# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

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

data_TC1010
_database_code_depnum_ccdc_archive 'CCDC 1894661'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-02-19 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 08 mars 2017                                             #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C34 H28'
_chemical_formula_sum            'C34 H28'
_chemical_formula_weight         436.56
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.0376(7)
_cell_length_b                   7.4582(4)
_cell_length_c                   14.0803(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.605(2)
_cell_angle_gamma                90
_cell_volume                     1264.04(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6506
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      27.47
_cell_measurement_wavelength     0.71073


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0593485
_diffrn_orient_matrix_UB_21      0.0568073
_diffrn_orient_matrix_UB_31      -0.0123528
_diffrn_orient_matrix_UB_12      0.0653397
_diffrn_orient_matrix_UB_22      0.0856265
_diffrn_orient_matrix_UB_32      0.0798525
_diffrn_orient_matrix_UB_13      0.0351301
_diffrn_orient_matrix_UB_23      0.0255828
_diffrn_orient_matrix_UB_33      -0.0561780


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             464
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_T_max  0.990

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software               : BIS V6.2.1/2016-03-01                             #
# Number of scans :  2                                                       #
# Option          : shutterless mode                                         #
#                                                                            #
#     Scan  Time(s)  Width  DX (mm)  Frames   Theta   Omega     Phi     Chi  #
#  1 Phi       40.0   1.00     34.0     216    0.27  270.94  220.00   23.00  #
#  2 Fast       5.0   1.00     34.0     180    0.00  360.00    0.00   54.74  #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 7.39
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0547
_diffrn_reflns_av_r_equivalents  0.0504
_diffrn_reflns_number            10774
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.894
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_reflns_number_total             2894
_reflns_number_gt                2381
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2023)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0473P)²+0.4817P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2894
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1335
_refine_ls_wR_factor_gt          0.1266
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.039

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.54048(11) 0.46074(19) 0.52445(10) 0.0296(3) Uani 1 1 d . . . . .
H1 H 0.571257 0.355161 0.497667 0.036 Uiso 1 1 calc R U . . .
C2 C 0.58757(11) 0.51986(18) 0.61567(10) 0.0271(3) Uani 1 1 d . . . . .
C3 C 0.54220(12) 0.6627(2) 0.66745(11) 0.0347(3) Uani 1 1 d . . . . .
H3 H 0.483184 0.730575 0.640222 0.042 Uiso 1 1 calc R U . . .
C4 C 0.58127(14) 0.7066(2) 0.75683(12) 0.0406(4) Uani 1 1 d . . . . .
H4 H 0.549632 0.804572 0.790142 0.049 Uiso 1 1 calc R U . . .
C5 C 0.66648(14) 0.6083(2) 0.79813(11) 0.0416(4) Uani 1 1 d . . . . .
H5 H 0.692251 0.636446 0.860376 0.050 Uiso 1 1 calc R U . . .
C6 C 0.71389(13) 0.4686(2) 0.74795(10) 0.0357(3) Uani 1 1 d . . . . .
H6 H 0.772697 0.401719 0.776239 0.043 Uiso 1 1 calc R U . . .
C7 C 0.67698(11) 0.42420(18) 0.65673(9) 0.0265(3) Uani 1 1 d . . . . .
C8 C 0.73355(10) 0.27555(18) 0.60516(9) 0.0256(3) Uani 1 1 d . . . . .
C9 C 0.72666(12) 0.09778(19) 0.63713(10) 0.0321(3) Uani 1 1 d . . . . .
H9 H 0.683430 0.071052 0.691381 0.039 Uiso 1 1 calc R U . . .
C10 C 0.78187(13) -0.0397(2) 0.59092(11) 0.0362(4) Uani 1 1 d . . . . .
H10 H 0.774541 -0.159474 0.612975 0.043 Uiso 1 1 calc R U . . .
C11 C 0.84790(12) -0.00399(19) 0.51256(11) 0.0331(3) Uani 1 1 d . . . . .
H11 H 0.886751 -0.097926 0.481706 0.040 Uiso 1 1 calc R U . . .
C12 C 0.85593(11) 0.17125(19) 0.48035(9) 0.0273(3) Uani 1 1 d . . . . .
C13 C 0.79818(10) 0.30971(18) 0.52603(9) 0.0246(3) Uani 1 1 d . . . . .
C14 C 0.82383(12) 0.48442(19) 0.47707(10) 0.0288(3) Uani 1 1 d . . . . .
H14A H 0.859657 0.570265 0.521414 0.035 Uiso 1 1 calc R U . . .
H14B H 0.755604 0.539508 0.450181 0.035 Uiso 1 1 calc R U . . .
C15 C 0.90252(11) 0.4291(2) 0.39944(9) 0.0314(3) Uani 1 1 d . . . . .
C16 C 0.91946(11) 0.2516(2) 0.40303(10) 0.0316(3) Uani 1 1 d . . . . .
H16 H 0.966171 0.186826 0.361241 0.038 Uiso 1 1 calc R U . . .
C17 C 0.95086(14) 0.5610(3) 0.33153(11) 0.0429(4) Uani 1 1 d . . . . .
H17A H 1.000354 0.498482 0.287722 0.064 Uiso 1 1 calc R U . . .
H17B H 0.993079 0.651854 0.366899 0.064 Uiso 1 1 calc R U . . .
H17C H 0.890857 0.619082 0.295406 0.064 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
C1 C1 1.324(3) 3_666 ?
C1 C2 1.466(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.4045(19) . ?
C2 C7 1.4100(18) . ?
C3 C4 1.378(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.4935(18) . ?
C8 C13 1.3892(19) . ?
C8 C9 1.4028(19) . ?
C9 C10 1.388(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.387(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.4046(18) . ?
C12 C16 1.465(2) . ?
C13 C14 1.5077(18) . ?
C14 C15 1.5112(19) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.341(2) . ?
C15 C17 1.494(2) . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C1 C2 126.75(17) 3_666 . ?
C1 C1 H1 116.6 3_666 . ?
C2 C1 H1 116.6 . . ?
C3 C2 C7 118.05(13) . . ?
C3 C2 C1 122.27(12) . . ?
C7 C2 C1 119.56(12) . . ?
C4 C3 C2 121.57(14) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 120.13(14) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 119.45(15) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C7 121.28(14) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C6 C7 C2 119.46(13) . . ?
C6 C7 C8 118.78(12) . . ?
C2 C7 C8 121.75(12) . . ?
C13 C8 C9 117.79(12) . . ?
C13 C8 C7 121.05(12) . . ?
C9 C8 C7 121.12(12) . . ?
C10 C9 C8 121.18(13) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 120.68(14) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C12 C11 C10 118.80(13) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
C11 C12 C13 120.43(13) . . ?
C11 C12 C16 131.83(13) . . ?
C13 C12 C16 107.72(12) . . ?
C8 C13 C12 121.10(13) . . ?
C8 C13 C14 130.12(12) . . ?
C12 C13 C14 108.74(12) . . ?
C13 C14 C15 103.18(11) . . ?
C13 C14 H14A 111.1 . . ?
C15 C14 H14A 111.1 . . ?
C13 C14 H14B 111.1 . . ?
C15 C14 H14B 111.1 . . ?
H14A C14 H14B 109.1 . . ?
C16 C15 C17 127.89(14) . . ?
C16 C15 C14 109.78(13) . . ?
C17 C15 C14 122.33(14) . . ?
C15 C16 C12 110.58(13) . . ?
C15 C16 H16 124.7 . . ?
C12 C16 H16 124.7 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1 C2 C3 6.7(3) 3_666 . . . ?
C1 C1 C2 C7 -177.56(18) 3_666 . . . ?
C7 C2 C3 C4 -1.6(2) . . . . ?
C1 C2 C3 C4 174.24(14) . . . . ?
C2 C3 C4 C5 -0.6(2) . . . . ?
C3 C4 C5 C6 1.6(3) . . . . ?
C4 C5 C6 C7 -0.4(3) . . . . ?
C5 C6 C7 C2 -1.8(2) . . . . ?
C5 C6 C7 C8 178.28(14) . . . . ?
C3 C2 C7 C6 2.8(2) . . . . ?
C1 C2 C7 C6 -173.18(13) . . . . ?
C3 C2 C7 C8 -177.35(12) . . . . ?
C1 C2 C7 C8 6.7(2) . . . . ?
C6 C7 C8 C13 -111.16(15) . . . . ?
C2 C7 C8 C13 68.96(17) . . . . ?
C6 C7 C8 C9 66.38(18) . . . . ?
C2 C7 C8 C9 -113.50(15) . . . . ?
C13 C8 C9 C10 -0.5(2) . . . . ?
C7 C8 C9 C10 -178.07(13) . . . . ?
C8 C9 C10 C11 1.5(2) . . . . ?
C9 C10 C11 C12 -1.2(2) . . . . ?
C10 C11 C12 C13 -0.1(2) . . . . ?
C10 C11 C12 C16 178.16(14) . . . . ?
C9 C8 C13 C12 -0.86(19) . . . . ?
C7 C8 C13 C12 176.76(12) . . . . ?
C9 C8 C13 C14 -178.27(13) . . . . ?
C7 C8 C13 C14 -0.7(2) . . . . ?
C11 C12 C13 C8 1.2(2) . . . . ?
C16 C12 C13 C8 -177.50(11) . . . . ?
C11 C12 C13 C14 179.08(12) . . . . ?
C16 C12 C13 C14 0.41(14) . . . . ?
C8 C13 C14 C15 177.39(13) . . . . ?
C12 C13 C14 C15 -0.27(14) . . . . ?
C13 C14 C15 C16 0.01(15) . . . . ?
C13 C14 C15 C17 -179.95(13) . . . . ?
C17 C15 C16 C12 -179.80(14) . . . . ?
C14 C15 C16 C12 0.24(16) . . . . ?
C11 C12 C16 C15 -178.87(14) . . . . ?
C13 C12 C16 C15 -0.42(15) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_TC1028
_database_code_depnum_ccdc_archive 'CCDC 1894662'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-02-19 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 18 mai 2017                                              #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C34 H28'
_chemical_formula_sum            'C34 H28'
_chemical_formula_weight         436.56
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4590(8)
_cell_length_b                   9.7392(7)
_cell_length_c                   13.9219(11)
_cell_angle_alpha                107.331(2)
_cell_angle_beta                 100.800(3)
_cell_angle_gamma                91.401(2)
_cell_volume                     1198.20(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9896
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      27.52
_cell_measurement_wavelength     0.71073


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0274896
_diffrn_orient_matrix_UB_21      0.1033889
_diffrn_orient_matrix_UB_31      -0.0149639
_diffrn_orient_matrix_UB_12      -0.0025912
_diffrn_orient_matrix_UB_22      0.0241907
_diffrn_orient_matrix_UB_32      0.1051796
_diffrn_orient_matrix_UB_13      0.0654246
_diffrn_orient_matrix_UB_23      0.0363181
_diffrn_orient_matrix_UB_33      0.0175584


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.120
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             464
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_T_max  0.992

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.1/2016-03-01                           #
# Number of scans            :  3                                              #
# Total length of scans      :   552.00 (deg.)                                 #
# Total number of frames     :      276                                        #
# Option                       : shutterless mode                              #
#                                                                              #
#     Scan  Time(s)  Width  DX (mm)  Frames   Theta   Omega     Phi     Chi    #
#  1 Phi       30.0   2.00     34.0     180    0.27  270.94  360.00   23.00    #
#  2 Omega     30.0   2.00     34.0      48    0.27    3.16    0.00  315.50    #
#  3 Omega     30.0   2.00     34.0      48    0.27    3.16  144.00  315.50    #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 7.39
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0505
_diffrn_reflns_av_r_equivalents  0.0721
_diffrn_reflns_number            27978
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.199
_diffrn_reflns_theta_max         27.569
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_reflns_number_total             5512
_reflns_number_gt                4439
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2014_4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2023)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0497P)²+0.5535P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5512
_refine_ls_number_parameters     309
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1275
_refine_ls_wR_factor_gt          0.1163
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.047

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C -0.28615(17) 0.94901(19) 0.21649(13) 0.0341(4) Uani 1 1 d . . . . .
H1A H -0.331267 1.015682 0.181789 0.051 Uiso 1 1 calc R U . . .
H1B H -0.320073 0.961786 0.280686 0.051 Uiso 1 1 calc R U . . .
H1C H -0.312319 0.849450 0.171702 0.051 Uiso 1 1 calc R U . . .
C2 C -0.12591(16) 0.97961(16) 0.23977(10) 0.0245(3) Uani 1 1 d . . . . .
C3 C -0.05007(17) 1.08082(16) 0.21849(11) 0.0263(3) Uani 1 1 d . . . . .
H3 H -0.091105 1.146411 0.184722 0.032 Uiso 1 1 calc R U . . .
C4 C 0.10474(16) 1.07628(14) 0.25449(10) 0.0221(3) Uani 1 1 d . . . . .
C5 C 0.22365(18) 1.15874(16) 0.25061(12) 0.0294(3) Uani 1 1 d . . . . .
H5 H 0.211899 1.233082 0.219174 0.035 Uiso 1 1 calc R U . . .
C6 C 0.36009(18) 1.13084(17) 0.29342(13) 0.0314(3) Uani 1 1 d . . . . .
H6 H 0.442554 1.187402 0.292122 0.038 Uiso 1 1 calc R U . . .
C7 C 0.37740(16) 1.02089(16) 0.33822(11) 0.0262(3) Uani 1 1 d . . . . .
H7 H 0.471884 1.003379 0.367027 0.031 Uiso 1 1 calc R U . . .
C8 C 0.25858(15) 0.93541(14) 0.34180(10) 0.0194(3) Uani 1 1 d . . . . .
C9 C 0.12229(15) 0.96481(13) 0.30006(9) 0.0184(3) Uani 1 1 d . . . . .
C10 C -0.02475(15) 0.89540(15) 0.29340(10) 0.0215(3) Uani 1 1 d . . . . .
H10A H -0.043243 0.904755 0.362648 0.026 Uiso 1 1 calc R U . . .
H10B H -0.034592 0.791891 0.252877 0.026 Uiso 1 1 calc R U . . .
C11 C 0.28048(14) 0.81997(14) 0.39249(10) 0.0198(3) Uani 1 1 d . . . . .
C12 C 0.24215(15) 0.83910(16) 0.48769(11) 0.0249(3) Uani 1 1 d . . . . .
H12 H 0.198167 0.923554 0.517873 0.030 Uiso 1 1 calc R U . . .
C13 C 0.26735(16) 0.73676(17) 0.53869(12) 0.0289(3) Uani 1 1 d . . . . .
H13 H 0.242847 0.752181 0.604011 0.035 Uiso 1 1 calc R U . . .
C14 C 0.32839(16) 0.61207(17) 0.49388(13) 0.0304(3) Uani 1 1 d . . . . .
H14 H 0.344481 0.540848 0.527906 0.036 Uiso 1 1 calc R U . . .
C15 C 0.36597(16) 0.59123(16) 0.39946(12) 0.0280(3) Uani 1 1 d . . . . .
H15 H 0.406599 0.504693 0.368903 0.034 Uiso 1 1 calc R U . . .
C16 C 0.34533(14) 0.69513(15) 0.34794(10) 0.0215(3) Uani 1 1 d . . . . .
C17 C 0.38873(16) 0.67180(14) 0.24753(11) 0.0241(3) Uani 1 1 d . . . . .
H17 H 0.319071 0.686515 0.193551 0.029 Uiso 1 1 calc R U . . .
C18 C 0.51581(16) 0.63226(14) 0.22573(10) 0.0231(3) Uani 1 1 d . . . . .
H18 H 0.522523 0.606586 0.155439 0.028 Uiso 1 1 calc R U . . .
C19 C 0.64772(15) 0.62414(14) 0.29965(10) 0.0195(3) Uani 1 1 d . . . . .
C20 C 0.68231(15) 0.72959(14) 0.39654(10) 0.0221(3) Uani 1 1 d . . . . .
H20 H 0.618239 0.802339 0.414114 0.026 Uiso 1 1 calc R U . . .
C21 C 0.80630(16) 0.73060(15) 0.46674(10) 0.0238(3) Uani 1 1 d . . . . .
H21 H 0.826784 0.803101 0.531774 0.029 Uiso 1 1 calc R U . . .
C22 C 0.90125(15) 0.62539(15) 0.44223(10) 0.0227(3) Uani 1 1 d . . . . .
H22 H 0.986665 0.624990 0.490484 0.027 Uiso 1 1 calc R U . . .
C23 C 0.87058(15) 0.52101(15) 0.34691(10) 0.0211(3) Uani 1 1 d . . . . .
H23 H 0.935987 0.449268 0.330408 0.025 Uiso 1 1 calc R U . . .
C24 C 0.74568(14) 0.51861(14) 0.27434(10) 0.0186(3) Uani 1 1 d . . . . .
C25 C 0.71737(15) 0.40159(14) 0.17352(10) 0.0191(3) Uani 1 1 d . . . . .
C26 C 0.58400(15) 0.31914(15) 0.13642(11) 0.0242(3) Uani 1 1 d . . . . .
H26 H 0.510532 0.340138 0.175462 0.029 Uiso 1 1 calc R U . . .
C27 C 0.55611(17) 0.20712(16) 0.04378(12) 0.0299(3) Uani 1 1 d . . . . .
H27 H 0.464417 0.153381 0.020654 0.036 Uiso 1 1 calc R U . . .
C28 C 0.66159(18) 0.17341(16) -0.01510(11) 0.0304(3) Uani 1 1 d . . . . .
H28 H 0.642717 0.097645 -0.078531 0.036 Uiso 1 1 calc R U . . .
C29 C 0.79483(16) 0.25286(15) 0.02087(10) 0.0247(3) Uani 1 1 d . . . . .
C30 C 0.82344(15) 0.36622(14) 0.11469(10) 0.0203(3) Uani 1 1 d . . . . .
C31 C 0.97629(15) 0.43015(15) 0.13210(10) 0.0231(3) Uani 1 1 d . . . . .
H31A H 1.034957 0.422246 0.196745 0.028 Uiso 1 1 calc R U . . .
H31B H 0.978487 0.532955 0.134852 0.028 Uiso 1 1 calc R U . . .
C32 C 1.03042(17) 0.33983(17) 0.03988(11) 0.0276(3) Uani 1 1 d . . . . .
C33 C 0.92538(18) 0.24045(17) -0.02197(11) 0.0307(3) Uani 1 1 d . . . . .
H33 H 0.934594 0.171726 -0.084758 0.037 Uiso 1 1 calc R U . . .
C34 C 1.18120(18) 0.3620(2) 0.02635(13) 0.0368(4) Uani 1 1 d . . . . .
H34A H 1.195538 0.290207 -0.036630 0.055 Uiso 1 1 calc R U . . .
H34B H 1.249450 0.351292 0.085464 0.055 Uiso 1 1 calc R U . . .
H34C H 1.197639 0.459179 0.021346 0.055 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
C1 C2 1.492(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.339(2) . ?
C2 C10 1.5103(18) . ?
C3 C4 1.462(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(2) . ?
C4 C9 1.4101(18) . ?
C5 C6 1.386(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.389(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.400(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.3849(19) . ?
C8 C11 1.4948(18) . ?
C9 C10 1.5061(19) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.3996(19) . ?
C11 C16 1.4032(19) . ?
C12 C13 1.387(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.4022(19) . ?
C15 H15 0.9500 . ?
C16 C17 1.485(2) . ?
C17 C18 1.332(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.4814(19) . ?
C18 H18 0.9500 . ?
C19 C20 1.4050(18) . ?
C19 C24 1.4114(18) . ?
C20 C21 1.377(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.387(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.3843(19) . ?
C22 H22 0.9500 . ?
C23 C24 1.3979(18) . ?
C23 H23 0.9500 . ?
C24 C25 1.4940(17) . ?
C25 C30 1.3974(19) . ?
C25 C26 1.401(2) . ?
C26 C27 1.394(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.392(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.4114(18) . ?
C29 C33 1.461(2) . ?
C30 C31 1.507(2) . ?
C31 C32 1.5099(19) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.342(2) . ?
C32 C34 1.492(2) . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 127.45(13) . . ?
C3 C2 C10 109.97(13) . . ?
C1 C2 C10 122.59(13) . . ?
C2 C3 C4 110.54(12) . . ?
C2 C3 H3 124.7 . . ?
C4 C3 H3 124.7 . . ?
C5 C4 C9 120.61(13) . . ?
C5 C4 C3 131.64(13) . . ?
C9 C4 C3 107.75(12) . . ?
C4 C5 C6 118.78(13) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C5 C6 C7 120.62(14) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C6 C7 C8 121.38(14) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C9 C8 C7 117.82(12) . . ?
C9 C8 C11 122.03(12) . . ?
C7 C8 C11 120.13(12) . . ?
C8 C9 C4 120.79(13) . . ?
C8 C9 C10 130.65(12) . . ?
C4 C9 C10 108.56(11) . . ?
C9 C10 C2 103.19(11) . . ?
C9 C10 H10A 111.1 . . ?
C2 C10 H10A 111.1 . . ?
C9 C10 H10B 111.1 . . ?
C2 C10 H10B 111.1 . . ?
H10A C10 H10B 109.1 . . ?
C12 C11 C16 119.42(12) . . ?
C12 C11 C8 119.84(12) . . ?
C16 C11 C8 120.68(12) . . ?
C13 C12 C11 121.07(13) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C14 C13 C12 119.62(14) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C15 C14 C13 119.93(13) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 121.40(14) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C15 C16 C11 118.51(13) . . ?
C15 C16 C17 120.55(13) . . ?
C11 C16 C17 120.92(12) . . ?
C18 C17 C16 126.36(13) . . ?
C18 C17 H17 116.8 . . ?
C16 C17 H17 116.8 . . ?
C17 C18 C19 126.80(13) . . ?
C17 C18 H18 116.6 . . ?
C19 C18 H18 116.6 . . ?
C20 C19 C24 118.12(12) . . ?
C20 C19 C18 119.44(12) . . ?
C24 C19 C18 122.34(12) . . ?
C21 C20 C19 121.94(13) . . ?
C21 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
C20 C21 C22 119.78(12) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C23 C22 C21 119.50(13) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 121.59(12) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C23 C24 C19 119.06(12) . . ?
C23 C24 C25 119.04(12) . . ?
C19 C24 C25 121.88(12) . . ?
C30 C25 C26 117.46(12) . . ?
C30 C25 C24 121.79(12) . . ?
C26 C25 C24 120.71(12) . . ?
C27 C26 C25 121.81(14) . . ?
C27 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C28 C27 C26 120.49(14) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C29 C28 C27 118.54(13) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
C28 C29 C30 121.09(13) . . ?
C28 C29 C33 130.83(13) . . ?
C30 C29 C33 108.07(13) . . ?
C25 C30 C29 120.60(13) . . ?
C25 C30 C31 131.22(12) . . ?
C29 C30 C31 108.18(12) . . ?
C30 C31 C32 103.49(12) . . ?
C30 C31 H31A 111.1 . . ?
C32 C31 H31A 111.1 . . ?
C30 C31 H31B 111.1 . . ?
C32 C31 H31B 111.1 . . ?
H31A C31 H31B 109.0 . . ?
C33 C32 C34 127.86(14) . . ?
C33 C32 C31 109.81(13) . . ?
C34 C32 C31 122.31(14) . . ?
C32 C33 C29 110.44(13) . . ?
C32 C33 H33 124.8 . . ?
C29 C33 H33 124.8 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 179.65(14) . . . . ?
C10 C2 C3 C4 -0.20(16) . . . . ?
C2 C3 C4 C5 -179.53(15) . . . . ?
C2 C3 C4 C9 0.12(16) . . . . ?
C9 C4 C5 C6 -0.8(2) . . . . ?
C3 C4 C5 C6 178.85(14) . . . . ?
C4 C5 C6 C7 0.8(2) . . . . ?
C5 C6 C7 C8 -0.1(2) . . . . ?
C6 C7 C8 C9 -0.7(2) . . . . ?
C6 C7 C8 C11 -178.71(14) . . . . ?
C7 C8 C9 C4 0.73(19) . . . . ?
C11 C8 C9 C4 178.74(12) . . . . ?
C7 C8 C9 C10 -178.94(13) . . . . ?
C11 C8 C9 C10 -0.9(2) . . . . ?
C5 C4 C9 C8 0.0(2) . . . . ?
C3 C4 C9 C8 -179.72(11) . . . . ?
C5 C4 C9 C10 179.71(12) . . . . ?
C3 C4 C9 C10 0.02(14) . . . . ?
C8 C9 C10 C2 179.58(13) . . . . ?
C4 C9 C10 C2 -0.12(14) . . . . ?
C3 C2 C10 C9 0.20(15) . . . . ?
C1 C2 C10 C9 -179.66(13) . . . . ?
C9 C8 C11 C12 -70.73(17) . . . . ?
C7 C8 C11 C12 107.23(15) . . . . ?
C9 C8 C11 C16 112.22(15) . . . . ?
C7 C8 C11 C16 -69.81(17) . . . . ?
C16 C11 C12 C13 0.1(2) . . . . ?
C8 C11 C12 C13 -177.03(13) . . . . ?
C11 C12 C13 C14 -1.5(2) . . . . ?
C12 C13 C14 C15 1.0(2) . . . . ?
C13 C14 C15 C16 0.8(2) . . . . ?
C14 C15 C16 C11 -2.2(2) . . . . ?
C14 C15 C16 C17 178.94(13) . . . . ?
C12 C11 C16 C15 1.8(2) . . . . ?
C8 C11 C16 C15 178.81(12) . . . . ?
C12 C11 C16 C17 -179.41(13) . . . . ?
C8 C11 C16 C17 -2.4(2) . . . . ?
C15 C16 C17 C18 -49.5(2) . . . . ?
C11 C16 C17 C18 131.71(15) . . . . ?
C16 C17 C18 C19 -9.8(2) . . . . ?
C17 C18 C19 C20 -38.1(2) . . . . ?
C17 C18 C19 C24 145.75(15) . . . . ?
C24 C19 C20 C21 -1.1(2) . . . . ?
C18 C19 C20 C21 -177.47(13) . . . . ?
C19 C20 C21 C22 0.2(2) . . . . ?
C20 C21 C22 C23 0.5(2) . . . . ?
C21 C22 C23 C24 -0.1(2) . . . . ?
C22 C23 C24 C19 -0.9(2) . . . . ?
C22 C23 C24 C25 -178.93(12) . . . . ?
C20 C19 C24 C23 1.48(19) . . . . ?
C18 C19 C24 C23 177.68(13) . . . . ?
C20 C19 C24 C25 179.46(12) . . . . ?
C18 C19 C24 C25 -4.3(2) . . . . ?
C23 C24 C25 C30 -48.62(18) . . . . ?
C19 C24 C25 C30 133.39(14) . . . . ?
C23 C24 C25 C26 128.85(14) . . . . ?
C19 C24 C25 C26 -49.14(18) . . . . ?
C30 C25 C26 C27 -0.9(2) . . . . ?
C24 C25 C26 C27 -178.45(13) . . . . ?
C25 C26 C27 C28 0.2(2) . . . . ?
C26 C27 C28 C29 0.5(2) . . . . ?
C27 C28 C29 C30 -0.4(2) . . . . ?
C27 C28 C29 C33 178.34(15) . . . . ?
C26 C25 C30 C29 0.94(19) . . . . ?
C24 C25 C30 C29 178.49(12) . . . . ?
C26 C25 C30 C31 -179.24(13) . . . . ?
C24 C25 C30 C31 -1.7(2) . . . . ?
C28 C29 C30 C25 -0.3(2) . . . . ?
C33 C29 C30 C25 -179.32(12) . . . . ?
C28 C29 C30 C31 179.83(13) . . . . ?
C33 C29 C30 C31 0.82(15) . . . . ?
C25 C30 C31 C32 179.25(13) . . . . ?
C29 C30 C31 C32 -0.91(14) . . . . ?
C30 C31 C32 C33 0.68(16) . . . . ?
C30 C31 C32 C34 -177.92(13) . . . . ?
C34 C32 C33 C29 178.29(14) . . . . ?
C31 C32 C33 C29 -0.21(17) . . . . ?
C28 C29 C33 C32 -179.27(15) . . . . ?
C30 C29 C33 C32 -0.39(17) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_TC1004
_database_code_depnum_ccdc_archive 'CCDC 2322681'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-02-19 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 22 fevrier 2017                                          #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H10 Br2'
_chemical_formula_sum            'C14 H10 Br2'
_chemical_formula_weight         338.04
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
_space_group_IT_number           60
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   13.8322(7)
_cell_length_b                   11.7938(6)
_cell_length_c                   15.1516(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2471.7(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2137
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      22.74
_cell_measurement_wavelength     0.71073


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0143200
_diffrn_orient_matrix_UB_21      -0.0745065
_diffrn_orient_matrix_UB_31      0.0378568
_diffrn_orient_matrix_UB_12      0.0632379
_diffrn_orient_matrix_UB_22      0.0054323
_diffrn_orient_matrix_UB_32      0.0346122
_diffrn_orient_matrix_UB_13      -0.0299800
_diffrn_orient_matrix_UB_23      0.0311121
_diffrn_orient_matrix_UB_33      0.0498916


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1312
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    6.527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.245
_exptl_absorpt_correction_T_max  0.376

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.33
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_source_current           30.
_diffrn_source_voltage           50.
_diffrn_source_power             1500.0
_diffrn_reflns_av_uneti/neti     0.0521
_diffrn_reflns_av_r_equivalents  0.0415
_diffrn_reflns_number            11228
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.638
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             2835
_reflns_number_gt                1667
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2014_4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  
'CRYSCALC (T. Roisnel, local program, ver. 2024)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0466P)²+0.1732P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2835
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1010
_refine_ls_wR_factor_gt          0.0850
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.077

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Br1 Br 0.40255(3) 0.13697(3) 0.58117(3) 0.05765(18) Uani 1 1 d . . . . .
Br2 Br 0.09903(3) 0.55196(4) 0.32693(3) 0.06028(18) Uani 1 1 d . . . . .
C1 C 0.2692(3) 0.1626(3) 0.6005(2) 0.0371(9) Uani 1 1 d . . . . .
C2 C 0.2210(3) 0.0839(3) 0.6519(3) 0.0479(10) Uani 1 1 d . . . . .
H2 H 0.253584 0.021341 0.674402 0.058 Uiso 1 1 calc R U . . .
C3 C 0.1246(3) 0.0992(4) 0.6692(3) 0.0558(12) Uani 1 1 d . . . . .
H3 H 0.091376 0.046525 0.703434 0.067 Uiso 1 1 calc R U . . .
C4 C 0.0768(3) 0.1923(4) 0.6361(3) 0.0562(12) Uani 1 1 d . . . . .
H4 H 0.011603 0.202608 0.648627 0.067 Uiso 1 1 calc R U . . .
C5 C 0.1246(3) 0.2698(3) 0.5848(3) 0.0468(10) Uani 1 1 d . . . . .
H5 H 0.091034 0.332065 0.562918 0.056 Uiso 1 1 calc R U . . .
C6 C 0.2232(3) 0.2573(3) 0.5646(2) 0.0363(9) Uani 1 1 d . . . . .
C7 C 0.2732(3) 0.3413(3) 0.5106(2) 0.0429(10) Uani 1 1 d . . . . .
H7 H 0.340276 0.342223 0.514734 0.051 Uiso 1 1 calc R U . . .
C8 C 0.2345(3) 0.4151(3) 0.4571(3) 0.0394(9) Uani 1 1 d . . . . .
H8 H 0.167933 0.410009 0.449606 0.047 Uiso 1 1 calc R U . . .
C9 C 0.2830(3) 0.5043(3) 0.4079(2) 0.0334(8) Uani 1 1 d . . . . .
C10 C 0.3813(3) 0.5263(3) 0.4173(3) 0.0465(10) Uani 1 1 d . . . . .
H10 H 0.417653 0.480487 0.454676 0.056 Uiso 1 1 calc R U . . .
C11 C 0.4264(3) 0.6132(3) 0.3735(3) 0.0530(12) Uani 1 1 d . . . . .
H11 H 0.492378 0.625245 0.381014 0.064 Uiso 1 1 calc R U . . .
C12 C 0.3735(3) 0.6831(3) 0.3179(3) 0.0553(12) Uani 1 1 d . . . . .
H12 H 0.403414 0.743289 0.289141 0.066 Uiso 1 1 calc R U . . .
C13 C 0.2773(3) 0.6629(3) 0.3058(3) 0.0494(11) Uani 1 1 d . . . . .
H13 H 0.241735 0.708408 0.267615 0.059 Uiso 1 1 calc R U . . .
C14 C 0.2324(3) 0.5749(3) 0.3504(2) 0.0375(9) Uani 1 1 d . . . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
Br1 C1 1.892(4) . ?
Br2 C14 1.897(4) . ?
C1 C2 1.382(5) . ?
C1 C6 1.396(5) . ?
C2 C3 1.371(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.406(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.459(5) . ?
C7 C8 1.304(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.453(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.392(5) . ?
C9 C14 1.395(5) . ?
C10 C11 1.372(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.387(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.365(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.386(5) . ?
C13 H13 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
C2 C1 C6 122.4(4) . . ?
C2 C1 Br1 116.8(3) . . ?
C6 C1 Br1 120.8(3) . . ?
C3 C2 C1 119.3(4) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 120.1(4) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.5(4) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 121.4(4) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 116.2(3) . . ?
C1 C6 C7 123.0(4) . . ?
C5 C6 C7 120.7(3) . . ?
C8 C7 C6 127.4(4) . . ?
C8 C7 H7 116.3 . . ?
C6 C7 H7 116.3 . . ?
C7 C8 C9 127.8(4) . . ?
C7 C8 H8 116.1 . . ?
C9 C8 H8 116.1 . . ?
C10 C9 C14 116.3(3) . . ?
C10 C9 C8 122.2(3) . . ?
C14 C9 C8 121.4(3) . . ?
C11 C10 C9 122.3(4) . . ?
C11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C10 C11 C12 119.8(4) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 120.2(4) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C9 121.8(4) . . ?
C13 C14 Br2 116.8(3) . . ?
C9 C14 Br2 121.3(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.6(6) . . . . ?
Br1 C1 C2 C3 179.0(3) . . . . ?
C1 C2 C3 C4 -0.3(6) . . . . ?
C2 C3 C4 C5 0.7(6) . . . . ?
C3 C4 C5 C6 -0.2(6) . . . . ?
C2 C1 C6 C5 1.1(5) . . . . ?
Br1 C1 C6 C5 -178.5(3) . . . . ?
C2 C1 C6 C7 179.8(3) . . . . ?
Br1 C1 C6 C7 0.2(5) . . . . ?
C4 C5 C6 C1 -0.7(6) . . . . ?
C4 C5 C6 C7 -179.4(4) . . . . ?
C1 C6 C7 C8 161.7(4) . . . . ?
C5 C6 C7 C8 -19.7(6) . . . . ?
C6 C7 C8 C9 175.2(4) . . . . ?
C7 C8 C9 C10 -4.3(6) . . . . ?
C7 C8 C9 C14 177.6(4) . . . . ?
C14 C9 C10 C11 0.7(6) . . . . ?
C8 C9 C10 C11 -177.5(4) . . . . ?
C9 C10 C11 C12 0.4(6) . . . . ?
C10 C11 C12 C13 -1.5(6) . . . . ?
C11 C12 C13 C14 1.5(6) . . . . ?
C12 C13 C14 C9 -0.3(6) . . . . ?
C12 C13 C14 Br2 -178.7(3) . . . . ?
C10 C9 C14 C13 -0.7(5) . . . . ?
C8 C9 C14 C13 177.4(3) . . . . ?
C10 C9 C14 Br2 177.5(3) . . . . ?
C8 C9 C14 Br2 -4.3(5) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_TC1002F1_2
_database_code_depnum_ccdc_archive 'CCDC 2322682'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-02-19 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 14 fevrier 2017                                          #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H10 Br2'
_chemical_formula_sum            'C14 H10 Br2'
_chemical_formula_weight         338.04
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.6067(17)
_cell_length_b                   14.7909(18)
_cell_length_c                   11.1941(15)
_cell_angle_alpha                90
_cell_angle_beta                 108.258(5)
_cell_angle_gamma                90
_cell_volume                     2453.9(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8920
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      27.48
_cell_measurement_wavelength     0.71073


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0063251
_diffrn_orient_matrix_UB_21      0.0935050
_diffrn_orient_matrix_UB_31      0.0081079
_diffrn_orient_matrix_UB_12      0.0487673
_diffrn_orient_matrix_UB_22      -0.0007610
_diffrn_orient_matrix_UB_32      0.0468204
_diffrn_orient_matrix_UB_13      0.0427479
_diffrn_orient_matrix_UB_23      0.0279789
_diffrn_orient_matrix_UB_33      -0.0440707


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.470
_exptl_crystal_size_min          0.310
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1312
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    6.575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.060
_exptl_absorpt_correction_T_max  0.130

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software               : BIS V6.2.1/2016-03-01                             #
# Number of scans :  2                                                       #
# Option          : shutterless mode                                         #
#                                                                            #
#     Scan  Time(s)  Width  DX (mm)  Frames   Theta   Omega     Phi     Chi  #
#  1 Phi        8.0   1.00     34.0     232    0.27  270.94  156.00   23.00  #
#  2 Fast       1.0   1.00     34.0     180    0.00  360.00    0.00   54.74  #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 7.39
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0588
_diffrn_reflns_av_r_equivalents  0.0578
_diffrn_reflns_number            23663
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.359
_diffrn_reflns_theta_max         27.569
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_reflns_number_total             5644
_reflns_number_gt                4522
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2014_4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2023)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0097P)²+2.8881P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5644
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0810
_refine_ls_wR_factor_gt          0.0744
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.116

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Br1 Br 0.38705(2) 0.33886(2) 0.60917(3) 0.02722(9) Uani 1 1 d . . . . .
Br2 Br 0.75847(2) 0.65380(2) 0.79638(3) 0.02577(9) Uani 1 1 d . . . . .
C1 C 0.48548(18) 0.3514(2) 0.5430(3) 0.0150(6) Uani 1 1 d . . . . .
C2 C 0.48351(19) 0.2987(2) 0.4399(3) 0.0192(6) Uani 1 1 d . . . . .
H2 H 0.434999 0.258137 0.404585 0.023 Uiso 1 1 calc R U . . .
C3 C 0.55361(19) 0.3063(2) 0.3890(3) 0.0199(6) Uani 1 1 d . . . . .
H3 H 0.553574 0.270702 0.318350 0.024 Uiso 1 1 calc R U . . .
C4 C 0.62391(19) 0.3663(2) 0.4417(3) 0.0203(6) Uani 1 1 d . . . . .
H4 H 0.671943 0.371496 0.406873 0.024 Uiso 1 1 calc R U . . .
C5 C 0.62432(18) 0.4184(2) 0.5446(3) 0.0166(6) Uani 1 1 d . . . . .
H5 H 0.672655 0.459403 0.579002 0.020 Uiso 1 1 calc R U . . .
C6 C 0.55485(18) 0.41210(19) 0.5992(3) 0.0141(6) Uani 1 1 d . . . . .
C7 C 0.55268(19) 0.4721(2) 0.7032(3) 0.0164(6) Uani 1 1 d . . . . .
H7 H 0.494874 0.493008 0.702156 0.020 Uiso 1 1 calc R U . . .
C8 C 0.62254(19) 0.5005(2) 0.7986(3) 0.0180(6) Uani 1 1 d . . . . .
H8 H 0.610154 0.545398 0.851656 0.022 Uiso 1 1 calc R U . . .
C9 C 0.71727(18) 0.4698(2) 0.8309(3) 0.0150(6) Uani 1 1 d . . . . .
C10 C 0.7405(2) 0.3801(2) 0.8614(3) 0.0209(6) Uani 1 1 d . . . . .
H10 H 0.694467 0.337162 0.857987 0.025 Uiso 1 1 calc R U . . .
C11 C 0.8304(2) 0.3520(2) 0.8969(3) 0.0255(7) Uani 1 1 d . . . . .
H11 H 0.845300 0.290444 0.917827 0.031 Uiso 1 1 calc R U . . .
C12 C 0.8975(2) 0.4137(2) 0.9014(3) 0.0255(7) Uani 1 1 d . . . . .
H12 H 0.958584 0.394280 0.925588 0.031 Uiso 1 1 calc R U . . .
C13 C 0.87712(19) 0.5034(2) 0.8714(3) 0.0221(7) Uani 1 1 d . . . . .
H13 H 0.923463 0.545718 0.873960 0.026 Uiso 1 1 calc R U . . .
C14 C 0.78735(19) 0.5305(2) 0.8372(3) 0.0161(6) Uani 1 1 d . . . . .
Br11 Br 0.73228(2) 0.63667(2) 0.14185(4) 0.02886(10) Uani 1 1 d . . . . .
Br12 Br 1.11193(2) 0.33138(2) 0.42239(3) 0.02786(9) Uani 1 1 d . . . . .
C21 C 0.7073(2) 0.51147(19) 0.1492(3) 0.0163(6) Uani 1 1 d . . . . .
C22 C 0.61771(19) 0.4841(2) 0.1181(3) 0.0200(6) Uani 1 1 d . . . . .
H22 H 0.570516 0.527536 0.097336 0.024 Uiso 1 1 calc R U . . .
C23 C 0.5982(2) 0.3934(2) 0.1177(3) 0.0208(6) Uani 1 1 d . . . . .
H23 H 0.537179 0.374028 0.095238 0.025 Uiso 1 1 calc R U . . .
C24 C 0.6674(2) 0.3298(2) 0.1500(3) 0.0199(6) Uani 1 1 d . . . . .
H24 H 0.653799 0.267213 0.149578 0.024 Uiso 1 1 calc R U . . .
C25 C 0.7563(2) 0.3587(2) 0.1827(3) 0.0176(6) Uani 1 1 d . . . . .
H25 H 0.803215 0.314978 0.205142 0.021 Uiso 1 1 calc R U . . .
C26 C 0.77876(18) 0.4502(2) 0.1837(3) 0.0148(6) Uani 1 1 d . . . . .
C27 C 0.87338(19) 0.4799(2) 0.2129(3) 0.0173(6) Uani 1 1 d . . . . .
H27 H 0.886049 0.519785 0.154111 0.021 Uiso 1 1 calc R U . . .
C28 C 0.94330(18) 0.4571(2) 0.3126(3) 0.0170(6) Uani 1 1 d . . . . .
H28 H 1.000770 0.477721 0.311818 0.020 Uiso 1 1 calc R U . . .
C29 C 0.94235(18) 0.40418(19) 0.4232(3) 0.0147(6) Uani 1 1 d . . . . .
C30 C 0.87275(18) 0.4142(2) 0.4779(3) 0.0170(6) Uani 1 1 d . . . . .
H30 H 0.823788 0.453614 0.439408 0.020 Uiso 1 1 calc R U . . .
C31 C 0.87394(19) 0.3683(2) 0.5861(3) 0.0192(6) Uani 1 1 d . . . . .
H31 H 0.825801 0.375766 0.620237 0.023 Uiso 1 1 calc R U . . .
C32 C 0.9456(2) 0.3112(2) 0.6449(3) 0.0204(6) Uani 1 1 d . . . . .
H32 H 0.946418 0.279551 0.719115 0.024 Uiso 1 1 calc R U . . .
C33 C 1.01599(19) 0.3006(2) 0.5950(3) 0.0198(6) Uani 1 1 d . . . . .
H33 H 1.065408 0.262105 0.634800 0.024 Uiso 1 1 calc R U . . .
C34 C 1.01312(18) 0.3469(2) 0.4863(3) 0.0163(6) Uani 1 1 d . . . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
Br1 C1 1.912(3) . ?
Br2 C14 1.900(3) . ?
C1 C2 1.385(4) . ?
C1 C6 1.395(4) . ?
C2 C3 1.387(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.405(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.473(4) . ?
C7 C8 1.333(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.479(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.390(4) . ?
C9 C14 1.399(4) . ?
C10 C11 1.397(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.378(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.382(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(4) . ?
C13 H13 0.9500 . ?
Br11 C21 1.900(3) . ?
Br12 C34 1.906(3) . ?
C21 C22 1.391(4) . ?
C21 C26 1.395(4) . ?
C22 C23 1.375(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.391(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.387(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.397(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.476(4) . ?
C27 C28 1.336(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.469(4) . ?
C28 H28 0.9500 . ?
C29 C34 1.395(4) . ?
C29 C30 1.412(4) . ?
C30 C31 1.383(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.392(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.389(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.385(4) . ?
C33 H33 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 123.3(3) . . ?
C2 C1 Br1 117.2(2) . . ?
C6 C1 Br1 119.5(2) . . ?
C1 C2 C3 118.8(3) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 121.5(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 116.2(3) . . ?
C1 C6 C7 122.5(3) . . ?
C5 C6 C7 121.1(3) . . ?
C8 C7 C6 127.4(3) . . ?
C8 C7 H7 116.3 . . ?
C6 C7 H7 116.3 . . ?
C7 C8 C9 127.1(3) . . ?
C7 C8 H8 116.4 . . ?
C9 C8 H8 116.4 . . ?
C10 C9 C14 117.4(3) . . ?
C10 C9 C8 121.1(3) . . ?
C14 C9 C8 121.4(3) . . ?
C9 C10 C11 121.0(3) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 120.9(3) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C14 118.6(3) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
C13 C14 C9 122.2(3) . . ?
C13 C14 Br2 119.0(2) . . ?
C9 C14 Br2 118.7(2) . . ?
C22 C21 C26 122.3(3) . . ?
C22 C21 Br11 118.5(2) . . ?
C26 C21 Br11 119.2(2) . . ?
C23 C22 C21 119.3(3) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 120.4(3) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C25 C24 C23 119.4(3) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 121.9(3) . . ?
C24 C25 H25 119.1 . . ?
C26 C25 H25 119.1 . . ?
C21 C26 C25 116.8(3) . . ?
C21 C26 C27 121.7(3) . . ?
C25 C26 C27 121.4(3) . . ?
C28 C27 C26 127.5(3) . . ?
C28 C27 H27 116.3 . . ?
C26 C27 H27 116.3 . . ?
C27 C28 C29 128.1(3) . . ?
C27 C28 H28 116.0 . . ?
C29 C28 H28 116.0 . . ?
C34 C29 C30 116.0(3) . . ?
C34 C29 C28 122.3(3) . . ?
C30 C29 C28 121.4(3) . . ?
C31 C30 C29 121.8(3) . . ?
C31 C30 H30 119.1 . . ?
C29 C30 H30 119.1 . . ?
C30 C31 C32 120.0(3) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C33 C32 C31 119.9(3) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C34 C33 C32 119.1(3) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C29 123.2(3) . . ?
C33 C34 Br12 117.6(2) . . ?
C29 C34 Br12 119.3(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.2(5) . . . . ?
Br1 C1 C2 C3 179.7(2) . . . . ?
C1 C2 C3 C4 -0.1(5) . . . . ?
C2 C3 C4 C5 0.0(5) . . . . ?
C3 C4 C5 C6 0.5(5) . . . . ?
C2 C1 C6 C5 0.6(4) . . . . ?
Br1 C1 C6 C5 -179.3(2) . . . . ?
C2 C1 C6 C7 175.6(3) . . . . ?
Br1 C1 C6 C7 -4.3(4) . . . . ?
C4 C5 C6 C1 -0.8(4) . . . . ?
C4 C5 C6 C7 -175.8(3) . . . . ?
C1 C6 C7 C8 147.0(3) . . . . ?
C5 C6 C7 C8 -38.2(5) . . . . ?
C6 C7 C8 C9 -8.0(5) . . . . ?
C7 C8 C9 C10 -61.0(4) . . . . ?
C7 C8 C9 C14 121.8(4) . . . . ?
C14 C9 C10 C11 0.0(5) . . . . ?
C8 C9 C10 C11 -177.3(3) . . . . ?
C9 C10 C11 C12 -0.3(5) . . . . ?
C10 C11 C12 C13 0.0(5) . . . . ?
C11 C12 C13 C14 0.5(5) . . . . ?
C12 C13 C14 C9 -0.8(5) . . . . ?
C12 C13 C14 Br2 179.7(2) . . . . ?
C10 C9 C14 C13 0.5(4) . . . . ?
C8 C9 C14 C13 177.9(3) . . . . ?
C10 C9 C14 Br2 -180.0(2) . . . . ?
C8 C9 C14 Br2 -2.6(4) . . . . ?
C26 C21 C22 C23 -1.8(5) . . . . ?
Br11 C21 C22 C23 177.2(2) . . . . ?
C21 C22 C23 C24 1.0(5) . . . . ?
C22 C23 C24 C25 0.1(5) . . . . ?
C23 C24 C25 C26 -0.4(5) . . . . ?
C22 C21 C26 C25 1.5(4) . . . . ?
Br11 C21 C26 C25 -177.5(2) . . . . ?
C22 C21 C26 C27 178.2(3) . . . . ?
Br11 C21 C26 C27 -0.9(4) . . . . ?
C24 C25 C26 C21 -0.4(4) . . . . ?
C24 C25 C26 C27 -177.1(3) . . . . ?
C21 C26 C27 C28 131.6(3) . . . . ?
C25 C26 C27 C28 -51.9(5) . . . . ?
C26 C27 C28 C29 -6.3(5) . . . . ?
C27 C28 C29 C34 146.6(3) . . . . ?
C27 C28 C29 C30 -38.7(5) . . . . ?
C34 C29 C30 C31 -1.4(4) . . . . ?
C28 C29 C30 C31 -176.4(3) . . . . ?
C29 C30 C31 C32 0.8(5) . . . . ?
C30 C31 C32 C33 0.1(5) . . . . ?
C31 C32 C33 C34 -0.4(5) . . . . ?
C32 C33 C34 C29 -0.2(5) . . . . ?
C32 C33 C34 Br12 179.3(2) . . . . ?
C30 C29 C34 C33 1.1(4) . . . . ?
C28 C29 C34 C33 176.1(3) . . . . ?
C30 C29 C34 Br12 -178.4(2) . . . . ?
C28 C29 C34 Br12 -3.4(4) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_TC1047
_database_code_depnum_ccdc_archive 'CCDC 1894663'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-02-19 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 01 septembre 2017                                        #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C46 H62 N6 Zr2'
_chemical_formula_sum            'C46 H62 N6 Zr2'
_chemical_formula_weight         881.45
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0140(7)
_cell_length_b                   9.0810(9)
_cell_length_c                   17.2090(16)
_cell_angle_alpha                80.724(3)
_cell_angle_beta                 78.474(3)
_cell_angle_gamma                64.123(3)
_cell_volume                     1100.20(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9717
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      27.53
_cell_measurement_wavelength     0.71073


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0600232
_diffrn_orient_matrix_UB_21      -0.0336997
_diffrn_orient_matrix_UB_31      0.1221205
_diffrn_orient_matrix_UB_12      0.1123865
_diffrn_orient_matrix_UB_22      -0.0466940
_diffrn_orient_matrix_UB_32      -0.0165845
_diffrn_orient_matrix_UB_13      0.0192860
_diffrn_orient_matrix_UB_23      0.0543965
_diffrn_orient_matrix_UB_33      0.0145295


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.270
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             460
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_T_max  0.871

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.1/2016-03-01                           #
# Number of scans            :  4                                              #
# Total length of scans  [*] :   552.00 (deg.)                                 #
# Total number of frames [*] :      552                                        #
#  [*] fast scan not included                                                  #
# Option                       : shutterless mode                              #
#                                                                              #
#     Scan Time(s)  Width  DX (mm)  Frames  Theta  Omega    Phi    Chi   T(K)  #
#  1 Phi       5.0   1.00     34.0     360   0.27 270.94 360.00  23.00 149.99  #
#  2 Omega     5.0   1.00     34.0      96   0.27   3.16 144.00 315.50 150.00  #
#  3 Omega     5.0   1.00     34.0      96   0.27   3.16   0.00 315.50 150.00  #
#  4 Fast      1.0   1.00     50.0     180   0.00 360.00   0.00  54.74 150.00  #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 7.39
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0193
_diffrn_reflns_av_r_equivalents  0.0271
_diffrn_reflns_number            26280
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.502
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             5066
_reflns_number_gt                4793
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2014_4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2023)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0234P)²+0.5973P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5066
_refine_ls_number_parameters     251
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0221
_refine_ls_wR_factor_ref         0.0567
_refine_ls_wR_factor_gt          0.0558
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.055

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.51794(2) 0.81723(2) 0.68894(2) 0.01381(5) Uani 1 1 d . . . . .
N1 N 0.72268(17) 0.67987(16) 0.75919(8) 0.0218(3) Uani 1 1 d . . . . .
N2 N 0.65253(19) 0.72946(17) 0.58075(8) 0.0239(3) Uani 1 1 d . . . . .
N3 N 0.51064(17) 1.04844(15) 0.68105(7) 0.0184(2) Uani 1 1 d . . . . .
C1 C 0.0526(2) 0.52537(18) 0.97063(8) 0.0186(3) Uani 1 1 d . . . . .
H1 H -0.003767 0.635639 0.948521 0.022 Uiso 1 1 calc R U . . .
C2 C 0.2477(2) 0.42591(18) 0.93720(8) 0.0172(3) Uani 1 1 d . . . . .
C3 C 0.3280(2) 0.25422(19) 0.95179(9) 0.0221(3) Uani 1 1 d . . . . .
H3 H 0.255810 0.202478 0.985161 0.027 Uiso 1 1 calc R U . . .
C4 C 0.5087(2) 0.15845(19) 0.91903(9) 0.0241(3) Uani 1 1 d . . . . .
H4 H 0.559500 0.042533 0.930128 0.029 Uiso 1 1 calc R U . . .
C5 C 0.6163(2) 0.2316(2) 0.86981(9) 0.0236(3) Uani 1 1 d . . . . .
H5 H 0.741088 0.166297 0.847376 0.028 Uiso 1 1 calc R U . . .
C6 C 0.5401(2) 0.40106(19) 0.85370(9) 0.0216(3) Uani 1 1 d . . . . .
H6 H 0.612932 0.450900 0.819308 0.026 Uiso 1 1 calc R U . . .
C7 C 0.3579(2) 0.49960(17) 0.88718(8) 0.0170(3) Uani 1 1 d . . . . .
C8 C 0.2855(2) 0.68102(18) 0.86964(8) 0.0175(3) Uani 1 1 d . . . . .
C9 C 0.2361(2) 0.7849(2) 0.92851(9) 0.0239(3) Uani 1 1 d . . . . .
H9 H 0.249220 0.739484 0.981849 0.029 Uiso 1 1 calc R U . . .
C10 C 0.1665(2) 0.9571(2) 0.91192(10) 0.0265(3) Uani 1 1 d . . . . .
H10 H 0.137141 1.023987 0.954182 0.032 Uiso 1 1 calc R U . . .
C11 C 0.1403(2) 1.03006(18) 0.83673(10) 0.0228(3) Uani 1 1 d . . . . .
H11 H 0.095069 1.145938 0.826546 0.027 Uiso 1 1 calc R U . . .
C12 C 0.18186(19) 0.92925(17) 0.77404(9) 0.0175(3) Uani 1 1 d . . . . .
C13 C 0.1590(2) 0.96381(18) 0.69152(9) 0.0207(3) Uani 1 1 d . . . . .
H13 H 0.113584 1.069786 0.663742 0.025 Uiso 1 1 calc R U . . .
C14 C 0.2152(2) 0.81392(19) 0.65864(9) 0.0211(3) Uani 1 1 d . . . . .
C15 C 0.2893(2) 0.68359(18) 0.71722(9) 0.0177(3) Uani 1 1 d . . . . .
H15 H 0.347880 0.569819 0.709339 0.021 Uiso 1 1 calc R U . . .
C16 C 0.26055(18) 0.75345(17) 0.79045(8) 0.0153(3) Uani 1 1 d . . . . .
C17 C 0.1973(3) 0.7944(2) 0.57599(10) 0.0321(4) Uani 1 1 d . . . . .
H17A H 0.132245 0.902931 0.548896 0.048 Uiso 1 1 calc R U . . .
H17B H 0.125495 0.729172 0.579025 0.048 Uiso 1 1 calc R U . . .
H17C H 0.322364 0.738522 0.546165 0.048 Uiso 1 1 calc R U . . .
C21 C 0.6966(3) 0.7344(2) 0.83743(11) 0.0331(4) Uani 1 1 d . . . . .
H21A H 0.704359 0.643603 0.878128 0.050 Uiso 1 1 calc R U . . .
H21B H 0.573358 0.826412 0.847044 0.050 Uiso 1 1 calc R U . . .
H21C H 0.794615 0.769844 0.839867 0.050 Uiso 1 1 calc R U . . .
C22 C 0.9038(2) 0.5439(2) 0.74200(13) 0.0368(4) Uani 1 1 d . . . . .
H22A H 1.003259 0.577831 0.744108 0.055 Uiso 1 1 calc R U . . .
H22B H 0.917338 0.511100 0.688758 0.055 Uiso 1 1 calc R U . . .
H22C H 0.913335 0.450972 0.781516 0.055 Uiso 1 1 calc R U . . .
C23 C 0.6910(3) 0.5650(2) 0.56393(14) 0.0452(5) Uani 1 1 d . . . . .
H23A H 0.627606 0.571885 0.519433 0.068 Uiso 1 1 calc R U . . .
H23B H 0.644866 0.509583 0.611142 0.068 Uiso 1 1 calc R U . . .
H23C H 0.826442 0.502543 0.549857 0.068 Uiso 1 1 calc R U . . .
C24 C 0.7182(3) 0.8159(2) 0.51160(10) 0.0341(4) Uani 1 1 d . . . . .
H24A H 0.852577 0.752393 0.495198 0.051 Uiso 1 1 calc R U . . .
H24B H 0.696662 0.924147 0.525194 0.051 Uiso 1 1 calc R U . . .
H24C H 0.649713 0.829380 0.467843 0.051 Uiso 1 1 calc R U . . .
C25 C 0.6989(2) 1.0423(2) 0.67216(10) 0.0277(3) Uani 1 1 d . . . . .
H25A H 0.719343 1.109908 0.623995 0.042 Uiso 1 1 calc R U . . .
H25B H 0.792050 0.928488 0.667889 0.042 Uiso 1 1 calc R U . . .
H25C H 0.711294 1.084456 0.718658 0.042 Uiso 1 1 calc R U . . .
C26 C 0.3723(2) 1.21642(19) 0.69107(10) 0.0252(3) Uani 1 1 d . . . . .
H26A H 0.380373 1.250743 0.740828 0.038 Uiso 1 1 calc R U . . .
H26B H 0.246530 1.222352 0.692892 0.038 Uiso 1 1 calc R U . . .
H26C H 0.396860 1.289291 0.646227 0.038 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 N2 2.0470(13) . ?
Zr1 N1 2.0566(13) . ?
Zr1 N3 2.0578(12) . ?
Zr1 C15 2.5416(14) . ?
Zr1 C13 2.5837(15) . ?
Zr1 C14 2.5949(15) . ?
Zr1 C16 2.6302(13) . ?
Zr1 C12 2.6355(14) . ?
N1 C22 1.449(2) . ?
N1 C21 1.454(2) . ?
N2 C23 1.453(2) . ?
N2 C24 1.456(2) . ?
N3 C26 1.4554(19) . ?
N3 C25 1.463(2) . ?
C1 C1 1.340(3) 2_567 ?
C1 C2 1.472(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.404(2) . ?
C2 C7 1.4125(19) . ?
C3 C4 1.380(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.398(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.4890(19) . ?
C8 C9 1.377(2) . ?
C8 C16 1.427(2) . ?
C9 C10 1.413(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.367(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.422(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.435(2) . ?
C12 C16 1.4397(19) . ?
C13 C14 1.410(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.418(2) . ?
C14 C17 1.503(2) . ?
C15 C16 1.434(2) . ?
C15 H15 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Zr1 N1 100.61(5) . . ?
N2 Zr1 N3 105.07(5) . . ?
N1 Zr1 N3 103.19(5) . . ?
N2 Zr1 C15 98.41(5) . . ?
N1 Zr1 C15 105.45(5) . . ?
N3 Zr1 C15 138.54(5) . . ?
N2 Zr1 C13 111.57(5) . . ?
N1 Zr1 C13 142.89(5) . . ?
N3 Zr1 C13 86.22(5) . . ?
C15 Zr1 C13 53.18(5) . . ?
N2 Zr1 C14 89.20(5) . . ?
N1 Zr1 C14 137.47(5) . . ?
N3 Zr1 C14 114.06(5) . . ?
C15 Zr1 C14 32.03(5) . . ?
C13 Zr1 C14 31.59(5) . . ?
N2 Zr1 C16 130.23(5) . . ?
N1 Zr1 C16 92.46(5) . . ?
N3 Zr1 C16 118.33(5) . . ?
C15 Zr1 C16 32.15(4) . . ?
C13 Zr1 C16 52.71(5) . . ?
C14 Zr1 C16 52.45(5) . . ?
N2 Zr1 C12 141.17(5) . . ?
N1 Zr1 C12 111.53(5) . . ?
N3 Zr1 C12 88.63(5) . . ?
C15 Zr1 C12 53.11(5) . . ?
C13 Zr1 C12 31.90(5) . . ?
C14 Zr1 C12 52.36(5) . . ?
C16 Zr1 C12 31.73(4) . . ?
C22 N1 C21 111.57(14) . . ?
C22 N1 Zr1 131.18(12) . . ?
C21 N1 Zr1 116.90(10) . . ?
C23 N2 C24 110.97(14) . . ?
C23 N2 Zr1 121.63(12) . . ?
C24 N2 Zr1 127.39(11) . . ?
C26 N3 C25 109.36(12) . . ?
C26 N3 Zr1 138.49(10) . . ?
C25 N3 Zr1 111.64(10) . . ?
C1 C1 C2 125.95(17) 2_567 . ?
C1 C1 H1 117.0 2_567 . ?
C2 C1 H1 117.0 . . ?
C3 C2 C7 117.88(13) . . ?
C3 C2 C1 121.02(13) . . ?
C7 C2 C1 121.06(13) . . ?
C4 C3 C2 121.88(14) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 119.97(14) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.44(14) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C7 121.16(14) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C6 C7 C2 119.66(13) . . ?
C6 C7 C8 118.78(12) . . ?
C2 C7 C8 121.56(13) . . ?
C9 C8 C16 117.59(13) . . ?
C9 C8 C7 121.93(13) . . ?
C16 C8 C7 120.47(13) . . ?
C8 C9 C10 121.93(15) . . ?
C8 C9 H9 119.0 . . ?
C10 C9 H9 119.0 . . ?
C11 C10 C9 121.79(14) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C10 C11 C12 118.74(14) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C11 C12 C13 133.42(14) . . ?
C11 C12 C16 119.30(13) . . ?
C13 C12 C16 107.26(13) . . ?
C11 C12 Zr1 120.47(10) . . ?
C13 C12 Zr1 72.06(8) . . ?
C16 C12 Zr1 73.93(7) . . ?
C14 C13 C12 108.45(13) . . ?
C14 C13 Zr1 74.64(8) . . ?
C12 C13 Zr1 76.04(8) . . ?
C14 C13 H13 125.8 . . ?
C12 C13 H13 125.8 . . ?
Zr1 C13 H13 115.6 . . ?
C13 C14 C15 108.46(13) . . ?
C13 C14 C17 126.07(14) . . ?
C15 C14 C17 125.46(15) . . ?
C13 C14 Zr1 73.77(8) . . ?
C15 C14 Zr1 71.91(8) . . ?
C17 C14 Zr1 121.03(11) . . ?
C14 C15 C16 108.10(13) . . ?
C14 C15 Zr1 76.05(8) . . ?
C16 C15 Zr1 77.33(8) . . ?
C14 C15 H15 125.9 . . ?
C16 C15 H15 126.0 . . ?
Zr1 C15 H15 113.1 . . ?
C8 C16 C15 131.98(13) . . ?
C8 C16 C12 120.52(13) . . ?
C15 C16 C12 107.38(12) . . ?
C8 C16 Zr1 123.79(9) . . ?
C15 C16 Zr1 70.52(8) . . ?
C12 C16 Zr1 74.34(8) . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C21 H21A 109.5 . . ?
N1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N1 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N2 C23 H23A 109.5 . . ?
N2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C24 H24A 109.5 . . ?
N2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 H26A 109.5 . . ?
N3 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N3 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1 C2 C3 15.3(3) 2_567 . . . ?
C1 C1 C2 C7 -166.92(18) 2_567 . . . ?
C7 C2 C3 C4 0.2(2) . . . . ?
C1 C2 C3 C4 178.01(14) . . . . ?
C2 C3 C4 C5 -0.2(2) . . . . ?
C3 C4 C5 C6 -0.4(2) . . . . ?
C4 C5 C6 C7 1.1(2) . . . . ?
C5 C6 C7 C2 -1.1(2) . . . . ?
C5 C6 C7 C8 178.24(14) . . . . ?
C3 C2 C7 C6 0.5(2) . . . . ?
C1 C2 C7 C6 -177.32(13) . . . . ?
C3 C2 C7 C8 -178.86(13) . . . . ?
C1 C2 C7 C8 3.3(2) . . . . ?
C6 C7 C8 C9 -117.13(16) . . . . ?
C2 C7 C8 C9 62.2(2) . . . . ?
C6 C7 C8 C16 64.44(19) . . . . ?
C2 C7 C8 C16 -116.19(15) . . . . ?
C16 C8 C9 C10 -1.2(2) . . . . ?
C7 C8 C9 C10 -179.68(14) . . . . ?
C8 C9 C10 C11 1.6(3) . . . . ?
C9 C10 C11 C12 0.9(2) . . . . ?
C10 C11 C12 C13 174.83(15) . . . . ?
C10 C11 C12 C16 -3.6(2) . . . . ?
C10 C11 C12 Zr1 -91.46(15) . . . . ?
C11 C12 C13 C14 -176.45(15) . . . . ?
C16 C12 C13 C14 2.16(16) . . . . ?
Zr1 C12 C13 C14 68.25(10) . . . . ?
C11 C12 C13 Zr1 115.30(16) . . . . ?
C16 C12 C13 Zr1 -66.09(9) . . . . ?
C12 C13 C14 C15 -5.17(16) . . . . ?
Zr1 C13 C14 C15 64.02(10) . . . . ?
C12 C13 C14 C17 173.93(14) . . . . ?
Zr1 C13 C14 C17 -116.88(15) . . . . ?
C12 C13 C14 Zr1 -69.19(10) . . . . ?
C13 C14 C15 C16 6.18(16) . . . . ?
C17 C14 C15 C16 -172.93(14) . . . . ?
Zr1 C14 C15 C16 71.40(10) . . . . ?
C13 C14 C15 Zr1 -65.23(10) . . . . ?
C17 C14 C15 Zr1 115.67(15) . . . . ?
C9 C8 C16 C15 -177.00(14) . . . . ?
C7 C8 C16 C15 1.5(2) . . . . ?
C9 C8 C16 C12 -1.6(2) . . . . ?
C7 C8 C16 C12 176.92(12) . . . . ?
C9 C8 C16 Zr1 89.42(15) . . . . ?
C7 C8 C16 Zr1 -92.09(14) . . . . ?
C14 C15 C16 C8 171.09(14) . . . . ?
Zr1 C15 C16 C8 -118.39(15) . . . . ?
C14 C15 C16 C12 -4.78(15) . . . . ?
Zr1 C15 C16 C12 65.75(9) . . . . ?
C14 C15 C16 Zr1 -70.53(10) . . . . ?
C11 C12 C16 C8 4.0(2) . . . . ?
C13 C12 C16 C8 -174.81(12) . . . . ?
Zr1 C12 C16 C8 120.35(12) . . . . ?
C11 C12 C16 C15 -179.54(12) . . . . ?
C13 C12 C16 C15 1.62(15) . . . . ?
Zr1 C12 C16 C15 -63.22(9) . . . . ?
C11 C12 C16 Zr1 -116.32(12) . . . . ?
C13 C12 C16 Zr1 64.84(9) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_NR2055
_database_code_depnum_ccdc_archive 'CCDC 2322680'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-02-19 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 08 avril 2016                                            #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H10 Br2'
_chemical_formula_sum            'C14 H10 Br2'
_chemical_formula_weight         338.04
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.7654(17)
_cell_length_b                   3.9608(7)
_cell_length_c                   15.486(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.132(6)
_cell_angle_gamma                90
_cell_volume                     598.09(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4249
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      27.45
_cell_measurement_wavelength     0.71073


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0087424
_diffrn_orient_matrix_UB_21      -0.1016833
_diffrn_orient_matrix_UB_31      0.0100796
_diffrn_orient_matrix_UB_12      -0.2479158
_diffrn_orient_matrix_UB_22      0.0168853
_diffrn_orient_matrix_UB_32      -0.0446857
_diffrn_orient_matrix_UB_13      0.0106062
_diffrn_orient_matrix_UB_23      -0.0107091
_diffrn_orient_matrix_UB_33      -0.0628900


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             328
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    6.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.076
_exptl_absorpt_correction_T_max  0.260

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software              : BIS 4.2.9/2015-10-22                               #
# Crystal to detector distance (mm) : 34.00                                  #
#  Number of scans :  3                                                      #
#  Option          : shutterless mode                                        #
#        Scan      Time per frame (s)        Frame width (deg)    Frames     #
#           1                     3.0          1.000                 64      #
#           2                     3.0          1.000                184      #
#           3                     1.0          1.000                180      #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 7.39
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0559
_diffrn_reflns_av_r_equivalents  0.0553
_diffrn_reflns_number            5389
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.634
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_reflns_number_total             1358
_reflns_number_gt                1201
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2023)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1058P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019_2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.062(7)
_refine_ls_number_reflns         1358
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1452
_refine_ls_wR_factor_gt          0.1401
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.537
_refine_diff_density_min         -1.610
_refine_diff_density_rms         0.256

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.5593(4) 0.5798(10) 0.5038(2) 0.0179(8) Uani 1 1 d . . . . .
H1 H 0.575981 0.711787 0.554551 0.021 Uiso 1 1 calc R U . . .
C2 C 0.6681(4) 0.5746(9) 0.4421(2) 0.0164(8) Uani 1 1 d . . . . .
C3 C 0.7979(5) 0.7046(9) 0.4671(3) 0.0188(9) Uani 1 1 d . . . . .
H3 H 0.813636 0.796154 0.523508 0.023 Uiso 1 1 calc R U . . .
C4 C 0.9035(5) 0.7016(10) 0.4108(3) 0.0210(9) Uani 1 1 d . . . . .
H4 H 0.990816 0.789168 0.429200 0.025 Uiso 1 1 calc R U . . .
C5 C 0.8827(4) 0.5714(10) 0.3276(2) 0.0198(8) Uani 1 1 d . . . . .
H5 H 0.954678 0.568033 0.288804 0.024 Uiso 1 1 calc R U . . .
C6 C 0.7538(4) 0.4470(10) 0.3032(2) 0.0162(8) Uani 1 1 d . . . . .
C7 C 0.6476(4) 0.4431(9) 0.3577(2) 0.0153(8) Uani 1 1 d . . . . .
H7 H 0.560941 0.352767 0.338771 0.018 Uiso 1 1 calc R U . . .
Br1 Br 0.72242(4) 0.27689(11) 0.18892(2) 0.0204(3) Uani 1 1 d . . . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
C1 C1 1.319(8) 3_666 ?
C1 C2 1.468(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.403(6) . ?
C2 C7 1.411(5) . ?
C3 C4 1.386(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.373(5) . ?
C6 Br1 1.902(4) . ?
C7 H7 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C1 C2 126.7(5) 3_666 . ?
C1 C1 H1 116.6 3_666 . ?
C2 C1 H1 116.6 . . ?
C3 C2 C7 118.2(4) . . ?
C3 C2 C1 119.4(3) . . ?
C7 C2 C1 122.5(3) . . ?
C4 C3 C2 121.0(4) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 120.6(4) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 118.0(4) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C7 C6 C5 122.8(3) . . ?
C7 C6 Br1 118.7(3) . . ?
C5 C6 Br1 118.6(3) . . ?
C6 C7 C2 119.4(3) . . ?
C6 C7 H7 120.3 . . ?
C2 C7 H7 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1 C2 C3 -167.9(5) 3_666 . . . ?
C1 C1 C2 C7 12.1(7) 3_666 . . . ?
C7 C2 C3 C4 -0.6(5) . . . . ?
C1 C2 C3 C4 179.5(4) . . . . ?
C2 C3 C4 C5 0.5(6) . . . . ?
C3 C4 C5 C6 0.2(6) . . . . ?
C4 C5 C6 C7 -0.9(6) . . . . ?
C4 C5 C6 Br1 178.7(3) . . . . ?
C5 C6 C7 C2 0.9(6) . . . . ?
Br1 C6 C7 C2 -178.7(3) . . . . ?
C3 C2 C7 C6 -0.1(5) . . . . ?
C1 C2 C7 C6 179.8(4) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_TC1042
_database_code_depnum_ccdc_archive 'CCDC 2322683'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-02-19 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 04 septembre 2017                                        #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C54 H56 Cl4 Zr2'
_chemical_formula_sum            'C54 H56 Cl4 Zr2'
_chemical_formula_weight         1029.22
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

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

_cell_length_a                   9.0237(12)
_cell_length_b                   13.1611(14)
_cell_length_c                   39.397(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.514(3)
_cell_angle_gamma                90
_cell_volume                     4674.4(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9906
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      27.47
_cell_measurement_wavelength     0.71073


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      0.0415162
_diffrn_orient_matrix_UB_21      0.0382506
_diffrn_orient_matrix_UB_31      0.0954845
_diffrn_orient_matrix_UB_12      -0.0368596
_diffrn_orient_matrix_UB_22      -0.0545774
_diffrn_orient_matrix_UB_32      0.0378898
_diffrn_orient_matrix_UB_13      0.0204795
_diffrn_orient_matrix_UB_23      -0.0149541
_diffrn_orient_matrix_UB_33      -0.0016176


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2112
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_T_max  0.945

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 7.39
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0714
_diffrn_reflns_av_r_equivalents  0.0525
_diffrn_reflns_number            25050
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.192
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.960
_reflns_number_total             10377
_reflns_number_gt                9653
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SIR2004 (Burla., 2005)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  
'CRYSCALC (T. Roisnel, local program, ver. 2024)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1051P)²+126.4650P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10377
_refine_ls_number_parameters     392
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.1098
_refine_ls_wR_factor_ref         0.2907
_refine_ls_wR_factor_gt          0.2868
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.194
_refine_diff_density_min         -2.630
_refine_diff_density_rms         0.215

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 -0.15814(11) 0.30285(8) 0.10249(3) 0.0143(2) Uani 1 1 d . . . . .
Cl1 Cl -0.4064(3) 0.3551(3) 0.11654(7) 0.0245(6) Uani 1 1 d . . . . .
Cl2 Cl -0.0640(4) 0.4756(2) 0.09633(8) 0.0254(6) Uani 1 1 d . . . . .
Zr2 Zr 0.07861(12) 0.29455(8) 0.39161(3) 0.0159(2) Uani 1 1 d . . . . .
Cl3 Cl -0.1783(3) 0.3522(2) 0.38940(7) 0.0232(6) Uani 1 1 d . . . . .
Cl4 Cl 0.1989(4) 0.4598(2) 0.38921(7) 0.0253(6) Uani 1 1 d . . . . .
C1 C -0.0486(15) 0.2354(10) 0.0495(3) 0.024(3) Uani 1 1 d . . . . .
C2 C -0.1431(16) 0.3153(9) 0.0381(3) 0.023(3) Uani 1 1 d . . . . .
C3 C -0.2918(14) 0.2867(10) 0.0441(3) 0.021(2) Uani 1 1 d . . . . .
C4 C -0.2883(15) 0.1889(8) 0.0585(3) 0.020(2) Uani 1 1 d . . . . .
C5 C -0.1414(15) 0.1559(10) 0.0610(3) 0.021(2) Uani 1 1 d . . . . .
C6 C 0.1174(16) 0.2289(10) 0.0453(3) 0.0285(13) Uani 1 1 d . . . . .
H6A H 0.162207 0.295813 0.049516 0.043 Uiso 1 1 calc R U . . .
H6B H 0.136595 0.207103 0.022103 0.043 Uiso 1 1 calc R U . . .
H6C H 0.160681 0.179679 0.061533 0.043 Uiso 1 1 calc R U . . .
C7 C -0.0984(17) 0.4081(10) 0.0198(3) 0.0285(13) Uani 1 1 d . . . . .
H7A H 0.008048 0.419942 0.023982 0.043 Uiso 1 1 calc R U . . .
H7B H -0.154163 0.466560 0.027808 0.043 Uiso 1 1 calc R U . . .
H7C H -0.119499 0.398999 -0.004673 0.043 Uiso 1 1 calc R U . . .
C8 C -0.4252(16) 0.3479(10) 0.0330(3) 0.0285(13) Uani 1 1 d . . . . .
H8A H -0.413153 0.417941 0.041051 0.043 Uiso 1 1 calc R U . . .
H8B H -0.514040 0.318144 0.042412 0.043 Uiso 1 1 calc R U . . .
H8C H -0.435749 0.347602 0.008095 0.043 Uiso 1 1 calc R U . . .
C9 C -0.4234(16) 0.1299(10) 0.0672(3) 0.0285(13) Uani 1 1 d . . . . .
H9A H -0.393693 0.062677 0.075774 0.043 Uiso 1 1 calc R U . . .
H9B H -0.488597 0.121999 0.046790 0.043 Uiso 1 1 calc R U . . .
H9C H -0.476446 0.166258 0.084644 0.043 Uiso 1 1 calc R U . . .
C10 C -0.0927(16) 0.0481(10) 0.0675(3) 0.0285(13) Uani 1 1 d . . . . .
H10A H -0.176071 0.008532 0.075597 0.043 Uiso 1 1 calc R U . . .
H10B H -0.010946 0.047235 0.084686 0.043 Uiso 1 1 calc R U . . .
H10C H -0.059356 0.018261 0.046336 0.043 Uiso 1 1 calc R U . . .
C11 C 0.0166(16) 0.1877(10) 0.1327(3) 0.0261(9) Uani 1 1 d . . . . .
H11 H 0.065272 0.141977 0.118165 0.031 Uiso 1 1 calc R U . . .
C12 C 0.0696(16) 0.2843(10) 0.1431(3) 0.0261(9) Uani 1 1 d . . . . .
C13 C 0.2140(15) 0.3273(10) 0.1346(3) 0.0261(9) Uani 1 1 d . . . . .
H13A H 0.293389 0.292869 0.147924 0.039 Uiso 1 1 calc R U . . .
H13B H 0.215781 0.400079 0.139936 0.039 Uiso 1 1 calc R U . . .
H13C H 0.229040 0.317715 0.110341 0.039 Uiso 1 1 calc R U . . .
C14 C -0.0422(16) 0.3302(10) 0.1624(3) 0.0261(9) Uani 1 1 d . . . . .
H14 H -0.038884 0.398112 0.170517 0.031 Uiso 1 1 calc R U . . .
C15 C -0.1580(16) 0.2616(10) 0.1677(3) 0.0261(9) Uani 1 1 d . . . . .
C16 C -0.1272(16) 0.1699(10) 0.1481(3) 0.0261(9) Uani 1 1 d . . . . .
C17 C -0.2261(16) 0.0892(10) 0.1466(3) 0.0261(9) Uani 1 1 d . . . . .
H17 H -0.205898 0.030631 0.133536 0.031 Uiso 1 1 calc R U . . .
C18 C -0.3534(16) 0.0950(11) 0.1643(3) 0.0261(9) Uani 1 1 d . . . . .
H18 H -0.423144 0.040858 0.163210 0.031 Uiso 1 1 calc R U . . .
C19 C -0.3803(16) 0.1826(10) 0.1843(3) 0.0261(9) Uani 1 1 d . . . . .
H19 H -0.469506 0.184926 0.196179 0.031 Uiso 1 1 calc R U . . .
C20 C -0.2851(16) 0.2642(10) 0.1875(3) 0.0261(9) Uani 1 1 d . . . . .
C21 C -0.3148(15) 0.3500(12) 0.2102(3) 0.0309(12) Uani 1 1 d . . . . .
C22 C -0.4508(16) 0.3981(12) 0.2079(3) 0.0309(12) Uani 1 1 d . . . . .
H22 H -0.522662 0.376045 0.191180 0.037 Uiso 1 1 calc R U . . .
C23 C -0.4864(16) 0.4784(12) 0.2294(3) 0.0309(12) Uani 1 1 d . . . . .
H23 H -0.578570 0.512815 0.226360 0.037 Uiso 1 1 calc R U . . .
C24 C -0.3843(16) 0.5075(12) 0.2555(3) 0.0309(12) Uani 1 1 d . . . . .
H24 H -0.407937 0.560116 0.270880 0.037 Uiso 1 1 calc R U . . .
C25 C -0.2464(16) 0.4575(12) 0.2586(3) 0.0309(12) Uani 1 1 d . . . . .
H25 H -0.176556 0.476729 0.276192 0.037 Uiso 1 1 calc R U . . .
C26 C -0.2108(16) 0.3791(12) 0.2358(3) 0.0309(12) Uani 1 1 d . . . . .
C27 C -0.0747(15) 0.3192(11) 0.2416(3) 0.028(3) Uani 1 1 d . . . . .
H27 H -0.081124 0.249981 0.234849 0.033 Uiso 1 1 calc R U . . .
C28 C 0.0612(15) 0.3496(10) 0.2554(3) 0.023(3) Uani 1 1 d . . . . .
H28 H 0.130213 0.296136 0.259725 0.028 Uiso 1 1 calc R U . . .
C29 C 0.1154(15) 0.4499(11) 0.2645(3) 0.0278(11) Uani 1 1 d . . . . .
C30 C 0.0846(15) 0.5332(11) 0.2441(3) 0.0278(11) Uani 1 1 d . . . . .
H30 H 0.019038 0.526002 0.224713 0.033 Uiso 1 1 calc R U . . .
C31 C 0.1473(15) 0.6266(11) 0.2514(3) 0.0278(11) Uani 1 1 d . . . . .
H31 H 0.130403 0.682029 0.236249 0.033 Uiso 1 1 calc R U . . .
C32 C 0.2357(15) 0.6393(11) 0.2810(3) 0.0278(11) Uani 1 1 d . . . . .
H32 H 0.274083 0.704418 0.286942 0.033 Uiso 1 1 calc R U . . .
C33 C 0.2673(15) 0.5550(11) 0.3018(3) 0.0278(11) Uani 1 1 d . . . . .
H33 H 0.328503 0.563754 0.321813 0.033 Uiso 1 1 calc R U . . .
C34 C 0.2121(15) 0.4600(11) 0.2940(3) 0.0278(11) Uani 1 1 d . . . . .
C35 C 0.2610(14) 0.3711(12) 0.3148(3) 0.029(3) Uani 1 1 d . . . . .
C36 C 0.1699(14) 0.2983(11) 0.3286(3) 0.023(2) Uani 1 1 d . . . . .
C37 C 0.2354(16) 0.2107(12) 0.3473(3) 0.032(3) Uani 1 1 d . . . . .
C38 C 0.1151(16) 0.1427(11) 0.3553(3) 0.028(3) Uani 1 1 d . . . . .
H38 H 0.124075 0.080518 0.367458 0.033 Uiso 1 1 calc R U . . .
C39 C -0.0155(15) 0.1853(10) 0.3418(3) 0.026(3) Uani 1 1 d . . . . .
C40 C -0.1653(17) 0.1349(12) 0.3411(3) 0.034(3) Uani 1 1 d . . . . .
H40A H -0.155119 0.065717 0.350146 0.052 Uiso 1 1 calc R U . . .
H40B H -0.206087 0.132132 0.317669 0.052 Uiso 1 1 calc R U . . .
H40C H -0.232190 0.173912 0.355083 0.052 Uiso 1 1 calc R U . . .
C41 C 0.0137(13) 0.2821(9) 0.3277(3) 0.017(2) Uani 1 1 d . . . . .
H41 H -0.059136 0.328547 0.319075 0.020 Uiso 1 1 calc R U . . .
C42 C 0.3924(19) 0.2046(16) 0.3539(4) 0.046(4) Uani 1 1 d . . . . .
H42 H 0.434978 0.149905 0.366645 0.055 Uiso 1 1 calc R U . . .
C43 C 0.4771(17) 0.2771(14) 0.3417(4) 0.041(4) Uani 1 1 d . . . . .
H43 H 0.581546 0.272868 0.345614 0.049 Uiso 1 1 calc R U . . .
C44 C 0.4154(16) 0.3641(12) 0.3222(4) 0.034(3) Uani 1 1 d . . . . .
H44 H 0.479647 0.415704 0.314577 0.041 Uiso 1 1 calc R U . . .
C51 C 0.2497(14) 0.2434(9) 0.4406(3) 0.0205(11) Uani 1 1 d . . . . .
C52 C 0.1513(14) 0.1599(9) 0.4338(3) 0.0205(11) Uani 1 1 d . . . . .
C53 C 0.0059(14) 0.1918(9) 0.4415(3) 0.0205(11) Uani 1 1 d . . . . .
C54 C 0.0174(13) 0.2932(10) 0.4544(3) 0.0205(11) Uani 1 1 d . . . . .
C55 C 0.1696(14) 0.3218(9) 0.4544(3) 0.0205(11) Uani 1 1 d . . . . .
C56 C 0.4150(15) 0.2434(12) 0.4393(3) 0.031(3) Uani 1 1 d . . . . .
H56A H 0.445412 0.292081 0.422112 0.046 Uiso 1 1 calc R U . . .
H56B H 0.449299 0.175276 0.433406 0.046 Uiso 1 1 calc R U . . .
H56C H 0.458677 0.262948 0.461566 0.046 Uiso 1 1 calc R U . . .
C57 C 0.1956(15) 0.0520(10) 0.4276(4) 0.027(3) Uani 1 1 d . . . . .
H57A H 0.217225 0.018086 0.449395 0.041 Uiso 1 1 calc R U . . .
H57B H 0.284169 0.050801 0.414068 0.041 Uiso 1 1 calc R U . . .
H57C H 0.114329 0.016509 0.415264 0.041 Uiso 1 1 calc R U . . .
C58 C -0.1325(15) 0.1293(10) 0.4398(4) 0.029(3) Uani 1 1 d . . . . .
H58A H -0.121428 0.073285 0.423735 0.043 Uiso 1 1 calc R U . . .
H58B H -0.216706 0.171892 0.432244 0.043 Uiso 1 1 calc R U . . .
H58C H -0.150219 0.101707 0.462388 0.043 Uiso 1 1 calc R U . . .
C59 C -0.1078(17) 0.3494(12) 0.4700(3) 0.033(3) Uani 1 1 d . . . . .
H59A H -0.113873 0.329144 0.493832 0.049 Uiso 1 1 calc R U . . .
H59B H -0.201336 0.332922 0.457628 0.049 Uiso 1 1 calc R U . . .
H59C H -0.089801 0.422692 0.468715 0.049 Uiso 1 1 calc R U . . .
C60 C 0.2299(17) 0.4173(10) 0.4699(3) 0.029(3) Uani 1 1 d . . . . .
H60A H 0.259182 0.405050 0.493797 0.044 Uiso 1 1 calc R U . . .
H60B H 0.153625 0.470295 0.468414 0.044 Uiso 1 1 calc R U . . .
H60C H 0.316544 0.439317 0.457676 0.044 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 Cl1 2.430(3) . ?
Zr1 Cl2 2.443(3) . ?
Zr1 C11 2.456(13) . ?
Zr1 C1 2.512(12) . ?
Zr1 C16 2.515(13) . ?
Zr1 C4 2.540(11) . ?
Zr1 C5 2.540(12) . ?
Zr1 C2 2.550(11) . ?
Zr1 C3 2.558(10) . ?
Zr1 C12 2.560(13) . ?
Zr1 C14 2.564(12) . ?
Zr1 C15 2.626(12) . ?
Zr2 Cl4 2.435(3) . ?
Zr2 Cl3 2.437(3) . ?
Zr2 C38 2.489(13) . ?
Zr2 C53 2.496(11) . ?
Zr2 C52 2.497(12) . ?
Zr2 C51 2.509(12) . ?
Zr2 C37 2.546(13) . ?
Zr2 C39 2.548(12) . ?
Zr2 C54 2.556(12) . ?
Zr2 C41 2.565(11) . ?
Zr2 C55 2.597(12) . ?
Zr2 C36 2.649(12) . ?
C1 C2 1.414(19) . ?
C1 C5 1.428(18) . ?
C1 C6 1.517(19) . ?
C2 C3 1.424(18) . ?
C2 C7 1.484(17) . ?
C3 C4 1.406(16) . ?
C3 C8 1.498(19) . ?
C4 C5 1.394(18) . ?
C4 C9 1.498(19) . ?
C5 C10 1.503(18) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.413(18) . ?
C11 C16 1.476(19) . ?
C11 H11 0.9500 . ?
C12 C14 1.42(2) . ?
C12 C13 1.473(19) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.404(19) . ?
C14 H14 0.9500 . ?
C15 C20 1.42(2) . ?
C15 C16 1.465(19) . ?
C16 C17 1.387(18) . ?
C17 C18 1.37(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.423(19) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(18) . ?
C19 H19 0.9500 . ?
C20 C21 1.47(2) . ?
C21 C22 1.38(2) . ?
C21 C26 1.40(2) . ?
C22 C23 1.40(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.403(19) . ?
C23 H23 0.9500 . ?
C24 C25 1.41(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.42(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.47(2) . ?
C27 C28 1.379(18) . ?
C27 H27 0.9500 . ?
C28 C29 1.447(19) . ?
C28 H28 0.9500 . ?
C29 C30 1.38(2) . ?
C29 C34 1.428(18) . ?
C30 C31 1.378(19) . ?
C30 H30 0.9500 . ?
C31 C32 1.394(18) . ?
C31 H31 0.9500 . ?
C32 C33 1.40(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.376(19) . ?
C33 H33 0.9500 . ?
C34 C35 1.49(2) . ?
C35 C36 1.389(19) . ?
C35 C44 1.414(17) . ?
C36 C41 1.425(16) . ?
C36 C37 1.477(18) . ?
C37 C42 1.43(2) . ?
C37 C38 1.45(2) . ?
C38 C39 1.390(19) . ?
C38 H38 0.9500 . ?
C39 C41 1.419(17) . ?
C39 C40 1.505(19) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41 0.9500 . ?
C42 C43 1.33(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.47(2) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C51 C55 1.386(18) . ?
C51 C52 1.430(17) . ?
C51 C56 1.495(18) . ?
C52 C53 1.423(18) . ?
C52 C57 1.498(17) . ?
C53 C54 1.430(17) . ?
C53 C58 1.495(17) . ?
C54 C55 1.424(17) . ?
C54 C59 1.504(18) . ?
C55 C60 1.490(17) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Zr1 Cl2 95.00(12) . . ?
Cl1 Zr1 C11 130.0(3) . . ?
Cl2 Zr1 C11 113.8(3) . . ?
Cl1 Zr1 C1 133.6(3) . . ?
Cl2 Zr1 C1 95.5(3) . . ?
C11 Zr1 C1 85.2(4) . . ?
Cl1 Zr1 C16 96.2(3) . . ?
Cl2 Zr1 C16 133.6(3) . . ?
C11 Zr1 C16 34.5(4) . . ?
C1 Zr1 C16 108.2(4) . . ?
Cl1 Zr1 C4 85.4(3) . . ?
Cl2 Zr1 C4 129.4(3) . . ?
C11 Zr1 C4 103.5(4) . . ?
C1 Zr1 C4 53.9(4) . . ?
C16 Zr1 C4 96.3(4) . . ?
Cl1 Zr1 C5 116.3(3) . . ?
Cl2 Zr1 C5 127.9(3) . . ?
C11 Zr1 C5 77.7(4) . . ?
C1 Zr1 C5 32.8(4) . . ?
C16 Zr1 C5 85.5(4) . . ?
C4 Zr1 C5 31.9(4) . . ?
Cl1 Zr1 C2 107.3(3) . . ?
Cl2 Zr1 C2 78.9(3) . . ?
C11 Zr1 C2 117.4(4) . . ?
C1 Zr1 C2 32.4(4) . . ?
C16 Zr1 C2 138.3(4) . . ?
C4 Zr1 C2 53.4(4) . . ?
C5 Zr1 C2 53.3(4) . . ?
Cl1 Zr1 C3 79.9(3) . . ?
Cl2 Zr1 C3 98.1(3) . . ?
C11 Zr1 C3 130.6(4) . . ?
C1 Zr1 C3 53.9(4) . . ?
C16 Zr1 C3 128.2(4) . . ?
C4 Zr1 C3 32.0(4) . . ?
C5 Zr1 C3 53.0(4) . . ?
C2 Zr1 C3 32.4(4) . . ?
Cl1 Zr1 C12 127.4(3) . . ?
Cl2 Zr1 C12 83.0(3) . . ?
C11 Zr1 C12 32.6(4) . . ?
C1 Zr1 C12 98.7(4) . . ?
C16 Zr1 C12 55.0(4) . . ?
C4 Zr1 C12 134.8(4) . . ?
C5 Zr1 C12 105.1(4) . . ?
C2 Zr1 C12 123.5(4) . . ?
C3 Zr1 C12 152.6(4) . . ?
Cl1 Zr1 C14 95.4(3) . . ?
Cl2 Zr1 C14 80.3(3) . . ?
C11 Zr1 C14 54.1(4) . . ?
C1 Zr1 C14 130.9(5) . . ?
C16 Zr1 C14 54.0(4) . . ?
C4 Zr1 C14 150.3(4) . . ?
C5 Zr1 C14 131.7(4) . . ?
C2 Zr1 C14 150.3(4) . . ?
C3 Zr1 C14 174.9(4) . . ?
C12 Zr1 C14 32.2(5) . . ?
Cl1 Zr1 C15 78.3(3) . . ?
Cl2 Zr1 C15 107.7(3) . . ?
C11 Zr1 C15 55.0(4) . . ?
C1 Zr1 C15 139.2(4) . . ?
C16 Zr1 C15 33.0(4) . . ?
C4 Zr1 C15 121.7(4) . . ?
C5 Zr1 C15 118.3(4) . . ?
C2 Zr1 C15 171.2(4) . . ?
C3 Zr1 C15 147.4(4) . . ?
C12 Zr1 C15 53.3(4) . . ?
C14 Zr1 C15 31.4(4) . . ?
Cl4 Zr2 Cl3 98.36(11) . . ?
Cl4 Zr2 C38 128.6(3) . . ?
Cl3 Zr2 C38 112.3(3) . . ?
Cl4 Zr2 C53 130.4(3) . . ?
Cl3 Zr2 C53 85.1(3) . . ?
C38 Zr2 C53 93.6(4) . . ?
Cl4 Zr2 C52 123.7(3) . . ?
Cl3 Zr2 C52 117.8(3) . . ?
C38 Zr2 C52 77.0(4) . . ?
C53 Zr2 C52 33.1(4) . . ?
Cl4 Zr2 C51 90.5(3) . . ?
Cl3 Zr2 C51 131.6(3) . . ?
C38 Zr2 C51 97.7(4) . . ?
C53 Zr2 C51 54.8(4) . . ?
C52 Zr2 C51 33.2(4) . . ?
Cl4 Zr2 C37 95.7(4) . . ?
Cl3 Zr2 C37 131.8(3) . . ?
C38 Zr2 C37 33.5(5) . . ?
C53 Zr2 C37 118.5(5) . . ?
C52 Zr2 C37 90.6(4) . . ?
C51 Zr2 C37 93.9(4) . . ?
Cl4 Zr2 C39 127.5(3) . . ?
Cl3 Zr2 C39 82.2(3) . . ?
C38 Zr2 C39 32.0(5) . . ?
C53 Zr2 C39 102.1(4) . . ?
C52 Zr2 C39 100.4(4) . . ?
C51 Zr2 C39 127.8(4) . . ?
C37 Zr2 C39 53.4(5) . . ?
Cl4 Zr2 C54 99.2(3) . . ?
Cl3 Zr2 C54 77.9(3) . . ?
C38 Zr2 C54 126.2(4) . . ?
C53 Zr2 C54 32.8(4) . . ?
C52 Zr2 C54 54.1(4) . . ?
C51 Zr2 C54 53.6(4) . . ?
C37 Zr2 C54 144.1(4) . . ?
C39 Zr2 C54 131.4(4) . . ?
Cl4 Zr2 C41 95.9(3) . . ?
Cl3 Zr2 C41 79.0(3) . . ?
C38 Zr2 C41 54.2(4) . . ?
C53 Zr2 C41 132.9(4) . . ?
C52 Zr2 C41 130.5(4) . . ?
C51 Zr2 C41 147.5(4) . . ?
C37 Zr2 C41 53.8(4) . . ?
C39 Zr2 C41 32.2(4) . . ?
C54 Zr2 C41 154.0(4) . . ?
Cl4 Zr2 C55 77.9(3) . . ?
Cl3 Zr2 C55 104.6(3) . . ?
C38 Zr2 C55 127.9(4) . . ?
C53 Zr2 C55 53.7(4) . . ?
C52 Zr2 C55 53.2(4) . . ?
C51 Zr2 C55 31.4(4) . . ?
C37 Zr2 C55 123.4(4) . . ?
C39 Zr2 C55 153.1(4) . . ?
C54 Zr2 C55 32.1(4) . . ?
C41 Zr2 C55 173.2(4) . . ?
Cl4 Zr2 C36 77.8(3) . . ?
Cl3 Zr2 C36 107.2(3) . . ?
C38 Zr2 C36 54.7(4) . . ?
C53 Zr2 C36 148.3(4) . . ?
C52 Zr2 C36 123.6(4) . . ?
C51 Zr2 C36 121.2(4) . . ?
C37 Zr2 C36 33.0(4) . . ?
C39 Zr2 C36 52.9(4) . . ?
C54 Zr2 C36 174.3(4) . . ?
C41 Zr2 C36 31.7(4) . . ?
C55 Zr2 C36 142.3(4) . . ?
C2 C1 C5 107.0(11) . . ?
C2 C1 C6 126.3(11) . . ?
C5 C1 C6 126.1(12) . . ?
C2 C1 Zr1 75.3(7) . . ?
C5 C1 Zr1 74.7(7) . . ?
C6 C1 Zr1 122.5(9) . . ?
C1 C2 C3 108.1(11) . . ?
C1 C2 C7 126.4(12) . . ?
C3 C2 C7 125.2(13) . . ?
C1 C2 Zr1 72.3(7) . . ?
C3 C2 Zr1 74.1(6) . . ?
C7 C2 Zr1 124.4(8) . . ?
C4 C3 C2 107.7(11) . . ?
C4 C3 C8 127.9(12) . . ?
C2 C3 C8 124.1(12) . . ?
C4 C3 Zr1 73.3(6) . . ?
C2 C3 Zr1 73.5(7) . . ?
C8 C3 Zr1 124.1(8) . . ?
C5 C4 C3 108.6(11) . . ?
C5 C4 C9 127.1(11) . . ?
C3 C4 C9 124.2(12) . . ?
C5 C4 Zr1 74.1(7) . . ?
C3 C4 Zr1 74.7(6) . . ?
C9 C4 Zr1 120.5(8) . . ?
C4 C5 C1 108.5(11) . . ?
C4 C5 C10 125.2(12) . . ?
C1 C5 C10 125.0(12) . . ?
C4 C5 Zr1 74.0(7) . . ?
C1 C5 Zr1 72.5(7) . . ?
C10 C5 Zr1 129.5(8) . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 108.3(12) . . ?
C12 C11 Zr1 77.7(8) . . ?
C16 C11 Zr1 74.9(8) . . ?
C12 C11 H11 125.8 . . ?
C16 C11 H11 125.8 . . ?
Zr1 C11 H11 113.8 . . ?
C11 C12 C14 107.4(12) . . ?
C11 C12 C13 124.8(13) . . ?
C14 C12 C13 127.8(12) . . ?
C11 C12 Zr1 69.6(7) . . ?
C14 C12 Zr1 74.0(7) . . ?
C13 C12 Zr1 121.0(8) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C12 110.9(12) . . ?
C15 C14 Zr1 76.8(7) . . ?
C12 C14 Zr1 73.7(7) . . ?
C15 C14 H14 124.6 . . ?
C12 C14 H14 124.6 . . ?
Zr1 C14 H14 116.6 . . ?
C14 C15 C20 133.9(13) . . ?
C14 C15 C16 106.9(12) . . ?
C20 C15 C16 119.2(12) . . ?
C14 C15 Zr1 71.9(7) . . ?
C20 C15 Zr1 124.6(9) . . ?
C16 C15 Zr1 69.3(6) . . ?
C17 C16 C15 121.1(13) . . ?
C17 C16 C11 132.8(13) . . ?
C15 C16 C11 106.1(11) . . ?
C17 C16 Zr1 116.8(8) . . ?
C15 C16 Zr1 77.6(7) . . ?
C11 C16 Zr1 70.6(7) . . ?
C18 C17 C16 119.2(13) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 119.5(12) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C20 C19 C18 124.2(13) . . ?
C20 C19 H19 117.9 . . ?
C18 C19 H19 117.9 . . ?
C19 C20 C15 116.6(12) . . ?
C19 C20 C21 121.6(13) . . ?
C15 C20 C21 121.8(12) . . ?
C22 C21 C26 119.2(13) . . ?
C22 C21 C20 119.7(13) . . ?
C26 C21 C20 120.9(13) . . ?
C21 C22 C23 122.2(14) . . ?
C21 C22 H22 118.9 . . ?
C23 C22 H22 118.9 . . ?
C22 C23 C24 119.2(13) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C23 C24 C25 119.0(13) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
C24 C25 C26 120.7(13) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C21 C26 C25 119.5(13) . . ?
C21 C26 C27 119.6(13) . . ?
C25 C26 C27 120.3(12) . . ?
C28 C27 C26 128.9(13) . . ?
C28 C27 H27 115.5 . . ?
C26 C27 H27 115.5 . . ?
C27 C28 C29 130.3(12) . . ?
C27 C28 H28 114.8 . . ?
C29 C28 H28 114.8 . . ?
C30 C29 C34 120.0(12) . . ?
C30 C29 C28 121.6(12) . . ?
C34 C29 C28 118.2(12) . . ?
C31 C30 C29 121.1(12) . . ?
C31 C30 H30 119.4 . . ?
C29 C30 H30 119.4 . . ?
C30 C31 C32 119.7(13) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C31 C32 C33 119.3(12) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C34 C33 C32 121.7(12) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
C33 C34 C29 118.0(13) . . ?
C33 C34 C35 119.8(12) . . ?
C29 C34 C35 122.1(12) . . ?
C36 C35 C44 117.9(13) . . ?
C36 C35 C34 126.4(11) . . ?
C44 C35 C34 115.5(13) . . ?
C35 C36 C41 134.0(12) . . ?
C35 C36 C37 120.2(12) . . ?
C41 C36 C37 105.6(11) . . ?
C35 C36 Zr2 126.5(9) . . ?
C41 C36 Zr2 70.9(6) . . ?
C37 C36 Zr2 69.7(7) . . ?
C42 C37 C38 132.1(15) . . ?
C42 C37 C36 120.3(15) . . ?
C38 C37 C36 107.6(12) . . ?
C42 C37 Zr2 118.5(10) . . ?
C38 C37 Zr2 71.1(7) . . ?
C36 C37 Zr2 77.4(7) . . ?
C39 C38 C37 107.4(12) . . ?
C39 C38 Zr2 76.4(8) . . ?
C37 C38 Zr2 75.4(8) . . ?
C39 C38 H38 126.3 . . ?
C37 C38 H38 126.3 . . ?
Zr2 C38 H38 114.3 . . ?
C38 C39 C41 110.0(12) . . ?
C38 C39 C40 125.1(13) . . ?
C41 C39 C40 124.8(12) . . ?
C38 C39 Zr2 71.6(7) . . ?
C41 C39 Zr2 74.5(7) . . ?
C40 C39 Zr2 122.1(9) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 C36 109.0(11) . . ?
C39 C41 Zr2 73.3(6) . . ?
C36 C41 Zr2 77.4(6) . . ?
C39 C41 H41 125.5 . . ?
C36 C41 H41 125.5 . . ?
Zr2 C41 H41 115.8 . . ?
C43 C42 C37 118.4(16) . . ?
C43 C42 H42 120.8 . . ?
C37 C42 H42 120.8 . . ?
C42 C43 C44 122.5(14) . . ?
C42 C43 H43 118.8 . . ?
C44 C43 H43 118.8 . . ?
C35 C44 C43 120.3(15) . . ?
C35 C44 H44 119.9 . . ?
C43 C44 H44 119.9 . . ?
C55 C51 C52 108.4(11) . . ?
C55 C51 C56 123.4(12) . . ?
C52 C51 C56 127.3(12) . . ?
C55 C51 Zr2 77.8(7) . . ?
C52 C51 Zr2 73.0(7) . . ?
C56 C51 Zr2 123.8(8) . . ?
C53 C52 C51 107.7(11) . . ?
C53 C52 C57 124.7(11) . . ?
C51 C52 C57 126.2(12) . . ?
C53 C52 Zr2 73.4(7) . . ?
C51 C52 Zr2 73.8(7) . . ?
C57 C52 Zr2 129.0(9) . . ?
C52 C53 C54 107.4(10) . . ?
C52 C53 C58 127.2(11) . . ?
C54 C53 C58 125.2(12) . . ?
C52 C53 Zr2 73.5(7) . . ?
C54 C53 Zr2 75.9(7) . . ?
C58 C53 Zr2 120.8(8) . . ?
C55 C54 C53 107.5(11) . . ?
C55 C54 C59 127.7(12) . . ?
C53 C54 C59 124.1(11) . . ?
C55 C54 Zr2 75.5(7) . . ?
C53 C54 Zr2 71.3(6) . . ?
C59 C54 Zr2 126.2(8) . . ?
C51 C55 C54 108.8(11) . . ?
C51 C55 C60 127.0(12) . . ?
C54 C55 C60 123.9(12) . . ?
C51 C55 Zr2 70.8(7) . . ?
C54 C55 Zr2 72.4(7) . . ?
C60 C55 Zr2 127.0(8) . . ?
C51 C56 H56A 109.5 . . ?
C51 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C51 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C52 C57 H57A 109.5 . . ?
C52 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C52 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C53 C58 H58A 109.5 . . ?
C53 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C53 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C54 C59 H59A 109.5 . . ?
C54 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C54 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C55 C60 H60A 109.5 . . ?
C55 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C55 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 2.5(13) . . . . ?
C6 C1 C2 C3 174.3(12) . . . . ?
Zr1 C1 C2 C3 -66.0(8) . . . . ?
C5 C1 C2 C7 -171.3(11) . . . . ?
C6 C1 C2 C7 0(2) . . . . ?
Zr1 C1 C2 C7 120.1(12) . . . . ?
C5 C1 C2 Zr1 68.5(8) . . . . ?
C6 C1 C2 Zr1 -119.7(13) . . . . ?
C1 C2 C3 C4 -1.0(13) . . . . ?
C7 C2 C3 C4 172.9(11) . . . . ?
Zr1 C2 C3 C4 -65.8(7) . . . . ?
C1 C2 C3 C8 -174.8(11) . . . . ?
C7 C2 C3 C8 -0.8(18) . . . . ?
Zr1 C2 C3 C8 120.4(11) . . . . ?
C1 C2 C3 Zr1 64.8(9) . . . . ?
C7 C2 C3 Zr1 -121.2(12) . . . . ?
C2 C3 C4 C5 -0.9(12) . . . . ?
C8 C3 C4 C5 172.5(11) . . . . ?
Zr1 C3 C4 C5 -66.9(8) . . . . ?
C2 C3 C4 C9 -177.2(11) . . . . ?
C8 C3 C4 C9 -3.8(18) . . . . ?
Zr1 C3 C4 C9 116.8(11) . . . . ?
C2 C3 C4 Zr1 66.0(8) . . . . ?
C8 C3 C4 Zr1 -120.6(12) . . . . ?
C3 C4 C5 C1 2.5(13) . . . . ?
C9 C4 C5 C1 178.6(11) . . . . ?
Zr1 C4 C5 C1 -64.8(8) . . . . ?
C3 C4 C5 C10 -165.3(11) . . . . ?
C9 C4 C5 C10 10.8(19) . . . . ?
Zr1 C4 C5 C10 127.4(11) . . . . ?
C3 C4 C5 Zr1 67.3(8) . . . . ?
C9 C4 C5 Zr1 -116.5(12) . . . . ?
C2 C1 C5 C4 -3.1(13) . . . . ?
C6 C1 C5 C4 -174.9(11) . . . . ?
Zr1 C1 C5 C4 65.8(8) . . . . ?
C2 C1 C5 C10 164.7(11) . . . . ?
C6 C1 C5 C10 -7(2) . . . . ?
Zr1 C1 C5 C10 -126.3(11) . . . . ?
C2 C1 C5 Zr1 -68.9(8) . . . . ?
C6 C1 C5 Zr1 119.3(13) . . . . ?
C16 C11 C12 C14 -4.5(13) . . . . ?
Zr1 C11 C12 C14 64.9(9) . . . . ?
C16 C11 C12 C13 176.4(11) . . . . ?
Zr1 C11 C12 C13 -114.3(12) . . . . ?
C16 C11 C12 Zr1 -69.4(9) . . . . ?
C11 C12 C14 C15 6.5(14) . . . . ?
C13 C12 C14 C15 -174.4(12) . . . . ?
Zr1 C12 C14 C15 68.5(9) . . . . ?
C11 C12 C14 Zr1 -62.0(8) . . . . ?
C13 C12 C14 Zr1 117.1(13) . . . . ?
C12 C14 C15 C20 172.5(14) . . . . ?
Zr1 C14 C15 C20 -120.9(15) . . . . ?
C12 C14 C15 C16 -5.8(14) . . . . ?
Zr1 C14 C15 C16 60.8(8) . . . . ?
C12 C14 C15 Zr1 -66.6(9) . . . . ?
C14 C15 C16 C17 -176.5(12) . . . . ?
C20 C15 C16 C17 4.9(18) . . . . ?
Zr1 C15 C16 C17 -114.0(12) . . . . ?
C14 C15 C16 C11 2.8(13) . . . . ?
C20 C15 C16 C11 -175.8(11) . . . . ?
Zr1 C15 C16 C11 65.3(8) . . . . ?
C14 C15 C16 Zr1 -62.5(9) . . . . ?
C20 C15 C16 Zr1 119.0(11) . . . . ?
C12 C11 C16 C17 -179.7(13) . . . . ?
Zr1 C11 C16 C17 109.0(14) . . . . ?
C12 C11 C16 C15 1.0(13) . . . . ?
Zr1 C11 C16 C15 -70.2(8) . . . . ?
C12 C11 C16 Zr1 71.3(9) . . . . ?
C15 C16 C17 C18 -1.1(18) . . . . ?
C11 C16 C17 C18 179.7(13) . . . . ?
Zr1 C16 C17 C18 -92.6(12) . . . . ?
C16 C17 C18 C19 -1.2(18) . . . . ?
C17 C18 C19 C20 -0.3(19) . . . . ?
C18 C19 C20 C15 4.0(19) . . . . ?
C18 C19 C20 C21 -176.1(12) . . . . ?
C14 C15 C20 C19 175.8(14) . . . . ?
C16 C15 C20 C19 -6.1(18) . . . . ?
Zr1 C15 C20 C19 77.8(14) . . . . ?
C14 C15 C20 C21 -4(2) . . . . ?
C16 C15 C20 C21 174.1(12) . . . . ?
Zr1 C15 C20 C21 -102.0(13) . . . . ?
C19 C20 C21 C22 -51.9(19) . . . . ?
C15 C20 C21 C22 127.9(15) . . . . ?
C19 C20 C21 C26 123.7(15) . . . . ?
C15 C20 C21 C26 -56.5(19) . . . . ?
C26 C21 C22 C23 3(2) . . . . ?
C20 C21 C22 C23 178.5(13) . . . . ?
C21 C22 C23 C24 -4(2) . . . . ?
C22 C23 C24 C25 2(2) . . . . ?
C23 C24 C25 C26 0(2) . . . . ?
C22 C21 C26 C25 0(2) . . . . ?
C20 C21 C26 C25 -176.0(13) . . . . ?
C22 C21 C26 C27 171.4(13) . . . . ?
C20 C21 C26 C27 -4(2) . . . . ?
C24 C25 C26 C21 -1(2) . . . . ?
C24 C25 C26 C27 -172.7(13) . . . . ?
C21 C26 C27 C28 154.4(14) . . . . ?
C25 C26 C27 C28 -34(2) . . . . ?
C26 C27 C28 C29 -8(2) . . . . ?
C27 C28 C29 C30 -41(2) . . . . ?
C27 C28 C29 C34 144.0(14) . . . . ?
C34 C29 C30 C31 1(2) . . . . ?
C28 C29 C30 C31 -174.2(12) . . . . ?
C29 C30 C31 C32 -4(2) . . . . ?
C30 C31 C32 C33 4(2) . . . . ?
C31 C32 C33 C34 -1(2) . . . . ?
C32 C33 C34 C29 -3(2) . . . . ?
C32 C33 C34 C35 173.6(12) . . . . ?
C30 C29 C34 C33 3(2) . . . . ?
C28 C29 C34 C33 177.8(12) . . . . ?
C30 C29 C34 C35 -173.6(12) . . . . ?
C28 C29 C34 C35 1.6(19) . . . . ?
C33 C34 C35 C36 131.0(15) . . . . ?
C29 C34 C35 C36 -53(2) . . . . ?
C33 C34 C35 C44 -45.8(19) . . . . ?
C29 C34 C35 C44 130.3(15) . . . . ?
C44 C35 C36 C41 178.1(14) . . . . ?
C34 C35 C36 C41 1(2) . . . . ?
C44 C35 C36 C37 -6(2) . . . . ?
C34 C35 C36 C37 176.8(12) . . . . ?
C44 C35 C36 Zr2 79.6(16) . . . . ?
C34 C35 C36 Zr2 -97.2(14) . . . . ?
C35 C36 C37 C42 5(2) . . . . ?
C41 C36 C37 C42 -178.0(12) . . . . ?
Zr2 C36 C37 C42 -115.8(13) . . . . ?
C35 C36 C37 C38 -173.6(12) . . . . ?
C41 C36 C37 C38 3.0(14) . . . . ?
Zr2 C36 C37 C38 65.2(9) . . . . ?
C35 C36 C37 Zr2 121.2(12) . . . . ?
C41 C36 C37 Zr2 -62.2(8) . . . . ?
C42 C37 C38 C39 -178.0(15) . . . . ?
C36 C37 C38 C39 0.9(15) . . . . ?
Zr2 C37 C38 C39 70.3(9) . . . . ?
C42 C37 C38 Zr2 111.7(16) . . . . ?
C36 C37 C38 Zr2 -69.4(9) . . . . ?
C37 C38 C39 C41 -4.5(15) . . . . ?
Zr2 C38 C39 C41 65.2(9) . . . . ?
C37 C38 C39 C40 173.5(12) . . . . ?
Zr2 C38 C39 C40 -116.8(13) . . . . ?
C37 C38 C39 Zr2 -69.7(9) . . . . ?
C38 C39 C41 C36 6.6(14) . . . . ?
C40 C39 C41 C36 -171.4(12) . . . . ?
Zr2 C39 C41 C36 69.9(8) . . . . ?
C38 C39 C41 Zr2 -63.3(9) . . . . ?
C40 C39 C41 Zr2 118.7(13) . . . . ?
C35 C36 C41 C39 170.2(15) . . . . ?
C37 C36 C41 C39 -5.7(13) . . . . ?
Zr2 C36 C41 C39 -67.1(8) . . . . ?
C35 C36 C41 Zr2 -122.7(16) . . . . ?
C37 C36 C41 Zr2 61.4(8) . . . . ?
C38 C37 C42 C43 176.3(14) . . . . ?
C36 C37 C42 C43 -3(2) . . . . ?
Zr2 C37 C42 C43 -94.1(15) . . . . ?
C37 C42 C43 C44 1(2) . . . . ?
C36 C35 C44 C43 5(2) . . . . ?
C34 C35 C44 C43 -177.9(13) . . . . ?
C42 C43 C44 C35 -2(2) . . . . ?
C55 C51 C52 C53 4.3(13) . . . . ?
C56 C51 C52 C53 174.0(12) . . . . ?
Zr2 C51 C52 C53 -66.1(8) . . . . ?
C55 C51 C52 C57 -162.8(12) . . . . ?
C56 C51 C52 C57 7(2) . . . . ?
Zr2 C51 C52 C57 126.8(12) . . . . ?
C55 C51 C52 Zr2 70.4(8) . . . . ?
C56 C51 C52 Zr2 -119.8(12) . . . . ?
C51 C52 C53 C54 -2.5(13) . . . . ?
C57 C52 C53 C54 164.8(11) . . . . ?
Zr2 C52 C53 C54 -69.0(8) . . . . ?
C51 C52 C53 C58 -177.1(11) . . . . ?
C57 C52 C53 C58 -10(2) . . . . ?
Zr2 C52 C53 C58 116.4(12) . . . . ?
C51 C52 C53 Zr2 66.4(8) . . . . ?
C57 C52 C53 Zr2 -126.3(12) . . . . ?
C52 C53 C54 C55 -0.1(13) . . . . ?
C58 C53 C54 C55 174.6(11) . . . . ?
Zr2 C53 C54 C55 -67.4(8) . . . . ?
C52 C53 C54 C59 -171.1(11) . . . . ?
C58 C53 C54 C59 3.6(18) . . . . ?
Zr2 C53 C54 C59 121.6(11) . . . . ?
C52 C53 C54 Zr2 67.3(8) . . . . ?
C58 C53 C54 Zr2 -117.9(12) . . . . ?
C52 C51 C55 C54 -4.4(13) . . . . ?
C56 C51 C55 C54 -174.6(11) . . . . ?
Zr2 C51 C55 C54 62.8(8) . . . . ?
C52 C51 C55 C60 170.5(11) . . . . ?
C56 C51 C55 C60 0.3(19) . . . . ?
Zr2 C51 C55 C60 -122.3(12) . . . . ?
C52 C51 C55 Zr2 -67.2(8) . . . . ?
C56 C51 C55 Zr2 122.6(12) . . . . ?
C53 C54 C55 C51 2.8(13) . . . . ?
C59 C54 C55 C51 173.4(12) . . . . ?
Zr2 C54 C55 C51 -61.8(8) . . . . ?
C53 C54 C55 C60 -172.3(11) . . . . ?
C59 C54 C55 C60 -1.7(19) . . . . ?
Zr2 C54 C55 C60 123.1(11) . . . . ?
C53 C54 C55 Zr2 64.5(8) . . . . ?
C59 C54 C55 Zr2 -124.9(12) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_NR2036
_database_code_depnum_ccdc_archive 'CCDC 2322679'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-02-19 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 22 mars 2016                                             #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C54 H56 Cl4 Zr2, 3(C7 H8) [+ solvent]'
_chemical_formula_sum            'C75 H80 Cl4 Zr2'
_chemical_formula_weight         1305.63
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.2349(11)
_cell_length_b                   16.0237(11)
_cell_length_c                   16.3054(12)
_cell_angle_alpha                118.098(2)
_cell_angle_beta                 103.060(3)
_cell_angle_gamma                90.216(2)
_cell_volume                     3392.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9781
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      27.48
_cell_measurement_wavelength     0.71073


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0364536
_diffrn_orient_matrix_UB_21      -0.0323191
_diffrn_orient_matrix_UB_31      -0.0473583
_diffrn_orient_matrix_UB_12      0.0508336
_diffrn_orient_matrix_UB_22      -0.0034046
_diffrn_orient_matrix_UB_32      -0.0499287
_diffrn_orient_matrix_UB_13      0.0343633
_diffrn_orient_matrix_UB_23      -0.0623397
_diffrn_orient_matrix_UB_33      -0.0105619


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.110
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1356
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_T_max  0.946

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 7.39
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0343
_diffrn_reflns_av_r_equivalents  0.0470
_diffrn_reflns_number            73247
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.514
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             15572
_reflns_number_gt                12535
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.

Squeeze procedure was used to remove the contribution of disordered solvent
molecule(s).
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2023)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0698P)²+7.9788P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15572
_refine_ls_number_parameters     601
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1492
_refine_ls_wR_factor_gt          0.1356
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.382
_refine_diff_density_min         -1.729
_refine_diff_density_rms         0.097

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.63459(2) 0.23735(2) 0.36679(2) 0.02051(8) Uani 1 1 d . . . . .
Cl1 Cl 0.74999(6) 0.15538(6) 0.41925(6) 0.03191(19) Uani 1 1 d . . . . .
Cl2 Cl 0.50804(6) 0.11021(6) 0.30800(6) 0.02969(18) Uani 1 1 d . . . . .
C1 C 0.6111(2) 0.2927(3) 0.2430(2) 0.0270(7) Uani 1 1 d . . . . .
C2 C 0.5844(3) 0.1928(3) 0.1908(2) 0.0300(7) Uani 1 1 d . . . . .
C3 C 0.6613(3) 0.1466(2) 0.2011(3) 0.0306(7) Uani 1 1 d . . . . .
C4 C 0.7379(2) 0.2177(3) 0.2583(3) 0.0290(7) Uani 1 1 d . . . . .
C5 C 0.7073(2) 0.3081(2) 0.2856(2) 0.0259(7) Uani 1 1 d . . . . .
C6 C 0.5539(3) 0.3668(3) 0.2376(3) 0.0364(8) Uani 1 1 d . . . . .
H6A H 0.550600 0.366905 0.176924 0.055 Uiso 1 1 calc R U . . .
H6B H 0.581206 0.429741 0.291708 0.055 Uiso 1 1 calc R U . . .
H6C H 0.492624 0.352292 0.240741 0.055 Uiso 1 1 calc R U . . .
C7 C 0.4910(3) 0.1459(3) 0.1257(3) 0.0448(10) Uani 1 1 d . . . . .
H7A H 0.485324 0.145046 0.064218 0.067 Uiso 1 1 calc R U . . .
H7B H 0.444994 0.181740 0.156197 0.067 Uiso 1 1 calc R U . . .
H7C H 0.481972 0.080299 0.114270 0.067 Uiso 1 1 calc R U . . .
C8 C 0.6641(3) 0.0410(3) 0.1544(3) 0.0437(10) Uani 1 1 d . . . . .
H8A H 0.608427 0.009200 0.153203 0.066 Uiso 1 1 calc R U . . .
H8B H 0.716867 0.027115 0.190969 0.066 Uiso 1 1 calc R U . . .
H8C H 0.669000 0.017581 0.088365 0.066 Uiso 1 1 calc R U . . .
C9 C 0.8353(3) 0.2017(3) 0.2792(4) 0.0440(10) Uani 1 1 d . . . . .
H9A H 0.864426 0.208187 0.234337 0.066 Uiso 1 1 calc R U . . .
H9B H 0.838546 0.137383 0.271476 0.066 Uiso 1 1 calc R U . . .
H9C H 0.866697 0.248903 0.345322 0.066 Uiso 1 1 calc R U . . .
C10 C 0.7669(3) 0.4016(3) 0.3331(3) 0.0332(8) Uani 1 1 d . . . . .
H10A H 0.820412 0.401605 0.379619 0.050 Uiso 1 1 calc R U . . .
H10B H 0.732969 0.453560 0.366484 0.050 Uiso 1 1 calc R U . . .
H10C H 0.786359 0.410794 0.284241 0.050 Uiso 1 1 calc R U . . .
C11 C 0.4399(3) 0.3535(3) 0.4019(3) 0.0368(8) Uani 1 1 d . . . . .
H11A H 0.436419 0.410022 0.393353 0.055 Uiso 1 1 calc R U . . .
H11B H 0.397159 0.353110 0.438560 0.055 Uiso 1 1 calc R U . . .
H11C H 0.424375 0.295885 0.338806 0.055 Uiso 1 1 calc R U . . .
C12 C 0.5347(2) 0.3555(2) 0.4557(3) 0.0292(7) Uani 1 1 d . . . . .
C13 C 0.5582(2) 0.3064(2) 0.5086(2) 0.0254(7) Uani 1 1 d . . . . .
H13 H 0.517417 0.264632 0.513015 0.031 Uiso 1 1 calc R U . . .
C14 C 0.6533(2) 0.3299(2) 0.5544(2) 0.0250(7) Uani 1 1 d . . . . .
C15 C 0.6895(3) 0.3919(2) 0.5248(2) 0.0285(7) Uani 1 1 d . . . . .
C16 C 0.6154(3) 0.4059(2) 0.4634(2) 0.0289(7) Uani 1 1 d . . . . .
H16 H 0.619438 0.443023 0.432638 0.035 Uiso 1 1 calc R U . . .
C17 C 0.7834(3) 0.4276(3) 0.5609(3) 0.0338(8) Uani 1 1 d . . . . .
H17 H 0.808420 0.467435 0.541237 0.041 Uiso 1 1 calc R U . . .
C18 C 0.8371(3) 0.4042(3) 0.6239(3) 0.0372(9) Uani 1 1 d . . . . .
H18 H 0.899873 0.428288 0.648211 0.045 Uiso 1 1 calc R U . . .
C19 C 0.8009(3) 0.3443(3) 0.6541(3) 0.0348(8) Uani 1 1 d . . . . .
H19 H 0.840341 0.329771 0.698433 0.042 Uiso 1 1 calc R U . . .
C20 C 0.7106(2) 0.3067(2) 0.6210(2) 0.0275(7) Uani 1 1 d . . . . .
C21 C 0.6742(2) 0.2449(2) 0.6533(2) 0.0258(7) Uani 1 1 d . . . . .
C22 C 0.6977(2) 0.2683(3) 0.7497(3) 0.0323(8) Uani 1 1 d . . . . .
H22 H 0.736820 0.325338 0.795854 0.039 Uiso 1 1 calc R U . . .
C23 C 0.6644(2) 0.2087(3) 0.7794(3) 0.0319(8) Uani 1 1 d . . . . .
H23 H 0.680876 0.225170 0.845449 0.038 Uiso 1 1 calc R U . . .
C24 C 0.6075(2) 0.1256(3) 0.7125(3) 0.0276(7) Uani 1 1 d . . . . .
H24 H 0.585246 0.085028 0.732977 0.033 Uiso 1 1 calc R U . . .
C25 C 0.5821(2) 0.1005(2) 0.6151(2) 0.0219(6) Uani 1 1 d . . . . .
C26 C 0.6170(2) 0.1605(2) 0.5863(2) 0.0231(6) Uani 1 1 d . . . . .
H26 H 0.601530 0.143453 0.520082 0.028 Uiso 1 1 calc R U . . .
C27 C 0.5195(2) 0.0132(2) 0.5460(2) 0.0216(6) Uani 1 1 d . . . . .
H27 H 0.505544 -0.028425 0.568965 0.026 Uiso 1 1 calc R U . . .
Zr2 Zr 0.20079(2) 0.26431(2) 0.63316(2) 0.02137(8) Uani 1 1 d . . . . .
Cl11 Cl 0.09985(6) 0.38852(6) 0.68758(6) 0.02998(18) Uani 1 1 d . . . . .
Cl12 Cl 0.29373(6) 0.34862(6) 0.58464(6) 0.03231(19) Uani 1 1 d . . . . .
C51 C 0.3129(2) 0.1957(2) 0.7167(3) 0.0284(7) Uani 1 1 d . . . . .
C52 C 0.3547(2) 0.2887(3) 0.7463(3) 0.0302(7) Uani 1 1 d . . . . .
C53 C 0.3009(3) 0.3563(3) 0.7998(3) 0.0330(8) Uani 1 1 d . . . . .
C54 C 0.2299(3) 0.3056(3) 0.8073(3) 0.0329(8) Uani 1 1 d . . . . .
C55 C 0.2361(2) 0.2071(3) 0.7559(3) 0.0296(7) Uani 1 1 d . . . . .
C56 C 0.3543(3) 0.1052(3) 0.6712(3) 0.0384(9) Uani 1 1 d . . . . .
H56A H 0.388387 0.108901 0.628582 0.058 Uiso 1 1 calc R U . . .
H56B H 0.306008 0.050946 0.633893 0.058 Uiso 1 1 calc R U . . .
H56C H 0.395359 0.096581 0.721621 0.058 Uiso 1 1 calc R U . . .
C57 C 0.4432(3) 0.3096(3) 0.7301(4) 0.0454(10) Uani 1 1 d . . . . .
H57A H 0.493395 0.306201 0.777640 0.068 Uiso 1 1 calc R U . . .
H57B H 0.448004 0.373637 0.736908 0.068 Uiso 1 1 calc R U . . .
H57C H 0.446069 0.262524 0.665200 0.068 Uiso 1 1 calc R U . . .
C58 C 0.3207(3) 0.4625(3) 0.8464(3) 0.0476(11) Uani 1 1 d . . . . .
H58A H 0.263474 0.490033 0.843760 0.071 Uiso 1 1 calc R U . . .
H58B H 0.356774 0.479254 0.812310 0.071 Uiso 1 1 calc R U . . .
H58C H 0.354862 0.487847 0.913716 0.071 Uiso 1 1 calc R U . . .
C59 C 0.1654(3) 0.3480(4) 0.8692(3) 0.0485(11) Uani 1 1 d . . . . .
H59A H 0.187379 0.346809 0.929901 0.073 Uiso 1 1 calc R U . . .
H59B H 0.105044 0.310813 0.835499 0.073 Uiso 1 1 calc R U . . .
H59C H 0.161516 0.414061 0.882575 0.073 Uiso 1 1 calc R U . . .
C60 C 0.1837(3) 0.1290(3) 0.7587(3) 0.0408(9) Uani 1 1 d . . . . .
H60A H 0.207373 0.131071 0.820795 0.061 Uiso 1 1 calc R U . . .
H60B H 0.190127 0.066978 0.706724 0.061 Uiso 1 1 calc R U . . .
H60C H 0.119310 0.138126 0.750284 0.061 Uiso 1 1 calc R U . . .
C61 C -0.0105(3) 0.1433(3) 0.5913(3) 0.0390(9) Uani 1 1 d . . . . .
H61A H 0.003617 0.200073 0.655004 0.058 Uiso 1 1 calc R U . . .
H61B H -0.010615 0.085918 0.598447 0.058 Uiso 1 1 calc R U . . .
H61C H -0.070522 0.143687 0.553788 0.058 Uiso 1 1 calc R U . . .
C62 C 0.0600(2) 0.1437(2) 0.5401(3) 0.0295(7) Uani 1 1 d . . . . .
C63 C 0.1381(3) 0.0944(2) 0.5335(3) 0.0310(8) Uani 1 1 d . . . . .
H63 H 0.156490 0.056301 0.563111 0.037 Uiso 1 1 calc R U . . .
C64 C 0.1837(3) 0.1122(2) 0.4751(3) 0.0287(7) Uani 1 1 d . . . . .
C65 C 0.1335(2) 0.1738(2) 0.4454(2) 0.0249(7) Uani 1 1 d . . . . .
C66 C 0.0591(2) 0.1941(2) 0.4885(2) 0.0257(7) Uani 1 1 d . . . . .
H66 H 0.015805 0.235033 0.483368 0.031 Uiso 1 1 calc R U . . .
C67 C 0.2617(3) 0.0785(3) 0.4411(3) 0.0377(9) Uani 1 1 d . . . . .
H67 H 0.296039 0.038676 0.460734 0.045 Uiso 1 1 calc R U . . .
C68 C 0.2861(3) 0.1042(3) 0.3803(3) 0.0406(9) Uani 1 1 d . . . . .
H68 H 0.337756 0.081576 0.357026 0.049 Uiso 1 1 calc R U . . .
C69 C 0.2360(3) 0.1642(3) 0.3507(3) 0.0337(8) Uani 1 1 d . . . . .
H69 H 0.255436 0.180379 0.308026 0.040 Uiso 1 1 calc R U . . .
C70 C 0.1608(2) 0.1996(2) 0.3812(2) 0.0265(7) Uani 1 1 d . . . . .
C71 C 0.1089(2) 0.2618(2) 0.3495(2) 0.0236(6) Uani 1 1 d . . . . .
C72 C 0.0877(3) 0.2396(3) 0.2526(3) 0.0295(7) Uani 1 1 d . . . . .
H72 H 0.106426 0.184015 0.206869 0.035 Uiso 1 1 calc R U . . .
C73 C 0.0396(3) 0.2981(3) 0.2233(2) 0.0303(7) Uani 1 1 d . . . . .
H73 H 0.026511 0.283205 0.157719 0.036 Uiso 1 1 calc R U . . .
C74 C 0.0104(2) 0.3786(2) 0.2893(2) 0.0257(7) Uani 1 1 d . . . . .
H74 H -0.023607 0.417736 0.268337 0.031 Uiso 1 1 calc R U . . .
C75 C 0.0307(2) 0.4024(2) 0.3862(2) 0.0205(6) Uani 1 1 d . . . . .
C76 C 0.0806(2) 0.3437(2) 0.4152(2) 0.0212(6) Uani 1 1 d . . . . .
H76 H 0.095522 0.359884 0.481209 0.025 Uiso 1 1 calc R U . . .
C77 C -0.0016(2) 0.4877(2) 0.4546(2) 0.0199(6) Uani 1 1 d . . . . .
H77 H -0.027084 0.529139 0.431610 0.024 Uiso 1 1 calc R U . . .
C101 C 0.9079(4) 0.2020(4) 0.8189(5) 0.0697(6) Uani 1 1 d . . . . .
H10D H 0.872173 0.231135 0.866157 0.105 Uiso 1 1 calc R U . . .
H10E H 0.866970 0.162467 0.754923 0.105 Uiso 1 1 calc R U . . .
H10F H 0.944291 0.252217 0.818354 0.105 Uiso 1 1 calc R U . . .
C102 C 0.9690(2) 0.1418(3) 0.8453(3) 0.0697(6) Uani 1 1 d G . . . .
C103 C 1.0298(3) 0.1793(2) 0.9355(3) 0.0697(6) Uani 1 1 d G . . . .
H103 H 1.033927 0.244894 0.980913 0.084 Uiso 1 1 calc R U . . .
C104 C 1.0846(2) 0.1207(3) 0.9594(2) 0.0697(6) Uani 1 1 d G . . . .
H104 H 1.126194 0.146313 1.021088 0.084 Uiso 1 1 calc R U . . .
C105 C 1.0786(2) 0.0247(2) 0.8930(3) 0.0697(6) Uani 1 1 d G . . . .
H105 H 1.116093 -0.015292 0.909313 0.084 Uiso 1 1 calc R U . . .
C106 C 1.0178(3) -0.0127(2) 0.8027(3) 0.0697(6) Uani 1 1 d G . . . .
H106 H 1.013724 -0.078318 0.757364 0.084 Uiso 1 1 calc R U . . .
C107 C 0.9630(2) 0.0458(3) 0.7789(2) 0.0697(6) Uani 1 1 d G . . . .
H107 H 0.921455 0.020261 0.717188 0.084 Uiso 1 1 calc R U . . .
C111 C 0.7722(6) 0.0039(5) -0.1062(5) 0.0929(9) Uani 1 1 d . . . . .
H11D H 0.735553 -0.048914 -0.110024 0.139 Uiso 1 1 calc R U . . .
H11E H 0.835509 0.007506 -0.073054 0.139 Uiso 1 1 calc R U . . .
H11F H 0.768836 -0.007022 -0.171235 0.139 Uiso 1 1 calc R U . . .
C112 C 0.7373(4) 0.0933(3) -0.0527(3) 0.0929(9) Uani 1 1 d G . . . .
C113 C 0.6456(3) 0.1046(3) -0.0680(3) 0.0929(9) Uani 1 1 d G . . . .
H113 H 0.601362 0.051494 -0.113423 0.111 Uiso 1 1 calc R U . . .
C114 C 0.6186(3) 0.1934(4) -0.0170(3) 0.0929(9) Uani 1 1 d G . . . .
H114 H 0.555976 0.201108 -0.027446 0.111 Uiso 1 1 calc R U . . .
C115 C 0.6834(4) 0.2711(3) 0.0495(3) 0.0929(9) Uani 1 1 d G . . . .
H115 H 0.664926 0.331832 0.084368 0.111 Uiso 1 1 calc R U . . .
C116 C 0.7750(3) 0.2599(3) 0.0648(3) 0.0929(9) Uani 1 1 d G . . . .
H116 H 0.819264 0.312944 0.110205 0.111 Uiso 1 1 calc R U . . .
C117 C 0.8020(3) 0.1710(4) 0.0137(3) 0.0929(9) Uani 1 1 d G . . . .
H117 H 0.864652 0.163331 0.024229 0.111 Uiso 1 1 calc R U . . .
C121 C 0.2618(5) 0.3724(6) 1.1920(6) 0.1024(10) Uani 1 1 d . . . . .
H12A H 0.286304 0.426798 1.256409 0.154 Uiso 1 1 calc R U . . .
H12B H 0.265733 0.312954 1.195353 0.154 Uiso 1 1 calc R U . . .
H12C H 0.198165 0.377205 1.167585 0.154 Uiso 1 1 calc R U . . .
C122 C 0.3134(3) 0.3725(5) 1.1286(4) 0.1024(10) Uani 1 1 d G . . . .
C123 C 0.3567(3) 0.4571(3) 1.1441(3) 0.1024(10) Uani 1 1 d G . . . .
H123 H 0.350864 0.516181 1.196260 0.123 Uiso 1 1 calc R U . . .
C124 C 0.4085(3) 0.4554(3) 1.0834(4) 0.1024(10) Uani 1 1 d G . . . .
H124 H 0.438100 0.513197 1.094002 0.123 Uiso 1 1 calc R U . . .
C125 C 0.4171(3) 0.3690(4) 1.0072(4) 0.1024(10) Uani 1 1 d G . . . .
H125 H 0.452477 0.367767 0.965646 0.123 Uiso 1 1 calc R U . . .
C126 C 0.3738(3) 0.2844(3) 0.9917(3) 0.1024(10) Uani 1 1 d G . . . .
H126 H 0.379616 0.225320 0.939546 0.123 Uiso 1 1 calc R U . . .
C127 C 0.3220(3) 0.2861(4) 1.0524(4) 0.1024(10) Uani 1 1 d G . . . .
H127 H 0.292379 0.228303 1.041803 0.123 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 Cl1 2.4380(9) . ?
Zr1 C16 2.464(3) . ?
Zr1 Cl2 2.4662(8) . ?
Zr1 C5 2.517(3) . ?
Zr1 C1 2.521(3) . ?
Zr1 C3 2.526(3) . ?
Zr1 C2 2.530(3) . ?
Zr1 C12 2.537(3) . ?
Zr1 C4 2.538(3) . ?
Zr1 C15 2.544(3) . ?
Zr1 C13 2.596(3) . ?
Zr1 C14 2.640(3) . ?
C1 C2 1.418(5) . ?
C1 C5 1.437(5) . ?
C1 C6 1.499(5) . ?
C2 C3 1.408(5) . ?
C2 C7 1.508(5) . ?
C3 C4 1.424(5) . ?
C3 C8 1.499(5) . ?
C4 C5 1.417(5) . ?
C4 C9 1.497(5) . ?
C5 C10 1.500(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.502(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.412(5) . ?
C12 C16 1.416(5) . ?
C13 C14 1.429(5) . ?
C13 H13 0.9500 . ?
C14 C20 1.426(5) . ?
C14 C15 1.446(4) . ?
C15 C17 1.419(5) . ?
C15 C16 1.425(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.360(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.426(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.476(5) . ?
C21 C22 1.390(5) . ?
C21 C26 1.397(5) . ?
C22 C23 1.395(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.383(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.397(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.400(4) . ?
C25 C27 1.468(4) . ?
C26 H26 0.9500 . ?
C27 C27 1.333(7) 2_656 ?
C27 H27 0.9500 . ?
Zr2 Cl12 2.4402(9) . ?
Zr2 C63 2.465(3) . ?
Zr2 Cl11 2.4677(8) . ?
Zr2 C53 2.494(4) . ?
Zr2 C51 2.520(3) . ?
Zr2 C54 2.521(4) . ?
Zr2 C62 2.525(4) . ?
Zr2 C55 2.527(3) . ?
Zr2 C52 2.532(3) . ?
Zr2 C64 2.534(3) . ?
Zr2 C66 2.582(3) . ?
Zr2 C65 2.629(3) . ?
C51 C52 1.426(5) . ?
C51 C55 1.428(5) . ?
C51 C56 1.503(5) . ?
C52 C53 1.430(5) . ?
C52 C57 1.497(5) . ?
C53 C54 1.412(6) . ?
C53 C58 1.496(5) . ?
C54 C55 1.411(5) . ?
C54 C59 1.501(5) . ?
C55 C60 1.506(5) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.504(5) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C66 1.412(5) . ?
C62 C63 1.426(5) . ?
C63 C64 1.423(5) . ?
C63 H63 0.9500 . ?
C64 C67 1.425(5) . ?
C64 C65 1.443(5) . ?
C65 C66 1.425(5) . ?
C65 C70 1.430(5) . ?
C66 H66 0.9500 . ?
C67 C68 1.357(6) . ?
C67 H67 0.9500 . ?
C68 C69 1.419(5) . ?
C68 H68 0.9500 . ?
C69 C70 1.371(5) . ?
C69 H69 0.9500 . ?
C70 C71 1.480(5) . ?
C71 C76 1.395(4) . ?
C71 C72 1.402(5) . ?
C72 C73 1.384(5) . ?
C72 H72 0.9500 . ?
C73 C74 1.392(5) . ?
C73 H73 0.9500 . ?
C74 C75 1.395(4) . ?
C74 H74 0.9500 . ?
C75 C76 1.397(4) . ?
C75 C77 1.473(4) . ?
C76 H76 0.9500 . ?
C77 C77 1.330(6) 2_566 ?
C77 H77 0.9500 . ?
C101 C102 1.482(6) . ?
C101 H10D 0.9800 . ?
C101 H10E 0.9800 . ?
C101 H10F 0.9800 . ?
C102 C103 1.3900 . ?
C102 C107 1.3900 . ?
C103 C104 1.3900 . ?
C103 H103 0.9500 . ?
C104 C105 1.3900 . ?
C104 H104 0.9500 . ?
C105 C106 1.3900 . ?
C105 H105 0.9500 . ?
C106 C107 1.3900 . ?
C106 H106 0.9500 . ?
C107 H107 0.9500 . ?
C111 C112 1.462(8) . ?
C111 H11D 0.9800 . ?
C111 H11E 0.9800 . ?
C111 H11F 0.9800 . ?
C112 C113 1.3900 . ?
C112 C117 1.3900 . ?
C113 C114 1.3900 . ?
C113 H113 0.9500 . ?
C114 C115 1.3900 . ?
C114 H114 0.9500 . ?
C115 C116 1.3900 . ?
C115 H115 0.9500 . ?
C116 C117 1.3900 . ?
C116 H116 0.9500 . ?
C117 H117 0.9500 . ?
C121 C122 1.433(9) . ?
C121 H12A 0.9800 . ?
C121 H12B 0.9800 . ?
C121 H12C 0.9800 . ?
C122 C123 1.3900 . ?
C122 C127 1.3900 . ?
C123 C124 1.3900 . ?
C123 H123 0.9500 . ?
C124 C125 1.3900 . ?
C124 H124 0.9500 . ?
C125 C126 1.3900 . ?
C125 H125 0.9500 . ?
C126 C127 1.3900 . ?
C126 H126 0.9500 . ?
C127 H127 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Zr1 C16 124.68(9) . . ?
Cl1 Zr1 Cl2 95.23(3) . . ?
C16 Zr1 Cl2 120.44(9) . . ?
Cl1 Zr1 C5 105.52(8) . . ?
C16 Zr1 C5 80.67(11) . . ?
Cl2 Zr1 C5 133.27(8) . . ?
Cl1 Zr1 C1 133.94(9) . . ?
C16 Zr1 C1 78.57(12) . . ?
Cl2 Zr1 C1 105.61(8) . . ?
C5 Zr1 C1 33.16(11) . . ?
Cl1 Zr1 C3 87.81(9) . . ?
C16 Zr1 C3 131.42(11) . . ?
Cl2 Zr1 C3 86.09(8) . . ?
C5 Zr1 C3 54.23(11) . . ?
C1 Zr1 C3 54.17(12) . . ?
Cl1 Zr1 C2 119.74(9) . . ?
C16 Zr1 C2 108.27(12) . . ?
Cl2 Zr1 C2 79.12(8) . . ?
C5 Zr1 C2 54.19(11) . . ?
C1 Zr1 C2 32.60(11) . . ?
C3 Zr1 C2 32.35(12) . . ?
Cl1 Zr1 C12 131.40(9) . . ?
C16 Zr1 C12 32.86(11) . . ?
Cl2 Zr1 C12 87.84(8) . . ?
C5 Zr1 C12 107.03(11) . . ?
C1 Zr1 C12 90.69(12) . . ?
C3 Zr1 C12 140.74(12) . . ?
C2 Zr1 C12 108.50(12) . . ?
Cl1 Zr1 C4 79.67(9) . . ?
C16 Zr1 C4 111.65(12) . . ?
Cl2 Zr1 C4 118.18(9) . . ?
C5 Zr1 C4 32.55(11) . . ?
C1 Zr1 C4 54.27(11) . . ?
C3 Zr1 C4 32.67(12) . . ?
C2 Zr1 C4 53.80(12) . . ?
C12 Zr1 C4 139.56(12) . . ?
Cl1 Zr1 C15 91.66(9) . . ?
C16 Zr1 C15 33.02(12) . . ?
Cl2 Zr1 C15 132.13(8) . . ?
C5 Zr1 C15 89.27(11) . . ?
C1 Zr1 C15 102.93(11) . . ?
C3 Zr1 C15 141.57(11) . . ?
C2 Zr1 C15 135.50(11) . . ?
C12 Zr1 C15 54.10(12) . . ?
C4 Zr1 C15 109.66(12) . . ?
Cl1 Zr1 C13 101.34(8) . . ?
C16 Zr1 C13 53.67(11) . . ?
Cl2 Zr1 C13 78.79(8) . . ?
C5 Zr1 C13 134.34(11) . . ?
C1 Zr1 C13 122.55(11) . . ?
C3 Zr1 C13 162.92(12) . . ?
C2 Zr1 C13 134.64(12) . . ?
C12 Zr1 C13 31.90(11) . . ?
C4 Zr1 C13 162.96(11) . . ?
C15 Zr1 C13 53.45(11) . . ?
Cl1 Zr1 C14 79.36(8) . . ?
C16 Zr1 C14 53.73(11) . . ?
Cl2 Zr1 C14 103.24(7) . . ?
C5 Zr1 C14 121.30(10) . . ?
C1 Zr1 C14 132.00(11) . . ?
C3 Zr1 C14 164.69(12) . . ?
C2 Zr1 C14 160.70(12) . . ?
C12 Zr1 C14 52.98(11) . . ?
C4 Zr1 C14 134.81(11) . . ?
C15 Zr1 C14 32.33(10) . . ?
C13 Zr1 C14 31.66(10) . . ?
C2 C1 C5 107.2(3) . . ?
C2 C1 C6 125.8(3) . . ?
C5 C1 C6 125.9(3) . . ?
C2 C1 Zr1 74.03(19) . . ?
C5 C1 Zr1 73.25(18) . . ?
C6 C1 Zr1 127.6(2) . . ?
C3 C2 C1 108.8(3) . . ?
C3 C2 C7 126.5(4) . . ?
C1 C2 C7 124.2(4) . . ?
C3 C2 Zr1 73.7(2) . . ?
C1 C2 Zr1 73.38(19) . . ?
C7 C2 Zr1 125.0(2) . . ?
C2 C3 C4 108.1(3) . . ?
C2 C3 C8 126.4(4) . . ?
C4 C3 C8 125.4(4) . . ?
C2 C3 Zr1 74.0(2) . . ?
C4 C3 Zr1 74.1(2) . . ?
C8 C3 Zr1 121.2(2) . . ?
C5 C4 C3 108.0(3) . . ?
C5 C4 C9 124.9(3) . . ?
C3 C4 C9 126.9(3) . . ?
C5 C4 Zr1 72.91(19) . . ?
C3 C4 Zr1 73.19(19) . . ?
C9 C4 Zr1 124.1(3) . . ?
C4 C5 C1 107.9(3) . . ?
C4 C5 C10 125.6(3) . . ?
C1 C5 C10 125.5(3) . . ?
C4 C5 Zr1 74.54(18) . . ?
C1 C5 Zr1 73.60(18) . . ?
C10 C5 Zr1 126.9(2) . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C16 108.0(3) . . ?
C13 C12 C11 124.8(3) . . ?
C16 C12 C11 127.2(3) . . ?
C13 C12 Zr1 76.4(2) . . ?
C16 C12 Zr1 70.74(19) . . ?
C11 C12 Zr1 119.0(2) . . ?
C12 C13 C14 108.9(3) . . ?
C12 C13 Zr1 71.72(19) . . ?
C14 C13 Zr1 75.84(19) . . ?
C12 C13 H13 125.6 . . ?
C14 C13 H13 125.6 . . ?
Zr1 C13 H13 118.7 . . ?
C20 C14 C13 132.3(3) . . ?
C20 C14 C15 120.6(3) . . ?
C13 C14 C15 107.0(3) . . ?
C20 C14 Zr1 124.3(2) . . ?
C13 C14 Zr1 72.50(18) . . ?
C15 C14 Zr1 70.20(18) . . ?
C17 C15 C16 133.5(3) . . ?
C17 C15 C14 119.2(3) . . ?
C16 C15 C14 107.2(3) . . ?
C17 C15 Zr1 119.7(3) . . ?
C16 C15 Zr1 70.39(19) . . ?
C14 C15 Zr1 77.47(19) . . ?
C12 C16 C15 108.8(3) . . ?
C12 C16 Zr1 76.40(19) . . ?
C15 C16 Zr1 76.6(2) . . ?
C12 C16 H16 125.6 . . ?
C15 C16 H16 125.6 . . ?
Zr1 C16 H16 113.7 . . ?
C18 C17 C15 119.4(3) . . ?
C18 C17 H17 120.3 . . ?
C15 C17 H17 120.3 . . ?
C17 C18 C19 121.2(3) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C20 C19 C18 122.3(3) . . ?
C20 C19 H19 118.9 . . ?
C18 C19 H19 118.9 . . ?
C19 C20 C14 117.3(3) . . ?
C19 C20 C21 121.5(3) . . ?
C14 C20 C21 121.2(3) . . ?
C22 C21 C26 118.9(3) . . ?
C22 C21 C20 120.9(3) . . ?
C26 C21 C20 120.1(3) . . ?
C21 C22 C23 120.6(3) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C24 C23 C22 119.9(3) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 120.8(3) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C24 C25 C26 118.6(3) . . ?
C24 C25 C27 119.7(3) . . ?
C26 C25 C27 121.7(3) . . ?
C21 C26 C25 121.1(3) . . ?
C21 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C27 C27 C25 126.3(4) 2_656 . ?
C27 C27 H27 116.8 2_656 . ?
C25 C27 H27 116.8 . . ?
Cl12 Zr2 C63 123.93(9) . . ?
Cl12 Zr2 Cl11 95.48(3) . . ?
C63 Zr2 Cl11 120.77(9) . . ?
Cl12 Zr2 C53 88.02(10) . . ?
C63 Zr2 C53 131.91(12) . . ?
Cl11 Zr2 C53 85.59(9) . . ?
Cl12 Zr2 C51 104.64(8) . . ?
C63 Zr2 C51 80.86(12) . . ?
Cl11 Zr2 C51 133.87(9) . . ?
C53 Zr2 C51 54.78(12) . . ?
Cl12 Zr2 C54 120.49(10) . . ?
C63 Zr2 C54 107.87(13) . . ?
Cl11 Zr2 C54 79.69(8) . . ?
C53 Zr2 C54 32.70(13) . . ?
C51 Zr2 C54 54.28(11) . . ?
Cl12 Zr2 C62 131.46(9) . . ?
C63 Zr2 C62 33.19(12) . . ?
Cl11 Zr2 C62 87.77(9) . . ?
C53 Zr2 C62 140.44(13) . . ?
C51 Zr2 C62 107.39(12) . . ?
C54 Zr2 C62 107.78(13) . . ?
Cl12 Zr2 C55 133.16(9) . . ?
C63 Zr2 C55 78.65(12) . . ?
Cl11 Zr2 C55 106.70(8) . . ?
C53 Zr2 C55 54.33(12) . . ?
C51 Zr2 C55 32.87(11) . . ?
C54 Zr2 C55 32.47(12) . . ?
C62 Zr2 C55 90.93(12) . . ?
Cl12 Zr2 C52 79.05(9) . . ?
C63 Zr2 C52 112.14(12) . . ?
Cl11 Zr2 C52 117.93(9) . . ?
C53 Zr2 C52 33.05(12) . . ?
C51 Zr2 C52 32.79(11) . . ?
C54 Zr2 C52 54.10(12) . . ?
C62 Zr2 C52 140.13(12) . . ?
C55 Zr2 C52 54.13(12) . . ?
Cl12 Zr2 C64 90.91(9) . . ?
C63 Zr2 C64 33.04(12) . . ?
Cl11 Zr2 C64 131.68(8) . . ?
C53 Zr2 C64 142.58(12) . . ?
C51 Zr2 C64 89.62(11) . . ?
C54 Zr2 C64 135.42(12) . . ?
C62 Zr2 C64 54.33(12) . . ?
C55 Zr2 C64 103.03(12) . . ?
C52 Zr2 C64 110.32(12) . . ?
Cl12 Zr2 C66 101.38(8) . . ?
C63 Zr2 C66 53.97(11) . . ?
Cl11 Zr2 C66 78.31(8) . . ?
C53 Zr2 C66 162.00(12) . . ?
C51 Zr2 C66 134.83(11) . . ?
C54 Zr2 C66 134.09(12) . . ?
C62 Zr2 C66 32.08(11) . . ?
C55 Zr2 C66 122.99(12) . . ?
C52 Zr2 C66 163.73(11) . . ?
C64 Zr2 C66 53.52(11) . . ?
Cl12 Zr2 C65 78.97(8) . . ?
C63 Zr2 C65 53.97(11) . . ?
Cl11 Zr2 C65 102.54(7) . . ?
C53 Zr2 C65 165.18(12) . . ?
C51 Zr2 C65 121.67(11) . . ?
C54 Zr2 C65 160.35(12) . . ?
C62 Zr2 C65 53.27(11) . . ?
C55 Zr2 C65 132.29(11) . . ?
C52 Zr2 C65 135.28(11) . . ?
C64 Zr2 C65 32.40(10) . . ?
C66 Zr2 C65 31.73(10) . . ?
C52 C51 C55 107.5(3) . . ?
C52 C51 C56 125.0(3) . . ?
C55 C51 C56 126.2(3) . . ?
C52 C51 Zr2 74.08(19) . . ?
C55 C51 Zr2 73.83(18) . . ?
C56 C51 Zr2 127.7(3) . . ?
C51 C52 C53 107.7(3) . . ?
C51 C52 C57 124.9(3) . . ?
C53 C52 C57 127.2(4) . . ?
C51 C52 Zr2 73.12(19) . . ?
C53 C52 Zr2 72.0(2) . . ?
C57 C52 Zr2 124.3(3) . . ?
C54 C53 C52 107.9(3) . . ?
C54 C53 C58 125.9(4) . . ?
C52 C53 C58 126.0(4) . . ?
C54 C53 Zr2 74.7(2) . . ?
C52 C53 Zr2 74.9(2) . . ?
C58 C53 Zr2 120.1(3) . . ?
C55 C54 C53 108.6(3) . . ?
C55 C54 C59 124.7(4) . . ?
C53 C54 C59 126.3(4) . . ?
C55 C54 Zr2 74.0(2) . . ?
C53 C54 Zr2 72.6(2) . . ?
C59 C54 Zr2 125.3(3) . . ?
C54 C55 C51 108.2(3) . . ?
C54 C55 C60 125.8(3) . . ?
C51 C55 C60 124.9(3) . . ?
C54 C55 Zr2 73.6(2) . . ?
C51 C55 Zr2 73.31(19) . . ?
C60 C55 Zr2 128.3(3) . . ?
C51 C56 H56A 109.5 . . ?
C51 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C51 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C52 C57 H57A 109.5 . . ?
C52 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C52 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C53 C58 H58A 109.5 . . ?
C53 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C53 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C54 C59 H59A 109.5 . . ?
C54 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C54 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C55 C60 H60A 109.5 . . ?
C55 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C55 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 H61A 109.5 . . ?
C62 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C62 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C66 C62 C63 107.7(3) . . ?
C66 C62 C61 124.8(3) . . ?
C63 C62 C61 127.5(3) . . ?
C66 C62 Zr2 76.2(2) . . ?
C63 C62 Zr2 71.1(2) . . ?
C61 C62 Zr2 118.9(3) . . ?
C64 C63 C62 108.3(3) . . ?
C64 C63 Zr2 76.2(2) . . ?
C62 C63 Zr2 75.7(2) . . ?
C64 C63 H63 125.8 . . ?
C62 C63 H63 125.8 . . ?
Zr2 C63 H63 114.5 . . ?
C63 C64 C67 132.7(3) . . ?
C63 C64 C65 107.8(3) . . ?
C67 C64 C65 119.4(3) . . ?
C63 C64 Zr2 70.78(19) . . ?
C67 C64 Zr2 120.2(3) . . ?
C65 C64 Zr2 77.43(19) . . ?
C66 C65 C70 132.7(3) . . ?
C66 C65 C64 106.9(3) . . ?
C70 C65 C64 120.3(3) . . ?
C66 C65 Zr2 72.32(19) . . ?
C70 C65 Zr2 124.1(2) . . ?
C64 C65 Zr2 70.18(19) . . ?
C62 C66 C65 109.2(3) . . ?
C62 C66 Zr2 71.7(2) . . ?
C65 C66 Zr2 75.95(19) . . ?
C62 C66 H66 125.4 . . ?
C65 C66 H66 125.4 . . ?
Zr2 C66 H66 118.7 . . ?
C68 C67 C64 118.9(3) . . ?
C68 C67 H67 120.5 . . ?
C64 C67 H67 120.5 . . ?
C67 C68 C69 121.4(3) . . ?
C67 C68 H68 119.3 . . ?
C69 C68 H68 119.3 . . ?
C70 C69 C68 122.7(4) . . ?
C70 C69 H69 118.6 . . ?
C68 C69 H69 118.6 . . ?
C69 C70 C65 117.2(3) . . ?
C69 C70 C71 122.3(3) . . ?
C65 C70 C71 120.6(3) . . ?
C76 C71 C72 118.7(3) . . ?
C76 C71 C70 120.8(3) . . ?
C72 C71 C70 120.4(3) . . ?
C73 C72 C71 120.3(3) . . ?
C73 C72 H72 119.8 . . ?
C71 C72 H72 119.8 . . ?
C72 C73 C74 120.3(3) . . ?
C72 C73 H73 119.8 . . ?
C74 C73 H73 119.8 . . ?
C73 C74 C75 120.5(3) . . ?
C73 C74 H74 119.7 . . ?
C75 C74 H74 119.7 . . ?
C74 C75 C76 118.7(3) . . ?
C74 C75 C77 119.5(3) . . ?
C76 C75 C77 121.9(3) . . ?
C71 C76 C75 121.5(3) . . ?
C71 C76 H76 119.3 . . ?
C75 C76 H76 119.3 . . ?
C77 C77 C75 126.3(4) 2_566 . ?
C77 C77 H77 116.9 2_566 . ?
C75 C77 H77 116.9 . . ?
C102 C101 H10D 109.5 . . ?
C102 C101 H10E 109.5 . . ?
H10D C101 H10E 109.5 . . ?
C102 C101 H10F 109.5 . . ?
H10D C101 H10F 109.5 . . ?
H10E C101 H10F 109.5 . . ?
C103 C102 C107 120.0 . . ?
C103 C102 C101 121.1(4) . . ?
C107 C102 C101 118.9(4) . . ?
C104 C103 C102 120.0 . . ?
C104 C103 H103 120.0 . . ?
C102 C103 H103 120.0 . . ?
C105 C104 C103 120.0 . . ?
C105 C104 H104 120.0 . . ?
C103 C104 H104 120.0 . . ?
C106 C105 C104 120.0 . . ?
C106 C105 H105 120.0 . . ?
C104 C105 H105 120.0 . . ?
C105 C106 C107 120.0 . . ?
C105 C106 H106 120.0 . . ?
C107 C106 H106 120.0 . . ?
C106 C107 C102 120.0 . . ?
C106 C107 H107 120.0 . . ?
C102 C107 H107 120.0 . . ?
C112 C111 H11D 109.5 . . ?
C112 C111 H11E 109.5 . . ?
H11D C111 H11E 109.5 . . ?
C112 C111 H11F 109.5 . . ?
H11D C111 H11F 109.5 . . ?
H11E C111 H11F 109.5 . . ?
C113 C112 C117 120.0 . . ?
C113 C112 C111 123.8(5) . . ?
C117 C112 C111 116.1(5) . . ?
C112 C113 C114 120.0 . . ?
C112 C113 H113 120.0 . . ?
C114 C113 H113 120.0 . . ?
C113 C114 C115 120.0 . . ?
C113 C114 H114 120.0 . . ?
C115 C114 H114 120.0 . . ?
C116 C115 C114 120.0 . . ?
C116 C115 H115 120.0 . . ?
C114 C115 H115 120.0 . . ?
C115 C116 C117 120.0 . . ?
C115 C116 H116 120.0 . . ?
C117 C116 H116 120.0 . . ?
C116 C117 C112 120.0 . . ?
C116 C117 H117 120.0 . . ?
C112 C117 H117 120.0 . . ?
C122 C121 H12A 109.5 . . ?
C122 C121 H12B 109.5 . . ?
H12A C121 H12B 109.5 . . ?
C122 C121 H12C 109.5 . . ?
H12A C121 H12C 109.5 . . ?
H12B C121 H12C 109.5 . . ?
C123 C122 C127 120.0 . . ?
C123 C122 C121 121.0(6) . . ?
C127 C122 C121 119.0(6) . . ?
C122 C123 C124 120.0 . . ?
C122 C123 H123 120.0 . . ?
C124 C123 H123 120.0 . . ?
C125 C124 C123 120.0 . . ?
C125 C124 H124 120.0 . . ?
C123 C124 H124 120.0 . . ?
C126 C125 C124 120.0 . . ?
C126 C125 H125 120.0 . . ?
C124 C125 H125 120.0 . . ?
C125 C126 C127 120.0 . . ?
C125 C126 H126 120.0 . . ?
C127 C126 H126 120.0 . . ?
C126 C127 C122 120.0 . . ?
C126 C127 H127 120.0 . . ?
C122 C127 H127 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 0.6(4) . . . . ?
C6 C1 C2 C3 169.1(3) . . . . ?
Zr1 C1 C2 C3 -65.7(2) . . . . ?
C5 C1 C2 C7 -172.4(3) . . . . ?
C6 C1 C2 C7 -3.8(6) . . . . ?
Zr1 C1 C2 C7 121.4(3) . . . . ?
C5 C1 C2 Zr1 66.3(2) . . . . ?
C6 C1 C2 Zr1 -125.2(3) . . . . ?
C1 C2 C3 C4 -1.4(4) . . . . ?
C7 C2 C3 C4 171.4(3) . . . . ?
Zr1 C2 C3 C4 -66.9(2) . . . . ?
C1 C2 C3 C8 -177.2(3) . . . . ?
C7 C2 C3 C8 -4.5(6) . . . . ?
Zr1 C2 C3 C8 117.3(4) . . . . ?
C1 C2 C3 Zr1 65.5(2) . . . . ?
C7 C2 C3 Zr1 -121.8(4) . . . . ?
C2 C3 C4 C5 1.7(4) . . . . ?
C8 C3 C4 C5 177.5(3) . . . . ?
Zr1 C3 C4 C5 -65.1(2) . . . . ?
C2 C3 C4 C9 -172.9(4) . . . . ?
C8 C3 C4 C9 3.0(6) . . . . ?
Zr1 C3 C4 C9 120.3(4) . . . . ?
C2 C3 C4 Zr1 66.8(2) . . . . ?
C8 C3 C4 Zr1 -117.4(4) . . . . ?
C3 C4 C5 C1 -1.3(4) . . . . ?
C9 C4 C5 C1 173.4(3) . . . . ?
Zr1 C4 C5 C1 -66.6(2) . . . . ?
C3 C4 C5 C10 -170.1(3) . . . . ?
C9 C4 C5 C10 4.6(6) . . . . ?
Zr1 C4 C5 C10 124.6(3) . . . . ?
C3 C4 C5 Zr1 65.3(2) . . . . ?
C9 C4 C5 Zr1 -120.0(4) . . . . ?
C2 C1 C5 C4 0.5(4) . . . . ?
C6 C1 C5 C4 -168.1(3) . . . . ?
Zr1 C1 C5 C4 67.2(2) . . . . ?
C2 C1 C5 C10 169.2(3) . . . . ?
C6 C1 C5 C10 0.7(6) . . . . ?
Zr1 C1 C5 C10 -124.0(3) . . . . ?
C2 C1 C5 Zr1 -66.8(2) . . . . ?
C6 C1 C5 Zr1 124.7(4) . . . . ?
C16 C12 C13 C14 3.2(4) . . . . ?
C11 C12 C13 C14 -176.5(3) . . . . ?
Zr1 C12 C13 C14 67.4(2) . . . . ?
C16 C12 C13 Zr1 -64.2(2) . . . . ?
C11 C12 C13 Zr1 116.1(3) . . . . ?
C12 C13 C14 C20 174.5(4) . . . . ?
Zr1 C13 C14 C20 -120.8(4) . . . . ?
C12 C13 C14 C15 -2.6(4) . . . . ?
Zr1 C13 C14 C15 62.1(2) . . . . ?
C12 C13 C14 Zr1 -64.7(2) . . . . ?
C20 C14 C15 C17 1.7(5) . . . . ?
C13 C14 C15 C17 179.2(3) . . . . ?
Zr1 C14 C15 C17 -117.2(3) . . . . ?
C20 C14 C15 C16 -176.5(3) . . . . ?
C13 C14 C15 C16 1.0(4) . . . . ?
Zr1 C14 C15 C16 64.6(2) . . . . ?
C20 C14 C15 Zr1 118.9(3) . . . . ?
C13 C14 C15 Zr1 -63.6(2) . . . . ?
C13 C12 C16 C15 -2.5(4) . . . . ?
C11 C12 C16 C15 177.2(3) . . . . ?
Zr1 C12 C16 C15 -70.5(2) . . . . ?
C13 C12 C16 Zr1 67.9(2) . . . . ?
C11 C12 C16 Zr1 -112.4(4) . . . . ?
C17 C15 C16 C12 -176.9(4) . . . . ?
C14 C15 C16 C12 0.9(4) . . . . ?
Zr1 C15 C16 C12 70.3(2) . . . . ?
C17 C15 C16 Zr1 112.8(4) . . . . ?
C14 C15 C16 Zr1 -69.4(2) . . . . ?
C16 C15 C17 C18 176.4(4) . . . . ?
C14 C15 C17 C18 -1.2(6) . . . . ?
Zr1 C15 C17 C18 -93.1(4) . . . . ?
C15 C17 C18 C19 0.2(6) . . . . ?
C17 C18 C19 C20 0.4(6) . . . . ?
C18 C19 C20 C14 0.1(6) . . . . ?
C18 C19 C20 C21 -179.8(4) . . . . ?
C13 C14 C20 C19 -177.9(4) . . . . ?
C15 C14 C20 C19 -1.1(5) . . . . ?
Zr1 C14 C20 C19 84.7(4) . . . . ?
C13 C14 C20 C21 2.0(6) . . . . ?
C15 C14 C20 C21 178.8(3) . . . . ?
Zr1 C14 C20 C21 -95.4(4) . . . . ?
C19 C20 C21 C22 44.3(5) . . . . ?
C14 C20 C21 C22 -135.7(4) . . . . ?
C19 C20 C21 C26 -134.2(4) . . . . ?
C14 C20 C21 C26 45.9(5) . . . . ?
C26 C21 C22 C23 -0.4(5) . . . . ?
C20 C21 C22 C23 -178.8(3) . . . . ?
C21 C22 C23 C24 0.0(6) . . . . ?
C22 C23 C24 C25 -0.4(5) . . . . ?
C23 C24 C25 C26 1.1(5) . . . . ?
C23 C24 C25 C27 -178.3(3) . . . . ?
C22 C21 C26 C25 1.2(5) . . . . ?
C20 C21 C26 C25 179.6(3) . . . . ?
C24 C25 C26 C21 -1.5(5) . . . . ?
C27 C25 C26 C21 177.9(3) . . . . ?
C24 C25 C27 C27 170.8(4) . . . 2_656 ?
C26 C25 C27 C27 -8.7(6) . . . 2_656 ?
C55 C51 C52 C53 -2.7(4) . . . . ?
C56 C51 C52 C53 -170.7(3) . . . . ?
Zr2 C51 C52 C53 64.2(2) . . . . ?
C55 C51 C52 C57 172.8(4) . . . . ?
C56 C51 C52 C57 4.8(6) . . . . ?
Zr2 C51 C52 C57 -120.4(4) . . . . ?
C55 C51 C52 Zr2 -66.8(2) . . . . ?
C56 C51 C52 Zr2 125.2(4) . . . . ?
C51 C52 C53 C54 3.2(4) . . . . ?
C57 C52 C53 C54 -172.1(4) . . . . ?
Zr2 C52 C53 C54 68.1(2) . . . . ?
C51 C52 C53 C58 178.6(4) . . . . ?
C57 C52 C53 C58 3.3(6) . . . . ?
Zr2 C52 C53 C58 -116.5(4) . . . . ?
C51 C52 C53 Zr2 -64.9(2) . . . . ?
C57 C52 C53 Zr2 119.8(4) . . . . ?
C52 C53 C54 C55 -2.5(4) . . . . ?
C58 C53 C54 C55 -177.9(3) . . . . ?
Zr2 C53 C54 C55 65.8(3) . . . . ?
C52 C53 C54 C59 170.4(3) . . . . ?
C58 C53 C54 C59 -5.0(6) . . . . ?
Zr2 C53 C54 C59 -121.4(4) . . . . ?
C52 C53 C54 Zr2 -68.2(2) . . . . ?
C58 C53 C54 Zr2 116.3(4) . . . . ?
C53 C54 C55 C51 0.8(4) . . . . ?
C59 C54 C55 C51 -172.2(3) . . . . ?
Zr2 C54 C55 C51 65.7(2) . . . . ?
C53 C54 C55 C60 169.4(3) . . . . ?
C59 C54 C55 C60 -3.6(6) . . . . ?
Zr2 C54 C55 C60 -125.8(4) . . . . ?
C53 C54 C55 Zr2 -64.8(3) . . . . ?
C59 C54 C55 Zr2 122.1(4) . . . . ?
C52 C51 C55 C54 1.2(4) . . . . ?
C56 C51 C55 C54 169.0(4) . . . . ?
Zr2 C51 C55 C54 -65.8(2) . . . . ?
C52 C51 C55 C60 -167.5(3) . . . . ?
C56 C51 C55 C60 0.3(6) . . . . ?
Zr2 C51 C55 C60 125.5(4) . . . . ?
C52 C51 C55 Zr2 67.0(2) . . . . ?
C56 C51 C55 Zr2 -125.2(4) . . . . ?
C66 C62 C63 C64 -1.9(4) . . . . ?
C61 C62 C63 C64 177.8(4) . . . . ?
Zr2 C62 C63 C64 -69.9(3) . . . . ?
C66 C62 C63 Zr2 68.0(2) . . . . ?
C61 C62 C63 Zr2 -112.3(4) . . . . ?
C62 C63 C64 C67 -176.7(4) . . . . ?
Zr2 C63 C64 C67 113.7(4) . . . . ?
C62 C63 C64 C65 0.3(4) . . . . ?
Zr2 C63 C64 C65 -69.3(2) . . . . ?
C62 C63 C64 Zr2 69.6(2) . . . . ?
C63 C64 C65 C66 1.3(4) . . . . ?
C67 C64 C65 C66 178.8(3) . . . . ?
Zr2 C64 C65 C66 -63.5(2) . . . . ?
C63 C64 C65 C70 -176.5(3) . . . . ?
C67 C64 C65 C70 1.0(5) . . . . ?
Zr2 C64 C65 C70 118.7(3) . . . . ?
C63 C64 C65 Zr2 64.8(2) . . . . ?
C67 C64 C65 Zr2 -117.7(3) . . . . ?
C63 C62 C66 C65 2.7(4) . . . . ?
C61 C62 C66 C65 -176.9(3) . . . . ?
Zr2 C62 C66 C65 67.3(2) . . . . ?
C63 C62 C66 Zr2 -64.6(2) . . . . ?
C61 C62 C66 Zr2 115.8(4) . . . . ?
C70 C65 C66 C62 174.9(4) . . . . ?
C64 C65 C66 C62 -2.5(4) . . . . ?
Zr2 C65 C66 C62 -64.6(2) . . . . ?
C70 C65 C66 Zr2 -120.5(4) . . . . ?
C64 C65 C66 Zr2 62.0(2) . . . . ?
C63 C64 C67 C68 175.8(4) . . . . ?
C65 C64 C67 C68 -0.9(6) . . . . ?
Zr2 C64 C67 C68 -93.2(4) . . . . ?
C64 C67 C68 C69 0.4(7) . . . . ?
C67 C68 C69 C70 0.0(7) . . . . ?
C68 C69 C70 C65 0.0(6) . . . . ?
C68 C69 C70 C71 -179.7(4) . . . . ?
C66 C65 C70 C69 -177.7(4) . . . . ?
C64 C65 C70 C69 -0.5(5) . . . . ?
Zr2 C65 C70 C69 85.0(4) . . . . ?
C66 C65 C70 C71 2.0(6) . . . . ?
C64 C65 C70 C71 179.2(3) . . . . ?
Zr2 C65 C70 C71 -95.2(3) . . . . ?
C69 C70 C71 C76 -135.4(4) . . . . ?
C65 C70 C71 C76 44.9(5) . . . . ?
C69 C70 C71 C72 44.2(5) . . . . ?
C65 C70 C71 C72 -135.5(3) . . . . ?
C76 C71 C72 C73 0.1(5) . . . . ?
C70 C71 C72 C73 -179.6(3) . . . . ?
C71 C72 C73 C74 -1.2(5) . . . . ?
C72 C73 C74 C75 1.3(5) . . . . ?
C73 C74 C75 C76 -0.2(5) . . . . ?
C73 C74 C75 C77 -179.6(3) . . . . ?
C72 C71 C76 C75 1.1(5) . . . . ?
C70 C71 C76 C75 -179.3(3) . . . . ?
C74 C75 C76 C71 -1.0(5) . . . . ?
C77 C75 C76 C71 178.4(3) . . . . ?
C74 C75 C77 C77 170.3(4) . . . 2_566 ?
C76 C75 C77 C77 -9.1(6) . . . 2_566 ?
C107 C102 C103 C104 0.0 . . . . ?
C101 C102 C103 C104 178.2(4) . . . . ?
C102 C103 C104 C105 0.0 . . . . ?
C103 C104 C105 C106 0.0 . . . . ?
C104 C105 C106 C107 0.0 . . . . ?
C105 C106 C107 C102 0.0 . . . . ?
C103 C102 C107 C106 0.0 . . . . ?
C101 C102 C107 C106 -178.3(4) . . . . ?
C117 C112 C113 C114 0.0 . . . . ?
C111 C112 C113 C114 -177.0(5) . . . . ?
C112 C113 C114 C115 0.0 . . . . ?
C113 C114 C115 C116 0.0 . . . . ?
C114 C115 C116 C117 0.0 . . . . ?
C115 C116 C117 C112 0.0 . . . . ?
C113 C112 C117 C116 0.0 . . . . ?
C111 C112 C117 C116 177.2(4) . . . . ?
C127 C122 C123 C124 0.0 . . . . ?
C121 C122 C123 C124 178.2(5) . . . . ?
C122 C123 C124 C125 0.0 . . . . ?
C123 C124 C125 C126 0.0 . . . . ?
C124 C125 C126 C127 0.0 . . . . ?
C125 C126 C127 C122 0.0 . . . . ?
C123 C122 C127 C126 0.0 . . . . ?
C121 C122 C127 C126 -178.2(4) . . . . ?

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#                                EMBEDDED FILES                                #
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#                                                                              #

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# .RES SHELXL file: sqz.res
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# ............... End of .HKL file ........................................... #
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#...............................................................................
# .FAB SHELXL file: sqz.fab
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# ............... End of .FAB file ........................................... #
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#===END OF CIF FILE FOR COMPOUND 1 (NR2036)                                    #
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#                                                                              #
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