# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# 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 
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data_cwmwm08
_database_code_depnum_ccdc_archive 'CCDC 1549636'
_audit_update_record             
;
2017-05-12 deposited with the CCDC.
2017-07-19 downloaded from the CCDC.
;

_vrf_PLAT302_cwmwm08             
;
PROBLEM: _G Anion/Solvent Disorder ............ Percentage = 41 
RESPONSE: The cocrystallized toluene solvent molecule is modeled
as disordered over a crystallographic inversion center (0.50:0.50).
;

_vrf_PLAT860_cwmwm08             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 6 
RESPONSE: Analogous bond lengths and angles were restrained to be
similar. Anisotropic displacement parameters for pairs of
symmetry related atoms were constrained to be equivalent.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            cwmwm08
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H18 Co N8 O10, B F4, C7 H8'
_chemical_formula_sum            'C25 H26 B Co F4 N8 O10'
_chemical_formula_weight         744.28

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.6690(16)
_cell_length_b                   15.7386(17)
_cell_length_c                   12.9152(14)
_cell_angle_alpha                90
_cell_angle_beta                 99.389(2)
_cell_angle_gamma                90
_cell_volume                     2941.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(5)
_cell_measurement_reflns_used    3787
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      37.11

_exptl_crystal_description       needle
_exptl_crystal_colour            pink-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_F_000             1520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.681
_shelx_estimated_absorpt_T_min   0.736
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6618
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2016a)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(5)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            64770
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.912
_diffrn_reflns_theta_max         38.792
_diffrn_reflns_theta_full        37.785
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8254
_reflns_number_gt                6347
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
; 
The cocrystallized toluene solvent molecule is modeled as
disordered over a crystallographic inversion center (0.50:0.50).
Analogous bond lengths and angles were restrained to be similar.
Anisotropic displacement parameters for pairs of symmetry related
atoms were constrained to be equivalent.

The NH₂ hydrogen atoms were found from the difference Fourier 
map and refined freely. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0696P)²+1.5871P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8254
_refine_ls_number_parameters     251
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1288
_refine_ls_wR_factor_gt          0.1181
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
CO1 Co 0.500000 0.84340(2) 0.250000 0.01333(5) Uani 1 2 d S T P . .
N1 N 0.59792(7) 0.92789(7) 0.25238(8) 0.01690(16) Uani 1 1 d . . . . .
H1C H 0.6259(15) 0.9211(14) 0.2013(18) 0.034(5) Uiso 1 1 d . . . . .
H1D H 0.5765(13) 0.9826(12) 0.2466(16) 0.023(4) Uiso 1 1 d . . . . .
C1 C 0.66364(8) 0.91553(8) 0.35183(10) 0.0196(2) Uani 1 1 d . . . . .
H1A H 0.705760 0.964852 0.365582 0.024 Uiso 1 1 calc R U . . .
H1B H 0.701122 0.863681 0.347822 0.024 Uiso 1 1 calc R U . . .
C2 C 0.60526(8) 0.90692(8) 0.43765(9) 0.0201(2) Uani 1 1 d . . . . .
H2A H 0.643174 0.885991 0.503154 0.024 Uiso 1 1 calc R U . . .
H2B H 0.578277 0.962494 0.452016 0.024 Uiso 1 1 calc R U . . .
N2 N 0.53141(7) 0.84531(6) 0.39887(8) 0.01585(15) Uani 1 1 d . . . . .
C3 C 0.49794(8) 0.79817(7) 0.46439(9) 0.01772(18) Uani 1 1 d . . . . .
H3 H 0.526076 0.800611 0.535993 0.021 Uiso 1 1 calc R U . . .
C4 C 0.41973(8) 0.74119(7) 0.43635(9) 0.01686(18) Uani 1 1 d . . . . .
C5 C 0.38363(8) 0.70339(8) 0.51862(9) 0.01895(19) Uani 1 1 d . . . . .
H5 H 0.412626 0.712122 0.589117 0.023 Uiso 1 1 calc R U . . .
C6 C 0.30516(9) 0.65295(7) 0.49702(10) 0.01908(19) Uani 1 1 d . . . . .
C7 C 0.26171(9) 0.63787(8) 0.39519(10) 0.0199(2) Uani 1 1 d . . . . .
H7 H 0.207595 0.603824 0.381677 0.024 Uiso 1 1 calc R U . . .
C8 C 0.29889(8) 0.67344(7) 0.31403(9) 0.01853(19) Uani 1 1 d . . . . .
C9 C 0.37862(8) 0.72713(7) 0.32924(9) 0.01621(17) Uani 1 1 d . . . . .
O1 O 0.40882(6) 0.75793(6) 0.24927(7) 0.01785(15) Uani 1 1 d . . . . .
N3 N 0.26362(8) 0.61900(7) 0.58258(9) 0.0229(2) Uani 1 1 d . . . . .
O2 O 0.30069(9) 0.63246(9) 0.67271(9) 0.0357(3) Uani 1 1 d . . . . .
O3 O 0.19035(7) 0.57919(7) 0.56021(9) 0.0282(2) Uani 1 1 d . . . . .
N4 N 0.25189(8) 0.65436(7) 0.20798(9) 0.0243(2) Uani 1 1 d . . . . .
O4 O 0.22104(9) 0.58143(7) 0.19280(9) 0.0358(3) Uani 1 1 d . . . . .
O5 O 0.24409(8) 0.70981(7) 0.14104(9) 0.0316(2) Uani 1 1 d . . . . .
B1 B 0.000000 0.64770(13) 0.250000 0.0216(3) Uani 1 2 d S T P . .
F1 F 0.06980(7) 0.69873(7) 0.22511(9) 0.0407(2) Uani 1 1 d . . . . .
F2 F -0.03368(7) 0.59460(6) 0.16498(7) 0.03189(19) Uani 1 1 d . . . . .
C10 C 0.606(2) 0.407(2) -0.0127(10) 0.0534(6) Uani 0.5 1 d D . P A -1
H10A H 0.616603 0.372994 0.051682 0.080 Uiso 0.5 1 calc R U P A -1
H10B H 0.663323 0.435654 -0.022017 0.080 Uiso 0.5 1 calc R U P A -1
H10C H 0.585581 0.369845 -0.072938 0.080 Uiso 0.5 1 calc R U P A -1
C11 C 0.5344(2) 0.4706(3) -0.0050(3) 0.0457(9) Uani 0.5 1 d D . P A -1
C12 C 0.513(3) 0.486(2) 0.0902(9) 0.048(2) Uani 0.5 1 d D . P A -1
H12 H 0.541747 0.455601 0.150260 0.057 Uiso 0.5 1 calc R U P A -1
C13 C 0.4425(3) 0.5528(3) 0.0987(3) 0.0460(8) Uani 0.5 1 d D . P A -1
H13 H 0.431070 0.568934 0.166275 0.055 Uiso 0.5 1 calc R U P A -1
C14 C 0.393(2) 0.592(2) 0.0102(9) 0.0534(6) Uani 0.5 1 d D . P A -1
H14 H 0.344293 0.631627 0.015111 0.064 Uiso 0.5 1 calc R U P A -1
C15 C 0.4182(3) 0.5701(4) -0.0867(4) 0.0634(15) Uani 0.5 1 d D . P A -1
H15 H 0.390445 0.598921 -0.148503 0.076 Uiso 0.5 1 calc R U P A -1
C16 C 0.488(2) 0.503(2) -0.0943(9) 0.048(2) Uani 0.5 1 d D . P A -1
H16 H 0.498609 0.482738 -0.160673 0.057 Uiso 0.5 1 calc R U P A -1


_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
CO1 O1 1.8958(9) 2_655 ?
CO1 O1 1.8959(9) . ?
CO1 N2 1.9029(10) 2_655 ?
CO1 N2 1.9029(10) . ?
CO1 N1 1.9540(10) . ?
CO1 N1 1.9541(10) 2_655 ?
N1 C1 1.4875(16) . ?
N1 H1C 0.84(2) . ?
N1 H1D 0.916(19) . ?
C1 C2 1.5133(18) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N2 1.4790(15) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N2 C3 1.2818(15) . ?
C3 C4 1.4547(16) . ?
C3 H3 0.9500 . ?
C4 C5 1.3952(16) . ?
C4 C9 1.4332(16) . ?
C5 C6 1.3886(17) . ?
C5 H5 0.9500 . ?
C6 C7 1.3852(18) . ?
C6 N3 1.4483(16) . ?
C7 C8 1.3770(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.4302(16) . ?
C8 N4 1.4607(16) . ?
C9 O1 1.2834(14) . ?
N3 O2 1.2202(16) . ?
N3 O3 1.2370(16) . ?
N4 O5 1.2206(15) . ?
N4 O4 1.2376(15) . ?
B1 F1 1.3798(16) . ?
B1 F1 1.3799(16) 2 ?
B1 F2 1.4040(15) . ?
B1 F2 1.4040(15) 2 ?
C10 C11 1.46(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C16 1.340(18) . ?
C11 C12 1.341(18) . ?
C12 C13 1.49(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.40(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.41(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.49(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 CO1 O1 89.61(6) 2_655 . ?
O1 CO1 N2 94.05(4) 2_655 2_655 ?
O1 CO1 N2 87.24(4) . 2_655 ?
O1 CO1 N2 87.24(4) 2_655 . ?
O1 CO1 N2 94.05(4) . . ?
N2 CO1 N2 178.18(6) 2_655 . ?
O1 CO1 N1 88.08(4) 2_655 . ?
O1 CO1 N1 177.62(4) . . ?
N2 CO1 N1 93.52(4) 2_655 . ?
N2 CO1 N1 85.24(4) . . ?
O1 CO1 N1 177.62(4) 2_655 2_655 ?
O1 CO1 N1 88.09(4) . 2_655 ?
N2 CO1 N1 85.25(4) 2_655 2_655 ?
N2 CO1 N1 93.52(4) . 2_655 ?
N1 CO1 N1 94.23(6) . 2_655 ?
C1 N1 CO1 107.20(7) . . ?
C1 N1 H1C 109.3(15) . . ?
CO1 N1 H1C 110.8(15) . . ?
C1 N1 H1D 111.0(12) . . ?
CO1 N1 H1D 113.4(12) . . ?
H1C N1 H1D 105.1(19) . . ?
N1 C1 C2 106.24(9) . . ?
N1 C1 H1A 110.5 . . ?
C2 C1 H1A 110.5 . . ?
N1 C1 H1B 110.5 . . ?
C2 C1 H1B 110.5 . . ?
H1A C1 H1B 108.7 . . ?
N2 C2 C1 106.35(9) . . ?
N2 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N2 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
C3 N2 C2 119.62(10) . . ?
C3 N2 CO1 127.02(8) . . ?
C2 N2 CO1 113.31(7) . . ?
N2 C3 C4 124.33(10) . . ?
N2 C3 H3 117.8 . . ?
C4 C3 H3 117.8 . . ?
C5 C4 C9 121.13(10) . . ?
C5 C4 C3 117.08(10) . . ?
C9 C4 C3 121.74(10) . . ?
C6 C5 C4 119.73(11) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C7 C6 C5 121.78(11) . . ?
C7 C6 N3 118.39(11) . . ?
C5 C6 N3 119.72(11) . . ?
C8 C7 C6 118.36(11) . . ?
C8 C7 H7 120.8 . . ?
C6 C7 H7 120.8 . . ?
C7 C8 C9 123.52(11) . . ?
C7 C8 N4 116.44(11) . . ?
C9 C8 N4 120.04(10) . . ?
O1 C9 C8 119.64(10) . . ?
O1 C9 C4 124.91(10) . . ?
C8 C9 C4 115.44(10) . . ?
C9 O1 CO1 126.86(7) . . ?
O2 N3 O3 123.08(12) . . ?
O2 N3 C6 119.10(11) . . ?
O3 N3 C6 117.80(11) . . ?
O5 N4 O4 124.15(12) . . ?
O5 N4 C8 119.51(11) . . ?
O4 N4 C8 116.34(11) . . ?
F1 B1 F1 108.82(17) . 2 ?
F1 B1 F2 110.13(6) . . ?
F1 B1 F2 110.41(7) 2 . ?
F1 B1 F2 110.41(7) . 2 ?
F1 B1 F2 110.13(6) 2 2 ?
F2 B1 F2 106.93(16) . 2 ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C16 C11 C12 124(3) . . ?
C16 C11 C10 118.0(14) . . ?
C12 C11 C10 117.6(14) . . ?
C11 C12 C13 117.7(15) . . ?
C11 C12 H12 121.2 . . ?
C13 C12 H12 121.2 . . ?
C14 C13 C12 122.1(14) . . ?
C14 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C13 C14 C15 116(2) . . ?
C13 C14 H14 122.1 . . ?
C15 C14 H14 122.1 . . ?
C14 C15 C16 121.5(14) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C11 C16 C15 118.1(15) . . ?
C11 C16 H16 120.9 . . ?
C15 C16 H16 120.9 . . ?

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
CO1 N1 C1 C2 -46.23(10) . . . . ?
N1 C1 C2 N2 47.62(12) . . . . ?
C1 C2 N2 C3 149.63(11) . . . . ?
C1 C2 N2 CO1 -28.10(11) . . . . ?
C2 N2 C3 C4 174.09(11) . . . . ?
CO1 N2 C3 C4 -8.52(17) . . . . ?
N2 C3 C4 C5 -171.18(11) . . . . ?
N2 C3 C4 C9 6.13(18) . . . . ?
C9 C4 C5 C6 -1.67(18) . . . . ?
C3 C4 C5 C6 175.66(11) . . . . ?
C4 C5 C6 C7 0.86(19) . . . . ?
C4 C5 C6 N3 -175.32(11) . . . . ?
C5 C6 C7 C8 0.83(19) . . . . ?
N3 C6 C7 C8 177.06(11) . . . . ?
C6 C7 C8 C9 -1.79(19) . . . . ?
C6 C7 C8 N4 178.76(11) . . . . ?
C7 C8 C9 O1 -179.85(11) . . . . ?
N4 C8 C9 O1 -0.42(17) . . . . ?
C7 C8 C9 C4 0.99(17) . . . . ?
N4 C8 C9 C4 -179.58(11) . . . . ?
C5 C4 C9 O1 -178.35(11) . . . . ?
C3 C4 C9 O1 4.45(18) . . . . ?
C5 C4 C9 C8 0.76(16) . . . . ?
C3 C4 C9 C8 -176.44(11) . . . . ?
C8 C9 O1 CO1 169.45(8) . . . . ?
C4 C9 O1 CO1 -11.47(17) . . . . ?
O1 CO1 O1 C9 94.87(10) 2_655 . . . ?
N2 CO1 O1 C9 -171.06(10) 2_655 . . . ?
N2 CO1 O1 C9 7.66(10) . . . . ?
N1 CO1 O1 C9 -85.73(10) 2_655 . . . ?
C7 C6 N3 O2 -179.34(13) . . . . ?
C5 C6 N3 O2 -3.03(19) . . . . ?
C7 C6 N3 O3 -1.09(17) . . . . ?
C5 C6 N3 O3 175.22(12) . . . . ?
C7 C8 N4 O5 141.23(14) . . . . ?
C9 C8 N4 O5 -38.24(19) . . . . ?
C7 C8 N4 O4 -37.81(18) . . . . ?
C9 C8 N4 O4 142.72(13) . . . . ?
C16 C11 C12 C13 -10(5) . . . . ?
C10 C11 C12 C13 178(2) . . . . ?
C11 C12 C13 C14 7(4) . . . . ?
C12 C13 C14 C15 -5(4) . . . . ?
C13 C14 C15 C16 6(4) . . . . ?
C12 C11 C16 C15 11(5) . . . . ?
C10 C11 C16 C15 -177(2) . . . . ?
C14 C15 C16 C11 -8(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1C O3 0.84(2) 2.19(2) 3.0181(15) 172(2) 8_565
N1 H1D F2 0.916(19) 2.504(19) 3.3427(15) 152.3(16) 3
N1 H1D F2 0.916(19) 2.24(2) 3.0396(14) 144.9(17) 4
C1 H1B O5 0.99 2.55 3.5046(17) 162.4 2_655
C2 H2A O4 0.99 2.58 3.4571(17) 147.7 8_566
C2 H2A O5 0.99 2.60 3.5606(16) 162.7 8_566
C2 H2A O5 0.99 2.60 3.5606(16) 162.7 8_566
C3 H3 F1 0.95 2.42 3.3607(16) 169.5 8_566
C3 H3 F2 0.95 2.60 3.1886(15) 120.8 8_566
C7 H7 F2 0.95 2.53 3.3777(17) 148.9 2

_refine_diff_density_max         1.141
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.098


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/toluene'
_chemical_properties_physical    ', Moisture-sensitive'
####################################################################### 
# 
# 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_cwmwm10
_database_code_depnum_ccdc_archive 'CCDC 1549635'
_audit_update_record             
;
2017-05-12 deposited with the CCDC.
2017-07-19 downloaded from the CCDC.
;

_vrf_PLAT007_cwmwm10             
; 
PROBLEM: _G Number of Unrefined Donor-H Atoms .............. 4 
RESPONSE: The NH~2~ hydrogen atoms were given a riding model due 
to disorder. 
;

_vrf_PLAT301_cwmwm10             
; 
PROBLEM: _G Main Residue Disorder ............ Percentage = 19 
RESPONSE: The ethane linkage is modeled as disordered over two 
positions (0.89:0.11). 
;

_vrf_PLAT302_cwmwm10             
; 
PROBLEM: _G Anion/Solvent Disorder ............ Percentage = 45 
RESPONSE: The anion site is modeled as a mixture of PF~6~^-^ and 
BF~4~^-^ (0.70:0.30). 
;

_vrf_PLAT860_cwmwm10             
; 
PROBLEM: _G Number of Least-Squares Restraints ............. 51 
RESPONSE: Analogous bond lengths and angles in all disordered 
moieties were restrained to be similar, respectively. Anisotropic 
displacement parameters for pairs of proximal atoms were 
constrained to be equivalent. 
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            cwmwm10
_chemical_melting_point          ?
_chemical_formula_moiety         
'C18 H20 Co N6 O6, 0.70(F6 P), 2(C7 H8), 0.30(B F4)'
_chemical_formula_sum            'C32 H36 B0.30 Co F5.39 N6 O6 P0.70'
_chemical_formula_weight         786.97

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.6579(11)
_cell_length_b                   18.1377(15)
_cell_length_c                   13.7492(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.4907(18)
_cell_angle_gamma                90
_cell_volume                     3405.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(5)
_cell_measurement_reflns_used    3983
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      35.63

_exptl_crystal_description       needle
_exptl_crystal_colour            pink-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_F_000             1622
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.620
_shelx_estimated_absorpt_T_min   0.755
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6514
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2016a)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(5)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            118185
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.867
_diffrn_reflns_theta_max         36.406
_diffrn_reflns_theta_full        36.319
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8288
_reflns_number_gt                6153
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
; 
The ethane linkage is modeled as disordered over two positions 
(0.89:0.11) and the anion site is modeled as a mixture of PF₆⁻ 
and BF₄⁻ (0.70:0.30). 
  
Analogous bond lengths and angles in all disordered moieties 
were restrained to be similar, respectively. Anisotropic 
displacement parameters for pairs of proximal atoms were 
constrained to be equivalent. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0478P)²+2.7873P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8288
_refine_ls_number_parameters     278
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1093
_refine_ls_wR_factor_gt          0.0980
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
CO1 Co 0.500000 0.64850(2) 0.750000 0.01627(6) Uani 1 2 d S T P A .
N1 N 0.39528(7) 0.57466(6) 0.74553(7) 0.01949(18) Uani 0.886(3) 1 d D . P A 1
H1E H 0.420241 0.529008 0.757556 0.023 Uiso 0.886(3) 1 calc R U P A 1
H1F H 0.349621 0.584828 0.791435 0.023 Uiso 0.886(3) 1 calc R U P A 1
C1 C 0.34976(10) 0.57697(8) 0.64664(10) 0.0210(3) Uani 0.886(3) 1 d D . P A 1
H1A H 0.304008 0.619137 0.641326 0.025 Uiso 0.886(3) 1 calc R U P A 1
H1B H 0.312885 0.530953 0.633754 0.025 Uiso 0.886(3) 1 calc R U P A 1
C2 C 0.43225(13) 0.58530(9) 0.57453(10) 0.0210(3) Uani 0.886(3) 1 d D . P A 1
H2A H 0.471225 0.539389 0.570767 0.025 Uiso 0.886(3) 1 calc R U P A 1
H2B H 0.406134 0.597002 0.508936 0.025 Uiso 0.886(3) 1 calc R U P A 1
N1' N 0.39528(7) 0.57466(6) 0.74553(7) 0.01949(18) Uani 0.114(3) 1 d D . P A 5
H1G H 0.407581 0.539416 0.791132 0.023 Uiso 0.114(3) 1 calc R U P A 5
H1H H 0.337455 0.596635 0.760539 0.023 Uiso 0.114(3) 1 calc R U P A 5
C1' C 0.3858(8) 0.5375(6) 0.6439(7) 0.0210(3) Uani 0.114(3) 1 d D . P A 5
H1C H 0.437754 0.500197 0.634173 0.025 Uiso 0.114(3) 1 calc R U P A 5
H1D H 0.321007 0.513911 0.635153 0.025 Uiso 0.114(3) 1 calc R U P A 5
C2' C 0.3980(9) 0.6018(7) 0.5761(8) 0.0210(3) Uani 0.114(3) 1 d D . P A 5
H2C H 0.339390 0.633868 0.577865 0.025 Uiso 0.114(3) 1 calc R U P A 5
H2D H 0.406923 0.584228 0.508581 0.025 Uiso 0.114(3) 1 calc R U P A 5
N2 N 0.49205(8) 0.64610(6) 0.61183(7) 0.01895(17) Uani 1 1 d D . . . .
C3 C 0.53057(9) 0.69240(7) 0.55281(8) 0.0189(2) Uani 1 1 d . . . . .
H3 H 0.514329 0.688181 0.485717 0.023 Uiso 1 1 calc R U . . .
C4 C 0.59673(8) 0.75026(7) 0.58167(8) 0.01777(19) Uani 1 1 d . . . . .
C5 C 0.63455(9) 0.79510(7) 0.50793(8) 0.0191(2) Uani 1 1 d . . . . .
H5 H 0.612375 0.789163 0.442726 0.023 Uiso 1 1 calc R U . . .
C6 C 0.70404(9) 0.84790(7) 0.53014(8) 0.01925(19) Uani 1 1 d . . . . .
C7 C 0.73928(9) 0.85728(7) 0.62568(9) 0.0220(2) Uani 1 1 d . . . . .
H7 H 0.787985 0.893237 0.639640 0.026 Uiso 1 1 calc R U . . .
C8 C 0.70264(10) 0.81403(7) 0.69843(9) 0.0225(2) Uani 1 1 d . . . . .
H8 H 0.726672 0.820425 0.762920 0.027 Uiso 1 1 calc R U . . .
C9 C 0.62959(9) 0.75982(7) 0.68007(8) 0.0189(2) Uani 1 1 d . . . . .
O1 O 0.59904(7) 0.72157(5) 0.75348(6) 0.02182(17) Uani 1 1 d . . . . .
N3 N 0.74719(8) 0.89048(6) 0.45324(8) 0.02153(19) Uani 1 1 d . . . . .
O2 O 0.81048(7) 0.93689(6) 0.47385(7) 0.0279(2) Uani 1 1 d . . . . .
O3 O 0.72080(8) 0.87831(6) 0.36806(7) 0.0278(2) Uani 1 1 d . . . . .
P1 P 0.500000 0.36565(5) 0.750000 0.01843(16) Uani 0.697(2) 2 d S T P B 1
F1 F 0.4551(2) 0.30444(11) 0.67959(18) 0.0245(3) Uani 0.697(2) 1 d . . P B 1
F2 F 0.45599(9) 0.42963(6) 0.67990(9) 0.0276(3) Uani 0.697(2) 1 d . . P B 1
F3 F 0.40097(9) 0.36775(9) 0.81154(9) 0.0286(3) Uani 0.697(2) 1 d . . P B 1
B1' B 0.4962(10) 0.3732(5) 0.7452(9) 0.01843(16) Uani 0.1513(12) 1 d D U P B -5
F1' F 0.4618(13) 0.3181(7) 0.6866(11) 0.0245(3) Uani 0.1513(12) 1 d D U P B -5
F2' F 0.4186(10) 0.4125(8) 0.7805(11) 0.063(4) Uani 0.1513(12) 1 d D U P B -5
F3' F 0.5448(9) 0.3413(6) 0.8218(7) 0.061(3) Uani 0.1513(12) 1 d D U P B -5
F4' F 0.5599(11) 0.4159(6) 0.6936(8) 0.068(4) Uani 0.1513(12) 1 d D U P B -5
C10 C 0.62594(14) 0.94461(10) -0.11927(12) 0.0406(4) Uani 1 1 d . . . . .
H10A H 0.584236 0.918057 -0.165852 0.061 Uiso 1 1 calc R U . . .
H10B H 0.693535 0.944992 -0.142612 0.061 Uiso 1 1 calc R U . . .
H10C H 0.602466 0.995414 -0.112724 0.061 Uiso 1 1 calc R U . . .
C11 C 0.62223(11) 0.90675(9) -0.02183(11) 0.0300(3) Uani 1 1 d . . . . .
C12 C 0.63938(12) 0.83137(9) -0.01294(11) 0.0322(3) Uani 1 1 d . . . . .
H12 H 0.653569 0.803239 -0.069370 0.039 Uiso 1 1 calc R U . . .
C13 C 0.63613(12) 0.79669(10) 0.07663(12) 0.0357(3) Uani 1 1 d . . . . .
H13 H 0.649101 0.745345 0.081297 0.043 Uiso 1 1 calc R U . . .
C14 C 0.61397(14) 0.83665(11) 0.15969(12) 0.0420(4) Uani 1 1 d . . . . .
H14 H 0.610833 0.812834 0.221123 0.050 Uiso 1 1 calc R U . . .
C15 C 0.59649(14) 0.91162(12) 0.15197(13) 0.0439(4) Uani 1 1 d . . . . .
H15 H 0.581386 0.939371 0.208484 0.053 Uiso 1 1 calc R U . . .
C16 C 0.60088(12) 0.94655(10) 0.06223(12) 0.0358(3) Uani 1 1 d . . . . .
H16 H 0.589216 0.998087 0.058023 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
CO1 O1 1.8940(9) 2_656 ?
CO1 O1 1.8940(9) . ?
CO1 N2 1.9024(10) . ?
CO1 N2 1.9025(10) 2_656 ?
CO1 N1 1.9600(11) . ?
CO1 N1' 1.9600(11) . ?
CO1 N1 1.9600(11) 2_656 ?
CO1 N1' 1.9600(11) 2_656 ?
N1 C1 1.4908(17) . ?
N1 H1E 0.9100 . ?
N1 H1F 0.9100 . ?
C1 C2 1.515(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N2 1.4624(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N1' C1' 1.556(9) . ?
N1' H1G 0.9100 . ?
N1' H1H 0.9100 . ?
C1' C2' 1.503(13) . ?
C1' H1C 0.9900 . ?
C1' H1D 0.9900 . ?
C2' N2 1.589(11) . ?
C2' H2C 0.9900 . ?
C2' H2D 0.9900 . ?
N2 C3 1.2837(15) . ?
C3 C4 1.4385(17) . ?
C3 H3 0.9500 . ?
C4 C5 1.4019(16) . ?
C4 C9 1.4323(16) . ?
C5 C6 1.3806(17) . ?
C5 H5 0.9500 . ?
C6 C7 1.4055(17) . ?
C6 N3 1.4395(15) . ?
C7 C8 1.3692(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.4218(17) . ?
C8 H8 0.9500 . ?
C9 O1 1.2967(14) . ?
N3 O2 1.2377(15) . ?
N3 O3 1.2422(14) . ?
P1 F1 1.5921(15) 2_656 ?
P1 F1 1.5921(15) . ?
P1 F3 1.6020(12) . ?
P1 F3 1.6020(12) 2_656 ?
P1 F2 1.6209(13) 2_656 ?
P1 F2 1.6209(13) . ?
B1' F1' 1.365(7) . ?
B1' F3' 1.367(7) . ?
B1' F4' 1.368(7) . ?
B1' F2' 1.369(7) . ?
C10 C11 1.507(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.392(2) . ?
C11 C16 1.396(2) . ?
C12 C13 1.384(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 CO1 O1 91.20(6) 2_656 . ?
O1 CO1 N2 87.49(4) 2_656 . ?
O1 CO1 N2 94.35(4) . . ?
O1 CO1 N2 94.35(4) 2_656 2_656 ?
O1 CO1 N2 87.49(4) . 2_656 ?
N2 CO1 N2 177.37(6) . 2_656 ?
O1 CO1 N1 87.51(4) 2_656 . ?
O1 CO1 N1 178.66(4) . . ?
N2 CO1 N1 85.27(4) . . ?
N2 CO1 N1 92.93(4) 2_656 . ?
O1 CO1 N1' 87.51(4) 2_656 . ?
O1 CO1 N1' 178.66(4) . . ?
N2 CO1 N1' 85.27(4) . . ?
N2 CO1 N1' 92.93(4) 2_656 . ?
O1 CO1 N1 178.67(4) 2_656 2_656 ?
O1 CO1 N1 87.51(4) . 2_656 ?
N2 CO1 N1 92.93(4) . 2_656 ?
N2 CO1 N1 85.27(4) 2_656 2_656 ?
N1 CO1 N1 93.79(6) . 2_656 ?
O1 CO1 N1' 178.67(4) 2_656 2_656 ?
O1 CO1 N1' 87.51(4) . 2_656 ?
N2 CO1 N1' 92.93(4) . 2_656 ?
N2 CO1 N1' 85.27(4) 2_656 2_656 ?
N1' CO1 N1' 93.79(6) . 2_656 ?
C1 N1 CO1 107.93(8) . . ?
C1 N1 H1E 110.1 . . ?
CO1 N1 H1E 110.1 . . ?
C1 N1 H1F 110.1 . . ?
CO1 N1 H1F 110.1 . . ?
H1E N1 H1F 108.4 . . ?
N1 C1 C2 107.04(11) . . ?
N1 C1 H1A 110.3 . . ?
C2 C1 H1A 110.3 . . ?
N1 C1 H1B 110.3 . . ?
C2 C1 H1B 110.3 . . ?
H1A C1 H1B 108.6 . . ?
N2 C2 C1 105.19(11) . . ?
N2 C2 H2A 110.7 . . ?
C1 C2 H2A 110.7 . . ?
N2 C2 H2B 110.7 . . ?
C1 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
C1' N1' CO1 112.3(4) . . ?
C1' N1' H1G 109.2 . . ?
CO1 N1' H1G 109.2 . . ?
C1' N1' H1H 109.2 . . ?
CO1 N1' H1H 109.2 . . ?
H1G N1' H1H 107.9 . . ?
C2' C1' N1' 102.3(7) . . ?
C2' C1' H1C 111.3 . . ?
N1' C1' H1C 111.3 . . ?
C2' C1' H1D 111.3 . . ?
N1' C1' H1D 111.3 . . ?
H1C C1' H1D 109.2 . . ?
C1' C2' N2 107.1(8) . . ?
C1' C2' H2C 110.3 . . ?
N2 C2' H2C 110.3 . . ?
C1' C2' H2D 110.3 . . ?
N2 C2' H2D 110.3 . . ?
H2C C2' H2D 108.6 . . ?
C3 N2 C2 120.15(10) . . ?
C3 N2 C2' 118.0(4) . . ?
C3 N2 CO1 126.59(9) . . ?
C2 N2 CO1 113.23(8) . . ?
C2' N2 CO1 111.1(4) . . ?
N2 C3 C4 124.25(10) . . ?
N2 C3 H3 117.9 . . ?
C4 C3 H3 117.9 . . ?
C5 C4 C9 119.90(11) . . ?
C5 C4 C3 117.27(10) . . ?
C9 C4 C3 122.68(10) . . ?
C6 C5 C4 119.96(11) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 121.32(11) . . ?
C5 C6 N3 119.65(11) . . ?
C7 C6 N3 118.85(11) . . ?
C8 C7 C6 119.28(12) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C7 C8 C9 121.80(11) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
O1 C9 C8 117.51(10) . . ?
O1 C9 C4 124.76(11) . . ?
C8 C9 C4 117.72(10) . . ?
C9 O1 CO1 126.10(8) . . ?
O2 N3 O3 122.22(11) . . ?
O2 N3 C6 119.09(11) . . ?
O3 N3 C6 118.67(11) . . ?
F1 P1 F1 91.6(2) 2_656 . ?
F1 P1 F3 91.01(12) 2_656 . ?
F1 P1 F3 90.89(13) . . ?
F1 P1 F3 90.89(13) 2_656 2_656 ?
F1 P1 F3 91.01(12) . 2_656 ?
F3 P1 F3 177.28(13) . 2_656 ?
F1 P1 F2 89.94(11) 2_656 2_656 ?
F1 P1 F2 178.46(12) . 2_656 ?
F3 P1 F2 88.82(7) . 2_656 ?
F3 P1 F2 89.23(8) 2_656 2_656 ?
F1 P1 F2 178.46(12) 2_656 . ?
F1 P1 F2 89.94(11) . . ?
F3 P1 F2 89.23(8) . . ?
F3 P1 F2 88.82(7) 2_656 . ?
F2 P1 F2 88.55(10) 2_656 . ?
F1' B1' F3' 107.9(8) . . ?
F1' B1' F4' 109.0(9) . . ?
F3' B1' F4' 109.4(8) . . ?
F1' B1' F2' 109.1(9) . . ?
F3' B1' F2' 108.6(8) . . ?
F4' B1' F2' 112.7(8) . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 118.12(15) . . ?
C12 C11 C10 121.24(14) . . ?
C16 C11 C10 120.63(15) . . ?
C13 C12 C11 121.18(15) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 120.24(17) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 119.24(16) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 120.50(17) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 120.71(17) . . ?
C15 C16 H16 119.6 . . ?
C11 C16 H16 119.6 . . ?

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
CO1 N1 C1 C2 41.19(12) . . . . ?
N1 C1 C2 N2 -49.21(15) . . . . ?
CO1 N1' C1' C2' -41.7(9) . . . . ?
N1' C1' C2' N2 48.5(10) . . . . ?
C1 C2 N2 C3 -142.12(12) . . . . ?
C1 C2 N2 CO1 35.91(14) . . . . ?
C1' C2' N2 C3 163.6(6) . . . . ?
C1' C2' N2 CO1 -38.2(10) . . . . ?
C2 N2 C3 C4 -174.74(13) . . . . ?
C2' N2 C3 C4 162.0(6) . . . . ?
CO1 N2 C3 C4 7.52(18) . . . . ?
N2 C3 C4 C5 178.33(11) . . . . ?
N2 C3 C4 C9 2.76(19) . . . . ?
C9 C4 C5 C6 0.61(17) . . . . ?
C3 C4 C5 C6 -175.09(11) . . . . ?
C4 C5 C6 C7 0.90(18) . . . . ?
C4 C5 C6 N3 175.99(11) . . . . ?
C5 C6 C7 C8 -1.16(19) . . . . ?
N3 C6 C7 C8 -176.29(12) . . . . ?
C6 C7 C8 C9 -0.1(2) . . . . ?
C7 C8 C9 O1 -179.81(12) . . . . ?
C7 C8 C9 C4 1.57(19) . . . . ?
C5 C4 C9 O1 179.69(11) . . . . ?
C3 C4 C9 O1 -4.85(19) . . . . ?
C5 C4 C9 C8 -1.81(17) . . . . ?
C3 C4 C9 C8 173.65(11) . . . . ?
C8 C9 O1 CO1 177.89(9) . . . . ?
C4 C9 O1 CO1 -3.60(18) . . . . ?
O1 CO1 O1 C9 -77.72(10) 2_656 . . . ?
N2 CO1 O1 C9 9.85(11) . . . . ?
N2 CO1 O1 C9 -172.03(11) 2_656 . . . ?
N1 CO1 O1 C9 102.60(10) 2_656 . . . ?
N1' CO1 O1 C9 102.60(10) 2_656 . . . ?
C5 C6 N3 O2 -178.92(11) . . . . ?
C7 C6 N3 O2 -3.71(17) . . . . ?
C5 C6 N3 O3 -0.27(17) . . . . ?
C7 C6 N3 O3 174.94(11) . . . . ?
C16 C11 C12 C13 -0.5(2) . . . . ?
C10 C11 C12 C13 179.88(15) . . . . ?
C11 C12 C13 C14 1.0(2) . . . . ?
C12 C13 C14 C15 -0.8(3) . . . . ?
C13 C14 C15 C16 0.1(3) . . . . ?
C14 C15 C16 C11 0.5(3) . . . . ?
C12 C11 C16 C15 -0.3(2) . . . . ?
C10 C11 C16 C15 179.37(16) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1E F2 0.92 2.15 2.9040(16) 139.1 .
N1 H1E F2 0.92 2.60 3.4727(17) 158.1 2_656
N1 H1F N3 0.92 2.67 3.5701(14) 167.6 8_466
N1 H1F O2 0.92 2.59 3.3618(14) 141.7 8_466
N1 H1F O3 0.92 2.15 3.0518(14) 164.7 8_466
C2 H2A F2 0.99 2.50 3.189(2) 126.2 .
N1' H1G F2' 0.92 2.31 2.997(16) 131.7 .
N1' H1G F4' 0.92 2.29 3.059(11) 141.5 2_656
N1' H1H O3 0.92 2.22 3.0518(14) 149.9 8_466
C1' H1C F4' 0.99 2.40 3.31(2) 152.3 .
C1' H1D O2 0.99 2.62 3.133(10) 112.1 3_445
C3 H3 F1 0.95 2.32 3.203(3) 154.8 5_666
C3 H3 F1' 0.95 2.40 3.300(15) 158.6 5_666
C3 H3 F3' 0.95 2.36 3.243(10) 154.8 6_565
C5 H5 F1 0.95 2.56 3.370(2) 143.8 5_666
C7 H7 F2 0.95 2.45 3.3168(18) 152.2 3
C7 H7 F3' 0.95 2.52 3.044(11) 114.7 4_656
C8 H8 F3 0.95 2.61 3.2609(18) 125.9 3
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.071


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/toluene'
_chemical_properties_physical    ', Moisture-sensitive'
