# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_Complex_1
_database_code_depnum_ccdc_archive 'CCDC 2400987'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-11-06 deposited with the CCDC.	2024-11-28 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 26 septembre 2023                                        #
#------------------------------------------------------------------------------#


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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C18 F15 Pb, C24 H60 Br3.44 Cl1.56 Mg3 O6 [+ solvent]'
_chemical_formula_sum            'C42 H58 Br3.44 Cl1.56 F15 Mg3 O6 Pb'
_chemical_formula_weight         1554.19
_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                   13.228(3)
_cell_length_b                   13.887(3)
_cell_length_c                   17.570(4)
_cell_angle_alpha                69.038(8)
_cell_angle_beta                 85.126(6)
_cell_angle_gamma                85.016(7)
_cell_volume                     2997.8(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    168(2)
_cell_measurement_reflns_used    9990
_cell_measurement_theta_min      2.3186
_cell_measurement_theta_max      27.3488
_cell_measurement_wavelength     0.710730


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

_diffrn_orient_matrix_UB_11      -0.0027578
_diffrn_orient_matrix_UB_21      -0.0690230
_diffrn_orient_matrix_UB_31      -0.0310659
_diffrn_orient_matrix_UB_12      -0.0049934
_diffrn_orient_matrix_UB_22      -0.0268506
_diffrn_orient_matrix_UB_32      0.0720606
_diffrn_orient_matrix_UB_13      -0.0552439
_diffrn_orient_matrix_UB_23      0.0153673
_diffrn_orient_matrix_UB_33      -0.0209636


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

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.180
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1516
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    5.293
_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  0.188
_exptl_absorpt_correction_T_max  0.386

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

# Software                   : BIS V6.2.15/2021-03-15 && APEX4server 2021.10-0 #
# Number of scans            :        6                                        #
# Total length of scans  [*] :   388.00 (deg.)                                 #
# Total exposition time  [*] :      2 h  9 min.                                #
#                                                                              #
#  [*] fast scan not included                                                  #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast     2.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 168.0 #
#  2 Fast@    2.0  1.00    34.0   180  180.0    0.0    0.0  180.0   54.7 150.0 #
#  3 Omega   20.0  1.00    34.0    97   97.0    0.1    2.7   72.0  -44.5 150.0 #
#  4 Omega   20.0  1.00    34.0    97   97.0    0.1    2.7  216.0  -44.5 150.0 #
#  5 Omega   20.0  1.00    34.0    97   97.0    0.1    2.7    0.0  -44.5 150.0 #
#  6 Omega   20.0  1.00    34.0    97   97.0    0.1    2.7  288.0  -44.5 150.0 #
#                                                                              #
#  @: attenuated beam                                                          #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean 7.39
_diffrn_ambient_temperature      168(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           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0689
_diffrn_reflns_av_r_equivalents  0.0635
_diffrn_reflns_number            44671
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.041
_diffrn_reflns_theta_max         27.613
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_reflns_number_total             13776
_reflns_number_gt                9556
_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, 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)+(0.0708P)²+13.3205P] 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         13776
_refine_ls_number_parameters     640
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1594
_refine_ls_wR_factor_gt          0.1394
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.753
_refine_diff_density_min         -2.203
_refine_diff_density_rms         0.156

#------------------------------------------------------------------------------#
#               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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 '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'
O O 0.0106 0.0060 '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
Mg1 Mg 0.15851(16) 0.46568(16) 0.68387(14) 0.0284(5) Uani 1 1 d . . . . .
Mg2 Mg 0.11793(15) 0.21776(16) 0.78381(13) 0.0258(4) Uani 1 1 d . . . . .
Mg3 Mg 0.33418(16) 0.27880(16) 0.67070(14) 0.0271(4) Uani 1 1 d . . . . .
Br1 Br -0.00207(6) 0.38195(6) 0.77809(5) 0.04191(18) Uani 1 1 d . . . . .
Br2 Br 0.26961(6) 0.09768(6) 0.75814(5) 0.04250(19) Uani 1 1 d . . . . .
Br3 Br 0.33417(5) 0.48161(5) 0.59546(5) 0.03794(17) Uani 1 1 d . . . . .
Br4 Br 0.14057(8) 0.31408(8) 0.62574(7) 0.0371(4) Uani 0.385(6) 1 d . . P . .
Cl4 Cl 0.14057(8) 0.31408(8) 0.62574(7) 0.0371(4) Uani 0.615(6) 1 d . . P . .
Br5 Br 0.25961(11) 0.33048(11) 0.79205(10) 0.0347(6) Uani 0.056(6) 1 d . . P .
.
Cl5 Cl 0.25961(11) 0.33048(11) 0.79205(10) 0.0347(6) Uani 0.944(6) 1 d . . P .
.
O1 O 0.0790(4) 0.5722(3) 0.5934(3) 0.0349(11) Uani 1 1 d . . . . .
C2 C -0.0034(6) 0.6349(6) 0.6142(5) 0.048(2) Uani 1 1 d . . . . .
H2A H 0.005732 0.708339 0.580949 0.058 Uiso 1 1 calc R U . . .
H2B H -0.001068 0.626848 0.672324 0.058 Uiso 1 1 calc R U . . .
C3 C -0.1048(7) 0.6072(9) 0.6005(7) 0.070(3) Uani 1 1 d . . . . .
H3A H -0.108434 0.617182 0.542683 0.105 Uiso 1 1 calc R U . . .
H3B H -0.157960 0.651429 0.616108 0.105 Uiso 1 1 calc R U . . .
H3C H -0.114651 0.534712 0.633738 0.105 Uiso 1 1 calc R U . . .
C4 C 0.0958(6) 0.5917(6) 0.5067(5) 0.0425(18) Uani 1 1 d . . . . .
H4A H 0.030628 0.588878 0.484008 0.051 Uiso 1 1 calc R U . . .
H4B H 0.143396 0.536635 0.498561 0.051 Uiso 1 1 calc R U . . .
C5 C 0.1378(8) 0.6928(7) 0.4619(6) 0.065(3) Uani 1 1 d . . . . .
H5A H 0.091162 0.747587 0.470005 0.097 Uiso 1 1 calc R U . . .
H5B H 0.146209 0.703264 0.403622 0.097 Uiso 1 1 calc R U . . .
H5C H 0.203929 0.694796 0.482416 0.097 Uiso 1 1 calc R U . . .
O11 O 0.1756(4) 0.5714(4) 0.7386(3) 0.0369(11) Uani 1 1 d . . . . .
C12 C 0.1514(6) 0.5570(6) 0.8231(5) 0.0422(17) Uani 1 1 d . . . . .
H12A H 0.209228 0.576990 0.845316 0.051 Uiso 1 1 calc R U . . .
H12B H 0.142076 0.482833 0.853871 0.051 Uiso 1 1 calc R U . . .
C13 C 0.0574(8) 0.6189(9) 0.8357(6) 0.073(3) Uani 1 1 d . . . . .
H13A H 0.067137 0.692549 0.807097 0.109 Uiso 1 1 calc R U . . .
H13B H 0.043568 0.605381 0.894128 0.109 Uiso 1 1 calc R U . . .
H13C H -0.000244 0.599173 0.813972 0.109 Uiso 1 1 calc R U . . .
C14 C 0.2287(8) 0.6649(6) 0.6940(6) 0.058(2) Uani 1 1 d . . . . .
H14A H 0.192694 0.724111 0.705712 0.070 Uiso 1 1 calc R U . . .
H14B H 0.227744 0.679390 0.634676 0.070 Uiso 1 1 calc R U . . .
C15 C 0.3371(8) 0.6543(9) 0.7174(8) 0.084(4) Uani 1 1 d . . . . .
H15A H 0.338154 0.651453 0.773858 0.125 Uiso 1 1 calc R U . . .
H15B H 0.373253 0.713777 0.680919 0.125 Uiso 1 1 calc R U . . .
H15C H 0.370348 0.590670 0.712623 0.125 Uiso 1 1 calc R U . . .
O21 O 0.0092(3) 0.1269(3) 0.7734(3) 0.0308(10) Uani 1 1 d . . . . .
C22 C -0.0842(5) 0.1123(6) 0.8243(4) 0.0351(15) Uani 1 1 d . . . . .
H22A H -0.076027 0.133541 0.871414 0.042 Uiso 1 1 calc R U . . .
H22B H -0.097509 0.037968 0.845785 0.042 Uiso 1 1 calc R U . . .
C23 C -0.1741(5) 0.1729(7) 0.7791(5) 0.0456(19) Uani 1 1 d . . . . .
H23A H -0.160788 0.246460 0.756593 0.068 Uiso 1 1 calc R U . . .
H23B H -0.234615 0.162850 0.816667 0.068 Uiso 1 1 calc R U . . .
H23C H -0.185395 0.149020 0.734519 0.068 Uiso 1 1 calc R U . . .
C24 C 0.0161(6) 0.0732(6) 0.7156(4) 0.0376(16) Uani 1 1 d . . . . .
H24A H 0.068135 0.104307 0.671692 0.045 Uiso 1 1 calc R U . . .
H24B H -0.049942 0.083131 0.690356 0.045 Uiso 1 1 calc R U . . .
C25 C 0.0428(6) -0.0400(6) 0.7537(5) 0.0452(19) Uani 1 1 d . . . . .
H25A H 0.101654 -0.050797 0.786777 0.068 Uiso 1 1 calc R U . . .
H25B H 0.059346 -0.069380 0.710789 0.068 Uiso 1 1 calc R U . . .
H25C H -0.015109 -0.073956 0.788553 0.068 Uiso 1 1 calc R U . . .
O31 O 0.1133(4) 0.1542(3) 0.9087(3) 0.0310(10) Uani 1 1 d . . . . .
C32 C 0.1030(6) 0.2150(6) 0.9619(5) 0.0413(17) Uani 1 1 d . . . . .
H32A H 0.114369 0.288109 0.928952 0.050 Uiso 1 1 calc R U . . .
H32B H 0.155393 0.189655 1.002676 0.050 Uiso 1 1 calc R U . . .
C33 C -0.0015(8) 0.2081(7) 1.0057(6) 0.060(2) Uani 1 1 d . . . . .
H33A H -0.053536 0.232290 0.965383 0.090 Uiso 1 1 calc R U . . .
H33B H -0.006748 0.251305 1.039519 0.090 Uiso 1 1 calc R U . . .
H33C H -0.011633 0.136193 1.040349 0.090 Uiso 1 1 calc R U . . .
C34 C 0.1356(5) 0.0454(6) 0.9508(5) 0.0384(16) Uani 1 1 d . . . . .
H34A H 0.127814 0.008173 0.913152 0.046 Uiso 1 1 calc R U . . .
H34B H 0.085258 0.020166 0.997421 0.046 Uiso 1 1 calc R U . . .
C35 C 0.2404(6) 0.0197(7) 0.9819(5) 0.054(2) Uani 1 1 d . . . . .
H35A H 0.290879 0.044869 0.936271 0.081 Uiso 1 1 calc R U . . .
H35B H 0.251280 -0.055351 1.008068 0.081 Uiso 1 1 calc R U . . .
H35C H 0.247548 0.052792 1.021821 0.081 Uiso 1 1 calc R U . . .
O41 O 0.3806(3) 0.2391(3) 0.5715(3) 0.0299(10) Uani 1 1 d . . . . .
C42 C 0.3575(6) 0.3018(6) 0.4883(5) 0.0422(17) Uani 1 1 d . . . . .
H42A H 0.317395 0.365295 0.488513 0.051 Uiso 1 1 calc R U . . .
H42B H 0.314912 0.262969 0.467020 0.051 Uiso 1 1 calc R U . . .
C43 C 0.4497(7) 0.3315(10) 0.4324(6) 0.076(3) Uani 1 1 d . . . . .
H43A H 0.496513 0.361973 0.456513 0.114 Uiso 1 1 calc R U . . .
H43B H 0.429973 0.382026 0.379768 0.114 Uiso 1 1 calc R U . . .
H43C H 0.483416 0.270030 0.424077 0.114 Uiso 1 1 calc R U . . .
C44 C 0.4338(6) 0.1415(6) 0.5791(5) 0.0392(16) Uani 1 1 d . . . . .
H44A H 0.448513 0.104627 0.637047 0.047 Uiso 1 1 calc R U . . .
H44B H 0.499638 0.154654 0.547047 0.047 Uiso 1 1 calc R U . . .
C45 C 0.3771(9) 0.0737(8) 0.5511(7) 0.078(3) Uani 1 1 d . . . . .
H45A H 0.308739 0.066486 0.577990 0.117 Uiso 1 1 calc R U . . .
H45B H 0.413199 0.005530 0.564893 0.117 Uiso 1 1 calc R U . . .
H45C H 0.371920 0.104416 0.491777 0.117 Uiso 1 1 calc R U . . .
O51 O 0.4743(3) 0.2523(4) 0.7193(3) 0.0362(11) Uani 1 1 d . . . . .
C52A C 0.5626(12) 0.2863(12) 0.6634(11) 0.047(3) Uani 0.5 1 d . . P A 1
H52A H 0.616553 0.229767 0.676205 0.056 Uiso 0.5 1 calc R U P A 1
H52B H 0.543576 0.300624 0.606969 0.056 Uiso 0.5 1 calc R U P A 1
C53A C 0.6030(11) 0.3785(12) 0.6677(12) 0.045(3) Uani 0.5 1 d . . P A 1
H53A H 0.662016 0.397631 0.628914 0.067 Uiso 0.5 1 calc R U P A 1
H53B H 0.550511 0.435333 0.653803 0.067 Uiso 0.5 1 calc R U P A 1
H53C H 0.623531 0.364436 0.723079 0.067 Uiso 0.5 1 calc R U P A 1
C54A C 0.5330(12) 0.1000(12) 0.8290(12) 0.046(3) Uani 0.5 1 d . . P A 1
H54A H 0.539635 0.072994 0.888200 0.068 Uiso 0.5 1 calc R U P A 1
H54B H 0.489669 0.056308 0.814364 0.068 Uiso 0.5 1 calc R U P A 1
H54C H 0.600405 0.099862 0.801121 0.068 Uiso 0.5 1 calc R U P A 1
C55A C 0.4861(14) 0.2086(14) 0.8035(12) 0.053(3) Uani 0.5 1 d . . P A 1
H55A H 0.418720 0.208432 0.832759 0.064 Uiso 0.5 1 calc R U P A 1
H55B H 0.529435 0.251979 0.819518 0.064 Uiso 0.5 1 calc R U P A 1
C52B C 0.6098(13) 0.3459(13) 0.6317(11) 0.047(3) Uani 0.5 1 d . . P A 2
H52C H 0.657059 0.400063 0.622461 0.070 Uiso 0.5 1 calc R U P A 2
H52D H 0.648245 0.280338 0.637580 0.070 Uiso 0.5 1 calc R U P A 2
H52E H 0.566804 0.364769 0.585118 0.070 Uiso 0.5 1 calc R U P A 2
C53B C 0.5460(11) 0.3349(12) 0.7059(11) 0.045(3) Uani 0.5 1 d . . P A 2
H53D H 0.507283 0.401116 0.700531 0.054 Uiso 0.5 1 calc R U P A 2
H53E H 0.588955 0.316445 0.753142 0.054 Uiso 0.5 1 calc R U P A 2
C54B C 0.5180(12) 0.1543(13) 0.7797(11) 0.046(3) Uani 0.5 1 d . . P A 2
H54D H 0.488847 0.094924 0.772744 0.055 Uiso 0.5 1 calc R U P A 2
H54E H 0.592344 0.148978 0.767715 0.055 Uiso 0.5 1 calc R U P A 2
C55B C 0.4994(14) 0.1478(14) 0.8617(11) 0.053(3) Uani 0.5 1 d . . P A 2
H55C H 0.529813 0.082305 0.897857 0.080 Uiso 0.5 1 calc R U P A 2
H55D H 0.529507 0.205416 0.869518 0.080 Uiso 0.5 1 calc R U P A 2
H55E H 0.425913 0.151311 0.874552 0.080 Uiso 0.5 1 calc R U P A 2
Pb1 Pb 0.75033(2) 0.85795(3) 0.81807(2) 0.04509(11) Uani 1 1 d . . . . .
C101 C 0.5680(7) 0.8478(15) 0.8299(15) 0.0477(15) Uani 0.5 1 d G . P B 1
C102 C 0.4979(11) 0.8594(14) 0.7722(11) 0.0477(15) Uani 0.5 1 d G . P B 1
C103 C 0.3948(10) 0.8534(12) 0.7953(8) 0.0477(15) Uani 0.5 1 d G . P B 1
C104 C 0.3619(7) 0.8358(12) 0.8761(8) 0.0477(15) Uani 0.5 1 d G . P B 1
C105 C 0.4320(11) 0.8242(13) 0.9339(9) 0.0477(15) Uani 0.5 1 d G . P B 1
C106 C 0.5351(10) 0.8302(14) 0.9107(14) 0.0477(15) Uani 0.5 1 d G . P B 1
F107 F 0.5311(9) 0.8743(10) 0.6968(9) 0.0562(9) Uani 0.5 1 d . . P B 1
F108 F 0.3292(8) 0.8689(9) 0.7389(7) 0.0562(9) Uani 0.5 1 d . . P B 1
F109 F 0.2639(8) 0.8310(9) 0.8951(7) 0.0562(9) Uani 0.5 1 d . . P B 1
F110 F 0.3977(8) 0.8043(9) 1.0122(8) 0.0562(9) Uani 0.5 1 d . . P B 1
F111 F 0.5842(10) 0.8028(9) 0.9676(10) 0.0562(9) Uani 0.5 1 d . . P B 1
C201 C 0.5768(14) 0.8610(17) 0.8190(18) 0.0477(15) Uani 0.5 1 d . . P B 2
C202 C 0.5134(14) 0.8720(17) 0.7584(16) 0.0477(15) Uani 0.5 1 d . . P B 2
C203 C 0.4108(13) 0.8600(15) 0.7709(13) 0.0477(15) Uani 0.5 1 d . . P B 2
C204 C 0.4192(13) 0.8162(15) 0.9099(14) 0.0477(15) Uani 0.5 1 d . . P B 2
C205 C 0.5218(14) 0.8307(17) 0.8955(16) 0.0477(15) Uani 0.5 1 d . . P B 2
C206 C 0.3655(13) 0.8306(15) 0.8460(13) 0.0477(15) Uani 0.5 1 d . . P B 2
F207 F 0.5472(9) 0.9002(10) 0.6781(9) 0.0562(9) Uani 0.5 1 d . . P B 2
F208 F 0.3496(8) 0.8768(9) 0.7057(7) 0.0562(9) Uani 0.5 1 d . . P B 2
F209 F 0.2624(8) 0.8195(9) 0.8603(7) 0.0562(9) Uani 0.5 1 d . . P B 2
F210 F 0.3800(8) 0.7885(9) 0.9873(8) 0.0562(9) Uani 0.5 1 d . . P B 2
F211 F 0.5927(10) 0.8310(9) 0.9644(10) 0.0562(9) Uani 0.5 1 d . . P B 2
C121 C 0.7587(6) 0.6838(7) 0.8308(5) 0.0466(19) Uani 1 1 d . . . . .
C122 C 0.7260(6) 0.6429(7) 0.7773(5) 0.0472(19) Uani 1 1 d . . . . .
C123 C 0.7254(7) 0.5396(7) 0.7908(6) 0.053(2) Uani 1 1 d . . . . .
C124 C 0.7575(7) 0.4705(7) 0.8623(6) 0.054(2) Uani 1 1 d . . . . .
C125 C 0.7910(7) 0.5066(8) 0.9188(6) 0.058(2) Uani 1 1 d . . . . .
C126 C 0.7906(7) 0.6087(8) 0.9024(5) 0.052(2) Uani 1 1 d . . . . .
F127 F 0.6900(4) 0.7086(4) 0.7053(3) 0.0658(14) Uani 1 1 d . . . . .
F128 F 0.6911(5) 0.5052(5) 0.7351(4) 0.0825(18) Uani 1 1 d . . . . .
F129 F 0.7551(4) 0.3687(4) 0.8777(4) 0.0698(15) Uani 1 1 d . . . . .
F130 F 0.8236(5) 0.4350(5) 0.9902(4) 0.0837(19) Uani 1 1 d . . . . .
F131 F 0.8269(5) 0.6394(5) 0.9598(3) 0.0754(17) Uani 1 1 d . . . . .
C141 C 0.7767(5) 0.9283(6) 0.6741(5) 0.0402(17) Uani 1 1 d . . . . .
C142 C 0.8523(5) 0.8912(5) 0.6321(5) 0.0368(16) Uani 1 1 d . . . . .
C143 C 0.8758(6) 0.9368(6) 0.5501(5) 0.0405(17) Uani 1 1 d . . . . .
C144 C 0.8222(6) 1.0259(6) 0.5066(5) 0.0417(17) Uani 1 1 d . . . . .
C145 C 0.7453(6) 1.0669(6) 0.5463(5) 0.0422(18) Uani 1 1 d . . . . .
C146 C 0.7269(5) 1.0183(6) 0.6279(5) 0.0412(17) Uani 1 1 d . . . . .
F147 F 0.9095(3) 0.8035(3) 0.6730(3) 0.0454(11) Uani 1 1 d . . . . .
F148 F 0.9513(4) 0.8971(4) 0.5108(3) 0.0534(12) Uani 1 1 d . . . . .
F149 F 0.8438(4) 1.0732(4) 0.4262(3) 0.0594(13) Uani 1 1 d . . . . .
F150 F 0.6936(4) 1.1549(4) 0.5026(3) 0.0575(13) Uani 1 1 d . . . . .
F151 F 0.6520(4) 1.0635(4) 0.6643(3) 0.0576(13) 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
Mg1 O1 2.038(5) . ?
Mg1 O11 2.059(5) . ?
Mg1 Br5 2.524(3) . ?
Mg1 Br1 2.657(2) . ?
Mg1 Br3 2.663(2) . ?
Mg1 Br4 2.683(2) . ?
Mg1 Mg2 3.326(3) . ?
Mg1 Mg3 3.388(3) . ?
Mg2 O31 2.049(5) . ?
Mg2 O21 2.054(5) . ?
Mg2 Br5 2.589(3) . ?
Mg2 Br2 2.610(2) . ?
Mg2 Br4 2.620(3) . ?
Mg2 Br1 2.639(2) . ?
Mg2 Mg3 3.332(3) . ?
Mg3 O41 2.040(5) . ?
Mg3 O51 2.056(5) . ?
Mg3 Br5 2.579(3) . ?
Mg3 Br2 2.608(2) . ?
Mg3 Br3 2.649(2) . ?
Mg3 Br4 2.697(2) . ?
O1 C2 1.440(8) . ?
O1 C4 1.450(9) . ?
C2 C3 1.488(13) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.473(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
O11 C12 1.436(9) . ?
O11 C14 1.460(9) . ?
C12 C13 1.497(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.505(15) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O21 C22 1.447(8) . ?
O21 C24 1.453(8) . ?
C22 C23 1.503(10) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.494(11) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
O31 C34 1.442(8) . ?
O31 C32 1.458(8) . ?
C32 C33 1.516(12) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.501(10) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
O41 C44 1.438(8) . ?
O41 C42 1.453(9) . ?
C42 C43 1.489(12) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.487(12) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
O51 C55A 1.400(19) . ?
O51 C52A 1.457(17) . ?
O51 C53B 1.493(14) . ?
O51 C54B 1.499(17) . ?
C52A C53A 1.46(2) . ?
C52A H52A 0.9900 . ?
C52A H52B 0.9900 . ?
C53A H53A 0.9800 . ?
C53A H53B 0.9800 . ?
C53A H53C 0.9800 . ?
C54A C55A 1.50(2) . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
C55A H55A 0.9900 . ?
C55A H55B 0.9900 . ?
C52B C53B 1.46(2) . ?
C52B H52C 0.9800 . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C53B H53D 0.9900 . ?
C53B H53E 0.9900 . ?
C54B C55B 1.41(3) . ?
C54B H54D 0.9900 . ?
C54B H54E 0.9900 . ?
C55B H55C 0.9800 . ?
C55B H55D 0.9800 . ?
C55B H55E 0.9800 . ?
Pb1 C201 2.291(18) . ?
Pb1 C121 2.341(9) . ?
Pb1 C141 2.370(8) . ?
Pb1 C101 2.415(9) . ?
C101 C102 1.3900 . ?
C101 C106 1.3900 . ?
C102 F107 1.31(2) . ?
C102 C103 1.3900 . ?
C103 F108 1.321(18) . ?
C103 C104 1.3900 . ?
C104 F109 1.312(14) . ?
C104 C105 1.3900 . ?
C105 F110 1.35(2) . ?
C105 C106 1.3900 . ?
C106 F111 1.17(2) . ?
C201 C202 1.37(3) . ?
C201 C205 1.41(2) . ?
C202 F207 1.37(3) . ?
C202 C203 1.37(2) . ?
C203 C206 1.34(3) . ?
C203 F208 1.40(2) . ?
C204 C206 1.33(3) . ?
C204 F210 1.34(2) . ?
C204 C205 1.38(2) . ?
C205 F211 1.59(3) . ?
C206 F209 1.377(19) . ?
C121 C122 1.375(11) . ?
C121 C126 1.386(12) . ?
C122 F127 1.365(9) . ?
C122 C123 1.368(13) . ?
C123 C124 1.355(13) . ?
C123 F128 1.356(10) . ?
C124 F129 1.343(10) . ?
C124 C125 1.380(13) . ?
C125 C126 1.342(13) . ?
C125 F130 1.368(10) . ?
C126 F131 1.363(9) . ?
C141 C142 1.367(10) . ?
C141 C146 1.370(11) . ?
C142 F147 1.371(8) . ?
C142 C143 1.369(11) . ?
C143 F148 1.356(8) . ?
C143 C144 1.372(11) . ?
C144 F149 1.345(9) . ?
C144 C145 1.382(11) . ?
C145 F150 1.350(8) . ?
C145 C146 1.359(11) . ?
C146 F151 1.362(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mg1 O11 92.0(2) . . ?
O1 Mg1 Br5 177.79(17) . . ?
O11 Mg1 Br5 89.94(17) . . ?
O1 Mg1 Br1 96.43(17) . . ?
O11 Mg1 Br1 95.89(16) . . ?
Br5 Mg1 Br1 84.50(8) . . ?
O1 Mg1 Br3 95.22(16) . . ?
O11 Mg1 Br3 99.70(16) . . ?
Br5 Mg1 Br3 83.34(7) . . ?
Br1 Mg1 Br3 160.17(9) . . ?
O1 Mg1 Br4 93.12(15) . . ?
O11 Mg1 Br4 174.66(18) . . ?
Br5 Mg1 Br4 85.02(8) . . ?
Br1 Mg1 Br4 81.91(7) . . ?
Br3 Mg1 Br4 81.48(7) . . ?
O1 Mg1 Mg2 129.05(17) . . ?
O11 Mg1 Mg2 124.69(17) . . ?
Br5 Mg1 Mg2 50.28(6) . . ?
Br1 Mg1 Mg2 50.85(5) . . ?
Br3 Mg1 Mg2 109.61(7) . . ?
Br4 Mg1 Mg2 50.31(6) . . ?
O1 Mg1 Mg3 128.73(16) . . ?
O11 Mg1 Mg3 125.92(17) . . ?
Br5 Mg1 Mg3 49.09(6) . . ?
Br1 Mg1 Mg3 110.34(8) . . ?
Br3 Mg1 Mg3 50.18(5) . . ?
Br4 Mg1 Mg3 51.14(6) . . ?
Mg2 Mg1 Mg3 59.50(6) . . ?
O31 Mg2 O21 93.9(2) . . ?
O31 Mg2 Br5 87.81(15) . . ?
O21 Mg2 Br5 177.57(17) . . ?
O31 Mg2 Br2 96.18(15) . . ?
O21 Mg2 Br2 94.01(15) . . ?
Br5 Mg2 Br2 84.06(7) . . ?
O31 Mg2 Br4 172.83(16) . . ?
O21 Mg2 Br4 93.30(16) . . ?
Br5 Mg2 Br4 85.03(8) . . ?
Br2 Mg2 Br4 83.54(7) . . ?
O31 Mg2 Br1 95.30(15) . . ?
O21 Mg2 Br1 97.98(15) . . ?
Br5 Mg2 Br1 83.60(7) . . ?
Br2 Mg2 Br1 162.77(9) . . ?
Br4 Mg2 Br1 83.46(7) . . ?
O31 Mg2 Mg1 122.05(15) . . ?
O21 Mg2 Mg1 131.31(16) . . ?
Br5 Mg2 Mg1 48.57(6) . . ?
Br2 Mg2 Mg1 111.47(8) . . ?
Br4 Mg2 Mg1 52.01(6) . . ?
Br1 Mg2 Mg1 51.34(5) . . ?
O31 Mg2 Mg3 122.52(16) . . ?
O21 Mg2 Mg3 127.86(16) . . ?
Br5 Mg2 Mg3 49.71(6) . . ?
Br2 Mg2 Mg3 50.29(5) . . ?
Br4 Mg2 Mg3 52.23(6) . . ?
Br1 Mg2 Mg3 112.51(8) . . ?
Mg1 Mg2 Mg3 61.18(6) . . ?
O41 Mg3 O51 95.8(2) . . ?
O41 Mg3 Br5 175.01(16) . . ?
O51 Mg3 Br5 89.14(16) . . ?
O41 Mg3 Br2 94.69(15) . . ?
O51 Mg3 Br2 95.50(16) . . ?
Br5 Mg3 Br2 84.30(8) . . ?
O41 Mg3 Br3 97.06(15) . . ?
O51 Mg3 Br3 99.36(15) . . ?
Br5 Mg3 Br3 82.59(7) . . ?
Br2 Mg3 Br3 159.98(9) . . ?
O41 Mg3 Br4 91.34(15) . . ?
O51 Mg3 Br4 172.62(18) . . ?
Br5 Mg3 Br4 83.68(7) . . ?
Br2 Mg3 Br4 82.09(7) . . ?
Br3 Mg3 Br4 81.48(7) . . ?
O41 Mg3 Mg2 126.00(15) . . ?
O51 Mg3 Mg2 123.22(17) . . ?
Br5 Mg3 Mg2 49.99(6) . . ?
Br2 Mg3 Mg2 50.35(5) . . ?
Br3 Mg3 Mg2 109.80(7) . . ?
Br4 Mg3 Mg2 50.17(6) . . ?
O41 Mg3 Mg1 128.66(16) . . ?
O51 Mg3 Mg1 124.46(16) . . ?
Br5 Mg3 Mg1 47.70(6) . . ?
Br2 Mg3 Mg1 109.67(8) . . ?
Br3 Mg3 Mg1 50.55(5) . . ?
Br4 Mg3 Mg1 50.79(6) . . ?
Mg2 Mg3 Mg1 59.32(6) . . ?
Mg2 Br1 Mg1 77.81(7) . . ?
Mg3 Br2 Mg2 79.36(7) . . ?
Mg3 Br3 Mg1 79.26(7) . . ?
Mg2 Br4 Mg1 77.68(7) . . ?
Mg2 Br4 Mg3 77.60(7) . . ?
Mg1 Br4 Mg3 78.07(7) . . ?
Mg1 Br5 Mg3 83.21(9) . . ?
Mg1 Br5 Mg2 81.15(8) . . ?
Mg3 Br5 Mg2 80.30(8) . . ?
C2 O1 C4 114.4(5) . . ?
C2 O1 Mg1 119.5(4) . . ?
C4 O1 Mg1 126.0(4) . . ?
O1 C2 C3 112.8(7) . . ?
O1 C2 H2A 109.0 . . ?
C3 C2 H2A 109.0 . . ?
O1 C2 H2B 109.0 . . ?
C3 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O1 C4 C5 112.4(7) . . ?
O1 C4 H4A 109.1 . . ?
C5 C4 H4A 109.1 . . ?
O1 C4 H4B 109.1 . . ?
C5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C12 O11 C14 113.6(6) . . ?
C12 O11 Mg1 125.8(4) . . ?
C14 O11 Mg1 120.1(5) . . ?
O11 C12 C13 112.7(7) . . ?
O11 C12 H12A 109.1 . . ?
C13 C12 H12A 109.1 . . ?
O11 C12 H12B 109.1 . . ?
C13 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
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 . . ?
O11 C14 C15 111.5(8) . . ?
O11 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
O11 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C22 O21 C24 113.6(5) . . ?
C22 O21 Mg2 121.5(4) . . ?
C24 O21 Mg2 125.0(4) . . ?
O21 C22 C23 112.7(6) . . ?
O21 C22 H22A 109.1 . . ?
C23 C22 H22A 109.1 . . ?
O21 C22 H22B 109.1 . . ?
C23 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O21 C24 C25 113.3(6) . . ?
O21 C24 H24A 108.9 . . ?
C25 C24 H24A 108.9 . . ?
O21 C24 H24B 108.9 . . ?
C25 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C34 O31 C32 113.9(5) . . ?
C34 O31 Mg2 121.7(4) . . ?
C32 O31 Mg2 123.7(4) . . ?
O31 C32 C33 111.4(6) . . ?
O31 C32 H32A 109.3 . . ?
C33 C32 H32A 109.3 . . ?
O31 C32 H32B 109.3 . . ?
C33 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O31 C34 C35 113.8(6) . . ?
O31 C34 H34A 108.8 . . ?
C35 C34 H34A 108.8 . . ?
O31 C34 H34B 108.8 . . ?
C35 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C44 O41 C42 113.7(5) . . ?
C44 O41 Mg3 122.2(4) . . ?
C42 O41 Mg3 124.0(4) . . ?
O41 C42 C43 113.3(7) . . ?
O41 C42 H42A 108.9 . . ?
C43 C42 H42A 108.9 . . ?
O41 C42 H42B 108.9 . . ?
C43 C42 H42B 108.9 . . ?
H42A C42 H42B 107.7 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O41 C44 C45 114.0(7) . . ?
O41 C44 H44A 108.8 . . ?
C45 C44 H44A 108.8 . . ?
O41 C44 H44B 108.8 . . ?
C45 C44 H44B 108.8 . . ?
H44A C44 H44B 107.7 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C55A O51 C52A 119.8(11) . . ?
C53B O51 C54B 108.0(10) . . ?
C55A O51 Mg3 122.3(8) . . ?
C52A O51 Mg3 117.8(8) . . ?
C53B O51 Mg3 123.7(7) . . ?
C54B O51 Mg3 128.0(7) . . ?
C53A C52A O51 113.1(13) . . ?
C53A C52A H52A 109.0 . . ?
O51 C52A H52A 109.0 . . ?
C53A C52A H52B 109.0 . . ?
O51 C52A H52B 109.0 . . ?
H52A C52A H52B 107.8 . . ?
C52A C53A H53A 109.5 . . ?
C52A C53A H53B 109.5 . . ?
H53A C53A H53B 109.5 . . ?
C52A C53A H53C 109.5 . . ?
H53A C53A H53C 109.5 . . ?
H53B C53A H53C 109.5 . . ?
C55A C54A H54A 109.5 . . ?
C55A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C55A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
O51 C55A C54A 112.6(15) . . ?
O51 C55A H55A 109.1 . . ?
C54A C55A H55A 109.1 . . ?
O51 C55A H55B 109.1 . . ?
C54A C55A H55B 109.1 . . ?
H55A C55A H55B 107.8 . . ?
C53B C52B H52C 109.5 . . ?
C53B C52B H52D 109.5 . . ?
H52C C52B H52D 109.5 . . ?
C53B C52B H52E 109.5 . . ?
H52C C52B H52E 109.5 . . ?
H52D C52B H52E 109.5 . . ?
C52B C53B O51 109.0(12) . . ?
C52B C53B H53D 109.9 . . ?
O51 C53B H53D 109.9 . . ?
C52B C53B H53E 109.9 . . ?
O51 C53B H53E 109.9 . . ?
H53D C53B H53E 108.3 . . ?
C55B C54B O51 113.6(14) . . ?
C55B C54B H54D 108.9 . . ?
O51 C54B H54D 108.9 . . ?
C55B C54B H54E 108.9 . . ?
O51 C54B H54E 108.9 . . ?
H54D C54B H54E 107.7 . . ?
C54B C55B H55C 109.5 . . ?
C54B C55B H55D 109.5 . . ?
H55C C55B H55D 109.5 . . ?
C54B C55B H55E 109.5 . . ?
H55C C55B H55E 109.5 . . ?
H55D C55B H55E 109.5 . . ?
C201 Pb1 C121 89.2(6) . . ?
C201 Pb1 C141 95.6(7) . . ?
C121 Pb1 C141 97.3(3) . . ?
C121 Pb1 C101 86.0(5) . . ?
C141 Pb1 C101 100.0(6) . . ?
C102 C101 C106 120.0 . . ?
C102 C101 Pb1 131.8(10) . . ?
C106 C101 Pb1 108.2(10) . . ?
F107 C102 C101 118.7(14) . . ?
F107 C102 C103 121.3(14) . . ?
C101 C102 C103 120.0 . . ?
F108 C103 C104 121.0(10) . . ?
F108 C103 C102 119.0(10) . . ?
C104 C103 C102 120.0 . . ?
F109 C104 C103 117.8(10) . . ?
F109 C104 C105 122.2(10) . . ?
C103 C104 C105 120.0 . . ?
F110 C105 C104 118.4(11) . . ?
F110 C105 C106 121.5(11) . . ?
C104 C105 C106 120.0 . . ?
F111 C106 C105 111.2(15) . . ?
F111 C106 C101 127.6(16) . . ?
C105 C106 C101 120.0 . . ?
C202 C201 C205 110.0(15) . . ?
C202 C201 Pb1 131.3(15) . . ?
C205 C201 Pb1 117.8(17) . . ?
F207 C202 C201 122.2(17) . . ?
F207 C202 C203 113.5(19) . . ?
C201 C202 C203 124.3(18) . . ?
C206 C203 C202 121.3(18) . . ?
C206 C203 F208 117.4(15) . . ?
C202 C203 F208 121.3(17) . . ?
C206 C204 F210 124.3(15) . . ?
C206 C204 C205 117.5(17) . . ?
F210 C204 C205 118.3(18) . . ?
C204 C205 C201 126.9(18) . . ?
C204 C205 F211 122.8(19) . . ?
C201 C205 F211 109.8(18) . . ?
C204 C206 C203 120.1(16) . . ?
C204 C206 F209 117.2(17) . . ?
C203 C206 F209 122.6(17) . . ?
C122 C121 C126 112.7(8) . . ?
C122 C121 Pb1 127.4(6) . . ?
C126 C121 Pb1 119.6(6) . . ?
F127 C122 C123 116.4(7) . . ?
F127 C122 C121 118.7(8) . . ?
C123 C122 C121 124.9(8) . . ?
C124 C123 F128 119.5(8) . . ?
C124 C123 C122 119.1(8) . . ?
F128 C123 C122 121.4(8) . . ?
F129 C124 C123 120.1(9) . . ?
F129 C124 C125 121.0(9) . . ?
C123 C124 C125 118.9(8) . . ?
C126 C125 F130 122.8(9) . . ?
C126 C125 C124 119.7(9) . . ?
F130 C125 C124 117.6(9) . . ?
C125 C126 F131 116.8(8) . . ?
C125 C126 C121 124.7(8) . . ?
F131 C126 C121 118.5(8) . . ?
C142 C141 C146 114.4(7) . . ?
C142 C141 Pb1 122.8(6) . . ?
C146 C141 Pb1 122.2(5) . . ?
C141 C142 F147 119.3(7) . . ?
C141 C142 C143 124.0(7) . . ?
F147 C142 C143 116.8(6) . . ?
F148 C143 C144 118.9(7) . . ?
F148 C143 C142 122.0(7) . . ?
C144 C143 C142 119.2(7) . . ?
F149 C144 C143 120.7(7) . . ?
F149 C144 C145 120.1(7) . . ?
C143 C144 C145 119.2(7) . . ?
F150 C145 C146 123.0(7) . . ?
F150 C145 C144 118.4(7) . . ?
C146 C145 C144 118.5(7) . . ?
C145 C146 F151 116.1(7) . . ?
C145 C146 C141 124.8(7) . . ?
F151 C146 C141 119.2(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 O1 C2 C3 69.8(9) . . . . ?
Mg1 O1 C2 C3 -109.3(7) . . . . ?
C2 O1 C4 C5 70.3(9) . . . . ?
Mg1 O1 C4 C5 -110.7(7) . . . . ?
C14 O11 C12 C13 81.4(9) . . . . ?
Mg1 O11 C12 C13 -106.9(8) . . . . ?
C12 O11 C14 C15 73.0(9) . . . . ?
Mg1 O11 C14 C15 -99.3(8) . . . . ?
C24 O21 C22 C23 -74.6(8) . . . . ?
Mg2 O21 C22 C23 104.7(6) . . . . ?
C22 O21 C24 C25 -77.6(7) . . . . ?
Mg2 O21 C24 C25 103.2(6) . . . . ?
C34 O31 C32 C33 -80.7(8) . . . . ?
Mg2 O31 C32 C33 108.2(7) . . . . ?
C32 O31 C34 C35 -69.7(8) . . . . ?
Mg2 O31 C34 C35 101.5(7) . . . . ?
C44 O41 C42 C43 -62.1(9) . . . . ?
Mg3 O41 C42 C43 122.1(7) . . . . ?
C42 O41 C44 C45 -60.2(9) . . . . ?
Mg3 O41 C44 C45 115.7(7) . . . . ?
C55A O51 C52A C53A -70.9(17) . . . . ?
Mg3 O51 C52A C53A 105.6(13) . . . . ?
C52A O51 C55A C54A -74.7(17) . . . . ?
Mg3 O51 C55A C54A 109.0(13) . . . . ?
C54B O51 C53B C52B 97.9(14) . . . . ?
Mg3 O51 C53B C52B -88.1(13) . . . . ?
C53B O51 C54B C55B 81.5(15) . . . . ?
Mg3 O51 C54B C55B -92.1(14) . . . . ?
C106 C101 C102 F107 -179.0(16) . . . . ?
Pb1 C101 C102 F107 3.5(14) . . . . ?
C106 C101 C102 C103 0.0 . . . . ?
Pb1 C101 C102 C103 -177.5(13) . . . . ?
F107 C102 C103 F108 -3.8(16) . . . . ?
C101 C102 C103 F108 177.2(14) . . . . ?
F107 C102 C103 C104 179.0(17) . . . . ?
C101 C102 C103 C104 0.0 . . . . ?
F108 C103 C104 F109 2.7(16) . . . . ?
C102 C103 C104 F109 179.9(14) . . . . ?
F108 C103 C104 C105 -177.2(15) . . . . ?
C102 C103 C104 C105 0.0 . . . . ?
F109 C104 C105 F110 2.0(15) . . . . ?
C103 C104 C105 F110 -178.1(14) . . . . ?
F109 C104 C105 C106 -179.9(15) . . . . ?
C103 C104 C105 C106 0.0 . . . . ?
F110 C105 C106 F111 9.4(16) . . . . ?
C104 C105 C106 F111 -168.6(15) . . . . ?
F110 C105 C106 C101 178.0(15) . . . . ?
C104 C105 C106 C101 0.0 . . . . ?
C102 C101 C106 F111 166.6(18) . . . . ?
Pb1 C101 C106 F111 -15.4(15) . . . . ?
C102 C101 C106 C105 0.0 . . . . ?
Pb1 C101 C106 C105 178.0(10) . . . . ?
C205 C201 C202 F207 -179.6(19) . . . . ?
Pb1 C201 C202 F207 -11(3) . . . . ?
C205 C201 C202 C203 3(2) . . . . ?
Pb1 C201 C202 C203 171.9(16) . . . . ?
F207 C202 C203 C206 178.7(18) . . . . ?
C201 C202 C203 C206 -4(3) . . . . ?
F207 C202 C203 F208 0(2) . . . . ?
C201 C202 C203 F208 177.1(17) . . . . ?
C206 C204 C205 C201 1(3) . . . . ?
F210 C204 C205 C201 -179.1(18) . . . . ?
C206 C204 C205 F211 171.6(17) . . . . ?
F210 C204 C205 F211 -9(2) . . . . ?
C202 C201 C205 C204 -2(2) . . . . ?
Pb1 C201 C205 C204 -172.3(16) . . . . ?
C202 C201 C205 F211 -173.3(16) . . . . ?
Pb1 C201 C205 F211 16.1(18) . . . . ?
F210 C204 C206 C203 178.8(17) . . . . ?
C205 C204 C206 C203 -1(2) . . . . ?
F210 C204 C206 F209 2(2) . . . . ?
C205 C204 C206 F209 -177.9(16) . . . . ?
C202 C203 C206 C204 3(3) . . . . ?
F208 C203 C206 C204 -178.2(16) . . . . ?
C202 C203 C206 F209 179.0(17) . . . . ?
F208 C203 C206 F209 -2(2) . . . . ?
C126 C121 C122 F127 178.3(7) . . . . ?
Pb1 C121 C122 F127 4.6(11) . . . . ?
C126 C121 C122 C123 -0.9(12) . . . . ?
Pb1 C121 C122 C123 -174.6(7) . . . . ?
F127 C122 C123 C124 -178.1(8) . . . . ?
C121 C122 C123 C124 1.1(14) . . . . ?
F127 C122 C123 F128 0.2(13) . . . . ?
C121 C122 C123 F128 179.5(8) . . . . ?
F128 C123 C124 F129 -0.1(13) . . . . ?
C122 C123 C124 F129 178.2(8) . . . . ?
F128 C123 C124 C125 -179.1(8) . . . . ?
C122 C123 C124 C125 -0.8(13) . . . . ?
F129 C124 C125 C126 -178.7(8) . . . . ?
C123 C124 C125 C126 0.4(14) . . . . ?
F129 C124 C125 F130 1.4(13) . . . . ?
C123 C124 C125 F130 -179.6(8) . . . . ?
F130 C125 C126 F131 1.5(13) . . . . ?
C124 C125 C126 F131 -178.4(8) . . . . ?
F130 C125 C126 C121 179.7(8) . . . . ?
C124 C125 C126 C121 -0.2(14) . . . . ?
C122 C121 C126 C125 0.5(13) . . . . ?
Pb1 C121 C126 C125 174.7(7) . . . . ?
C122 C121 C126 F131 178.7(8) . . . . ?
Pb1 C121 C126 F131 -7.1(11) . . . . ?
C146 C141 C142 F147 177.7(6) . . . . ?
Pb1 C141 C142 F147 6.6(9) . . . . ?
C146 C141 C142 C143 -1.9(11) . . . . ?
Pb1 C141 C142 C143 -173.1(6) . . . . ?
C141 C142 C143 F148 -179.8(7) . . . . ?
F147 C142 C143 F148 0.6(11) . . . . ?
C141 C142 C143 C144 1.0(12) . . . . ?
F147 C142 C143 C144 -178.7(7) . . . . ?
F148 C143 C144 F149 0.2(11) . . . . ?
C142 C143 C144 F149 179.5(7) . . . . ?
F148 C143 C144 C145 -180.0(7) . . . . ?
C142 C143 C144 C145 -0.7(11) . . . . ?
F149 C144 C145 F150 -0.5(11) . . . . ?
C143 C144 C145 F150 179.7(7) . . . . ?
F149 C144 C145 C146 -178.7(7) . . . . ?
C143 C144 C145 C146 1.5(11) . . . . ?
F150 C145 C146 F151 0.2(11) . . . . ?
C144 C145 C146 F151 178.3(7) . . . . ?
F150 C145 C146 C141 179.2(7) . . . . ?
C144 C145 C146 C141 -2.7(12) . . . . ?
C142 C141 C146 C145 2.8(11) . . . . ?
Pb1 C141 C146 C145 174.0(6) . . . . ?
C142 C141 C146 F151 -178.2(6) . . . . ?
Pb1 C141 C146 F151 -7.0(10) . . . . ?

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

#...............................................................................
# .RES SHELXL file: sqz.res
#...............................................................................



# ............... End of .RES file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .HKL SHELXL file: sqz.hkl
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .FAB SHELXL file: sqz.fab
#...............................................................................


####################################################################### 
# 
# 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_Complex_2
_database_code_depnum_ccdc_archive 'CCDC 2400988'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-11-06 deposited with the CCDC.	2024-11-28 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 24 novembre 2023                                         #
#------------------------------------------------------------------------------#


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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H8 F10 O2 Pb'
_chemical_formula_sum            'C16 H8 F10 O2 Pb'
_chemical_formula_weight         629.41
_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                   7.8568(8)
_cell_length_b                   7.9859(8)
_cell_length_c                   15.6528(15)
_cell_angle_alpha                95.693(3)
_cell_angle_beta                 91.114(4)
_cell_angle_gamma                115.308(3)
_cell_volume                     881.38(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9904
_cell_measurement_theta_min      2.8416
_cell_measurement_theta_max      27.5009
_cell_measurement_wavelength     0.710730


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

_diffrn_orient_matrix_UB_11      -0.0144571
_diffrn_orient_matrix_UB_21      -0.1403673
_diffrn_orient_matrix_UB_31      -0.0020318
_diffrn_orient_matrix_UB_12      0.1084959
_diffrn_orient_matrix_UB_22      -0.0724276
_diffrn_orient_matrix_UB_32      0.0494432
_diffrn_orient_matrix_UB_13      -0.0201457
_diffrn_orient_matrix_UB_23      -0.0032567
_diffrn_orient_matrix_UB_33      0.0610337


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

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.372
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             584
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    9.682
_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  0.235
_exptl_absorpt_correction_T_max  0.461

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

# Software                   : BIS V6.2.15/2021-03-15 && APEX4server 2021.10-0 #
# Number of scans            :        5                                        #
# Total length of scans  [*] :   291.00 (deg.)                                 #
# Total exposition time  [*] :      1 h 37 min.                                #
#                                                                              #
#  [*] fast scan not included                                                  #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast     2.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Fast@    2.0  1.00    34.0   180  180.0    0.0    0.0  180.0   54.7 150.0 #
#  3 Omega   20.0  1.00    34.0    97   97.0    0.1    2.7   72.0  -44.5 150.0 #
#  4 Omega   20.0  1.00    34.0    97   97.0    0.1    2.7  144.0  -44.5 150.0 #
#  5 Omega   20.0  1.00    34.0    97   97.0    0.1    2.7  288.0  -44.5 150.0 #
#                                                                              #
#  @: attenuated beam                                                          #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_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           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0338
_diffrn_reflns_av_r_equivalents  0.0322
_diffrn_reflns_number            10064
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.622
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.985
_reflns_number_total             3994
_reflns_number_gt                3859
_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 2018_2 (Sheldrick, 2018)'
_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)+4.7867P] 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         3994
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0578
_refine_ls_wR_factor_gt          0.0572
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.806
_refine_diff_density_min         -1.857
_refine_diff_density_rms         0.142

#------------------------------------------------------------------------------#
#               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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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
Pb1 Pb 0.03876(2) 0.00177(2) 0.23949(2) 0.01971(6) Uani 1 1 d . . . . .
C1 C 0.1275(6) 0.2269(6) 0.1423(3) 0.0207(8) Uani 1 1 d . . . . .
C2 C 0.1945(6) 0.1891(6) 0.0661(3) 0.0211(8) Uani 1 1 d . . . . .
C3 C 0.2497(7) 0.3078(6) 0.0030(3) 0.0250(9) Uani 1 1 d . . . . .
C4 C 0.2359(7) 0.4744(6) 0.0164(3) 0.0273(10) Uani 1 1 d . . . . .
C5 C 0.1686(7) 0.5192(6) 0.0916(3) 0.0253(9) Uani 1 1 d . . . . .
C6 C 0.1169(6) 0.3962(6) 0.1524(3) 0.0223(8) Uani 1 1 d . . . . .
F7 F 0.2104(4) 0.0261(4) 0.04946(18) 0.0309(6) Uani 1 1 d . . . . .
F8 F 0.3163(5) 0.2641(5) -0.07039(19) 0.0405(7) Uani 1 1 d . . . . .
F9 F 0.2891(5) 0.5926(5) -0.0437(2) 0.0425(8) Uani 1 1 d . . . . .
F10 F 0.1537(5) 0.6811(4) 0.1037(2) 0.0373(7) Uani 1 1 d . . . . .
F11 F 0.0501(4) 0.4481(4) 0.22453(18) 0.0325(6) Uani 1 1 d . . . . .
C21 C 0.1182(7) 0.2231(6) 0.3613(3) 0.0238(9) Uani 1 1 d . . . . .
C22 C 0.2711(7) 0.3961(6) 0.3735(3) 0.0245(9) Uani 1 1 d . . . . .
C23 C 0.3132(7) 0.5157(7) 0.4486(3) 0.0303(10) Uani 1 1 d . . . . .
C24 C 0.2016(8) 0.4630(8) 0.5159(3) 0.0343(11) Uani 1 1 d . . . . .
C25 C 0.0464(8) 0.2910(8) 0.5081(3) 0.0331(11) Uani 1 1 d . . . . .
C26 C 0.0088(7) 0.1775(7) 0.4312(3) 0.0278(10) Uani 1 1 d . . . . .
F27 F 0.3890(4) 0.4560(4) 0.30961(19) 0.0327(6) Uani 1 1 d . . . . .
F28 F 0.4635(5) 0.6854(4) 0.4567(2) 0.0438(8) Uani 1 1 d . . . . .
F29 F 0.2416(6) 0.5772(5) 0.5907(2) 0.0529(9) Uani 1 1 d . . . . .
F30 F -0.0631(5) 0.2398(6) 0.5743(2) 0.0494(9) Uani 1 1 d . . . . .
F31 F -0.1465(4) 0.0105(4) 0.4252(2) 0.0366(7) Uani 1 1 d . . . . .
O41 O 0.3908(5) 0.0693(5) 0.2529(2) 0.0313(8) Uani 1 1 d . . . . .
C42 C 0.4526(7) -0.0272(8) 0.3103(3) 0.0333(11) Uani 1 1 d . . . . .
H42A H 0.342174 -0.118852 0.336071 0.040 Uiso 1 1 calc R U . . .
H42B H 0.538317 0.063287 0.357491 0.040 Uiso 1 1 calc R U . . .
C43 C 0.5534(7) -0.1262(7) 0.2625(3) 0.0289(10) Uani 1 1 d . . . . .
H43A H 0.600481 -0.187087 0.302960 0.035 Uiso 1 1 calc R U . . .
H43B H 0.465028 -0.223943 0.218356 0.035 Uiso 1 1 calc R U . . .
O44 O 0.7088(4) 0.0054(5) 0.2220(2) 0.0262(7) Uani 1 1 d . . . . .
C45 C 0.6410(7) 0.0943(7) 0.1633(3) 0.0258(9) Uani 1 1 d . . . . .
H45A H 0.549237 -0.000774 0.119264 0.031 Uiso 1 1 calc R U . . .
H45B H 0.747551 0.181175 0.133604 0.031 Uiso 1 1 calc R U . . .
C46 C 0.5483(6) 0.1993(6) 0.2126(3) 0.0239(9) Uani 1 1 d . . . . .
H46A H 0.639784 0.293874 0.256833 0.029 Uiso 1 1 calc R U . . .
H46B H 0.504194 0.264303 0.173130 0.029 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
Pb1 C21 2.343(5) . ?
Pb1 C1 2.355(4) . ?
Pb1 O41 2.581(3) . ?
Pb1 O44 2.614(3) 1_455 ?
C1 C2 1.371(6) . ?
C1 C6 1.384(6) . ?
C2 F7 1.360(5) . ?
C2 C3 1.383(6) . ?
C3 F8 1.347(5) . ?
C3 C4 1.377(7) . ?
C4 F9 1.343(5) . ?
C4 C5 1.376(7) . ?
C5 F10 1.343(5) . ?
C5 C6 1.377(6) . ?
C6 F11 1.356(5) . ?
C21 C22 1.381(7) . ?
C21 C26 1.384(6) . ?
C22 F27 1.356(5) . ?
C22 C23 1.376(7) . ?
C23 F28 1.356(6) . ?
C23 C24 1.366(8) . ?
C24 F29 1.353(6) . ?
C24 C25 1.385(8) . ?
C25 F30 1.340(6) . ?
C25 C26 1.379(7) . ?
C26 F31 1.363(6) . ?
O41 C46 1.439(5) . ?
O41 C42 1.442(6) . ?
C42 C43 1.501(7) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 O44 1.436(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
O44 C45 1.438(5) . ?
C45 C46 1.498(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?

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
C21 Pb1 C1 93.89(15) . . ?
C21 Pb1 O41 84.28(14) . . ?
C1 Pb1 O41 86.08(13) . . ?
C21 Pb1 O44 89.94(13) . 1_455 ?
C1 Pb1 O44 84.18(12) . 1_455 ?
O41 Pb1 O44 168.31(10) . 1_455 ?
C2 C1 C6 114.8(4) . . ?
C2 C1 Pb1 118.1(3) . . ?
C6 C1 Pb1 127.1(3) . . ?
F7 C2 C1 119.6(4) . . ?
F7 C2 C3 116.2(4) . . ?
C1 C2 C3 124.2(4) . . ?
F8 C3 C4 119.7(4) . . ?
F8 C3 C2 121.6(4) . . ?
C4 C3 C2 118.6(4) . . ?
F9 C4 C5 120.5(4) . . ?
F9 C4 C3 119.9(4) . . ?
C5 C4 C3 119.7(4) . . ?
F10 C5 C4 119.3(4) . . ?
F10 C5 C6 121.5(4) . . ?
C4 C5 C6 119.2(4) . . ?
F11 C6 C5 116.1(4) . . ?
F11 C6 C1 120.3(4) . . ?
C5 C6 C1 123.5(4) . . ?
C22 C21 C26 114.7(4) . . ?
C22 C21 Pb1 126.8(3) . . ?
C26 C21 Pb1 118.5(3) . . ?
F27 C22 C23 116.5(4) . . ?
F27 C22 C21 120.1(4) . . ?
C23 C22 C21 123.4(4) . . ?
F28 C23 C24 119.4(5) . . ?
F28 C23 C22 121.0(5) . . ?
C24 C23 C22 119.5(5) . . ?
F29 C24 C23 120.6(5) . . ?
F29 C24 C25 119.4(5) . . ?
C23 C24 C25 120.0(5) . . ?
F30 C25 C26 121.9(5) . . ?
F30 C25 C24 119.9(5) . . ?
C26 C25 C24 118.2(4) . . ?
F31 C26 C25 116.7(4) . . ?
F31 C26 C21 119.1(4) . . ?
C25 C26 C21 124.2(5) . . ?
C46 O41 C42 110.6(3) . . ?
C46 O41 Pb1 129.8(3) . . ?
C42 O41 Pb1 119.5(3) . . ?
O41 C42 C43 110.4(4) . . ?
O41 C42 H42A 109.6 . . ?
C43 C42 H42A 109.6 . . ?
O41 C42 H42B 109.6 . . ?
C43 C42 H42B 109.6 . . ?
H42A C42 H42B 108.1 . . ?
O44 C43 C42 109.6(4) . . ?
O44 C43 H43A 109.8 . . ?
C42 C43 H43A 109.8 . . ?
O44 C43 H43B 109.8 . . ?
C42 C43 H43B 109.8 . . ?
H43A C43 H43B 108.2 . . ?
C43 O44 C45 109.9(3) . . ?
C43 O44 Pb1 118.8(2) . 1_655 ?
C45 O44 Pb1 130.1(2) . 1_655 ?
O44 C45 C46 109.0(4) . . ?
O44 C45 H45A 109.9 . . ?
C46 C45 H45A 109.9 . . ?
O44 C45 H45B 109.9 . . ?
C46 C45 H45B 109.9 . . ?
H45A C45 H45B 108.3 . . ?
O41 C46 C45 108.8(4) . . ?
O41 C46 H46A 109.9 . . ?
C45 C46 H46A 109.9 . . ?
O41 C46 H46B 109.9 . . ?
C45 C46 H46B 109.9 . . ?
H46A C46 H46B 108.3 . . ?

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 F7 -179.9(4) . . . . ?
Pb1 C1 C2 F7 -1.0(6) . . . . ?
C6 C1 C2 C3 0.5(7) . . . . ?
Pb1 C1 C2 C3 179.3(4) . . . . ?
F7 C2 C3 F8 -0.3(7) . . . . ?
C1 C2 C3 F8 179.3(4) . . . . ?
F7 C2 C3 C4 179.8(4) . . . . ?
C1 C2 C3 C4 -0.6(7) . . . . ?
F8 C3 C4 F9 -0.1(7) . . . . ?
C2 C3 C4 F9 179.8(4) . . . . ?
F8 C3 C4 C5 -179.7(4) . . . . ?
C2 C3 C4 C5 0.2(7) . . . . ?
F9 C4 C5 F10 1.1(7) . . . . ?
C3 C4 C5 F10 -179.3(4) . . . . ?
F9 C4 C5 C6 -179.3(4) . . . . ?
C3 C4 C5 C6 0.2(7) . . . . ?
F10 C5 C6 F11 0.2(7) . . . . ?
C4 C5 C6 F11 -179.4(4) . . . . ?
F10 C5 C6 C1 179.2(4) . . . . ?
C4 C5 C6 C1 -0.3(7) . . . . ?
C2 C1 C6 F11 179.0(4) . . . . ?
Pb1 C1 C6 F11 0.3(6) . . . . ?
C2 C1 C6 C5 0.0(7) . . . . ?
Pb1 C1 C6 C5 -178.7(3) . . . . ?
C26 C21 C22 F27 179.8(4) . . . . ?
Pb1 C21 C22 F27 2.9(6) . . . . ?
C26 C21 C22 C23 -0.1(7) . . . . ?
Pb1 C21 C22 C23 -177.1(3) . . . . ?
F27 C22 C23 F28 1.1(7) . . . . ?
C21 C22 C23 F28 -178.9(4) . . . . ?
F27 C22 C23 C24 -179.2(4) . . . . ?
C21 C22 C23 C24 0.8(7) . . . . ?
F28 C23 C24 F29 -1.1(7) . . . . ?
C22 C23 C24 F29 179.2(4) . . . . ?
F28 C23 C24 C25 179.2(4) . . . . ?
C22 C23 C24 C25 -0.5(8) . . . . ?
F29 C24 C25 F30 0.5(7) . . . . ?
C23 C24 C25 F30 -179.9(5) . . . . ?
F29 C24 C25 C26 179.9(4) . . . . ?
C23 C24 C25 C26 -0.4(8) . . . . ?
F30 C25 C26 F31 0.5(7) . . . . ?
C24 C25 C26 F31 -179.0(4) . . . . ?
F30 C25 C26 C21 -179.4(5) . . . . ?
C24 C25 C26 C21 1.1(7) . . . . ?
C22 C21 C26 F31 179.3(4) . . . . ?
Pb1 C21 C26 F31 -3.5(6) . . . . ?
C22 C21 C26 C25 -0.8(7) . . . . ?
Pb1 C21 C26 C25 176.4(4) . . . . ?
C46 O41 C42 C43 -57.4(5) . . . . ?
Pb1 O41 C42 C43 124.4(3) . . . . ?
O41 C42 C43 O44 56.8(5) . . . . ?
C42 C43 O44 C45 -59.3(5) . . . . ?
C42 C43 O44 Pb1 132.2(3) . . . 1_655 ?
C43 O44 C45 C46 61.9(5) . . . . ?
Pb1 O44 C45 C46 -131.4(3) 1_655 . . . ?
C42 O41 C46 C45 59.3(5) . . . . ?
Pb1 O41 C46 C45 -122.8(4) . . . . ?
O44 C45 C46 O41 -61.2(5) . . . . ?

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

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



# ............... End of .RES file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .HKL SHELXL file: job.hkl
#...............................................................................


####################################################################### 
# 
# 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_Pb_C6F5_4
_database_code_depnum_ccdc_archive 'CCDC 2400989'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-11-06 deposited with the CCDC.	2024-11-28 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 24 novembre 2023                                         #
#------------------------------------------------------------------------------#


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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H8 F10 O2 Pb'
_chemical_formula_sum            'C16 H8 F10 O2 Pb'
_chemical_formula_weight         629.41
_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                   7.8568(8)
_cell_length_b                   7.9859(8)
_cell_length_c                   15.6528(15)
_cell_angle_alpha                95.693(3)
_cell_angle_beta                 91.114(4)
_cell_angle_gamma                115.308(3)
_cell_volume                     881.38(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9904
_cell_measurement_theta_min      2.8416
_cell_measurement_theta_max      27.5009
_cell_measurement_wavelength     0.710730


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

_diffrn_orient_matrix_UB_11      -0.0144571
_diffrn_orient_matrix_UB_21      -0.1403673
_diffrn_orient_matrix_UB_31      -0.0020318
_diffrn_orient_matrix_UB_12      0.1084959
_diffrn_orient_matrix_UB_22      -0.0724276
_diffrn_orient_matrix_UB_32      0.0494432
_diffrn_orient_matrix_UB_13      -0.0201457
_diffrn_orient_matrix_UB_23      -0.0032567
_diffrn_orient_matrix_UB_33      0.0610337


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

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.372
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             584
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    9.682
_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  0.235
_exptl_absorpt_correction_T_max  0.461

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

# Software                   : BIS V6.2.15/2021-03-15 && APEX4server 2021.10-0 #
# Number of scans            :        5                                        #
# Total length of scans  [*] :   291.00 (deg.)                                 #
# Total exposition time  [*] :      1 h 37 min.                                #
#                                                                              #
#  [*] fast scan not included                                                  #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast     2.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Fast@    2.0  1.00    34.0   180  180.0    0.0    0.0  180.0   54.7 150.0 #
#  3 Omega   20.0  1.00    34.0    97   97.0    0.1    2.7   72.0  -44.5 150.0 #
#  4 Omega   20.0  1.00    34.0    97   97.0    0.1    2.7  144.0  -44.5 150.0 #
#  5 Omega   20.0  1.00    34.0    97   97.0    0.1    2.7  288.0  -44.5 150.0 #
#                                                                              #
#  @: attenuated beam                                                          #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_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           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0338
_diffrn_reflns_av_r_equivalents  0.0322
_diffrn_reflns_number            10064
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.622
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.985
_reflns_number_total             3994
_reflns_number_gt                3859
_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 2018_2 (Sheldrick, 2018)'
_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)+4.7867P] 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         3994
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0578
_refine_ls_wR_factor_gt          0.0572
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.806
_refine_diff_density_min         -1.857
_refine_diff_density_rms         0.142

#------------------------------------------------------------------------------#
#               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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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
Pb1 Pb 0.03876(2) 0.00177(2) 0.23949(2) 0.01971(6) Uani 1 1 d . . . . .
C1 C 0.1275(6) 0.2269(6) 0.1423(3) 0.0207(8) Uani 1 1 d . . . . .
C2 C 0.1945(6) 0.1891(6) 0.0661(3) 0.0211(8) Uani 1 1 d . . . . .
C3 C 0.2497(7) 0.3078(6) 0.0030(3) 0.0250(9) Uani 1 1 d . . . . .
C4 C 0.2359(7) 0.4744(6) 0.0164(3) 0.0273(10) Uani 1 1 d . . . . .
C5 C 0.1686(7) 0.5192(6) 0.0916(3) 0.0253(9) Uani 1 1 d . . . . .
C6 C 0.1169(6) 0.3962(6) 0.1524(3) 0.0223(8) Uani 1 1 d . . . . .
F7 F 0.2104(4) 0.0261(4) 0.04946(18) 0.0309(6) Uani 1 1 d . . . . .
F8 F 0.3163(5) 0.2641(5) -0.07039(19) 0.0405(7) Uani 1 1 d . . . . .
F9 F 0.2891(5) 0.5926(5) -0.0437(2) 0.0425(8) Uani 1 1 d . . . . .
F10 F 0.1537(5) 0.6811(4) 0.1037(2) 0.0373(7) Uani 1 1 d . . . . .
F11 F 0.0501(4) 0.4481(4) 0.22453(18) 0.0325(6) Uani 1 1 d . . . . .
C21 C 0.1182(7) 0.2231(6) 0.3613(3) 0.0238(9) Uani 1 1 d . . . . .
C22 C 0.2711(7) 0.3961(6) 0.3735(3) 0.0245(9) Uani 1 1 d . . . . .
C23 C 0.3132(7) 0.5157(7) 0.4486(3) 0.0303(10) Uani 1 1 d . . . . .
C24 C 0.2016(8) 0.4630(8) 0.5159(3) 0.0343(11) Uani 1 1 d . . . . .
C25 C 0.0464(8) 0.2910(8) 0.5081(3) 0.0331(11) Uani 1 1 d . . . . .
C26 C 0.0088(7) 0.1775(7) 0.4312(3) 0.0278(10) Uani 1 1 d . . . . .
F27 F 0.3890(4) 0.4560(4) 0.30961(19) 0.0327(6) Uani 1 1 d . . . . .
F28 F 0.4635(5) 0.6854(4) 0.4567(2) 0.0438(8) Uani 1 1 d . . . . .
F29 F 0.2416(6) 0.5772(5) 0.5907(2) 0.0529(9) Uani 1 1 d . . . . .
F30 F -0.0631(5) 0.2398(6) 0.5743(2) 0.0494(9) Uani 1 1 d . . . . .
F31 F -0.1465(4) 0.0105(4) 0.4252(2) 0.0366(7) Uani 1 1 d . . . . .
O41 O 0.3908(5) 0.0693(5) 0.2529(2) 0.0313(8) Uani 1 1 d . . . . .
C42 C 0.4526(7) -0.0272(8) 0.3103(3) 0.0333(11) Uani 1 1 d . . . . .
H42A H 0.342174 -0.118852 0.336071 0.040 Uiso 1 1 calc R U . . .
H42B H 0.538317 0.063287 0.357491 0.040 Uiso 1 1 calc R U . . .
C43 C 0.5534(7) -0.1262(7) 0.2625(3) 0.0289(10) Uani 1 1 d . . . . .
H43A H 0.600481 -0.187087 0.302960 0.035 Uiso 1 1 calc R U . . .
H43B H 0.465028 -0.223943 0.218356 0.035 Uiso 1 1 calc R U . . .
O44 O 0.7088(4) 0.0054(5) 0.2220(2) 0.0262(7) Uani 1 1 d . . . . .
C45 C 0.6410(7) 0.0943(7) 0.1633(3) 0.0258(9) Uani 1 1 d . . . . .
H45A H 0.549237 -0.000774 0.119264 0.031 Uiso 1 1 calc R U . . .
H45B H 0.747551 0.181175 0.133604 0.031 Uiso 1 1 calc R U . . .
C46 C 0.5483(6) 0.1993(6) 0.2126(3) 0.0239(9) Uani 1 1 d . . . . .
H46A H 0.639784 0.293874 0.256833 0.029 Uiso 1 1 calc R U . . .
H46B H 0.504194 0.264303 0.173130 0.029 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
Pb1 C21 2.343(5) . ?
Pb1 C1 2.355(4) . ?
Pb1 O41 2.581(3) . ?
Pb1 O44 2.614(3) 1_455 ?
C1 C2 1.371(6) . ?
C1 C6 1.384(6) . ?
C2 F7 1.360(5) . ?
C2 C3 1.383(6) . ?
C3 F8 1.347(5) . ?
C3 C4 1.377(7) . ?
C4 F9 1.343(5) . ?
C4 C5 1.376(7) . ?
C5 F10 1.343(5) . ?
C5 C6 1.377(6) . ?
C6 F11 1.356(5) . ?
C21 C22 1.381(7) . ?
C21 C26 1.384(6) . ?
C22 F27 1.356(5) . ?
C22 C23 1.376(7) . ?
C23 F28 1.356(6) . ?
C23 C24 1.366(8) . ?
C24 F29 1.353(6) . ?
C24 C25 1.385(8) . ?
C25 F30 1.340(6) . ?
C25 C26 1.379(7) . ?
C26 F31 1.363(6) . ?
O41 C46 1.439(5) . ?
O41 C42 1.442(6) . ?
C42 C43 1.501(7) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 O44 1.436(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
O44 C45 1.438(5) . ?
C45 C46 1.498(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?

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
C21 Pb1 C1 93.89(15) . . ?
C21 Pb1 O41 84.28(14) . . ?
C1 Pb1 O41 86.08(13) . . ?
C21 Pb1 O44 89.94(13) . 1_455 ?
C1 Pb1 O44 84.18(12) . 1_455 ?
O41 Pb1 O44 168.31(10) . 1_455 ?
C2 C1 C6 114.8(4) . . ?
C2 C1 Pb1 118.1(3) . . ?
C6 C1 Pb1 127.1(3) . . ?
F7 C2 C1 119.6(4) . . ?
F7 C2 C3 116.2(4) . . ?
C1 C2 C3 124.2(4) . . ?
F8 C3 C4 119.7(4) . . ?
F8 C3 C2 121.6(4) . . ?
C4 C3 C2 118.6(4) . . ?
F9 C4 C5 120.5(4) . . ?
F9 C4 C3 119.9(4) . . ?
C5 C4 C3 119.7(4) . . ?
F10 C5 C4 119.3(4) . . ?
F10 C5 C6 121.5(4) . . ?
C4 C5 C6 119.2(4) . . ?
F11 C6 C5 116.1(4) . . ?
F11 C6 C1 120.3(4) . . ?
C5 C6 C1 123.5(4) . . ?
C22 C21 C26 114.7(4) . . ?
C22 C21 Pb1 126.8(3) . . ?
C26 C21 Pb1 118.5(3) . . ?
F27 C22 C23 116.5(4) . . ?
F27 C22 C21 120.1(4) . . ?
C23 C22 C21 123.4(4) . . ?
F28 C23 C24 119.4(5) . . ?
F28 C23 C22 121.0(5) . . ?
C24 C23 C22 119.5(5) . . ?
F29 C24 C23 120.6(5) . . ?
F29 C24 C25 119.4(5) . . ?
C23 C24 C25 120.0(5) . . ?
F30 C25 C26 121.9(5) . . ?
F30 C25 C24 119.9(5) . . ?
C26 C25 C24 118.2(4) . . ?
F31 C26 C25 116.7(4) . . ?
F31 C26 C21 119.1(4) . . ?
C25 C26 C21 124.2(5) . . ?
C46 O41 C42 110.6(3) . . ?
C46 O41 Pb1 129.8(3) . . ?
C42 O41 Pb1 119.5(3) . . ?
O41 C42 C43 110.4(4) . . ?
O41 C42 H42A 109.6 . . ?
C43 C42 H42A 109.6 . . ?
O41 C42 H42B 109.6 . . ?
C43 C42 H42B 109.6 . . ?
H42A C42 H42B 108.1 . . ?
O44 C43 C42 109.6(4) . . ?
O44 C43 H43A 109.8 . . ?
C42 C43 H43A 109.8 . . ?
O44 C43 H43B 109.8 . . ?
C42 C43 H43B 109.8 . . ?
H43A C43 H43B 108.2 . . ?
C43 O44 C45 109.9(3) . . ?
C43 O44 Pb1 118.8(2) . 1_655 ?
C45 O44 Pb1 130.1(2) . 1_655 ?
O44 C45 C46 109.0(4) . . ?
O44 C45 H45A 109.9 . . ?
C46 C45 H45A 109.9 . . ?
O44 C45 H45B 109.9 . . ?
C46 C45 H45B 109.9 . . ?
H45A C45 H45B 108.3 . . ?
O41 C46 C45 108.8(4) . . ?
O41 C46 H46A 109.9 . . ?
C45 C46 H46A 109.9 . . ?
O41 C46 H46B 109.9 . . ?
C45 C46 H46B 109.9 . . ?
H46A C46 H46B 108.3 . . ?

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 F7 -179.9(4) . . . . ?
Pb1 C1 C2 F7 -1.0(6) . . . . ?
C6 C1 C2 C3 0.5(7) . . . . ?
Pb1 C1 C2 C3 179.3(4) . . . . ?
F7 C2 C3 F8 -0.3(7) . . . . ?
C1 C2 C3 F8 179.3(4) . . . . ?
F7 C2 C3 C4 179.8(4) . . . . ?
C1 C2 C3 C4 -0.6(7) . . . . ?
F8 C3 C4 F9 -0.1(7) . . . . ?
C2 C3 C4 F9 179.8(4) . . . . ?
F8 C3 C4 C5 -179.7(4) . . . . ?
C2 C3 C4 C5 0.2(7) . . . . ?
F9 C4 C5 F10 1.1(7) . . . . ?
C3 C4 C5 F10 -179.3(4) . . . . ?
F9 C4 C5 C6 -179.3(4) . . . . ?
C3 C4 C5 C6 0.2(7) . . . . ?
F10 C5 C6 F11 0.2(7) . . . . ?
C4 C5 C6 F11 -179.4(4) . . . . ?
F10 C5 C6 C1 179.2(4) . . . . ?
C4 C5 C6 C1 -0.3(7) . . . . ?
C2 C1 C6 F11 179.0(4) . . . . ?
Pb1 C1 C6 F11 0.3(6) . . . . ?
C2 C1 C6 C5 0.0(7) . . . . ?
Pb1 C1 C6 C5 -178.7(3) . . . . ?
C26 C21 C22 F27 179.8(4) . . . . ?
Pb1 C21 C22 F27 2.9(6) . . . . ?
C26 C21 C22 C23 -0.1(7) . . . . ?
Pb1 C21 C22 C23 -177.1(3) . . . . ?
F27 C22 C23 F28 1.1(7) . . . . ?
C21 C22 C23 F28 -178.9(4) . . . . ?
F27 C22 C23 C24 -179.2(4) . . . . ?
C21 C22 C23 C24 0.8(7) . . . . ?
F28 C23 C24 F29 -1.1(7) . . . . ?
C22 C23 C24 F29 179.2(4) . . . . ?
F28 C23 C24 C25 179.2(4) . . . . ?
C22 C23 C24 C25 -0.5(8) . . . . ?
F29 C24 C25 F30 0.5(7) . . . . ?
C23 C24 C25 F30 -179.9(5) . . . . ?
F29 C24 C25 C26 179.9(4) . . . . ?
C23 C24 C25 C26 -0.4(8) . . . . ?
F30 C25 C26 F31 0.5(7) . . . . ?
C24 C25 C26 F31 -179.0(4) . . . . ?
F30 C25 C26 C21 -179.4(5) . . . . ?
C24 C25 C26 C21 1.1(7) . . . . ?
C22 C21 C26 F31 179.3(4) . . . . ?
Pb1 C21 C26 F31 -3.5(6) . . . . ?
C22 C21 C26 C25 -0.8(7) . . . . ?
Pb1 C21 C26 C25 176.4(4) . . . . ?
C46 O41 C42 C43 -57.4(5) . . . . ?
Pb1 O41 C42 C43 124.4(3) . . . . ?
O41 C42 C43 O44 56.8(5) . . . . ?
C42 C43 O44 C45 -59.3(5) . . . . ?
C42 C43 O44 Pb1 132.2(3) . . . 1_655 ?
C43 O44 C45 C46 61.9(5) . . . . ?
Pb1 O44 C45 C46 -131.4(3) 1_655 . . . ?
C42 O41 C46 C45 59.3(5) . . . . ?
Pb1 O41 C46 C45 -122.8(4) . . . . ?
O44 C45 C46 O41 -61.2(5) . . . . ?

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

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



# ............... End of .RES file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .HKL SHELXL file: job.hkl
#...............................................................................


####################################################################### 
# 
# 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_MgBr2_DMAP_2
_database_code_depnum_ccdc_archive 'CCDC 2400991'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-11-06 deposited with the CCDC.	2024-11-28 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 08 novembre 2023                                         #
#------------------------------------------------------------------------------#


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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H20 Br2 Mg N4'
_chemical_formula_sum            'C14 H20 Br2 Mg N4'
_chemical_formula_weight         428.47
_chemical_compound_source        'synthesis as described'

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

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_IT_number           56
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   14.220(4)
_cell_length_b                   14.478(4)
_cell_length_c                   17.924(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3690.2(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1394
_cell_measurement_theta_min      2.6864
_cell_measurement_theta_max      22.2035
_cell_measurement_wavelength     0.710730


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

_diffrn_orient_matrix_UB_11      0.0044462
_diffrn_orient_matrix_UB_21      -0.0567469
_diffrn_orient_matrix_UB_31      0.0412972
_diffrn_orient_matrix_UB_12      0.0524682
_diffrn_orient_matrix_UB_22      -0.0236712
_diffrn_orient_matrix_UB_32      -0.0381757
_diffrn_orient_matrix_UB_13      0.0361110
_diffrn_orient_matrix_UB_23      0.0268374
_diffrn_orient_matrix_UB_33      0.0329897


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

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1712
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    4.426
_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  0.743
_exptl_absorpt_correction_T_max  0.876

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

# Software                   : BIS V6.2.15/2021-03-15 && APEX4 2022.10-0       #
# Number of scans            :        2                                        #
# Total length of scans  [*] :    97.00 (deg.)                                 #
# Total exposition time  [*] :      2 h 41 min.                                #
#                                                                              #
#  [*] fast scan not included                                                  #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast    10.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Omega  100.0  1.00    34.0    97   97.0    0.1    2.7    0.0  -44.5 150.0 #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_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           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.1393
_diffrn_reflns_av_r_equivalents  0.1237
_diffrn_reflns_number            13800
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.007
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_reflns_number_total             4193
_reflns_number_gt                1938
_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 2018_2 (Sheldrick, 2018)'
_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.
;

# start Validation Reply Form
_vrf_PLATxxx_job                 
;
PROBLEM:
RESPONSE:
blablabla
;
# end Validation Reply Form

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0404P)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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4193
_refine_ls_number_parameters     195
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1422
_refine_ls_wR_factor_gt          0.1116
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.978
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.112

#------------------------------------------------------------------------------#
#               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'
Mg Mg 0.0486 0.0363 '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'

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 0.88510(5) 0.31155(5) 0.32817(4) 0.0443(2) Uani 1 1 d . . . . .
Mg1 Mg 0.750000 0.250000 0.39679(16) 0.0302(7) Uani 1 2 d S T P . .
Br2 Br 0.88605(6) 0.80281(5) 0.94890(4) 0.0483(2) Uani 1 1 d . . . . .
Mg2 Mg 0.750000 0.750000 0.87815(17) 0.0355(8) Uani 1 2 d S T P . .
C1 C 0.5721(5) 0.3985(4) 0.5508(3) 0.0388(17) Uani 1 1 d . . . . .
H1 H 0.516016 0.382243 0.576409 0.047 Uiso 1 1 calc R U . . .
C2 C 0.6142(5) 0.3363(4) 0.5031(3) 0.0330(15) Uani 1 1 d . . . . .
H2 H 0.585066 0.277750 0.496753 0.040 Uiso 1 1 calc R U . . .
N3 N 0.6938(4) 0.3529(3) 0.4650(3) 0.0319(13) Uani 1 1 d . . . . .
C4 C 0.7309(5) 0.4376(4) 0.4744(3) 0.0345(16) Uani 1 1 d . . . . .
H4 H 0.786708 0.451980 0.447715 0.041 Uiso 1 1 calc R U . . .
C5 C 0.6939(5) 0.5045(4) 0.5199(3) 0.0352(16) Uani 1 1 d . . . . .
H5 H 0.723265 0.563325 0.523301 0.042 Uiso 1 1 calc R U . . .
C6 C 0.6126(5) 0.4858(4) 0.5612(3) 0.0328(14) Uani 1 1 d . . . . .
N7 N 0.5745(4) 0.5498(3) 0.6082(3) 0.0403(14) Uani 1 1 d . . . . .
C8 C 0.4949(6) 0.5254(5) 0.6561(4) 0.063(2) Uani 1 1 d . . . . .
H8A H 0.440189 0.510639 0.625028 0.094 Uiso 1 1 calc R U . . .
H8B H 0.479750 0.577595 0.688758 0.094 Uiso 1 1 calc R U . . .
H8C H 0.511387 0.471553 0.686545 0.094 Uiso 1 1 calc R U . . .
C9 C 0.6141(6) 0.6408(4) 0.6171(4) 0.0486(19) Uani 1 1 d . . . . .
H9A H 0.623791 0.668797 0.567962 0.073 Uiso 1 1 calc R U . . .
H9B H 0.674524 0.636192 0.643181 0.073 Uiso 1 1 calc R U . . .
H9C H 0.570938 0.679226 0.646335 0.073 Uiso 1 1 calc R U . . .
C11 C 0.8766(5) 0.6016(4) 0.6968(4) 0.0361(16) Uani 1 1 d . . . . .
H11 H 0.923031 0.619010 0.661393 0.043 Uiso 1 1 calc R U . . .
C12 C 0.8494(5) 0.6626(4) 0.7502(4) 0.0384(17) Uani 1 1 d . . . . .
H12 H 0.879620 0.721136 0.750801 0.046 Uiso 1 1 calc R U . . .
N13 N 0.7826(4) 0.6469(3) 0.8026(3) 0.0341(13) Uani 1 1 d . . . . .
C14 C 0.7421(5) 0.5621(4) 0.7977(4) 0.0380(17) Uani 1 1 d . . . . .
H14 H 0.693519 0.547611 0.832212 0.046 Uiso 1 1 calc R U . . .
C15 C 0.7663(5) 0.4966(4) 0.7468(3) 0.0359(16) Uani 1 1 d . . . . .
H15 H 0.735030 0.438585 0.747298 0.043 Uiso 1 1 calc R U . . .
C16 C 0.8367(5) 0.5133(4) 0.6936(3) 0.0318(15) Uani 1 1 d . . . . .
N17 N 0.8652(4) 0.4511(3) 0.6438(3) 0.0395(15) Uani 1 1 d . . . . .
C18 C 0.9348(6) 0.4746(5) 0.5871(4) 0.055(2) Uani 1 1 d . . . . .
H18A H 0.912533 0.527678 0.558144 0.082 Uiso 1 1 calc R U . . .
H18B H 0.944071 0.421706 0.553844 0.082 Uiso 1 1 calc R U . . .
H18C H 0.994520 0.490261 0.611318 0.082 Uiso 1 1 calc R U . . .
C19 C 0.8297(6) 0.3555(4) 0.6464(4) 0.057(2) Uani 1 1 d . . . . .
H19A H 0.832710 0.332453 0.697715 0.086 Uiso 1 1 calc R U . . .
H19B H 0.868408 0.316285 0.614055 0.086 Uiso 1 1 calc R U . . .
H19C H 0.764374 0.354181 0.628980 0.086 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
Br1 Mg1 2.4490(16) . ?
Mg1 N3 2.087(5) . ?
Mg1 N3 2.087(5) 2_655 ?
Br2 Mg2 2.4363(18) . ?
Mg2 N13 2.068(6) . ?
Mg2 N13 2.068(6) 2_665 ?
C1 C2 1.378(8) . ?
C1 C6 1.402(8) . ?
C1 H1 0.9500 . ?
C2 N3 1.343(8) . ?
C2 H2 0.9500 . ?
N3 C4 1.345(7) . ?
C4 C5 1.372(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(9) . ?
C5 H5 0.9500 . ?
C6 N7 1.365(8) . ?
N7 C9 1.441(8) . ?
N7 C8 1.464(9) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.358(8) . ?
C11 C16 1.400(8) . ?
C11 H11 0.9500 . ?
C12 N13 1.356(8) . ?
C12 H12 0.9500 . ?
N13 C14 1.358(7) . ?
C14 C15 1.361(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.405(9) . ?
C15 H15 0.9500 . ?
C16 N17 1.330(7) . ?
N17 C18 1.458(9) . ?
N17 C19 1.475(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 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
N3 Mg1 N3 108.3(3) . 2_655 ?
N3 Mg1 Br1 104.69(15) . 2_655 ?
N3 Mg1 Br1 109.56(15) 2_655 2_655 ?
N3 Mg1 Br1 109.56(15) . . ?
N3 Mg1 Br1 104.69(15) 2_655 . ?
Br1 Mg1 Br1 119.70(12) 2_655 . ?
N13 Mg2 N13 98.2(3) . 2_665 ?
N13 Mg2 Br2 112.93(15) . . ?
N13 Mg2 Br2 106.97(15) 2_665 . ?
N13 Mg2 Br2 106.97(15) . 2_665 ?
N13 Mg2 Br2 112.93(15) 2_665 2_665 ?
Br2 Mg2 Br2 117.26(13) . 2_665 ?
C2 C1 C6 119.6(6) . . ?
C2 C1 H1 120.2 . . ?
C6 C1 H1 120.2 . . ?
N3 C2 C1 124.3(6) . . ?
N3 C2 H2 117.8 . . ?
C1 C2 H2 117.8 . . ?
C2 N3 C4 115.5(5) . . ?
C2 N3 Mg1 119.5(4) . . ?
C4 N3 Mg1 125.0(4) . . ?
N3 C4 C5 124.6(6) . . ?
N3 C4 H4 117.7 . . ?
C5 C4 H4 117.7 . . ?
C4 C5 C6 119.6(6) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
N7 C6 C5 121.5(6) . . ?
N7 C6 C1 122.1(6) . . ?
C5 C6 C1 116.4(6) . . ?
C6 N7 C9 122.3(6) . . ?
C6 N7 C8 120.3(6) . . ?
C9 N7 C8 117.3(5) . . ?
N7 C8 H8A 109.5 . . ?
N7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N7 C9 H9A 109.5 . . ?
N7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C11 C16 120.5(6) . . ?
C12 C11 H11 119.7 . . ?
C16 C11 H11 119.7 . . ?
N13 C12 C11 125.3(6) . . ?
N13 C12 H12 117.3 . . ?
C11 C12 H12 117.3 . . ?
C12 N13 C14 113.9(6) . . ?
C12 N13 Mg2 119.3(4) . . ?
C14 N13 Mg2 126.8(5) . . ?
N13 C14 C15 124.5(6) . . ?
N13 C14 H14 117.8 . . ?
C15 C14 H14 117.8 . . ?
C14 C15 C16 121.1(6) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
N17 C16 C11 121.5(6) . . ?
N17 C16 C15 123.8(6) . . ?
C11 C16 C15 114.7(6) . . ?
C16 N17 C18 121.1(6) . . ?
C16 N17 C19 120.7(6) . . ?
C18 N17 C19 118.2(6) . . ?
N17 C18 H18A 109.5 . . ?
N17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N17 C19 H19A 109.5 . . ?
N17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
C6 C1 C2 N3 0.5(10) . . . . ?
C1 C2 N3 C4 -1.7(9) . . . . ?
C1 C2 N3 Mg1 178.7(5) . . . . ?
C2 N3 C4 C5 0.9(9) . . . . ?
Mg1 N3 C4 C5 -179.4(5) . . . . ?
N3 C4 C5 C6 1.0(10) . . . . ?
C4 C5 C6 N7 178.6(6) . . . . ?
C4 C5 C6 C1 -2.1(9) . . . . ?
C2 C1 C6 N7 -179.3(6) . . . . ?
C2 C1 C6 C5 1.4(9) . . . . ?
C5 C6 N7 C9 1.3(10) . . . . ?
C1 C6 N7 C9 -177.8(6) . . . . ?
C5 C6 N7 C8 -174.1(7) . . . . ?
C1 C6 N7 C8 6.7(10) . . . . ?
C16 C11 C12 N13 -1.5(11) . . . . ?
C11 C12 N13 C14 -0.5(10) . . . . ?
C11 C12 N13 Mg2 -179.1(5) . . . . ?
C12 N13 C14 C15 1.6(9) . . . . ?
Mg2 N13 C14 C15 -180.0(5) . . . . ?
N13 C14 C15 C16 -0.7(10) . . . . ?
C12 C11 C16 N17 -177.0(6) . . . . ?
C12 C11 C16 C15 2.4(9) . . . . ?
C14 C15 C16 N17 178.0(6) . . . . ?
C14 C15 C16 C11 -1.4(9) . . . . ?
C11 C16 N17 C18 -4.3(9) . . . . ?
C15 C16 N17 C18 176.3(6) . . . . ?
C11 C16 N17 C19 173.5(6) . . . . ?
C15 C16 N17 C19 -5.9(10) . . . . ?

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

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



# ............... End of .RES file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .HKL SHELXL file: job.hkl
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR COMPOUND 5 (MgBr2_DMAP_2)                              #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################



################################################################################
#                                                                              #
#                            END OF GLOBAL CIF FILE                            #
#                                                                              #
################################################################################

####################################################################### 
# 
# 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_F5C6_3_Sn_C6F5_3_dioxane
_database_code_depnum_ccdc_archive 'CCDC 2400990'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL' 'ISCR CNRS Univ Rennes'
_audit_update_record             
;
2024-11-06 deposited with the CCDC.	2024-11-28 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 30 novembre 2023                                         #
#------------------------------------------------------------------------------#


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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C36 F30 Sn2, C4 H8 O2'
_chemical_formula_sum            'C40 H8 F30 O2 Sn2'
_chemical_formula_weight         1327.84
_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                   9.9952(10)
_cell_length_b                   10.1428(11)
_cell_length_c                   10.8362(12)
_cell_angle_alpha                95.488(4)
_cell_angle_beta                 95.241(4)
_cell_angle_gamma                112.298(4)
_cell_volume                     1002.00(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9351
_cell_measurement_theta_min      2.1922
_cell_measurement_theta_max      27.5131
_cell_measurement_wavelength     0.710730


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

_diffrn_orient_matrix_UB_11      0.0243890
_diffrn_orient_matrix_UB_21      -0.0252379
_diffrn_orient_matrix_UB_31      0.1033929
_diffrn_orient_matrix_UB_12      -0.0735434
_diffrn_orient_matrix_UB_22      0.0349667
_diffrn_orient_matrix_UB_32      0.0703956
_diffrn_orient_matrix_UB_13      -0.0505392
_diffrn_orient_matrix_UB_23      -0.0785320
_diffrn_orient_matrix_UB_33      0.0064524


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

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             634
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    1.427
_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  0.743
_exptl_absorpt_correction_T_max  0.945

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

# Software                   : BIS V6.2.15/2021-03-15 && APEX4 2022.10-0       #
# Total number of scans:        5                                              #
#                                                                              #
# ....[fast scans included]       :                                            #
#    . Total number of frames :      651                                       #
#    . Total length of scans  :   651.00 (deg.)                                #
#    . Mean rotation speed    :    20.09 sec./deg.                             #
#    . Total exposition time  :      3 h 38 min.                               #
#                                                                              #
#                                                                              #
# ....[fast scans excluded]       :                                            #
#    . Total number of frames :      291                                       #
#    . Total length of scans  :   291.00 (deg.)                                #
#    . Mean rotation speed    :    40.00 sec./deg.                             #
#    . Total exposition time  :      3 h 38 min.                               #
#                                                                              #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast     4.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Fast@    4.0  1.00    34.0   180  180.0    0.0    0.0  180.0   54.7 150.0 #
#  3 Omega   40.0  1.00    34.0    97   97.0    0.1    2.7   72.0  -44.5 150.0 #
#  4 Omega   40.0  1.00    34.0    97   97.0    0.1    2.7  288.0  -44.5 150.0 #
#  5 Omega   40.0  1.00    34.0    97   97.0    0.1    2.7  216.0  -44.5 150.0 #
#                                                                              #
#  @: attenuated beam                                                          #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_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           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0393
_diffrn_reflns_av_r_equivalents  0.0298
_diffrn_reflns_number            10571
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.436
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.984
_reflns_number_total             4532
_reflns_number_gt                3911
_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 2018_2 (Sheldrick, 2018)'
_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)+(0.0399P)²+5.4117P] 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         4532
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.1095
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         2.298
_refine_diff_density_min         -1.676
_refine_diff_density_rms         0.142

#------------------------------------------------------------------------------#
#               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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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
Sn1 Sn 0.49647(3) 0.13580(3) 0.49855(3) 0.02084(10) Uani 1 1 d . . . . .
C1 C 0.3205(5) 0.1501(5) 0.5912(4) 0.0229(8) Uani 1 1 d . . . . .
C2 C 0.3267(5) 0.2766(5) 0.6549(4) 0.0273(9) Uani 1 1 d . . . . .
C3 C 0.2126(6) 0.2853(6) 0.7125(5) 0.0344(11) Uani 1 1 d . . . . .
C4 C 0.0874(6) 0.1639(6) 0.7068(5) 0.0360(12) Uani 1 1 d . . . . .
C5 C 0.0780(5) 0.0342(6) 0.6463(5) 0.0333(11) Uani 1 1 d . . . . .
C6 C 0.1945(5) 0.0301(5) 0.5897(4) 0.0283(9) Uani 1 1 d . . . . .
F7 F 0.4459(4) 0.3979(3) 0.6599(3) 0.0407(7) Uani 1 1 d . . . . .
F8 F 0.2211(4) 0.4088(4) 0.7747(3) 0.0488(8) Uani 1 1 d . . . . .
F9 F -0.0278(4) 0.1699(4) 0.7565(3) 0.0490(9) Uani 1 1 d . . . . .
F10 F -0.0438(3) -0.0849(4) 0.6423(3) 0.0455(8) Uani 1 1 d . . . . .
F11 F 0.1807(3) -0.0968(3) 0.5261(3) 0.0349(6) Uani 1 1 d . . . . .
C12 C 0.4727(5) 0.1901(4) 0.3129(4) 0.0206(8) Uani 1 1 d . . . . .
C13 C 0.5424(5) 0.1511(5) 0.2217(4) 0.0260(9) Uani 1 1 d . . . . .
C14 C 0.5393(6) 0.1935(5) 0.1039(4) 0.0301(10) Uani 1 1 d . . . . .
C15 C 0.4635(6) 0.2782(5) 0.0767(4) 0.0317(10) Uani 1 1 d . . . . .
C16 C 0.3935(5) 0.3201(5) 0.1659(4) 0.0277(9) Uani 1 1 d . . . . .
C17 C 0.3974(5) 0.2755(5) 0.2823(4) 0.0242(9) Uani 1 1 d . . . . .
F18 F 0.6198(3) 0.0709(3) 0.2461(3) 0.0368(7) Uani 1 1 d . . . . .
F19 F 0.6090(4) 0.1532(4) 0.0184(3) 0.0479(8) Uani 1 1 d . . . . .
F20 F 0.4609(4) 0.3205(4) -0.0367(3) 0.0473(8) Uani 1 1 d . . . . .
F21 F 0.3222(4) 0.4051(3) 0.1400(3) 0.0420(7) Uani 1 1 d . . . . .
F22 F 0.3307(3) 0.3216(3) 0.3674(3) 0.0318(6) Uani 1 1 d . . . . .
C23 C 0.6905(5) 0.3008(5) 0.5987(4) 0.0239(9) Uani 1 1 d . . . . .
C24 C 0.7776(6) 0.4229(5) 0.5523(5) 0.0315(10) Uani 1 1 d . . . . .
C25 C 0.9002(6) 0.5267(5) 0.6223(5) 0.0364(11) Uani 1 1 d . . . . .
C26 C 0.9393(6) 0.5136(5) 0.7436(5) 0.0357(11) Uani 1 1 d . . . . .
C27 C 0.8554(6) 0.3939(6) 0.7940(5) 0.0370(11) Uani 1 1 d . . . . .
C28 C 0.7346(6) 0.2917(5) 0.7212(4) 0.0288(10) Uani 1 1 d . . . . .
F29 F 0.7434(4) 0.4419(4) 0.4346(3) 0.0527(10) Uani 1 1 d . . . . .
F30 F 0.9819(4) 0.6429(4) 0.5737(4) 0.0571(10) Uani 1 1 d . . . . .
F31 F 1.0591(4) 0.6140(4) 0.8121(4) 0.0525(9) Uani 1 1 d . . . . .
F32 F 0.8927(5) 0.3799(4) 0.9121(3) 0.0622(11) Uani 1 1 d . . . . .
F33 F 0.6564(4) 0.1745(4) 0.7708(3) 0.0480(9) Uani 1 1 d . . . . .
C51 C 0.1228(7) -0.0300(7) 0.9856(6) 0.0453(14) Uani 1 1 d . . . . .
H51A H 0.164084 -0.025165 1.073282 0.054 Uiso 1 1 calc R U . . .
H51B H 0.184835 -0.056159 0.930026 0.054 Uiso 1 1 calc R U . . .
O52 O 0.1243(4) 0.1080(5) 0.9655(4) 0.0431(9) Uani 1 1 d . . . . .
C53 C 0.0288(7) 0.1430(7) 1.0402(5) 0.0432(13) Uani 1 1 d . . . . .
H53A H 0.026807 0.236288 1.022737 0.052 Uiso 1 1 calc R U . . .
H53B H 0.066710 0.153566 1.129776 0.052 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
Sn1 C23 2.132(4) . ?
Sn1 C1 2.147(4) . ?
Sn1 C12 2.152(4) . ?
Sn1 Sn1 2.7855(6) 2_656 ?
C1 C6 1.377(6) . ?
C1 C2 1.375(6) . ?
C2 F7 1.342(6) . ?
C2 C3 1.376(7) . ?
C3 F8 1.334(6) . ?
C3 C4 1.374(8) . ?
C4 F9 1.334(6) . ?
C4 C5 1.377(8) . ?
C5 F10 1.345(6) . ?
C5 C6 1.377(7) . ?
C6 F11 1.353(6) . ?
C12 C13 1.371(6) . ?
C12 C17 1.390(6) . ?
C13 F18 1.346(5) . ?
C13 C14 1.387(6) . ?
C14 F19 1.331(6) . ?
C14 C15 1.379(7) . ?
C15 F20 1.341(5) . ?
C15 C16 1.369(7) . ?
C16 F21 1.344(5) . ?
C16 C17 1.382(6) . ?
C17 F22 1.333(5) . ?
C23 C28 1.382(6) . ?
C23 C24 1.388(6) . ?
C24 F29 1.341(6) . ?
C24 C25 1.372(7) . ?
C25 F30 1.342(6) . ?
C25 C26 1.370(8) . ?
C26 F31 1.338(6) . ?
C26 C27 1.383(8) . ?
C27 F32 1.336(6) . ?
C27 C28 1.369(7) . ?
C28 F33 1.344(5) . ?
C51 O52 1.431(7) . ?
C51 C53 1.494(9) 2_557 ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
O52 C53 1.426(7) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?

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
C23 Sn1 C1 105.82(17) . . ?
C23 Sn1 C12 106.89(16) . . ?
C1 Sn1 C12 108.51(16) . . ?
C23 Sn1 Sn1 111.62(12) . 2_656 ?
C1 Sn1 Sn1 110.27(11) . 2_656 ?
C12 Sn1 Sn1 113.38(11) . 2_656 ?
C6 C1 C2 116.6(4) . . ?
C6 C1 Sn1 120.7(3) . . ?
C2 C1 Sn1 122.7(3) . . ?
F7 C2 C3 117.8(4) . . ?
F7 C2 C1 119.8(4) . . ?
C3 C2 C1 122.4(5) . . ?
F8 C3 C2 121.5(5) . . ?
F8 C3 C4 119.1(5) . . ?
C2 C3 C4 119.4(5) . . ?
F9 C4 C5 119.0(5) . . ?
F9 C4 C3 120.9(5) . . ?
C5 C4 C3 120.1(5) . . ?
F10 C5 C4 120.0(4) . . ?
F10 C5 C6 121.3(5) . . ?
C4 C5 C6 118.7(5) . . ?
F11 C6 C1 119.2(4) . . ?
F11 C6 C5 117.9(4) . . ?
C1 C6 C5 122.8(5) . . ?
C13 C12 C17 116.8(4) . . ?
C13 C12 Sn1 120.7(3) . . ?
C17 C12 Sn1 122.3(3) . . ?
F18 C13 C12 119.8(4) . . ?
F18 C13 C14 117.7(4) . . ?
C12 C13 C14 122.5(4) . . ?
F19 C14 C15 120.5(4) . . ?
F19 C14 C13 120.4(4) . . ?
C15 C14 C13 119.1(4) . . ?
F20 C15 C16 120.6(4) . . ?
F20 C15 C14 119.4(5) . . ?
C16 C15 C14 119.9(4) . . ?
F21 C16 C15 119.8(4) . . ?
F21 C16 C17 120.4(4) . . ?
C15 C16 C17 119.8(4) . . ?
F22 C17 C16 117.9(4) . . ?
F22 C17 C12 120.3(4) . . ?
C16 C17 C12 121.8(4) . . ?
C28 C23 C24 115.4(4) . . ?
C28 C23 Sn1 119.4(3) . . ?
C24 C23 Sn1 125.2(3) . . ?
F29 C24 C25 117.7(4) . . ?
F29 C24 C23 119.8(5) . . ?
C25 C24 C23 122.5(5) . . ?
F30 C25 C26 119.2(5) . . ?
F30 C25 C24 120.6(5) . . ?
C26 C25 C24 120.1(5) . . ?
F31 C26 C25 120.4(5) . . ?
F31 C26 C27 120.2(5) . . ?
C25 C26 C27 119.4(5) . . ?
F32 C27 C28 121.1(5) . . ?
F32 C27 C26 119.9(5) . . ?
C28 C27 C26 119.0(5) . . ?
F33 C28 C27 118.1(4) . . ?
F33 C28 C23 118.2(4) . . ?
C27 C28 C23 123.7(4) . . ?
O52 C51 C53 111.1(5) . 2_557 ?
O52 C51 H51A 109.4 . . ?
C53 C51 H51A 109.4 2_557 . ?
O52 C51 H51B 109.4 . . ?
C53 C51 H51B 109.4 2_557 . ?
H51A C51 H51B 108.0 . . ?
C53 O52 C51 109.8(4) . . ?
O52 C53 C51 111.7(5) . 2_557 ?
O52 C53 H53A 109.3 . . ?
C51 C53 H53A 109.3 2_557 . ?
O52 C53 H53B 109.3 . . ?
C51 C53 H53B 109.3 2_557 . ?
H53A C53 H53B 107.9 . . ?

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 F7 -179.8(4) . . . . ?
Sn1 C1 C2 F7 0.6(6) . . . . ?
C6 C1 C2 C3 -1.3(7) . . . . ?
Sn1 C1 C2 C3 179.1(3) . . . . ?
F7 C2 C3 F8 -2.0(7) . . . . ?
C1 C2 C3 F8 179.5(4) . . . . ?
F7 C2 C3 C4 178.5(4) . . . . ?
C1 C2 C3 C4 0.0(7) . . . . ?
F8 C3 C4 F9 3.7(7) . . . . ?
C2 C3 C4 F9 -176.8(4) . . . . ?
F8 C3 C4 C5 -178.1(4) . . . . ?
C2 C3 C4 C5 1.5(7) . . . . ?
F9 C4 C5 F10 -2.6(7) . . . . ?
C3 C4 C5 F10 179.1(4) . . . . ?
F9 C4 C5 C6 176.7(4) . . . . ?
C3 C4 C5 C6 -1.6(7) . . . . ?
C2 C1 C6 F11 178.5(4) . . . . ?
Sn1 C1 C6 F11 -1.8(6) . . . . ?
C2 C1 C6 C5 1.2(7) . . . . ?
Sn1 C1 C6 C5 -179.1(4) . . . . ?
F10 C5 C6 F11 2.2(7) . . . . ?
C4 C5 C6 F11 -177.2(4) . . . . ?
F10 C5 C6 C1 179.5(4) . . . . ?
C4 C5 C6 C1 0.2(7) . . . . ?
C17 C12 C13 F18 178.6(4) . . . . ?
Sn1 C12 C13 F18 3.8(6) . . . . ?
C17 C12 C13 C14 0.0(7) . . . . ?
Sn1 C12 C13 C14 -174.8(4) . . . . ?
F18 C13 C14 F19 1.1(7) . . . . ?
C12 C13 C14 F19 179.8(4) . . . . ?
F18 C13 C14 C15 -178.6(4) . . . . ?
C12 C13 C14 C15 0.0(8) . . . . ?
F19 C14 C15 F20 -0.3(8) . . . . ?
C13 C14 C15 F20 179.5(5) . . . . ?
F19 C14 C15 C16 -179.4(5) . . . . ?
C13 C14 C15 C16 0.4(8) . . . . ?
F20 C15 C16 F21 -0.4(7) . . . . ?
C14 C15 C16 F21 178.7(5) . . . . ?
F20 C15 C16 C17 -180.0(4) . . . . ?
C14 C15 C16 C17 -0.9(8) . . . . ?
F21 C16 C17 F22 -1.1(7) . . . . ?
C15 C16 C17 F22 178.4(4) . . . . ?
F21 C16 C17 C12 -178.6(4) . . . . ?
C15 C16 C17 C12 0.9(7) . . . . ?
C13 C12 C17 F22 -177.9(4) . . . . ?
Sn1 C12 C17 F22 -3.2(6) . . . . ?
C13 C12 C17 C16 -0.4(7) . . . . ?
Sn1 C12 C17 C16 174.3(3) . . . . ?
C28 C23 C24 F29 -179.7(5) . . . . ?
Sn1 C23 C24 F29 -1.6(7) . . . . ?
C28 C23 C24 C25 0.8(7) . . . . ?
Sn1 C23 C24 C25 178.8(4) . . . . ?
F29 C24 C25 F30 0.1(8) . . . . ?
C23 C24 C25 F30 179.7(5) . . . . ?
F29 C24 C25 C26 179.3(5) . . . . ?
C23 C24 C25 C26 -1.2(8) . . . . ?
F30 C25 C26 F31 -1.3(8) . . . . ?
C24 C25 C26 F31 179.6(5) . . . . ?
F30 C25 C26 C27 -179.9(5) . . . . ?
C24 C25 C26 C27 0.9(8) . . . . ?
F31 C26 C27 F32 1.3(8) . . . . ?
C25 C26 C27 F32 179.9(5) . . . . ?
F31 C26 C27 C28 -179.0(5) . . . . ?
C25 C26 C27 C28 -0.3(8) . . . . ?
F32 C27 C28 F33 -1.8(8) . . . . ?
C26 C27 C28 F33 178.5(5) . . . . ?
F32 C27 C28 C23 179.7(5) . . . . ?
C26 C27 C28 C23 -0.1(8) . . . . ?
C24 C23 C28 F33 -178.7(4) . . . . ?
Sn1 C23 C28 F33 3.1(6) . . . . ?
C24 C23 C28 C27 -0.1(7) . . . . ?
Sn1 C23 C28 C27 -178.3(4) . . . . ?
C53 C51 O52 C53 55.9(7) 2_557 . . . ?
C51 O52 C53 C51 -56.3(6) . . . 2_557 ?

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

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



# ............... End of .RES file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .HKL SHELXL file: job.hkl
#...............................................................................


