?
O7 Zr1 Zr2 35.7(2) . 5_656 ?
O7 Zr1 Zr2 91.4(3) . 29 ?
O7 Zr1 O1 142.2(2) . . ?
O7 Zr1 O1 142.2(2) . 29 ?
O7 Zr1 O8 80.9(4) . 29 ?
O7 Zr1 O8 80.9(4) . . ?
O3 Zr1 Zr2 89.9(3) 29 . ?
O3 Zr1 Zr2 35.7(3) . . ?
O3 Zr1 Zr2 34.3(2) . 5_656 ?
O3 Zr1 Zr2 90.0(3) . 29 ?
O3 Zr1 Zr2 35.7(3) 29 29 ?
O3 Zr1 Zr2 88.7(2) . 25_656 ?
O3 Zr1 Zr2 88.7(2) 29 5_656 ?
O3 Zr1 Zr2 34.3(2) 29 25_656 ?
O3 Zr1 O1 142.5(3) . 29 ?
O3 Zr1 O1 142.5(3) 29 . ?
O3 Zr1 O1 78.9(3) 29 29 ?
O3 Zr1 O1 78.9(3) . . ?
O3 Zr1 O7 70.0(3) . . ?
O3 Zr1 O7 70.0(3) 29 . ?
O3 Zr1 O3 107.8(5) 29 . ?
O3 Zr1 O8 82.1(5) . . ?
O3 Zr1 O8 82.1(5) 29 29 ?
O3 Zr1 O8 142.8(3) 29 . ?
O3 Zr1 O8 142.8(3) . 29 ?
O4 Zr1 Zr2 89.4(4) . 5_656 ?
O4 Zr1 Zr2 34.8(2) . 29 ?
O4 Zr1 Zr2 89.4(4) . 25_656 ?
O4 Zr1 Zr2 34.8(2) . . ?
O4 Zr1 O1 77.8(4) . 29 ?
O4 Zr1 O1 77.8(4) . . ?
O4 Zr1 O7 110.0(6) . . ?
O4 Zr1 O3 70.5(4) . . ?
O4 Zr1 O3 70.5(4) . 29 ?
O4 Zr1 O8 143.8(3) . . ?
O4 Zr1 O8 143.8(3) . 29 ?
O8 Zr1 Zr2 80.2(3) 29 25_656 ?
O8 Zr1 Zr2 80.2(3) . 5_656 ?
O8 Zr1 Zr2 170.4(3) 29 . ?
O8 Zr1 Zr2 113.7(2) . 25_656 ?
O8 Zr1 Zr2 170.4(3) . 29 ?
O8 Zr1 Zr2 114.0(4) . . ?
O8 Zr1 Zr2 113.7(2) 29 5_656 ?
O8 Zr1 Zr2 114.0(4) 29 29 ?
O8 Zr1 O1 115.3(4) 29 . ?
O8 Zr1 O1 74.0(3) 29 29 ?
O8 Zr1 O1 74.0(3) . . ?
O8 Zr1 O1 115.3(4) . 29 ?
O8 Zr1 O8 70.5(7) 29 . ?
C1 O2 Zr2 135.1(7) . . ?
C1 O1 Zr1 131.9(6) . . ?
Zr2 O7 Zr2 107.2(5) 5_656 25_656 ?
Zr1 O7 Zr2 109.0(4) . 5_656 ?
Zr1 O7 Zr2 109.0(4) . 25_656 ?
Zr2 O3 Zr2 110.7(4) 5_656 . ?
Zr2 O3 Zr1 111.3(4) 5_656 . ?
Zr1 O3 Zr2 108.9(4) . . ?
C15 O12 Zr2 139.7(9) . 7_547 ?
B2 O11 B1 118.0(12) . . ?
C9 O5 Zr2 115.3(13) . . ?
C7 C2 C1 121.7(10) . . ?
C3 C2 C7 118.0(9) . . ?
C3 C2 C1 120.2(10) . . ?
C2 C7 C6 120.9(9) . . ?
C7 C6 C5 121.4(9) . . ?
O2 C1 O1 125.4(10) . . ?
O2 C1 C2 117.7(11) . . ?
O1 C1 C2 116.8(9) . . ?
O12 C15 O12 115.5(14) 22_655 . ?
O12 C15 C14 122.2(7) . . ?
O12 C15 C14 122.2(7) 22_655 . ?
Zr2 O4 Zr2 110.5(6) . 29 ?
Zr1 O4 Zr2 110.7(5) . 29 ?
Zr1 O4 Zr2 110.7(5) . . ?
C6 C5 C4 116.2(10) . . ?
C6 C5 B1 122.3(9) . . ?
C4 C5 B1 121.4(10) . . ?
C13 C14 C15 122.0(8) . . ?
C13 C14 C15 122.0(8) 22_655 . ?
C13 C14 C13 116.0(17) 22_655 . ?
C2 C3 C4 122.3(10) . . ?
C14 C13 C12 123.2(16) . . ?
C12 C11 C12 122.0(17) . 22_655 ?
C12 C11 B2 118.1(10) 22_655 . ?
C12 C11 B2 118.1(10) . . ?
C3 C4 C5 121.0(11) . . ?
C11 C12 C13 117.2(17) . . ?
C10 O6 Zr2 127.6(14) . . ?
C8 O8 Zr1 114.5(12) . . ?
C8 O8 C10 117.4(14) . 5_656 ?
C10 O8 Zr1 126.7(10) 5_656 . ?
O11 B2 O11 123.8(17) 22_655 . ?
O11 B2 C11 118.1(9) . . ?
O11 B2 C11 118.1(9) 22_655 . ?
B1 O10 B1 121.1(13) 22_655 . ?
C8 O9 B1 119.8(14) . 7_546 ?
O8 C8 C8 110.5(11) . 29 ?
O9 C8 O8 111.0(18) . . ?
O9 C8 C8 121.0(12) . 29 ?
O11 B1 C5 112.3(9) . . ?
O11 B1 O9 99.0(13) . 7_546 ?
C5 B1 O9 99.1(13) . 7_546 ?
O10 B1 O11 117.3(12) . . ?
O10 B1 C5 121.4(12) . . ?
O10 B1 O9 102.0(10) . 7_546 ?
O5 C9 O5 149(2) . 5_656 ?
O6 C10 O8 121.4(18) . 5_656 ?

_smtbx_masks_special_details     ?
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 -0.172 -0.252 -0.700 17865.3 3001.6 ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.477
_oxdiff_exptl_absorpt_empirical_full_min 0.579
####################################################################### 
# 
# 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_BUT-101(Zn)
_database_code_depnum_ccdc_archive 'CCDC 1888830'
loop_
_audit_author_name
_audit_author_address
'Xiang-Jing Kong'
;Beijing University of Technology
China
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2017-11-02
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.06(C252 H162 N18 O72 Zn18)'
_chemical_formula_sum            'C14 H9 N O4 Zn'
_chemical_formula_weight         320.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Zn'
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      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m'
_space_group_name_Hall           '-R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   18.4038(8)
_cell_length_b                   18.4038(8)
_cell_length_c                   34.5026(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10120.4(10)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    4009
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      74.3480
_cell_measurement_theta_min      3.7380
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.591
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    0.947
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2916
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7259
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.038
_diffrn_reflns_theta_min         3.776
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -78.00   3.00   1.00    3.00    --  -41.81  19.00  90.00   81
  2  ω      1.00  33.00   1.00    3.00    --   41.81 -99.00 120.00   32
  3  ω     75.00 117.00   1.00   15.00    --  107.13-125.00 150.00   42
  4  ω    101.00 160.00   1.00   15.00    --  107.13 125.00-120.00   59
  5  ω     37.00 109.00   1.00   15.00    --  107.13 -94.00   0.00   72
  6  ω     41.00 129.00   1.00   15.00    --  107.13 -45.00 -30.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0110792000
_diffrn_orient_matrix_UB_12      -0.0691803000
_diffrn_orient_matrix_UB_13      -0.0285618000
_diffrn_orient_matrix_UB_21      0.0352892000
_diffrn_orient_matrix_UB_22      -0.0354859000
_diffrn_orient_matrix_UB_23      0.0305055000
_diffrn_orient_matrix_UB_31      -0.0892328000
_diffrn_orient_matrix_UB_32      -0.0573906000
_diffrn_orient_matrix_UB_33      0.0155598000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2002
_reflns_number_total             2221
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2221
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0602
_refine_ls_restrained_S_all      1.145
_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)+(0.0720P)²+97.4730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1673
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.19509(2) -0.19509(2) 0.36809(2) 0.0168(2) Uani 1 2 d S T P . .
O002 O 0.1897(2) -0.03612(19) 0.33432(8) 0.0377(8) Uani 1 1 d . . . . .
O003 O 0.2315(2) -0.0768(2) 0.38638(8) 0.0420(8) Uani 1 1 d . . . . .
N1 N 0.4764(3) 0.23822(14) 0.58674(11) 0.0366(13) Uani 1 2 d S T P . .
H1A H 0.5090 0.2936 0.5889 0.044 Uiso 0.5 1 calc R . . . .
H1B H 0.5090 0.2155 0.5889 0.044 Uiso 0.5 1 calc R . . . .
C2 C 0.2480(3) 0.0594(3) 0.38584(10) 0.0283(9) Uani 1 1 d . . . . .
C3 C 0.2293(4) 0.11465(18) 0.36818(14) 0.0246(11) Uani 1 2 d S T P . .
H3 H 0.2037 0.1018 0.3440 0.030 Uiso 1 2 calc RS T P . .
C1 C 0.2215(3) -0.0243(3) 0.36762(10) 0.0290(9) Uani 1 1 d . . . . .
C6 C 0.3575(4) 0.1787(2) 0.47753(15) 0.0308(12) Uani 1 2 d S T P . .
C9 C 0.4383(4) 0.21916(18) 0.54889(14) 0.0322(13) Uani 1 2 d S T P . .
C5 C 0.3113(4) 0.1556(2) 0.43942(14) 0.0302(13) Uani 1 2 d S T P . .
C4 C 0.2892(3) 0.0795(3) 0.42117(11) 0.0323(9) Uani 1 1 d . . . . .
H4 H 0.3023 0.0420 0.4329 0.039 Uiso 1 1 calc R . . . .
C7 C 0.3758(5) 0.2486(4) 0.49590(17) 0.078(2) Uani 1 1 d . U . . .
H7 H 0.3579 0.2834 0.4852 0.093 Uiso 1 1 calc R . . . .
C8 C 0.4213(5) 0.2734(5) 0.53094(16) 0.079(2) Uani 1 1 d . U . . .
H8 H 0.4391 0.3263 0.5414 0.094 Uiso 1 1 calc R . . . .


_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 Zn1 3.0059(12) 31_545 ?
Zn1 O002 2.042(3) 16_545 ?
Zn1 O002 2.042(3) 31_545 ?
Zn1 O003 2.032(3) 22 ?
Zn1 O003 2.032(3) . ?
Zn1 N1 2.078(4) 20_556 ?
O002 Zn1 2.042(3) 31_545 ?
O002 C1 1.258(5) . ?
O003 C1 1.249(5) . ?
N1 Zn1 2.078(4) 21_556 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C9 1.440(6) . ?
C2 C3 1.369(5) . ?
C2 C1 1.502(5) . ?
C2 C4 1.384(5) . ?
C3 C2 1.369(5) 24 ?
C3 H3 0.9300 . ?
C6 C5 1.507(7) . ?
C6 C7 1.318(6) 24 ?
C6 C7 1.318(6) . ?
C9 C8 1.338(7) . ?
C9 C8 1.338(7) 24 ?
C5 C4 1.398(5) 24 ?
C5 C4 1.398(5) . ?
C4 H4 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.410(7) . ?
C8 H8 0.9300 . ?

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
O002 Zn1 Zn1 75.90(8) 16_545 31_545 ?
O002 Zn1 Zn1 75.90(8) 31_545 31_545 ?
O002 Zn1 O002 87.6(2) 31_545 16_545 ?
O002 Zn1 N1 101.03(12) 31_545 20_556 ?
O002 Zn1 N1 101.03(12) 16_545 20_556 ?
O003 Zn1 Zn1 81.98(8) . 31_545 ?
O003 Zn1 Zn1 81.98(8) 22 31_545 ?
O003 Zn1 O002 157.87(12) . 31_545 ?
O003 Zn1 O002 87.52(14) . 16_545 ?
O003 Zn1 O002 157.88(12) 22 16_545 ?
O003 Zn1 O002 87.52(14) 22 31_545 ?
O003 Zn1 O003 88.9(2) . 22 ?
O003 Zn1 N1 101.09(12) . 20_556 ?
O003 Zn1 N1 101.08(12) 22 20_556 ?
N1 Zn1 Zn1 175.65(13) 20_556 31_545 ?
C1 O002 Zn1 132.2(3) . 31_545 ?
C1 O003 Zn1 124.7(3) . . ?
Zn1 N1 H1A 108.8 21_556 . ?
Zn1 N1 H1B 108.8 21_556 . ?
H1A N1 H1B 107.7 . . ?
C9 N1 Zn1 113.6(3) . 21_556 ?
C9 N1 H1A 108.8 . . ?
C9 N1 H1B 108.8 . . ?
C3 C2 C1 120.2(3) . . ?
C3 C2 C4 120.0(4) . . ?
C4 C2 C1 119.7(3) . . ?
C2 C3 C2 120.6(5) . 24 ?
C2 C3 H3 119.7 . . ?
C2 C3 H3 119.7 24 . ?
O002 C1 C2 116.3(3) . . ?
O003 C1 O002 125.1(4) . . ?
O003 C1 C2 118.5(3) . . ?
C7 C6 C5 121.9(3) . . ?
C7 C6 C5 121.9(3) 24 . ?
C7 C6 C7 116.0(6) . 24 ?
C8 C9 N1 120.3(3) 24 . ?
C8 C9 N1 120.3(3) . . ?
C8 C9 C8 119.3(6) . 24 ?
C4 C5 C6 121.1(2) . . ?
C4 C5 C6 121.1(2) 24 . ?
C4 C5 C4 117.9(5) 24 . ?
C2 C4 C5 120.7(4) . . ?
C2 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C7 H7 118.4 . . ?
C6 C7 C8 123.3(5) . . ?
C8 C7 H7 118.4 . . ?
C9 C8 C7 118.6(6) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?

_smtbx_masks_special_details     ?
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 -0.365 -0.953 -0.867 5685.2 1522.6 ?


_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.273
_oxdiff_exptl_absorpt_empirical_full_min 0.830
####################################################################### 
# 
# 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_BUT-106
_database_code_depnum_ccdc_archive 'CCDC 1888837'
loop_
_audit_author_name
_audit_author_address
'Xiang-Jing Kong'
;Beijing University of Technology
China
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-08-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C640 H368 Cd28 N32 O192)'
_chemical_formula_sum            'C160 H96 Cd7 N8 O48'
_chemical_formula_weight         3685.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Cd'
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'
Cd Cd 0.1185 4.6533 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   32.872(2)
_cell_length_b                   19.2171(7)
_cell_length_c                   32.400(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.239(9)
_cell_angle_gamma                90
_cell_volume                     19748(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4236
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      54.1240
_cell_measurement_theta_min      3.6010
_shelx_estimated_absorpt_T_max   0.854
_shelx_estimated_absorpt_T_min   0.442
_exptl_absorpt_coefficient_mu    6.500
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             7328
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            36069
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        65.996
_diffrn_reflns_theta_max         65.996
_diffrn_reflns_theta_min         3.409
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -102.00 -22.00   1.00   15.00    --  -41.81 -38.00-180.00   80
  2  ω   -116.00 -20.00   1.00   15.00    --  -41.81 -38.00 -60.00   96
  3  ω      4.00  45.00   1.00   15.00    --   41.81 -99.00  90.00   41
  4  ω     36.00  66.00   1.00   15.00    --   41.81-125.00-150.00   30
  5  ω     81.00 126.00   1.00   40.00    --  107.13  45.00  90.00   45
  6  ω    148.00 177.00   1.00   40.00    --  107.13  30.00  60.00   29
  7  ω    100.00 126.00   1.00   40.00    --  107.13 -61.00-150.00   26
  8  ω     42.00  69.00   1.00   40.00    --  107.13-125.00  90.00   27
  9  ω     92.00 121.00   1.00   40.00    --  107.13-125.00  90.00   29
 10  ω     39.00 110.00   1.00   40.00    --  107.13-125.00 -30.00   71
 11  ω     36.00  71.00   1.00   40.00    --  107.13 -61.00-150.00   35
 12  ω     78.00 178.00   1.00   40.00    --  107.13  77.00 120.00  100
 13  ω     79.00 122.00   1.00   40.00    --  107.13  30.00  60.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0361255000
_diffrn_orient_matrix_UB_12      0.0331576000
_diffrn_orient_matrix_UB_13      -0.0153229000
_diffrn_orient_matrix_UB_21      0.0160837000
_diffrn_orient_matrix_UB_22      0.0363854000
_diffrn_orient_matrix_UB_23      0.0436198000
_diffrn_orient_matrix_UB_31      0.0281553000
_diffrn_orient_matrix_UB_32      -0.0633528000
_diffrn_orient_matrix_UB_33      0.0170293000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7168
_reflns_number_total             17166
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.912
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         17166
_refine_ls_number_restraints     1059
_refine_ls_R_factor_all          0.1747
_refine_ls_R_factor_gt           0.1068
_refine_ls_restrained_S_all      0.923
_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)+(0.1981P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2963
_refine_ls_wR_factor_ref         0.3422
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C12-N1 = C21-N2
 1.48 with sigma of 0.02
 C61-N4 = C50-N3
 1.48 with sigma of 0.02
 C58-C57
 1.48 with sigma of 0.02
 C58-O13 = C58-O14
 1.25 with sigma of 0.02
 C72-C71
 1.5 with sigma of 0.01
 C40-C37
 1.5 with sigma of 0.01
 C1-C2
 1.48 with sigma of 0.02
 C1-O1 = C1-O2
 1.26 with sigma of 0.02
 C30-C31
 1.48 with sigma of 0.02
 C31-O21 = C31-O22
 1.26 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(Cd2) \\sim Ueq, Uanis(Cd3) \\sim Ueq, Uanis(Cd5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Cd4(0.66667) Cd5(0.33333)
6.a Rotating group:
 O10(H10A,H10B)
6.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C28(H28), C9(H9), C64(H64), C26(H26), C51(H51), C62(H62), C76(H76),
 C81(H81), C24(H24), C69(H69), C49(H49), C33(H33), C4(H4), C66(H66), C46(H46),
 C13(H13), C47(H47), C22(H22), C29(H29), C55(H55), C44(H44), C38(H38), C7(H7),
 C60(H60), C73(H73), C43(H43), C11(H11), C15(H15), C36(H36), C6(H6), C74(H74),
 C77(H77), C39(H39), C20(H20), C56(H56), C70(H70), C80(H80), C3(H3), C19(H19),
 C35(H35), C59(H59), C32(H32), C16(H16)
;
_atom_sites_solution_hydrogens   mixed
_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
Cd1 Cd 0.500000 0.44010(4) 0.250000 0.0833(4) Uani 1 2 d S TU P . .
Cd2 Cd 0.66178(3) 1.36536(5) 0.60811(5) 0.1424(5) Uani 1 1 d . U . . .
Cd3 Cd 0.62973(4) 1.42613(6) 0.70165(6) 0.1631(6) Uani 1 1 d . U . . .
Cd4 Cd 0.26479(4) 0.77024(6) 0.64520(5) 0.1005(4) Uani 0.6667 1 d . U . . .
Cd5 Cd 0.24553(7) 0.77656(12) 0.58500(11) 0.1094(9) Uani 0.3333 1 d . U . . .
O15 O 0.5287(2) 0.8317(4) 0.5003(3) 0.106(2) Uani 1 1 d . U . . .
O16 O 0.3500(3) 0.2935(4) 0.4940(3) 0.112(3) Uani 1 1 d . U . . .
O18 O 0.4485(3) 0.3899(4) 0.2738(3) 0.107(2) Uani 1 1 d . U . . .
O19 O 0.5629(3) 0.5138(4) 0.2954(3) 0.122(3) Uani 1 1 d . U . . .
C52 C 0.6256(3) 0.9043(5) 0.4183(3) 0.078(2) Uani 1 1 d . U . . .
O8 O 0.5931(3) 1.3196(6) 0.7008(5) 0.155(3) Uani 1 1 d . U . . .
O20 O 0.4993(3) 0.5276(4) 0.2993(3) 0.123(3) Uani 1 1 d . U . . .
C27 C 0.3458(3) -0.0012(6) 0.4090(4) 0.092(3) Uani 1 1 d . U . . .
N2 N 0.3318(3) 0.2301(6) 0.4901(4) 0.113(3) Uani 1 1 d D U . . .
C63 C 0.5299(3) 1.0420(6) 0.5889(4) 0.085(2) Uani 1 1 d . U . . .
C53 C 0.6166(3) 0.8422(5) 0.3977(3) 0.081(2) Uani 1 1 d . U . . .
H53 H 0.631175 0.829382 0.377890 0.097 Uiso 1 1 calc R . . . .
C28 C 0.3461(3) -0.0447(5) 0.4434(4) 0.093(3) Uani 1 1 d . U . . .
H28 H 0.349705 -0.025406 0.470410 0.111 Uiso 1 1 calc R . . . .
C65 C 0.4810(3) 0.9467(6) 0.5801(4) 0.086(2) Uani 1 1 d . U . . .
N3 N 0.5492(3) 0.8863(5) 0.4948(4) 0.110(3) Uani 1 1 d D U . . .
C68 C 0.4427(3) 0.9128(5) 0.5906(4) 0.086(2) Uani 1 1 d . U . . .
C9 C 0.2613(3) 0.2918(5) 0.5970(4) 0.091(3) Uani 1 1 d . U . . .
H9 H 0.249934 0.306638 0.618915 0.109 Uiso 1 1 calc R . . . .
C64 C 0.4964(3) 1.0073(5) 0.5998(3) 0.073(2) Uani 1 1 d . U . . .
H64 H 0.484787 1.025892 0.620633 0.088 Uiso 1 1 calc R . . . .
O17 O 0.5077(3) 0.3428(5) 0.3063(4) 0.141(3) Uani 1 1 d . U . . .
C26 C 0.3749(3) 0.1125(5) 0.3924(4) 0.086(3) Uani 1 1 d . U . . .
H26 H 0.385119 0.089709 0.371912 0.103 Uiso 1 1 calc R . . . .
O5 O 0.3024(3) 0.8071(5) 0.5895(4) 0.142(3) Uani 1 1 d . U . . .
C75 C 0.5470(3) 1.1086(6) 0.6098(4) 0.095(3) Uani 1 1 d . U . . .
C50 C 0.5744(3) 0.8767(6) 0.4585(4) 0.091(3) Uani 1 1 d D U . . .
C23 C 0.3525(3) 0.0756(5) 0.4166(4) 0.082(2) Uani 1 1 d . U . . .
N4 N 0.5568(3) 0.9400(5) 0.5045(4) 0.108(3) Uani 1 1 d D U . . .
C5 C 0.2779(3) 0.4155(6) 0.5859(5) 0.102(3) Uani 1 1 d . U . . .
O11 O 0.5675(3) 1.4838(5) 0.6717(5) 0.166(4) Uani 1 1 d . U . . .
C42 C 0.5503(4) 0.6096(6) 0.3345(4) 0.095(3) Uani 1 1 d . U . . .
C8 C 0.2793(4) 0.3396(7) 0.5759(4) 0.103(3) Uani 1 1 d . U . . .
O1 O 0.2579(3) 0.6734(5) 0.5901(4) 0.152(3) Uani 1 1 d D U . . .
C51 C 0.6041(3) 0.9228(5) 0.4482(3) 0.082(2) Uani 1 1 d . U . . .
H51 H 0.609141 0.965894 0.461575 0.099 Uiso 1 1 calc R . . . .
C62 C 0.5453(3) 1.0117(8) 0.5568(4) 0.104(3) Uani 1 1 d . U . . .
H62 H 0.566251 1.034918 0.547872 0.125 Uiso 1 1 calc R . . . .
O7 O 0.6120(4) 1.3452(5) 0.6431(5) 0.173(4) Uani 1 1 d . U . . .
C54 C 0.6595(4) 0.9514(5) 0.4092(4) 0.090(3) Uani 1 1 d . U . . .
C25 C 0.3817(4) 0.1846(5) 0.3995(4) 0.091(3) Uani 1 1 d . U . . .
C10 C 0.2596(4) 0.2204(6) 0.5861(4) 0.103(3) Uani 1 1 d . U . . .
C76 C 0.5520(4) 1.1209(6) 0.6521(4) 0.098(3) Uani 1 1 d . U . . .
H76 H 0.545283 1.086555 0.669411 0.118 Uiso 1 1 calc R . . . .
C81 C 0.5555(3) 1.1637(7) 0.5836(5) 0.113(3) Uani 1 1 d . U . . .
H81 H 0.550844 1.157450 0.554304 0.135 Uiso 1 1 calc R . . . .
C24 C 0.3653(3) 0.2177(5) 0.4303(4) 0.090(3) Uani 1 1 d . U . . .
H24 H 0.368730 0.265478 0.434212 0.109 Uiso 1 1 calc R . . . .
O24 O 0.1704(4) 0.0298(5) 0.6996(5) 0.168(4) Uani 1 1 d . U . . .
C45 C 0.5740(3) 0.7327(5) 0.3809(4) 0.090(3) Uani 1 1 d . U . . .
O2 O 0.2761(4) 0.6528(5) 0.6503(5) 0.171(4) Uani 1 1 d D U . . .
C69 C 0.4381(4) 0.9129(6) 0.6311(4) 0.103(3) Uani 1 1 d . U . . .
H69 H 0.458569 0.932807 0.653370 0.124 Uiso 1 1 calc R . . . .
N1 N 0.3120(4) 0.1967(4) 0.5012(4) 0.114(3) Uani 1 1 d D U . . .
C37 C 0.4482(4) 0.3058(6) 0.3272(4) 0.111(4) Uani 1 1 d D U . . .
C48 C 0.5860(3) 0.7973(5) 0.4053(4) 0.083(2) Uani 1 1 d . U . . .
C30 C 0.3342(3) -0.1447(6) 0.3994(6) 0.113(3) Uani 1 1 d D U . . .
C49 C 0.5654(3) 0.8147(6) 0.4371(4) 0.088(3) Uani 1 1 d . U . . .
H49 H 0.545862 0.784291 0.443376 0.106 Uiso 1 1 calc R . . . .
O23 O 0.1552(3) -0.0326(5) 0.6434(5) 0.170(5) Uani 1 1 d . U . . .
C33 C 0.3392(5) -0.0290(7) 0.3693(5) 0.121(4) Uani 1 1 d . U . . .
H33 H 0.338634 -0.000975 0.345718 0.146 Uiso 1 1 calc R . . . .
O21 O 0.3419(5) -0.2598(6) 0.4251(5) 0.180(4) Uani 1 1 d D U . . .
C4 C 0.2823(4) 0.4380(6) 0.6272(5) 0.108(3) Uani 1 1 d . U . . .
H4 H 0.287387 0.405957 0.649514 0.130 Uiso 1 1 calc R . . . .
C40 C 0.4708(4) 0.3484(6) 0.3009(4) 0.104(3) Uani 1 1 d D U . . .
C66 C 0.4989(4) 0.9167(7) 0.5505(4) 0.098(3) Uani 1 1 d . U . . .
H66 H 0.489269 0.873607 0.538882 0.118 Uiso 1 1 calc R . . . .
C46 C 0.5327(3) 0.7089(6) 0.3689(4) 0.101(3) Uani 1 1 d . U . . .
H46 H 0.512284 0.735325 0.376779 0.122 Uiso 1 1 calc R . . . .
C13 C 0.2997(4) 0.3156(8) 0.5457(4) 0.113(3) Uani 1 1 d . U . . .
H13 H 0.313582 0.347424 0.532615 0.135 Uiso 1 1 calc R . . . .
C47 C 0.5205(4) 0.6504(6) 0.3469(4) 0.108(4) Uani 1 1 d . U . . .
H47 H 0.492327 0.637015 0.339836 0.129 Uiso 1 1 calc R . . . .
C22 C 0.3369(3) 0.1096(6) 0.4465(4) 0.088(2) Uani 1 1 d . U . . .
H22 H 0.321194 0.084680 0.461495 0.105 Uiso 1 1 calc R . . . .
C29 C 0.3413(3) -0.1131(6) 0.4385(5) 0.108(3) Uani 1 1 d . U . . .
H29 H 0.342888 -0.140538 0.462493 0.130 Uiso 1 1 calc R . . . .
C14 C 0.2356(4) 0.1675(6) 0.6078(5) 0.109(3) Uani 1 1 d . U . . .
C55 C 0.6870(3) 0.9854(5) 0.4429(4) 0.097(3) Uani 1 1 d . U . . .
H55 H 0.683788 0.980432 0.470441 0.116 Uiso 1 1 calc R . . . .
C44 C 0.6025(4) 0.6928(6) 0.3692(4) 0.102(3) Uani 1 1 d . U . . .
H44 H 0.630460 0.707259 0.376096 0.123 Uiso 1 1 calc R . . . .
C38 C 0.4635(4) 0.2405(6) 0.3431(5) 0.124(4) Uani 1 1 d . U . . .
H38 H 0.487775 0.222636 0.337393 0.149 Uiso 1 1 calc R . . . .
O6 O 0.3315(3) 0.8174(7) 0.6563(5) 0.170(4) Uani 1 1 d . U . . .
C34 C 0.4043(4) 0.2265(5) 0.3735(4) 0.094(3) Uani 1 1 d . U . . .
C21 C 0.3440(4) 0.1803(6) 0.4551(4) 0.098(3) Uani 1 1 d D U . . .
C7 C 0.2670(4) 0.5335(8) 0.5618(6) 0.136(4) Uani 1 1 d . U . . .
H7 H 0.262084 0.564934 0.539250 0.163 Uiso 1 1 calc R . . . .
C72 C 0.3304(4) 0.8218(7) 0.6151(8) 0.142(4) Uani 1 1 d D U . . .
O22 O 0.3110(4) -0.2495(6) 0.3614(5) 0.198(6) Uani 1 1 d D U . . .
C12 C 0.2998(5) 0.2451(9) 0.5346(4) 0.131(4) Uani 1 1 d D U . . .
C60 C 0.6640(5) 0.9598(7) 0.3679(5) 0.122(4) Uani 1 1 d . U . . .
H60 H 0.646675 0.936981 0.344528 0.147 Uiso 1 1 calc R . . . .
C71 C 0.3704(4) 0.8560(6) 0.6096(7) 0.134(4) Uani 1 1 d D U . . .
C73 C 0.3743(4) 0.8551(7) 0.5671(6) 0.132(4) Uani 1 1 d . U . . .
H73 H 0.353025 0.835980 0.545210 0.159 Uiso 1 1 calc R . . . .
C61 C 0.5309(4) 0.9492(9) 0.5377(4) 0.117(3) Uani 1 1 d D U . . .
C1 C 0.2684(6) 0.6282(7) 0.6128(6) 0.166(5) Uani 1 1 d D U . . .
C79 C 0.5951(5) 1.3054(8) 0.6652(8) 0.140(4) Uani 1 1 d . U . . .
C43 C 0.5916(4) 0.6290(6) 0.3464(4) 0.103(3) Uani 1 1 d . U . . .
H43 H 0.612184 0.601342 0.339801 0.124 Uiso 1 1 calc R . . . .
C41 C 0.5373(4) 0.5466(6) 0.3079(4) 0.100(3) Uani 1 1 d . U . . .
C11 C 0.2785(5) 0.1998(7) 0.5546(4) 0.120(4) Uani 1 1 d . U . . .
H11 H 0.276857 0.153209 0.546644 0.144 Uiso 1 1 calc R . . . .
C57 C 0.7234(5) 1.0359(6) 0.3988(8) 0.142(5) Uani 1 1 d D U . . .
C15 C 0.2387(4) 0.1741(6) 0.6479(5) 0.104(3) Uani 1 1 d . U . . .
H15 H 0.254437 0.209324 0.664256 0.124 Uiso 1 1 calc R . . . .
C36 C 0.4100(4) 0.3282(6) 0.3328(4) 0.110(4) Uani 1 1 d . U . . .
H36 H 0.397256 0.368334 0.319293 0.132 Uiso 1 1 calc R . . . .
C6 C 0.2707(4) 0.4653(8) 0.5553(5) 0.120(3) Uani 1 1 d . U . . .
H6 H 0.268075 0.450892 0.527361 0.145 Uiso 1 1 calc R . . . .
C2 C 0.2707(4) 0.5550(7) 0.6021(7) 0.130(4) Uani 1 1 d D U . . .
C74 C 0.4120(4) 0.8846(6) 0.5578(5) 0.116(3) Uani 1 1 d . U . . .
H74 H 0.415025 0.884222 0.530103 0.139 Uiso 1 1 calc R . . . .
C77 C 0.5665(4) 1.1824(7) 0.6688(5) 0.114(3) Uani 1 1 d . U . . .
H77 H 0.569347 1.190405 0.697763 0.136 Uiso 1 1 calc R . . . .
C39 C 0.4423(4) 0.2027(5) 0.3672(4) 0.108(4) Uani 1 1 d . U . . .
H39 H 0.453621 0.160812 0.379442 0.130 Uiso 1 1 calc R . . . .
C20 C 0.2120(5) 0.1167(5) 0.5830(5) 0.131(4) Uani 1 1 d . U . . .
H20 H 0.209254 0.116001 0.553698 0.157 Uiso 1 1 calc R . . . .
C56 C 0.7186(4) 1.0260(6) 0.4363(6) 0.130(4) Uani 1 1 d . U . . .
H56 H 0.737172 1.047159 0.459565 0.156 Uiso 1 1 calc R . . . .
C70 C 0.4018(4) 0.8825(7) 0.6391(6) 0.124(4) Uani 1 1 d . U . . .
H70 H 0.400044 0.881130 0.667265 0.149 Uiso 1 1 calc R . . . .
C80 C 0.5706(4) 1.2253(8) 0.6022(6) 0.123(4) Uani 1 1 d . U . . .
H80 H 0.576160 1.261103 0.585150 0.147 Uiso 1 1 calc R . . . .
C78 C 0.5777(4) 1.2357(7) 0.6438(6) 0.115(3) Uani 1 1 d . U . . .
O10 O 0.6313(5) 1.4563(7) 0.7685(5) 0.197(4) Uani 1 1 d . U . . .
H10A H 0.647146 1.422472 0.795797 0.296 Uiso 1 1 d GR . . . .
H10B H 0.601799 1.458084 0.779109 0.296 Uiso 1 1 d GR . . . .
C3 C 0.2790(4) 0.5094(7) 0.6359(5) 0.125(4) Uani 1 1 d . U . . .
H3 H 0.282497 0.525202 0.663738 0.150 Uiso 1 1 calc R . . . .
C19 C 0.1931(5) 0.0686(6) 0.6006(6) 0.145(5) Uani 1 1 d . U . . .
H19 H 0.179349 0.031466 0.584288 0.174 Uiso 1 1 calc R . . . .
C17 C 0.1940(4) 0.0740(6) 0.6433(6) 0.128(4) Uani 1 1 d . U . . .
C35 C 0.3908(4) 0.2895(5) 0.3591(4) 0.109(4) Uani 1 1 d . U . . .
H35 H 0.367874 0.308529 0.366832 0.131 Uiso 1 1 calc R . . . .
C59 C 0.6978(5) 1.0071(9) 0.3638(6) 0.149(5) Uani 1 1 d . U . . .
H59 H 0.701353 1.017067 0.336868 0.179 Uiso 1 1 calc R . . . .
C32 C 0.3332(5) -0.1022(8) 0.3648(5) 0.133(4) Uani 1 1 d . U . . .
H32 H 0.328551 -0.122002 0.337740 0.160 Uiso 1 1 calc R . . . .
C16 C 0.2169(5) 0.1249(8) 0.6651(6) 0.139(5) Uani 1 1 d . U . . .
H16 H 0.218648 0.128035 0.694103 0.167 Uiso 1 1 calc R . . . .
O3 O 0.2712(6) 0.7891(11) 0.7183(5) 0.255(7) Uani 1 1 d . U . . .
C18 C 0.1716(6) 0.0195(9) 0.6614(9) 0.166(5) Uani 1 1 d . U . . .
C31 C 0.3275(5) -0.2209(7) 0.3932(6) 0.142(5) Uani 1 1 d D U . . .
O13 O 0.7931(5) 1.0892(7) 0.4284(6) 0.214(5) Uani 1 1 d D U . . .
O14 O 0.7622(4) 1.1096(7) 0.3655(6) 0.235(7) Uani 1 1 d D U . . .
C58 C 0.7604(5) 1.0802(10) 0.3969(7) 0.191(6) Uani 1 1 d D U . . .
O4 O 0.2230(8) 0.772(2) 0.5065(6) 0.45(3) Uani 1 1 d . U . . .
O9 O 0.6910(4) 1.3600(10) 0.7257(10) 0.356(13) Uani 1 1 d . U . . .
O12 O 0.6089(7) 1.4034(10) 0.5506(7) 0.291(10) Uani 1 1 d . 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
Cd1 O18 2.253(7) . ?
Cd1 O18 2.253(7) 2_655 ?
Cd1 O19 2.617(9) . ?
Cd1 O19 2.617(9) 2_655 ?
Cd1 O20 2.323(8) 2_655 ?
Cd1 O20 2.323(8) . ?
Cd1 O17 2.579(9) . ?
Cd1 O17 2.579(9) 2_655 ?
Cd1 C40 2.752(9) . ?
Cd1 C40 2.752(9) 2_655 ?
Cd2 O7 2.254(10) . ?
Cd2 O23 2.308(10) 3_565 ?
Cd2 O21 2.284(12) 5_666 ?
Cd2 O22 2.504(13) 5_666 ?
Cd2 O13 2.299(12) 7_676 ?
Cd2 O14 2.467(14) 7_676 ?
Cd2 O12 2.307(19) . ?
Cd3 O8 2.371(10) . ?
Cd3 O11 2.303(12) . ?
Cd3 O7 2.405(12) . ?
Cd3 O24 2.411(9) 3_565 ?
Cd3 O23 2.391(14) 3_565 ?
Cd3 C79 2.715(18) . ?
Cd3 O10 2.228(14) . ?
Cd3 O9 2.335(16) . ?
Cd4 Cd5 1.890(4) . ?
Cd4 O5 2.541(11) . ?
Cd4 O1 2.548(11) . ?
Cd4 O2 2.287(9) . ?
Cd4 O6 2.313(10) . ?
Cd4 O22 2.476(14) 7_556 ?
Cd4 O3 2.350(16) . ?
Cd4 O14 2.466(11) 5_676 ?
Cd5 O5 1.928(10) . ?
Cd5 O1 2.022(10) . ?
Cd5 O4 2.46(2) . ?
O15 N3 1.284(11) . ?
O16 N2 1.350(12) . ?
O18 C40 1.268(14) . ?
O19 C41 1.205(14) . ?
C52 C53 1.362(13) . ?
C52 C51 1.385(15) . ?
C52 C54 1.522(15) . ?
O8 C79 1.20(2) . ?
O20 C41 1.261(14) . ?
C27 C28 1.391(15) . ?
C27 C23 1.502(15) . ?
C27 C33 1.356(17) . ?
N2 N1 1.041(12) . ?
N2 C21 1.614(13) . ?
C63 C64 1.409(13) . ?
C63 C75 1.489(16) . ?
C63 C62 1.397(16) . ?
C53 C48 1.394(14) . ?
C28 C29 1.330(16) . ?
C65 C68 1.533(15) . ?
C65 C64 1.360(14) . ?
C65 C66 1.378(15) . ?
N3 C50 1.618(13) . ?
N3 N4 1.088(12) . ?
C68 C69 1.361(16) . ?
C68 C74 1.371(16) . ?
C9 C8 1.369(16) . ?
C9 C10 1.414(15) . ?
O17 C40 1.183(14) . ?
C26 C23 1.400(13) . ?
C26 C25 1.414(14) . ?
O5 C72 1.101(19) . ?
C75 C76 1.356(16) . ?
C75 C81 1.429(16) . ?
C50 C51 1.422(15) . ?
C50 C49 1.372(15) . ?
C23 C22 1.374(15) . ?
N4 C61 1.548(13) . ?
C5 C8 1.498(17) . ?
C5 C4 1.378(17) . ?
C5 C6 1.352(17) . ?
C42 C47 1.392(16) . ?
C42 C43 1.362(15) . ?
C42 C41 1.482(15) . ?
C8 C13 1.400(17) . ?
O1 C1 1.133(14) . ?
C62 C61 1.375(19) . ?
O7 C79 1.273(18) . ?
C54 C55 1.385(15) . ?
C54 C60 1.393(17) . ?
C25 C24 1.403(15) . ?
C25 C34 1.497(15) . ?
C10 C14 1.562(19) . ?
C10 C11 1.385(18) . ?
C76 C77 1.335(16) . ?
C81 C80 1.362(19) . ?
C24 C21 1.397(15) . ?
O24 C18 1.26(2) . ?
C45 C48 1.470(14) . ?
C45 C46 1.387(14) . ?
C45 C44 1.340(15) . ?
O2 C1 1.265(15) . ?
C69 C70 1.410(16) . ?
N1 C12 1.557(14) . ?
C37 C40 1.510(9) . ?
C37 C38 1.400(16) . ?
C37 C36 1.384(16) . ?
C48 C49 1.412(15) . ?
C30 C29 1.367(19) . ?
C30 C32 1.38(2) . ?
C30 C31 1.485(14) . ?
O23 C18 1.212(19) . ?
C33 C32 1.424(18) . ?
O21 C31 1.264(14) . ?
C4 C3 1.410(16) . ?
C66 C61 1.376(18) . ?
C46 C47 1.336(15) . ?
C13 C12 1.403(19) . ?
C22 C21 1.393(16) . ?
C14 C15 1.281(17) . ?
C14 C20 1.368(17) . ?
C55 C56 1.362(16) . ?
C44 C43 1.426(15) . ?
C38 C39 1.382(15) . ?
O6 C72 1.33(2) . ?
C34 C39 1.395(15) . ?
C34 C35 1.332(14) . ?
C7 C6 1.34(2) . ?
C7 C2 1.34(2) . ?
C72 C71 1.522(9) . ?
O22 C31 1.169(14) . ?
C12 C11 1.38(2) . ?
C60 C59 1.47(2) . ?
C71 C73 1.42(2) . ?
C71 C70 1.31(2) . ?
C73 C74 1.46(2) . ?
C1 C2 1.455(15) . ?
C79 C78 1.55(2) . ?
C57 C56 1.28(2) . ?
C57 C59 1.34(2) . ?
C57 C58 1.499(15) . ?
C15 C16 1.387(18) . ?
C36 C35 1.400(15) . ?
C2 C3 1.37(2) . ?
C77 C78 1.413(18) . ?
C20 C19 1.32(2) . ?
C80 C78 1.32(2) . ?
C19 C17 1.38(2) . ?
C17 C16 1.321(18) . ?
C17 C18 1.49(2) . ?
O13 C58 1.284(16) . ?
O14 C58 1.179(15) . ?

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
O18 Cd1 O18 129.3(4) . 2_655 ?
O18 Cd1 O19 82.5(3) . 2_655 ?
O18 Cd1 O19 126.4(3) . . ?
O18 Cd1 O19 126.4(3) 2_655 2_655 ?
O18 Cd1 O19 82.5(3) 2_655 . ?
O18 Cd1 O20 86.0(3) 2_655 2_655 ?
O18 Cd1 O20 133.6(3) . 2_655 ?
O18 Cd1 O20 133.6(3) 2_655 . ?
O18 Cd1 O20 86.0(3) . . ?
O18 Cd1 O17 52.4(3) 2_655 2_655 ?
O18 Cd1 O17 52.4(3) . . ?
O18 Cd1 O17 89.4(3) 2_655 . ?
O18 Cd1 O17 89.4(3) . 2_655 ?
O18 Cd1 C40 110.0(3) . 2_655 ?
O18 Cd1 C40 27.1(3) . . ?
O18 Cd1 C40 27.1(3) 2_655 2_655 ?
O18 Cd1 C40 110.0(3) 2_655 . ?
O19 Cd1 O19 114.4(4) 2_655 . ?
O19 Cd1 C40 111.0(4) . . ?
O19 Cd1 C40 109.6(4) 2_655 . ?
O19 Cd1 C40 111.0(4) 2_655 2_655 ?
O19 Cd1 C40 109.6(4) . 2_655 ?
O20 Cd1 O19 81.1(3) 2_655 . ?
O20 Cd1 O19 51.0(3) 2_655 2_655 ?
O20 Cd1 O19 51.0(3) . . ?
O20 Cd1 O19 81.1(3) . 2_655 ?
O20 Cd1 O20 87.3(5) . 2_655 ?
O20 Cd1 O17 174.0(3) . 2_655 ?
O20 Cd1 O17 174.0(3) 2_655 . ?
O20 Cd1 O17 93.2(4) . . ?
O20 Cd1 O17 93.2(4) 2_655 2_655 ?
O20 Cd1 C40 89.0(3) . . ?
O20 Cd1 C40 160.6(4) 2_655 . ?
O20 Cd1 C40 160.6(4) . 2_655 ?
O20 Cd1 C40 89.0(3) 2_655 2_655 ?
O17 Cd1 O19 94.5(3) . . ?
O17 Cd1 O19 135.0(3) . 2_655 ?
O17 Cd1 O19 135.0(3) 2_655 . ?
O17 Cd1 O19 94.5(3) 2_655 2_655 ?
O17 Cd1 O17 87.0(5) . 2_655 ?
O17 Cd1 C40 25.4(3) . . ?
O17 Cd1 C40 88.5(3) 2_655 . ?
O17 Cd1 C40 25.4(3) 2_655 2_655 ?
O17 Cd1 C40 88.5(3) . 2_655 ?
C40 Cd1 C40 100.4(5) 2_655 . ?
O7 Cd2 O23 73.9(4) . 3_565 ?
O7 Cd2 O21 97.4(4) . 5_666 ?
O7 Cd2 O22 83.1(5) . 5_666 ?
O7 Cd2 O13 167.2(4) . 7_676 ?
O7 Cd2 O14 131.5(5) . 7_676 ?
O7 Cd2 O12 88.2(7) . . ?
O23 Cd2 O22 129.0(5) 3_565 5_666 ?
O23 Cd2 O14 83.1(5) 3_565 7_676 ?
O23 Cd2 O12 89.0(7) 3_565 . ?
O21 Cd2 O23 170.8(4) 5_666 3_565 ?
O21 Cd2 O22 50.7(4) 5_666 5_666 ?
O21 Cd2 O13 93.2(4) 5_666 7_676 ?
O21 Cd2 O14 105.1(5) 5_666 7_676 ?
O21 Cd2 O12 87.9(7) 5_666 . ?
O13 Cd2 O23 95.1(5) 7_676 3_565 ?
O13 Cd2 O22 109.2(5) 7_676 5_666 ?
O13 Cd2 O14 51.2(5) 7_676 7_676 ?
O13 Cd2 O12 85.0(7) 7_676 . ?
O14 Cd2 O22 79.2(4) 7_676 5_666 ?
O12 Cd2 O22 135.7(6) . 5_666 ?
O12 Cd2 O14 134.2(6) . 7_676 ?
O8 Cd3 O7 54.2(4) . . ?
O8 Cd3 O24 175.5(4) . 3_565 ?
O8 Cd3 O23 124.0(4) . 3_565 ?
O8 Cd3 C79 26.3(4) . . ?
O11 Cd3 O8 91.0(4) . . ?
O11 Cd3 O7 88.5(4) . . ?
O11 Cd3 O24 91.6(4) . 3_565 ?
O11 Cd3 O23 87.9(4) . 3_565 ?
O11 Cd3 C79 90.2(4) . . ?
O11 Cd3 O9 173.9(6) . . ?
O7 Cd3 O24 122.2(4) . 3_565 ?
O7 Cd3 C79 28.0(5) . . ?
O24 Cd3 C79 150.1(6) 3_565 . ?
O23 Cd3 O7 69.7(3) 3_565 . ?
O23 Cd3 O24 52.6(4) 3_565 3_565 ?
O23 Cd3 C79 97.7(5) 3_565 . ?
O10 Cd3 O8 96.8(5) . . ?
O10 Cd3 O11 94.4(5) . . ?
O10 Cd3 O7 151.0(4) . . ?
O10 Cd3 O24 86.6(5) . 3_565 ?
O10 Cd3 O23 139.1(4) . 3_565 ?
O10 Cd3 C79 123.1(5) . . ?
O10 Cd3 O9 91.1(8) . . ?
O9 Cd3 O8 85.7(6) . . ?
O9 Cd3 O7 85.4(6) . . ?
O9 Cd3 O24 91.3(6) . 3_565 ?
O9 Cd3 O23 89.7(8) . 3_565 ?
O9 Cd3 C79 84.6(6) . . ?
Cd5 Cd4 O5 48.9(3) . . ?
Cd5 Cd4 O1 51.7(3) . . ?
Cd5 Cd4 O2 98.2(4) . . ?
Cd5 Cd4 O6 100.5(4) . . ?
Cd5 Cd4 O22 82.2(4) . 7_556 ?
Cd5 Cd4 O3 161.3(5) . . ?
Cd5 Cd4 O14 77.5(5) . 5_676 ?
O5 Cd4 O1 71.1(3) . . ?
O2 Cd4 O5 103.1(4) . . ?
O2 Cd4 O1 46.6(4) . . ?
O2 Cd4 O6 104.2(5) . . ?
O2 Cd4 O22 89.3(4) . 7_556 ?
O2 Cd4 O3 96.3(6) . . ?
O2 Cd4 O14 168.7(5) . 5_676 ?
O6 Cd4 O5 51.9(4) . . ?
O6 Cd4 O1 107.5(5) . . ?
O6 Cd4 O22 165.5(4) . 7_556 ?
O6 Cd4 O3 87.3(7) . . ?
O6 Cd4 O14 86.9(4) . 5_676 ?
O22 Cd4 O5 130.5(5) 7_556 . ?
O22 Cd4 O1 85.4(3) 7_556 . ?
O3 Cd4 O5 137.8(6) . . ?
O3 Cd4 O1 141.9(6) . . ?
O3 Cd4 O22 86.1(6) . 7_556 ?
O3 Cd4 O14 86.0(6) . 5_676 ?
O14 Cd4 O5 82.2(3) 5_676 . ?
O14 Cd4 O1 128.6(5) 5_676 . ?
O14 Cd4 O22 79.8(4) 5_676 7_556 ?
Cd4 Cd5 O5 83.4(4) . . ?
Cd4 Cd5 O1 81.2(4) . . ?
Cd4 Cd5 O4 173.9(10) . . ?
O5 Cd5 O1 97.0(4) . . ?
O5 Cd5 O4 96.4(6) . . ?
O1 Cd5 O4 92.8(10) . . ?
C40 O18 Cd1 99.0(7) . . ?
C41 O19 Cd1 87.4(8) . . ?
C53 C52 C51 118.8(9) . . ?
C53 C52 C54 120.1(10) . . ?
C51 C52 C54 121.1(9) . . ?
C79 O8 Cd3 93.0(10) . . ?
C41 O20 Cd1 100.0(8) . . ?
C28 C27 C23 119.2(11) . . ?
C33 C27 C28 119.2(12) . . ?
C33 C27 C23 121.5(11) . . ?
O16 N2 C21 114.4(9) . . ?
N1 N2 O16 145.8(13) . . ?
N1 N2 C21 99.8(11) . . ?
C64 C63 C75 121.3(9) . . ?
C62 C63 C64 116.6(11) . . ?
C62 C63 C75 122.1(10) . . ?
C52 C53 C48 122.0(10) . . ?
C29 C28 C27 121.6(13) . . ?
C64 C65 C68 119.0(10) . . ?
C64 C65 C66 120.7(11) . . ?
C66 C65 C68 120.2(10) . . ?
O15 N3 C50 113.1(9) . . ?
N4 N3 O15 145.6(13) . . ?
N4 N3 C50 101.3(10) . . ?
C69 C68 C65 121.4(10) . . ?
C69 C68 C74 120.0(12) . . ?
C74 C68 C65 118.5(11) . . ?
C8 C9 C10 121.4(11) . . ?
C65 C64 C63 120.4(10) . . ?
C40 O17 Cd1 85.5(7) . . ?
C23 C26 C25 119.4(10) . . ?
Cd5 O5 Cd4 47.6(3) . . ?
C72 O5 Cd4 90.2(13) . . ?
C72 O5 Cd5 137.5(14) . . ?
C76 C75 C63 122.8(10) . . ?
C76 C75 C81 118.7(12) . . ?
C81 C75 C63 118.4(12) . . ?
C51 C50 N3 127.9(10) . . ?
C49 C50 N3 112.6(9) . . ?
C49 C50 C51 119.5(10) . . ?
C26 C23 C27 118.7(10) . . ?
C22 C23 C27 121.3(9) . . ?
C22 C23 C26 120.1(10) . . ?
N3 N4 C61 100.5(11) . . ?
C4 C5 C8 121.0(13) . . ?
C6 C5 C8 122.6(14) . . ?
C6 C5 C4 116.3(13) . . ?
C47 C42 C41 120.7(10) . . ?
C43 C42 C47 119.2(11) . . ?
C43 C42 C41 120.1(11) . . ?
C9 C8 C5 120.2(11) . . ?
C9 C8 C13 118.5(12) . . ?
C13 C8 C5 121.3(13) . . ?
Cd5 O1 Cd4 47.1(2) . . ?
C1 O1 Cd4 98.5(12) . . ?
C1 O1 Cd5 145.6(13) . . ?
C52 C51 C50 120.8(9) . . ?
C61 C62 C63 123.4(11) . . ?
Cd2 O7 Cd3 103.2(4) . . ?
C79 O7 Cd2 150.4(10) . . ?
C79 O7 Cd3 89.7(12) . . ?
C55 C54 C52 119.1(11) . . ?
C55 C54 C60 119.3(12) . . ?
C60 C54 C52 121.6(11) . . ?
C26 C25 C34 121.1(10) . . ?
C24 C25 C26 119.0(10) . . ?
C24 C25 C34 119.8(9) . . ?
C9 C10 C14 120.8(11) . . ?
C11 C10 C9 117.7(13) . . ?
C11 C10 C14 121.5(11) . . ?
C77 C76 C75 120.0(12) . . ?
C80 C81 C75 119.1(14) . . ?
C21 C24 C25 121.3(10) . . ?
C18 O24 Cd3 93.3(11) . 3_435 ?
C46 C45 C48 122.2(10) . . ?
C44 C45 C48 121.9(10) . . ?
C44 C45 C46 115.9(10) . . ?
C1 O2 Cd4 108.1(10) . . ?
C68 C69 C70 119.4(13) . . ?
N2 N1 C12 99.8(12) . . ?
C38 C37 C40 120.7(11) . . ?
C36 C37 C40 120.3(11) . . ?
C36 C37 C38 118.8(9) . . ?
C53 C48 C45 122.1(10) . . ?
C53 C48 C49 119.3(10) . . ?
C49 C48 C45 118.6(9) . . ?
C29 C30 C32 116.8(12) . . ?
C29 C30 C31 123.1(14) . . ?
C32 C30 C31 120.1(15) . . ?
C50 C49 C48 119.5(10) . . ?
Cd2 O23 Cd3 102.0(4) 3_435 3_435 ?
C18 O23 Cd2 148.5(11) . 3_435 ?
C18 O23 Cd3 95.6(15) . 3_435 ?
C27 C33 C32 118.0(14) . . ?
C31 O21 Cd2 100.2(11) . 5_666 ?
C5 C4 C3 120.3(14) . . ?
O18 C40 Cd1 54.0(5) . . ?
O18 C40 C37 116.7(11) . . ?
O17 C40 Cd1 69.1(6) . . ?
O17 C40 O18 123.0(10) . . ?
O17 C40 C37 120.3(12) . . ?
C37 C40 Cd1 170.2(9) . . ?
C61 C66 C65 121.3(12) . . ?
C47 C46 C45 124.2(12) . . ?
C8 C13 C12 122.1(14) . . ?
C46 C47 C42 119.4(11) . . ?
C23 C22 C21 122.1(10) . . ?
C28 C29 C30 122.4(13) . . ?
C15 C14 C10 118.5(11) . . ?
C15 C14 C20 123.1(15) . . ?
C20 C14 C10 118.4(14) . . ?
C56 C55 C54 120.9(14) . . ?
C45 C44 C43 122.6(11) . . ?
C39 C38 C37 119.6(11) . . ?
C72 O6 Cd4 95.4(8) . . ?
C39 C34 C25 120.2(9) . . ?
C35 C34 C25 121.2(10) . . ?
C35 C34 C39 118.4(10) . . ?
C24 C21 N2 110.8(10) . . ?
C22 C21 N2 131.3(10) . . ?
C22 C21 C24 118.0(11) . . ?
C6 C7 C2 117.8(16) . . ?
O5 C72 O6 122.5(14) . . ?
O5 C72 C71 127(2) . . ?
O6 C72 C71 110.3(17) . . ?
Cd4 O22 Cd2 97.9(5) 7_556 5_666 ?
C31 O22 Cd2 92.0(11) . 5_666 ?
C31 O22 Cd4 112.1(13) . 7_556 ?
C13 C12 N1 140.6(15) . . ?
C11 C12 N1 101.9(13) . . ?
C11 C12 C13 116.9(13) . . ?
C54 C60 C59 115.8(15) . . ?
C73 C71 C72 114.1(17) . . ?
C70 C71 C72 128.5(19) . . ?
C70 C71 C73 117.3(12) . . ?
C71 C73 C74 119.4(13) . . ?
C62 C61 N4 103.1(11) . . ?
C62 C61 C66 117.4(12) . . ?
C66 C61 N4 139.5(14) . . ?
O1 C1 O2 106.8(14) . . ?
O1 C1 C2 127.6(18) . . ?
O2 C1 C2 125.6(16) . . ?
O8 C79 Cd3 60.7(9) . . ?
O8 C79 O7 123.0(17) . . ?
O8 C79 C78 121.3(15) . . ?
O7 C79 Cd3 62.3(9) . . ?
O7 C79 C78 115.7(18) . . ?
C78 C79 Cd3 176.8(10) . . ?
C42 C43 C44 118.6(11) . . ?
O19 C41 O20 120.8(11) . . ?
O19 C41 C42 120.2(11) . . ?
O20 C41 C42 118.9(11) . . ?
C12 C11 C10 123.2(12) . . ?
C56 C57 C59 122.2(14) . . ?
C56 C57 C58 115.2(19) . . ?
C59 C57 C58 122.5(19) . . ?
C14 C15 C16 115.3(13) . . ?
C37 C36 C35 119.0(11) . . ?
C7 C6 C5 125.7(17) . . ?
C7 C2 C1 122.3(17) . . ?
C7 C2 C3 121.8(14) . . ?
C3 C2 C1 115.9(17) . . ?
C68 C74 C73 119.1(15) . . ?
C76 C77 C78 121.8(14) . . ?
C38 C39 C34 120.9(11) . . ?
C19 C20 C14 120.3(16) . . ?
C57 C56 C55 121.7(16) . . ?
C71 C70 C69 124.7(16) . . ?
C78 C80 C81 121.8(13) . . ?
C77 C78 C79 119.5(16) . . ?
C80 C78 C79 122.1(14) . . ?
C80 C78 C77 118.3(14) . . ?
C2 C3 C4 118.2(15) . . ?
C20 C19 C17 119.3(13) . . ?
C19 C17 C18 117.5(15) . . ?
C16 C17 C19 116.7(16) . . ?
C16 C17 C18 125.7(19) . . ?
C34 C35 C36 122.3(11) . . ?
C57 C59 C60 120.0(15) . . ?
C30 C32 C33 121.9(15) . . ?
C17 C16 C15 125.0(17) . . ?
O24 C18 C17 115.0(16) . . ?
O23 C18 O24 118(2) . . ?
O23 C18 C17 127(2) . . ?
O21 C31 C30 117.5(14) . . ?
O22 C31 C30 126.9(16) . . ?
O22 C31 O21 115.5(15) . . ?
C58 O13 Cd2 99.2(11) . 7_676 ?
Cd2 O14 Cd4 99.2(5) 7_676 5_676 ?
C58 O14 Cd2 93.9(12) . 7_676 ?
C58 O14 Cd4 118.1(14) . 5_676 ?
O13 C58 C57 124.2(16) . . ?
O14 C58 C57 122.0(18) . . ?
O14 C58 O13 113.7(16) . . ?

_smtbx_masks_special_details     ?
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 -0.879 -0.214 0.471 7448.3 1816.9 ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.732
####################################################################### 
# 
# 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_BUT-107
_database_code_depnum_ccdc_archive 'CCDC 1888838'
loop_
_audit_author_name
_audit_author_address
'Xiang-Jing Kong'
;Beijing University of Technology
China
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-08-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H22 In N2 O8'
_chemical_formula_sum            'C40 H22 In N2 O8'
_chemical_formula_weight         773.41
_chemical_melting_point          ?
_chemical_oxdiff_formula         'In C N O'
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'
In In 0.0822 5.0449 '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           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   32.0315(3)
_cell_length_b                   28.2049(3)
_cell_length_c                   19.8600(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17942.4(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    22196
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      66.1650
_cell_measurement_theta_min      2.6260
_shelx_estimated_absorpt_T_max   0.856
_shelx_estimated_absorpt_T_min   0.683
_exptl_absorpt_coefficient_mu    2.291
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light gold'
_exptl_crystal_density_diffrn    0.573
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            79338
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         2.618
_diffrn_ambient_temperature      243(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     42.00  67.20   0.40    1.00    --    5.00  32.00-174.00   63
  2  ω    -32.00  -6.00   0.40    1.00    --  -45.20  32.00-174.00   65
  3  ω   -108.00 -82.00   0.40    1.00    --  -45.20 -32.00  26.00   65
  4  ω    -87.00 -61.00   0.40   20.00    -- -100.10  32.00-174.00   65
  5  ω   -163.00-137.00   0.40   20.00    -- -100.10 -32.00  26.00   65
  6  ω     -8.00  90.00   0.40    1.00    --    5.00  57.00  30.00  245
  7  ω   -130.00 -34.00   0.40    1.00    --  -45.20 -38.00 -60.00  240
  8  ω   -112.00 -70.00   0.40    1.00    --  -45.20 -72.00 -90.00  105
  9  ω   -117.00 -89.00   0.40   20.00    -- -100.10 -19.00 -30.00   70
 10  ω   -187.00 -89.00   0.40   20.00    -- -100.10 -72.00 -60.00  245
 11  ω   -114.00 -32.00   0.40   20.00    -- -100.10  72.00  30.00  205
 12  ω   -185.00 -97.00   0.40   20.00    -- -100.10 -19.00  60.00  220
 13  ω   -169.00-119.80   0.40   20.00    -- -100.10 -19.00 -30.00  123
 14  ω    -47.00 -21.00   0.40   20.00    -- -100.10  72.00-150.00   65
 15  ω   -106.00 -14.80   0.40   20.00    -- -100.10  57.00 -60.00  228
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0026852000
_diffrn_orient_matrix_UB_12      0.0541606000
_diffrn_orient_matrix_UB_13      0.0085864000
_diffrn_orient_matrix_UB_21      -0.0439016000
_diffrn_orient_matrix_UB_22      0.0052362000
_diffrn_orient_matrix_UB_23      -0.0307307000
_diffrn_orient_matrix_UB_31      -0.0194890000
_diffrn_orient_matrix_UB_32      -0.0043418000
_diffrn_orient_matrix_UB_33      0.0707358000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11575
_reflns_number_total             15832
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         15832
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0706
_refine_ls_restrained_S_all      1.038
_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)+(0.1672P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2197
_refine_ls_wR_factor_ref         0.2308
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C32(H32), C18(H18), C39(H39), C40(H40), C33(H33), C26(H26),
 C29(H29), C19(H19), C13(H13), C28(H28), C16(H16), C35(H35), C22(H22), C36(H36),
  C15(H15), C11(H11), C3(H3), C4(H4), C9(H9), C7(H7), C6(H6)
;
_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
In1 In 0.53728(2) 0.39158(2) 0.84639(2) 0.08557(14) Uani 1 1 d . . . . .
O1 O 0.50223(10) 0.39967(10) 0.75259(16) 0.1056(8) Uani 1 1 d . . . . .
O6 O 0.09855(8) 0.42249(10) 0.12136(15) 0.0993(7) Uani 1 1 d . . . . .
O3 O 0.44418(11) 0.83241(11) 0.42111(17) 0.1154(9) Uani 1 1 d . . . . .
O5 O 0.09679(9) 0.38707(11) 0.21853(16) 0.1076(8) Uani 1 1 d . . . . .
O4 O 0.46674(10) 0.81331(12) 0.32328(18) 0.1111(9) Uani 1 1 d . . . . .
O7 O 0.51204(9) 0.43004(10) -0.06427(16) 0.1087(8) Uani 1 1 d . . . . .
O8 O 0.47003(10) 0.37742(15) -0.1070(2) 0.1218(10) Uani 1 1 d . . . . .
O2 O 0.52549(12) 0.46604(12) 0.79019(17) 0.1204(10) Uani 1 1 d . . . . .
C31 C 0.11675(13) 0.40880(16) 0.1736(2) 0.0955(10) Uani 1 1 d . . . . .
C30 C 0.16225(11) 0.41684(15) 0.1813(2) 0.0949(10) Uani 1 1 d . . . . .
C20 C 0.45298(14) 0.80080(16) 0.3788(2) 0.0993(11) Uani 1 1 d . . . . .
C38 C 0.47791(14) 0.40820(18) -0.0632(2) 0.1005(11) Uani 1 1 d . . . . .
C37 C 0.44809(13) 0.41665(16) -0.0082(2) 0.1005(11) Uani 1 1 d . . . . .
C34 C 0.39218(12) 0.43490(16) 0.0972(2) 0.0998(11) Uani 1 1 d . . . . .
C1 C 0.50666(13) 0.44340(16) 0.7470(2) 0.1018(11) Uani 1 1 d . . . . .
C17 C 0.44790(14) 0.75012(14) 0.3961(2) 0.0990(11) Uani 1 1 d . . . . .
C25 C 0.36376(13) 0.44469(17) 0.1530(2) 0.1028(12) Uani 1 1 d . . . . .
C27 C 0.24839(12) 0.43259(18) 0.1939(2) 0.1072(12) Uani 1 1 d . . . . .
C2 C 0.48910(14) 0.46771(15) 0.6855(2) 0.1081(13) Uani 1 1 d . . . . .
C24 C 0.32141(13) 0.43367(19) 0.1489(2) 0.1070(13) Uani 1 1 d . . . . .
H24 H 0.311416 0.419489 0.109848 0.128 Uiso 1 1 calc R . . . .
N2 N 0.36486(17) 0.5011(2) 0.3229(3) 0.161(2) Uani 1 1 d . . . . .
C14 C 0.43660(16) 0.65452(15) 0.4238(2) 0.1113(13) Uani 1 1 d . . . . .
C32 C 0.18543(12) 0.43473(17) 0.1278(2) 0.1037(11) Uani 1 1 d . . . . .
H32 H 0.172348 0.441872 0.087238 0.124 Uiso 1 1 calc R . . . .
C18 C 0.43740(16) 0.73531(16) 0.4600(2) 0.1116(13) Uani 1 1 d . . . . .
H18 H 0.433840 0.757632 0.494000 0.134 Uiso 1 1 calc R . . . .
C39 C 0.42765(14) 0.46299(17) 0.0877(3) 0.1125(13) Uani 1 1 d . . . . .
H39 H 0.433170 0.488011 0.116858 0.135 Uiso 1 1 calc R . . . .
C40 C 0.45435(14) 0.45362(18) 0.0352(3) 0.1133(14) Uani 1 1 d . . . . .
H40 H 0.477475 0.473067 0.029056 0.136 Uiso 1 1 calc R . . . .
C23 C 0.29348(13) 0.44301(18) 0.2009(2) 0.1073(12) Uani 1 1 d . . . . .
C33 C 0.22734(13) 0.44180(18) 0.1347(2) 0.1095(13) Uani 1 1 d . . . . .
H33 H 0.242325 0.453290 0.098108 0.131 Uiso 1 1 calc R . . . .
C26 C 0.37769(14) 0.46601(18) 0.2117(2) 0.1131(13) Uani 1 1 d . . . . .
H26 H 0.405674 0.474280 0.215910 0.136 Uiso 1 1 calc R . . . .
C12 C 0.43160(19) 0.60323(15) 0.4361(3) 0.1154(15) Uani 1 1 d . . . . .
C29 C 0.18283(13) 0.4063(2) 0.2405(2) 0.1144(13) Uani 1 1 d . . . . .
H29 H 0.168150 0.393173 0.276306 0.137 Uiso 1 1 calc R . . . .
C19 C 0.43215(17) 0.68830(16) 0.4741(2) 0.1152(14) Uani 1 1 d . . . . .
H19 H 0.425560 0.678858 0.517704 0.138 Uiso 1 1 calc R . . . .
C13 C 0.44446(16) 0.58203(15) 0.4969(2) 0.1130(14) Uani 1 1 d . . . . .
H13 H 0.455101 0.601066 0.531015 0.136 Uiso 1 1 calc R . . . .
C28 C 0.22509(14) 0.4151(2) 0.2469(2) 0.1185(14) Uani 1 1 d . . . . .
H28 H 0.238141 0.409089 0.287857 0.142 Uiso 1 1 calc R . . . .
C5 C 0.45623(16) 0.51089(16) 0.5705(3) 0.1196(16) Uani 1 1 d . . . . .
C21 C 0.35049(14) 0.4751(2) 0.2639(2) 0.1179(14) Uani 1 1 d . . . . .
C16 C 0.4530(2) 0.71687(19) 0.3465(2) 0.1256(17) Uani 1 1 d . . . . .
H16 H 0.460166 0.726431 0.303198 0.151 Uiso 1 1 calc R . . . .
C35 C 0.38511(15) 0.3983(2) 0.0514(3) 0.1255(17) Uani 1 1 d . . . . .
H35 H 0.361119 0.379903 0.055406 0.151 Uiso 1 1 calc R . . . .
N1 N 0.3972(2) 0.4968(3) 0.3408(3) 0.167(2) Uani 1 1 d . . . . .
C22 C 0.30892(14) 0.4630(2) 0.2591(3) 0.1237(15) Uani 1 1 d . . . . .
H22 H 0.291167 0.468372 0.295341 0.148 Uiso 1 1 calc R . . . .
C36 C 0.41303(15) 0.38870(18) 0.0001(3) 0.1231(16) Uani 1 1 d . . . . .
H36 H 0.408216 0.363393 -0.028923 0.148 Uiso 1 1 calc R . . . .
C15 C 0.4476(2) 0.66940(18) 0.3602(2) 0.1302(18) Uani 1 1 d . . . . .
H15 H 0.451410 0.647181 0.326169 0.156 Uiso 1 1 calc R . . . .
C8 C 0.44168(17) 0.53376(16) 0.5070(3) 0.1192(16) Uani 1 1 d . . . . .
C11 C 0.41398(18) 0.57388(19) 0.3859(2) 0.1273(16) Uani 1 1 d . . . . .
H11 H 0.403844 0.586963 0.346187 0.153 Uiso 1 1 calc R . . . .
C3 C 0.4710(2) 0.44284(19) 0.6362(3) 0.149(2) Uani 1 1 d . . . . .
H3 H 0.469104 0.410056 0.640123 0.179 Uiso 1 1 calc R . . . .
C10 C 0.4121(2) 0.5271(2) 0.3963(3) 0.1362(18) Uani 1 1 d . . . . .
C4 C 0.4554(2) 0.46433(19) 0.5808(3) 0.149(2) Uani 1 1 d . . . . .
H4 H 0.443335 0.445357 0.547831 0.179 Uiso 1 1 calc R . . . .
C9 C 0.4244(2) 0.50663(18) 0.4553(3) 0.148(2) Uani 1 1 d . . . . .
H9 H 0.421302 0.474105 0.461115 0.178 Uiso 1 1 calc R . . . .
C7 C 0.4886(3) 0.51583(19) 0.6804(3) 0.178(3) Uani 1 1 d . . . . .
H7 H 0.499915 0.534550 0.714373 0.213 Uiso 1 1 calc R . . . .
C6 C 0.4707(3) 0.5368(2) 0.6230(4) 0.173(3) Uani 1 1 d . U . . .
H6 H 0.468717 0.569699 0.620936 0.208 Uiso 1 1 calc R . . . .


_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
In1 O1 2.187(3) . ?
In1 O6 2.241(2) 6_656 ?
In1 O3 2.311(3) 8_656 ?
In1 O5 2.305(3) 6_656 ?
In1 O4 2.259(3) 8_656 ?
In1 O7 2.231(3) 1_556 ?
In1 O8 2.379(3) 1_556 ?
In1 O2 2.408(3) . ?
In1 C31 2.622(4) 6_656 ?
In1 C20 2.659(4) 8_656 ?
In1 C38 2.657(5) 1_556 ?
In1 C1 2.645(4) . ?
O1 C1 1.247(5) . ?
O6 C31 1.251(5) . ?
O3 C20 1.257(5) . ?
O5 C31 1.257(5) . ?
O4 C20 1.239(6) . ?
O7 C38 1.255(5) . ?
O8 C38 1.254(6) . ?
O2 C1 1.228(5) . ?
C31 C30 1.483(5) . ?
C30 C32 1.391(6) . ?
C30 C29 1.380(6) . ?
C20 C17 1.479(6) . ?
C38 C37 1.470(7) . ?
C37 C40 1.368(7) . ?
C37 C36 1.382(6) . ?
C34 C25 1.460(6) . ?
C34 C39 1.398(6) . ?
C34 C35 1.396(7) . ?
C1 C2 1.509(5) . ?
C17 C18 1.378(6) . ?
C17 C16 1.370(7) . ?
C25 C24 1.394(6) . ?
C25 C26 1.385(6) . ?
C27 C23 1.480(6) . ?
C27 C33 1.380(6) . ?
C27 C28 1.381(6) . ?
C2 C3 1.337(7) . ?
C2 C7 1.361(7) . ?
C24 C23 1.391(6) . ?
N2 C21 1.458(7) . ?
N2 N1 1.101(7) . ?
C14 C12 1.476(6) . ?
C14 C19 1.388(7) . ?
C14 C15 1.377(7) . ?
C32 C33 1.364(6) . ?
C18 C19 1.366(6) . ?
C39 C40 1.373(7) . ?
C23 C22 1.378(6) . ?
C26 C21 1.378(7) . ?
C12 C13 1.408(6) . ?
C12 C11 1.413(7) . ?
C29 C28 1.382(6) . ?
C13 C8 1.379(6) . ?
C5 C8 1.492(6) . ?
C5 C4 1.329(7) . ?
C5 C6 1.354(8) . ?
C21 C22 1.378(6) . ?
C16 C15 1.377(7) . ?
C35 C36 1.382(7) . ?
N1 C10 1.473(7) . ?
C8 C9 1.395(7) . ?
C11 C10 1.337(7) . ?
C3 C4 1.352(7) . ?
C10 C9 1.366(7) . ?
C7 C6 1.408(8) . ?

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 In1 O6 130.73(10) . 6_656 ?
O1 In1 O3 138.96(11) . 8_656 ?
O1 In1 O5 87.36(11) . 6_656 ?
O1 In1 O4 84.24(12) . 8_656 ?
O1 In1 O7 116.15(12) . 1_556 ?
O1 In1 O8 83.36(13) . 1_556 ?
O1 In1 O2 55.51(11) . . ?
O1 In1 C31 110.49(12) . 6_656 ?
O1 In1 C20 111.53(13) . 8_656 ?
O1 In1 C38 100.94(14) . 1_556 ?
O1 In1 C1 27.90(12) . . ?
O6 In1 O3 82.66(11) 6_656 8_656 ?
O6 In1 O5 57.11(11) 6_656 6_656 ?
O6 In1 O4 119.21(11) 6_656 8_656 ?
O6 In1 O8 138.34(13) 6_656 1_556 ?
O6 In1 O2 86.02(11) 6_656 . ?
O6 In1 C31 28.47(12) 6_656 6_656 ?
O6 In1 C20 101.69(12) 6_656 8_656 ?
O6 In1 C38 111.41(14) 6_656 1_556 ?
O6 In1 C1 108.85(11) 6_656 . ?
O3 In1 O8 82.03(13) 8_656 1_556 ?
O3 In1 O2 165.41(12) 8_656 . ?
O3 In1 C31 88.94(12) 8_656 6_656 ?
O3 In1 C20 28.21(12) 8_656 8_656 ?
O3 In1 C38 82.95(13) 8_656 1_556 ?
O3 In1 C1 166.84(14) 8_656 . ?
O5 In1 O3 96.13(12) 6_656 8_656 ?
O5 In1 O8 163.25(13) 6_656 1_556 ?
O5 In1 O2 85.33(12) 6_656 . ?
O5 In1 C31 28.64(12) 6_656 6_656 ?
O5 In1 C20 89.15(12) 6_656 8_656 ?
O5 In1 C38 168.43(14) 6_656 1_556 ?
O5 In1 C1 85.40(13) 6_656 . ?
O4 In1 O3 55.89(12) 8_656 8_656 ?
O4 In1 O5 83.07(11) 8_656 6_656 ?
O4 In1 O8 82.15(13) 8_656 1_556 ?
O4 In1 O2 138.53(11) 8_656 . ?
O4 In1 C31 101.86(13) 8_656 6_656 ?
O4 In1 C20 27.68(14) 8_656 8_656 ?
O4 In1 C38 105.61(14) 8_656 1_556 ?
O4 In1 C1 111.56(14) 8_656 . ?
O7 In1 O6 84.32(11) 1_556 6_656 ?
O7 In1 O3 86.19(12) 1_556 8_656 ?
O7 In1 O5 140.47(11) 1_556 6_656 ?
O7 In1 O4 128.04(11) 1_556 8_656 ?
O7 In1 O8 56.21(12) 1_556 1_556 ?
O7 In1 O2 83.56(12) 1_556 . ?
O7 In1 C31 112.48(14) 1_556 6_656 ?
O7 In1 C20 108.55(13) 1_556 8_656 ?
O7 In1 C38 28.06(13) 1_556 1_556 ?
O7 In1 C1 100.98(14) 1_556 . ?
O8 In1 O2 100.66(14) 1_556 . ?
O8 In1 C31 165.79(14) 1_556 6_656 ?
O8 In1 C20 81.39(14) 1_556 8_656 ?
O8 In1 C38 28.15(13) 1_556 1_556 ?
O8 In1 C1 92.73(14) 1_556 . ?
O2 In1 C31 85.44(13) . 6_656 ?
O2 In1 C20 166.07(14) . 8_656 ?
O2 In1 C38 92.71(14) . 1_556 ?
O2 In1 C1 27.62(12) . . ?
C31 In1 C20 95.80(13) 6_656 8_656 ?
C31 In1 C38 139.88(16) 6_656 1_556 ?
C31 In1 C1 98.31(12) 6_656 . ?
C38 In1 C20 95.17(14) 1_556 8_656 ?
C1 In1 C20 139.16(15) . 8_656 ?
C1 In1 C38 98.14(14) . 1_556 ?
C1 O1 In1 96.9(3) . . ?
C31 O6 In1 92.9(2) . 6_556 ?
C20 O3 In1 91.5(3) . 8_665 ?
C31 O5 In1 89.8(3) . 6_556 ?
C20 O4 In1 94.4(3) . 8_665 ?
C38 O7 In1 95.2(3) . 1_554 ?
C38 O8 In1 88.4(3) . 1_554 ?
C1 O2 In1 87.0(2) . . ?
O6 C31 In1 58.60(19) . 6_556 ?
O6 C31 O5 120.1(4) . . ?
O6 C31 C30 119.7(4) . . ?
O5 C31 In1 61.5(2) . 6_556 ?
O5 C31 C30 120.1(4) . . ?
C30 C31 In1 176.6(3) . 6_556 ?
C32 C30 C31 120.1(4) . . ?
C29 C30 C31 121.6(4) . . ?
C29 C30 C32 118.3(4) . . ?
O3 C20 In1 60.3(2) . 8_665 ?
O3 C20 C17 120.4(4) . . ?
O4 C20 In1 57.9(2) . 8_665 ?
O4 C20 O3 118.2(4) . . ?
O4 C20 C17 121.4(5) . . ?
C17 C20 In1 179.3(4) . 8_665 ?
O7 C38 In1 56.7(2) . 1_554 ?
O7 C38 C37 119.9(5) . . ?
O8 C38 In1 63.5(2) . 1_554 ?
O8 C38 O7 120.2(4) . . ?
O8 C38 C37 119.8(4) . . ?
C37 C38 In1 174.6(3) . 1_554 ?
C40 C37 C38 119.8(4) . . ?
C40 C37 C36 118.6(4) . . ?
C36 C37 C38 121.6(5) . . ?
C39 C34 C25 120.1(4) . . ?
C35 C34 C25 122.3(4) . . ?
C35 C34 C39 117.6(4) . . ?
O1 C1 In1 55.17(19) . . ?
O1 C1 C2 118.6(4) . . ?
O2 C1 In1 65.4(2) . . ?
O2 C1 O1 120.5(4) . . ?
O2 C1 C2 120.8(4) . . ?
C2 C1 In1 173.3(4) . . ?
C18 C17 C20 122.3(4) . . ?
C16 C17 C20 118.8(4) . . ?
C16 C17 C18 119.0(4) . . ?
C24 C25 C34 121.3(4) . . ?
C26 C25 C34 121.3(4) . . ?
C26 C25 C24 117.3(4) . . ?
C33 C27 C23 121.3(4) . . ?
C33 C27 C28 116.9(4) . . ?
C28 C27 C23 121.8(4) . . ?
C3 C2 C1 121.1(4) . . ?
C3 C2 C7 117.6(4) . . ?
C7 C2 C1 121.2(5) . . ?
C23 C24 C25 122.7(4) . . ?
N1 N2 C21 120.1(6) . . ?
C19 C14 C12 122.8(4) . . ?
C15 C14 C12 118.6(5) . . ?
C15 C14 C19 118.5(4) . . ?
C33 C32 C30 120.1(4) . . ?
C19 C18 C17 120.9(5) . . ?
C40 C39 C34 120.0(5) . . ?
C37 C40 C39 122.3(4) . . ?
C24 C23 C27 121.4(4) . . ?
C22 C23 C27 120.6(4) . . ?
C22 C23 C24 118.0(4) . . ?
C32 C33 C27 122.7(4) . . ?
C21 C26 C25 120.7(4) . . ?
C13 C12 C14 121.8(4) . . ?
C13 C12 C11 118.2(4) . . ?
C11 C12 C14 120.0(4) . . ?
C28 C29 C30 120.5(4) . . ?
C18 C19 C14 120.4(4) . . ?
C8 C13 C12 121.7(4) . . ?
C29 C28 C27 121.5(4) . . ?
C4 C5 C8 123.4(5) . . ?
C4 C5 C6 115.0(5) . . ?
C6 C5 C8 121.6(4) . . ?
C26 C21 N2 119.9(4) . . ?
C22 C21 N2 119.1(5) . . ?
C22 C21 C26 120.8(4) . . ?
C17 C16 C15 120.5(4) . . ?
C36 C35 C34 121.3(4) . . ?
N2 N1 C10 118.8(7) . . ?
C21 C22 C23 120.4(5) . . ?
C37 C36 C35 120.2(5) . . ?
C16 C15 C14 120.7(5) . . ?
C13 C8 C5 122.0(4) . . ?
C13 C8 C9 117.4(4) . . ?
C9 C8 C5 120.6(4) . . ?
C10 C11 C12 119.3(4) . . ?
C2 C3 C4 121.4(5) . . ?
C11 C10 N1 118.2(5) . . ?
C11 C10 C9 122.4(5) . . ?
C9 C10 N1 119.4(5) . . ?
C5 C4 C3 124.1(5) . . ?
C10 C9 C8 121.0(5) . . ?
C2 C7 C6 119.0(6) . . ?
C5 C6 C7 122.4(6) . . ?

_smtbx_masks_special_details     ?
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 -0.021 -0.875 -0.103 13030.8 3416.2 ?

_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 1.357
_oxdiff_exptl_absorpt_empirical_full_min 0.818
####################################################################### 
# 
# 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_BUT-105
_database_code_depnum_ccdc_archive 'CCDC 1888839'
loop_
_audit_author_name
_audit_author_address
'Xiang-Jing Kong'
;Beijing University of Technology
China
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-08-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.06(C1440 H792 N72 O432 Zn90)'
_chemical_formula_sum            'C80 H44 N4 O24 Zn5'
_chemical_formula_weight         1772.04
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Zn C H O N'
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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   54.3601(10)
_cell_length_b                   54.3601(10)
_cell_length_c                   42.0659(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     107652(5)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    8546
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      47.2140
_cell_measurement_theta_min      2.3630
_shelx_estimated_absorpt_T_max   0.962
_shelx_estimated_absorpt_T_min   0.841
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    0.492
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             16092
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       63
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            116821
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        65.073
_diffrn_reflns_theta_max         65.073
_diffrn_reflns_theta_min         2.301
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -56.00   1.05   0.35   20.00    --  -45.20  71.00  85.00  163
  2  ω   -177.00 -97.90   0.35   60.00    -- -100.10 -71.00 -44.00  226
  3  ω   -181.00-107.15   0.35   60.00    -- -100.10 -59.00-103.00  211
  4  ω   -120.00 -35.30   0.35   20.00    --  -45.20 -19.00   0.00  242
  5  ω   -168.00 -95.90   0.35   60.00    -- -100.10 -57.00-150.00  206
  6  ω   -113.00 -18.85   0.35   60.00    -- -100.10  57.00-180.00  269
  7  ω   -118.00 -93.50   0.35   60.00    -- -100.10 -38.00 -60.00   70
  8  ω   -100.00 -17.05   0.35   60.00    -- -100.10  72.00 -30.00  237
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0245149000
_diffrn_orient_matrix_UB_12      -0.0126348000
_diffrn_orient_matrix_UB_13      -0.0242570000
_diffrn_orient_matrix_UB_21      -0.0090295000
_diffrn_orient_matrix_UB_22      0.0214335000
_diffrn_orient_matrix_UB_23      0.0107339000
_diffrn_orient_matrix_UB_31      0.0197098000
_diffrn_orient_matrix_UB_32      0.0212543000
_diffrn_orient_matrix_UB_33      -0.0252391000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7124
_reflns_number_total             20392
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         20392
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0938
_refine_ls_restrained_S_all      1.013
_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)+(0.1500P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2655
_refine_ls_wR_factor_ref         0.3082
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1-O3
 1.24 with sigma of 0.02
 C1-O2
 1.24 with sigma of 0.01
 C21-N2
 1.45 with sigma of 0.01
 C10-N1
 1.48 with sigma of 0.01
 O2-O3
 2.2 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C35(H35), C28(H28), C13(H13), C32(H32), C36(H36), C22(H22),
 C29(H29), C40(H40), C3(H3), C16(H16), C20(H20), C15(H15), C19(H19), C9(H9),
 C39(H39), C26(H26), C4(H4), C11(H11), C31(H31), C6(H6), C7(H7)
;
_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 0.333333 0.23361(2) 0.416667 0.1699(5) Uani 1 2 d S T P . .
Zn2 Zn 0.36319(2) 0.29111(2) 0.46296(2) 0.1762(4) Uani 1 1 d . . . . .
Zn3 Zn 0.07193(2) 0.45607(2) 0.24653(3) 0.2196(5) Uani 1 1 d . . . . .
O4 O 0.14153(9) 0.36429(12) 0.58036(11) 0.1749(15) Uani 1 1 d . . . . .
O10 O 0.23547(9) 0.33953(11) 0.13465(13) 0.1835(16) Uani 1 1 d . . . . .
O1 O 0.36503(10) 0.27631(7) 0.42040(9) 0.1949(16) Uani 1 1 d . . . . .
O6 O 0.06588(11) 0.40787(9) 0.30059(11) 0.1895(15) Uani 1 1 d . . . . .
O11 O 0.24078(9) 0.30796(10) 0.16376(10) 0.1874(16) Uani 1 1 d . . . . .
O7 O 0.09173(9) 0.43643(10) 0.26105(13) 0.1982(17) Uani 1 1 d . . . . .
C38 C 0.23369(13) 0.32682(18) 0.1607(2) 0.176(2) Uani 1 1 d . . . . .
O2 O 0.33077(15) 0.29382(12) 0.45378(13) 0.241(3) Uani 1 1 d D . . . .
O5 O 0.14671(9) 0.40139(11) 0.55317(12) 0.2043(17) Uani 1 1 d . . . . .
C24 C 0.17653(11) 0.37129(11) 0.26890(12) 0.1466(15) Uani 1 1 d . . . . .
H24 H 0.170502 0.373210 0.248833 0.176 Uiso 1 1 calc R . . . .
C33 C 0.08732(18) 0.41871(15) 0.28314(18) 0.177(2) Uani 1 1 d . . . . .
C8 C 0.24518(14) 0.34443(12) 0.44224(16) 0.1545(17) Uani 1 1 d . . . . .
N1 N 0.21713(15) 0.35920(13) 0.36712(16) 0.221(3) Uani 1 1 d D . . . .
C35 C 0.20667(11) 0.36498(12) 0.21282(14) 0.1501(16) Uani 1 1 d . . . . .
H35 H 0.202182 0.379318 0.210716 0.180 Uiso 1 1 calc R . . . .
C27 C 0.14752(13) 0.38982(13) 0.29238(14) 0.1484(16) Uani 1 1 d . . . . .
C23 C 0.19493(12) 0.36073(12) 0.27152(14) 0.1529(16) Uani 1 1 d . . . . .
C5 C 0.26487(15) 0.33506(13) 0.44978(15) 0.1536(17) Uani 1 1 d . . . . .
C25 C 0.16686(13) 0.37908(12) 0.29544(14) 0.1524(16) Uani 1 1 d . . . . .
N2 N 0.20158(12) 0.36570(13) 0.36538(13) 0.192(2) Uani 1 1 d D . . . .
C18 C 0.15098(17) 0.38076(19) 0.5574(2) 0.184(3) Uani 1 1 d . . . . .
C34 C 0.20443(11) 0.35217(14) 0.24236(17) 0.1588(18) Uani 1 1 d . . . . .
C28 C 0.12530(15) 0.38191(13) 0.31420(13) 0.1625(18) Uani 1 1 d . . . . .
H28 H 0.123664 0.370189 0.331131 0.195 Uiso 1 1 calc R . . . .
C13 C 0.23091(13) 0.35055(12) 0.46505(15) 0.1559(17) Uani 1 1 d . . . . .
H13 H 0.234033 0.348141 0.486273 0.187 Uiso 1 1 calc R . . . .
C32 C 0.14965(13) 0.40783(14) 0.26815(15) 0.1647(18) Uani 1 1 d . . . . .
H32 H 0.163970 0.413181 0.253107 0.198 Uiso 1 1 calc R . . . .
C36 C 0.21561(11) 0.35605(13) 0.18692(14) 0.1579(17) Uani 1 1 d . . . . .
H36 H 0.216581 0.364255 0.167226 0.189 Uiso 1 1 calc R . . . .
C22 C 0.20562(13) 0.35950(13) 0.30231(16) 0.172(2) Uani 1 1 d . . . . .
H22 H 0.219017 0.353778 0.304765 0.206 Uiso 1 1 calc R . . . .
C14 C 0.19683(13) 0.36566(14) 0.48365(17) 0.1554(19) Uani 1 1 d . . . . .
C2 C 0.3037(2) 0.31739(18) 0.4632(3) 0.193(3) Uani 1 1 d . . . . .
C1 C 0.3265(3) 0.30972(19) 0.46655(18) 0.224(5) Uani 1 1 d D . . . .
C30 C 0.10919(13) 0.40907(12) 0.28710(17) 0.1546(17) Uani 1 1 d . . . . .
C29 C 0.10570(15) 0.39101(14) 0.31133(15) 0.1668(19) Uani 1 1 d . . . . .
H29 H 0.090639 0.384966 0.325513 0.200 Uiso 1 1 calc R . . . .
C37 C 0.22327(11) 0.33514(15) 0.18911(17) 0.1579(18) Uani 1 1 d . . . . .
C12 C 0.21248(14) 0.35992(13) 0.45838(16) 0.1639(18) Uani 1 1 d . . . . .
C21 C 0.19506(17) 0.36728(17) 0.32864(14) 0.190(2) Uani 1 1 d D . . . .
C40 C 0.21052(13) 0.32970(15) 0.24422(15) 0.175(2) Uani 1 1 d . . . . .
H40 H 0.207817 0.320074 0.263327 0.211 Uiso 1 1 calc R . . . .
C3 C 0.2909(3) 0.31122(17) 0.4381(2) 0.209(4) Uani 1 1 d . . . . .
H3 H 0.294491 0.300534 0.423555 0.251 Uiso 1 1 calc R . . . .
C16 C 0.17269(13) 0.35508(15) 0.53478(15) 0.1654(19) Uani 1 1 d . . . . .
H16 H 0.165957 0.343213 0.552426 0.198 Uiso 1 1 calc R . . . .
C20 C 0.19135(15) 0.38645(18) 0.48149(18) 0.186(2) Uani 1 1 d . . . . .
H20 H 0.197324 0.397616 0.463259 0.224 Uiso 1 1 calc R . . . .
O3 O 0.34067(16) 0.32016(14) 0.4923(2) 0.283(3) Uani 1 1 d D . . . .
C10 C 0.2216(2) 0.35699(16) 0.40375(14) 0.190(3) Uani 1 1 d D . . . .
C15 C 0.18774(13) 0.34997(14) 0.51117(17) 0.1621(18) Uani 1 1 d . . . . .
H15 H 0.191743 0.335384 0.514223 0.195 Uiso 1 1 calc R . . . .
C19 C 0.17759(15) 0.39286(15) 0.5039(3) 0.190(2) Uani 1 1 d . . . . .
H19 H 0.174472 0.408011 0.500678 0.228 Uiso 1 1 calc R . . . .
C9 C 0.24079(16) 0.34851(14) 0.4107(2) 0.181(2) Uani 1 1 d . . . . .
H9 H 0.250704 0.345533 0.394514 0.218 Uiso 1 1 calc R . . . .
C39 C 0.22033(14) 0.32198(15) 0.2182(2) 0.182(2) Uani 1 1 d . . . . .
H39 H 0.225059 0.307797 0.220146 0.218 Uiso 1 1 calc R . . . .
C17 C 0.16791(13) 0.37681(17) 0.5322(2) 0.168(2) Uani 1 1 d . . . . .
C26 C 0.17705(16) 0.37724(15) 0.32481(15) 0.181(2) Uani 1 1 d . . . . .
H26 H 0.171244 0.383093 0.342658 0.217 Uiso 1 1 calc R . . . .
C4 C 0.2711(2) 0.31923(17) 0.42983(16) 0.203(3) Uani 1 1 d . . . . .
H4 H 0.261928 0.313649 0.410288 0.243 Uiso 1 1 calc R . . . .
O12 O 0.23559(13) 0.35607(14) 0.35040(12) 0.246(2) Uani 1 1 d . . . . .
C11 C 0.20780(13) 0.36287(13) 0.42523(18) 0.169(2) Uani 1 1 d . . . . .
H11 H 0.195173 0.368839 0.419144 0.203 Uiso 1 1 calc R . . . .
C31 C 0.13155(15) 0.41793(13) 0.26562(15) 0.170(2) Uani 1 1 d . . . . .
H31 H 0.134000 0.430750 0.249606 0.204 Uiso 1 1 calc R . . . .
C6 C 0.28068(18) 0.34371(15) 0.4773(2) 0.198(2) Uani 1 1 d . . . . .
H6 H 0.277929 0.355260 0.491451 0.238 Uiso 1 1 calc R . . . .
O8 O 0.06710(16) 0.4524(2) 0.19797(18) 0.382(6) Uani 1 1 d . . . . .
C7 C 0.30047(17) 0.33579(16) 0.48449(19) 0.210(3) Uani 1 1 d . . . . .
H7 H 0.311426 0.342344 0.502830 0.252 Uiso 1 1 calc R . . . .
O9 O 0.11246(18) 0.49278(13) 0.2368(2) 0.358(5) 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
Zn1 O4 2.046(5) 20_556 ?
Zn1 O4 2.046(5) 28 ?
Zn1 O10 2.179(5) 4 ?
Zn1 O10 2.179(5) 8 ?
Zn1 O1 2.094(4) 12 ?
Zn1 O1 2.094(4) . ?
Zn2 O1 1.986(4) . ?
Zn2 O6 1.903(5) 36 ?
Zn2 O11 1.905(4) 8 ?
Zn2 O2 1.881(7) . ?
Zn3 O1 2.062(5) 30_455 ?
Zn3 O7 1.955(5) . ?
Zn3 O5 2.005(5) 10_455 ?
Zn3 O8 2.057(8) . ?
Zn3 O9 2.147(7) . ?
O4 C18 1.240(9) . ?
O10 C38 1.274(8) . ?
O6 C33 1.248(7) . ?
O11 C38 1.269(8) . ?
O7 C33 1.272(7) . ?
C38 C37 1.486(9) . ?
O2 C1 1.135(8) . ?
O5 C18 1.267(8) . ?
C24 C23 1.384(6) . ?
C24 C25 1.388(6) . ?
C33 C30 1.529(9) . ?
C8 C5 1.432(8) . ?
C8 C13 1.375(7) . ?
C8 C9 1.387(8) . ?
N1 N2 1.070(6) . ?
N1 C10 1.574(7) . ?
N1 O12 1.304(7) . ?
C35 C34 1.400(7) . ?
C35 C36 1.376(7) . ?
C27 C25 1.441(7) . ?
C27 C28 1.402(7) . ?
C27 C32 1.377(7) . ?
C23 C34 1.493(7) . ?
C23 C22 1.435(7) . ?
C5 C4 1.360(8) . ?
C5 C6 1.377(8) . ?
C25 C26 1.378(7) . ?
N2 C21 1.598(6) . ?
C18 C17 1.488(10) . ?
C34 C40 1.418(8) . ?
C28 C29 1.386(7) . ?
C13 C12 1.361(7) . ?
C32 C31 1.349(7) . ?
C36 C37 1.395(7) . ?
C22 C21 1.406(8) . ?
C14 C12 1.489(8) . ?
C14 C20 1.308(8) . ?
C14 C15 1.375(7) . ?
C2 C1 1.500(12) . ?
C2 C3 1.219(10) . ?
C2 C7 1.416(10) . ?
C1 O3 1.285(9) . ?
C30 C29 1.361(7) . ?
C30 C31 1.393(7) . ?
C37 C39 1.387(8) . ?
C12 C11 1.441(8) . ?
C21 C26 1.344(8) . ?
C40 C39 1.371(8) . ?
C3 C4 1.390(11) . ?
C16 C15 1.400(7) . ?
C16 C17 1.335(8) . ?
C20 C19 1.353(9) . ?
C10 C9 1.365(10) . ?
C10 C11 1.313(9) . ?
C19 C17 1.412(9) . ?
C6 C7 1.378(9) . ?

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
O4 Zn1 O4 91.3(3) 20_556 28 ?
O4 Zn1 O10 86.78(18) 20_556 4 ?
O4 Zn1 O10 86.78(19) 28 8 ?
O4 Zn1 O10 90.77(18) 20_556 8 ?
O4 Zn1 O10 90.77(18) 28 4 ?
O4 Zn1 O1 179.20(18) 20_556 12 ?
O4 Zn1 O1 88.59(19) 28 12 ?
O4 Zn1 O1 88.59(19) 20_556 . ?
O4 Zn1 O1 179.19(19) 28 . ?
O10 Zn1 O10 176.5(2) 8 4 ?
O1 Zn1 O10 90.02(16) . 4 ?
O1 Zn1 O10 90.01(16) 12 8 ?
O1 Zn1 O10 92.43(16) 12 4 ?
O1 Zn1 O10 92.43(16) . 8 ?
O1 Zn1 O1 91.6(2) 12 . ?
O6 Zn2 O1 103.76(19) 36 . ?
O6 Zn2 O11 108.4(2) 36 8 ?
O11 Zn2 O1 113.92(16) 8 . ?
O2 Zn2 O1 94.9(2) . . ?
O2 Zn2 O6 120.0(2) . 36 ?
O2 Zn2 O11 114.8(2) . 8 ?
O1 Zn3 O9 175.8(3) 30_455 . ?
O7 Zn3 O1 95.24(17) . 30_455 ?
O7 Zn3 O5 113.6(2) . 10_455 ?
O7 Zn3 O8 109.6(3) . . ?
O7 Zn3 O9 88.7(3) . . ?
O5 Zn3 O1 94.01(17) 10_455 30_455 ?
O5 Zn3 O8 135.6(3) 10_455 . ?
O5 Zn3 O9 85.6(3) 10_455 . ?
O8 Zn3 O1 91.9(3) . 30_455 ?
O8 Zn3 O9 85.5(4) . . ?
C18 O4 Zn1 122.0(4) . 21_556 ?
C38 O10 Zn1 141.6(5) . 15_554 ?
Zn2 O1 Zn1 109.68(17) . . ?
Zn2 O1 Zn3 109.3(2) . 36 ?
Zn3 O1 Zn1 112.83(15) 36 . ?
C33 O6 Zn2 131.5(5) . 30_455 ?
C38 O11 Zn2 117.4(5) . 15_554 ?
C33 O7 Zn3 134.0(5) . . ?
O10 C38 C37 117.6(7) . . ?
O11 C38 O10 123.6(6) . . ?
O11 C38 C37 118.8(8) . . ?
C1 O2 Zn2 121.2(7) . . ?
C18 O5 Zn3 114.2(6) . 10_455 ?
C23 C24 C25 121.7(5) . . ?
O6 C33 O7 124.4(7) . . ?
O6 C33 C30 118.5(7) . . ?
O7 C33 C30 117.0(7) . . ?
C13 C8 C5 122.9(6) . . ?
C13 C8 C9 117.8(7) . . ?
C9 C8 C5 119.2(7) . . ?
N2 N1 C10 105.7(7) . . ?
N2 N1 O12 142.5(8) . . ?
O12 N1 C10 111.0(7) . . ?
C36 C35 C34 119.0(5) . . ?
C28 C27 C25 120.6(6) . . ?
C32 C27 C25 122.3(6) . . ?
C32 C27 C28 117.1(6) . . ?
C24 C23 C34 119.9(5) . . ?
C24 C23 C22 119.0(5) . . ?
C22 C23 C34 121.1(5) . . ?
C4 C5 C8 123.7(7) . . ?
C4 C5 C6 115.1(7) . . ?
C6 C5 C8 121.0(6) . . ?
C24 C25 C27 121.1(5) . . ?
C26 C25 C24 118.1(6) . . ?
C26 C25 C27 120.7(6) . . ?
N1 N2 C21 108.5(7) . . ?
O4 C18 O5 123.8(9) . . ?
O4 C18 C17 120.9(7) . . ?
O5 C18 C17 115.3(8) . . ?
C35 C34 C23 122.1(5) . . ?
C35 C34 C40 118.5(5) . . ?
C40 C34 C23 119.3(6) . . ?
C29 C28 C27 122.1(6) . . ?
C12 C13 C8 123.8(6) . . ?
C31 C32 C27 121.9(5) . . ?
C35 C36 C37 122.5(5) . . ?
C21 C22 C23 117.5(5) . . ?
C20 C14 C12 122.2(7) . . ?
C20 C14 C15 115.4(7) . . ?
C15 C14 C12 122.5(6) . . ?
C3 C2 C1 116.4(10) . . ?
C3 C2 C7 119.1(9) . . ?
C7 C2 C1 123.4(10) . . ?
O2 C1 C2 132.8(9) . . ?
O2 C1 O3 115.5(10) . . ?
O3 C1 C2 110.5(9) . . ?
C29 C30 C33 118.5(7) . . ?
C29 C30 C31 121.2(6) . . ?
C31 C30 C33 120.3(7) . . ?
C30 C29 C28 117.9(6) . . ?
C36 C37 C38 120.6(7) . . ?
C39 C37 C38 121.0(7) . . ?
C39 C37 C36 118.3(5) . . ?
C13 C12 C14 122.4(6) . . ?
C13 C12 C11 116.4(6) . . ?
C11 C12 C14 121.1(7) . . ?
C22 C21 N2 127.7(7) . . ?
C26 C21 N2 111.3(6) . . ?
C26 C21 C22 121.0(5) . . ?
C39 C40 C34 120.9(6) . . ?
C2 C3 C4 123.8(9) . . ?
C17 C16 C15 120.6(7) . . ?
C14 C20 C19 124.6(8) . . ?
C9 C10 N1 114.1(8) . . ?
C11 C10 N1 121.7(9) . . ?
C11 C10 C9 124.2(6) . . ?
C14 C15 C16 122.6(6) . . ?
C20 C19 C17 120.7(7) . . ?
C10 C9 C8 118.6(7) . . ?
C40 C39 C37 120.5(6) . . ?
C16 C17 C18 118.5(8) . . ?
C16 C17 C19 116.0(7) . . ?
C19 C17 C18 125.3(8) . . ?
C21 C26 C25 122.5(6) . . ?
C5 C4 C3 121.3(7) . . ?
C10 C11 C12 119.0(6) . . ?
C32 C31 C30 119.7(6) . . ?
C7 C6 C5 122.0(6) . . ?
C6 C7 C2 118.3(8) . . ?

_smtbx_masks_special_details     ?
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 -0.137 -0.164 -0.689 82515.3 16536.3 ?

_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 1.734
_oxdiff_exptl_absorpt_empirical_full_min 0.473
