# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1406792'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H16 B Mo N6 O2 P3'
_chemical_formula_sum            'C17 H16 B Mo N6 O2 P3'
_chemical_formula_weight         536.02

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'
O O 0.0106 0.0060 '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'
B B 0.0013 0.0007 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7379(7)
_cell_length_b                   9.9570(3)
_cell_length_c                   13.2391(9)
_cell_angle_alpha                104.609(4)
_cell_angle_beta                 96.252(7)
_cell_angle_gamma                107.110(3)
_cell_volume                     1044.19(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    22540
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536
_exptl_absorpt_coefficient_mu    0.886
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.042
0 0 -1 0.045
0 1 0 0.166
0 -1 0 0.110
-1 0 0 0.096
1 0 0 0.054


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22413
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4771
_reflns_number_gt                4429
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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     
'calc w=1/[σ²(Fo²)+(0.0222P)²+0.9353P] 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         4771
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0221
_refine_ls_wR_factor_ref         0.0565
_refine_ls_wR_factor_gt          0.0538
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.835636(17) -0.177224(15) 0.159370(11) 0.01347(5) Uani 1 1 d . . .
P3 P 0.75171(6) 0.03268(6) 0.50525(4) 0.02337(11) Uani 1 1 d . . .
P2 P 0.69395(6) 0.22741(5) 0.09058(4) 0.02170(11) Uani 1 1 d . . .
P1 P 1.42600(6) 0.03490(6) 0.24805(4) 0.02239(11) Uani 1 1 d . . .
N6 N 0.92988(18) 0.10044(15) 0.36908(11) 0.0148(3) Uani 1 1 d . . .
N1 N 1.10564(18) -0.05057(16) 0.21273(12) 0.0170(3) Uani 1 1 d . . .
O1 O 0.46004(17) -0.32368(16) 0.12596(12) 0.0286(3) Uani 1 1 d . . .
N5 N 0.84306(18) -0.04595(15) 0.32378(11) 0.0151(3) Uani 1 1 d . . .
C16 C 0.5989(2) -0.26633(19) 0.13577(14) 0.0191(4) Uani 1 1 d . . .
N2 N 1.15904(18) 0.09632(16) 0.26496(12) 0.0153(3) Uani 1 1 d . . .
N4 N 0.91323(17) 0.17140(15) 0.20526(11) 0.0147(3) Uani 1 1 d . . .
C17 C 0.8174(3) -0.3340(2) 0.22457(16) 0.0236(4) Uani 1 1 d . . .
C9 C 0.8914(2) 0.1572(2) 0.46199(14) 0.0200(4) Uani 1 1 d . . .
H9 H 0.9364 0.2566 0.5003 0.024 Uiso 1 1 d R . .
C12 C 1.3214(2) 0.5447(2) 0.52374(16) 0.0243(4) Uani 1 1 d . . .
H12 H 1.3590 0.5755 0.5970 0.029 Uiso 1 1 d R . .
C13 C 1.3686(2) 0.6412(2) 0.46525(17) 0.0240(4) Uani 1 1 d . . .
H13 H 1.4379 0.7373 0.4988 0.029 Uiso 1 1 d R . .
C7 C 0.8535(2) 0.27853(19) 0.19623(15) 0.0184(3) Uani 1 1 d . . .
H7 H 0.8953 0.3732 0.2436 0.022 Uiso 1 1 d R . .
N3 N 0.82903(17) 0.03849(15) 0.13092(11) 0.0149(3) Uani 1 1 d . . .
C4 C 1.2321(2) -0.0966(2) 0.19932(15) 0.0209(4) Uani 1 1 d . . .
H4 H 1.2178 -0.1947 0.1654 0.025 Uiso 1 1 d R . .
C11 C 1.2168(2) 0.4014(2) 0.47343(15) 0.0204(4) Uani 1 1 d . . .
H11 H 1.1899 0.3367 0.5136 0.024 Uiso 1 1 d R . .
C5 C 1.3230(2) 0.1560(2) 0.28754(15) 0.0198(4) Uani 1 1 d . . .
H5 H 1.3765 0.2558 0.3219 0.024 Uiso 1 1 d R . .
C2 C 0.8985(3) -0.2731(2) 0.00526(15) 0.0251(4) Uani 1 1 d . . .
H2 H 0.9905 -0.2123 -0.0100 0.030 Uiso 1 1 d R . .
O2 O 0.7973(2) -0.42462(17) 0.26657(13) 0.0397(4) Uani 1 1 d . . .
C6 C 0.7132(2) 0.0535(2) 0.06530(15) 0.0188(3) Uani 1 1 d . . .
H6 H 0.6453 -0.0253 0.0085 0.023 Uiso 1 1 d R . .
C8 C 0.7472(2) -0.0954(2) 0.38729(14) 0.0182(3) Uani 1 1 d . . .
H8 H 0.6813 -0.1935 0.3695 0.022 Uiso 1 1 d R . .
B1 B 1.0404(2) 0.1827(2) 0.30229(15) 0.0146(4) Uani 1 1 d . . .
C1 C 0.9080(3) -0.3728(2) 0.06223(16) 0.0265(4) Uani 1 1 d . . .
H1A H 0.8137 -0.4321 0.0763 0.032 Uiso 1 1 d R . .
H1B H 1.0090 -0.3793 0.0860 0.032 Uiso 1 1 d R . .
C14 C 1.3122(2) 0.5934(2) 0.35646(17) 0.0246(4) Uani 1 1 d . . .
H14 H 1.3452 0.6571 0.3162 0.030 Uiso 1 1 d R . .
C10 C 1.1517(2) 0.35118(19) 0.36447(14) 0.0171(3) Uani 1 1 d . . .
C3 C 0.7420(3) -0.2714(2) -0.02720(15) 0.0272(4) Uani 1 1 d . . .
H3A H 0.6524 -0.3335 -0.0107 0.033 Uiso 1 1 d R . .
H3B H 0.7273 -0.2079 -0.0653 0.033 Uiso 1 1 d R . .
C15 C 1.2057(2) 0.4508(2) 0.30676(15) 0.0209(4) Uani 1 1 d . . .
H15 H 1.1697 0.4203 0.2333 0.025 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C17 1.942(2) . ?
Mo1 C16 1.9498(19) . ?
Mo1 N5 2.2214(14) . ?
Mo1 C2 2.2239(18) . ?
Mo1 N1 2.2567(15) . ?
Mo1 N3 2.2880(14) . ?
Mo1 C1 2.3418(18) . ?
Mo1 C3 2.3643(19) . ?
P3 C9 1.7254(19) . ?
P3 C8 1.7377(18) . ?
P2 C7 1.7198(19) . ?
P2 C6 1.7412(19) . ?
P1 C5 1.7213(19) . ?
P1 C4 1.741(2) . ?
N6 C9 1.340(2) . ?
N6 N5 1.3671(19) . ?
N6 B1 1.572(2) . ?
N1 C4 1.328(2) . ?
N1 N2 1.361(2) . ?
O1 C16 1.156(2) . ?
N5 C8 1.331(2) . ?
N2 C5 1.345(2) . ?
N2 B1 1.575(2) . ?
N4 C7 1.343(2) . ?
N4 N3 1.3688(19) . ?
N4 B1 1.562(2) . ?
C17 O2 1.156(2) . ?
C9 H9 0.9300 . ?
C12 C13 1.380(3) . ?
C12 C11 1.392(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.380(3) . ?
C13 H13 0.9300 . ?
C7 H7 0.9300 . ?
N3 C6 1.328(2) . ?
C4 H4 0.9301 . ?
C11 C10 1.394(3) . ?
C11 H11 0.9300 . ?
C5 H5 0.9300 . ?
C2 C3 1.395(3) . ?
C2 C1 1.405(3) . ?
C2 H2 0.9300 . ?
C6 H6 0.9299 . ?
C8 H8 0.9300 . ?
B1 C10 1.615(2) . ?
C1 H1A 0.9300 . ?
C1 H1B 0.9300 . ?
C14 C15 1.390(3) . ?
C14 H14 0.9301 . ?
C10 C15 1.406(3) . ?
C3 H3A 0.9300 . ?
C3 H3B 0.9301 . ?
C15 H15 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C17 Mo1 C16 79.15(8) . . ?
C17 Mo1 N5 83.03(7) . . ?
C16 Mo1 N5 91.05(6) . . ?
C17 Mo1 C2 101.12(8) . . ?
C16 Mo1 C2 104.17(8) . . ?
N5 Mo1 C2 164.70(7) . . ?
C17 Mo1 N1 100.50(7) . . ?
C16 Mo1 N1 170.44(6) . . ?
N5 Mo1 N1 79.44(5) . . ?
C2 Mo1 N1 85.31(6) . . ?
C17 Mo1 N3 161.43(7) . . ?
C16 Mo1 N3 94.86(6) . . ?
N5 Mo1 N3 79.50(5) . . ?
C2 Mo1 N3 97.38(7) . . ?
N1 Mo1 N3 82.49(5) . . ?
C17 Mo1 C1 65.80(8) . . ?
C16 Mo1 C1 101.46(7) . . ?
N5 Mo1 C1 143.05(7) . . ?
C2 Mo1 C1 35.72(8) . . ?
N1 Mo1 C1 86.94(6) . . ?
N3 Mo1 C1 132.77(7) . . ?
C17 Mo1 C3 111.63(8) . . ?
C16 Mo1 C3 73.61(8) . . ?
N5 Mo1 C3 155.57(7) . . ?
C2 Mo1 C3 35.22(8) . . ?
N1 Mo1 C3 114.98(7) . . ?
N3 Mo1 C3 82.93(6) . . ?
C1 Mo1 C3 60.48(7) . . ?
C9 P3 C8 85.29(9) . . ?
C7 P2 C6 85.22(9) . . ?
C5 P1 C4 84.92(9) . . ?
C9 N6 N5 112.72(14) . . ?
C9 N6 B1 128.74(15) . . ?
N5 N6 B1 118.03(13) . . ?
C4 N1 N2 110.04(15) . . ?
C4 N1 Mo1 129.61(12) . . ?
N2 N1 Mo1 120.33(11) . . ?
C8 N5 N6 110.24(14) . . ?
C8 N5 Mo1 123.91(12) . . ?
N6 N5 Mo1 125.38(11) . . ?
O1 C16 Mo1 175.94(16) . . ?
C5 N2 N1 112.80(14) . . ?
C5 N2 B1 124.14(15) . . ?
N1 N2 B1 122.90(14) . . ?
C7 N4 N3 113.17(14) . . ?
C7 N4 B1 124.90(14) . . ?
N3 N4 B1 120.79(13) . . ?
O2 C17 Mo1 174.93(18) . . ?
N6 C9 P3 115.11(13) . . ?
N6 C9 H9 122.5 . . ?
P3 C9 H9 122.4 . . ?
C13 C12 C11 120.19(18) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 119.23(17) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.4 . . ?
N4 C7 P2 114.96(13) . . ?
N4 C7 H7 122.5 . . ?
P2 C7 H7 122.5 . . ?
C6 N3 N4 109.59(14) . . ?
C6 N3 Mo1 125.99(11) . . ?
N4 N3 Mo1 121.06(11) . . ?
N1 C4 P1 116.96(14) . . ?
N1 C4 H4 121.6 . . ?
P1 C4 H4 121.5 . . ?
C12 C11 C10 122.16(18) . . ?
C12 C11 H11 119.0 . . ?
C10 C11 H11 118.9 . . ?
N2 C5 P1 115.26(14) . . ?
N2 C5 H5 122.2 . . ?
P1 C5 H5 122.5 . . ?
C3 C2 C1 115.70(19) . . ?
C3 C2 Mo1 77.89(11) . . ?
C1 C2 Mo1 76.72(11) . . ?
C3 C2 H2 122.1 . . ?
C1 C2 H2 122.2 . . ?
Mo1 C2 H2 114.5 . . ?
N3 C6 P2 116.97(13) . . ?
N3 C6 H6 121.6 . . ?
P2 C6 H6 121.4 . . ?
N5 C8 P3 116.56(13) . . ?
N5 C8 H8 121.7 . . ?
P3 C8 H8 121.7 . . ?
N4 B1 N6 102.67(13) . . ?
N4 B1 N2 110.84(14) . . ?
N6 B1 N2 108.64(13) . . ?
N4 B1 C10 111.94(14) . . ?
N6 B1 C10 115.30(14) . . ?
N2 B1 C10 107.40(14) . . ?
C2 C1 Mo1 67.56(10) . . ?
C2 C1 H1A 120.2 . . ?
Mo1 C1 H1A 84.7 . . ?
C2 C1 H1B 119.8 . . ?
Mo1 C1 H1B 118.3 . . ?
H1A C1 H1B 120.0 . . ?
C13 C14 C15 120.38(18) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C11 C10 C15 116.17(16) . . ?
C11 C10 B1 123.34(16) . . ?
C15 C10 B1 119.97(16) . . ?
C2 C3 Mo1 66.88(11) . . ?
C2 C3 H3A 120.0 . . ?
Mo1 C3 H3A 84.5 . . ?
C2 C3 H3B 120.0 . . ?
Mo1 C3 H3B 119.2 . . ?
H3A C3 H3B 120.0 . . ?
C14 C15 C10 121.77(17) . . ?
C14 C15 H15 119.1 . . ?
C10 C15 H15 119.1 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.069
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1406793'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 B2 Fe N12 P6, 2(C7 H8)'
_chemical_formula_sum            'C38 H38 B2 Fe N12 P6'
_chemical_formula_weight         926.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9810(6)
_cell_length_b                   13.5289(12)
_cell_length_c                   15.9001(10)
_cell_angle_alpha                91.940(5)
_cell_angle_beta                 99.962(4)
_cell_angle_gamma                111.752(5)
_cell_volume                     2148.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    36636
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    0.620
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.113
-1 0 0 0.097
0 -1 0 0.112
0 1 0 0.118
0 0 1 0.235
0 0 -1 0.215
1 1 0 0.103


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36582
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         27.47
_reflns_number_total             9655
_reflns_number_gt                7845
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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     
'calc w=1/[σ²(Fo²)+(0.0292P)²+2.4198P] 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         9655
_refine_ls_number_parameters     535
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.0970
_refine_ls_wR_factor_gt          0.0854
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.0000 0.0000 0.01633(10) Uani 1 2 d S . .
Fe2 Fe 0.0000 0.5000 0.5000 0.01397(10) Uani 1 2 d S . .
P5 P 0.03403(7) 0.38016(5) 0.23831(4) 0.02541(14) Uani 1 1 d . . .
P6 P 0.40450(6) 0.56444(5) 0.66876(4) 0.02600(14) Uani 1 1 d . . .
P4 P -0.24858(6) 0.16586(5) 0.55398(4) 0.02281(13) Uani 1 1 d . . .
P1 P -0.04023(6) 0.00287(5) 0.27892(4) 0.02598(14) Uani 1 1 d . . .
P3 P 0.27651(7) -0.17569(6) -0.01483(5) 0.03448(17) Uani 1 1 d . . .
P2 P 0.26922(7) 0.35101(5) 0.04843(4) 0.03223(16) Uani 1 1 d . . .
C7 C 0.3998(2) 0.09436(18) 0.20533(14) 0.0210(5) Uani 1 1 d . . .
N7 N -0.07821(18) 0.35148(14) 0.52819(11) 0.0163(4) Uani 1 1 d . . .
N11 N 0.17254(18) 0.51024(14) 0.56518(11) 0.0165(4) Uani 1 1 d . . .
N1 N 0.01180(18) -0.00635(15) 0.12521(12) 0.0190(4) Uani 1 1 d . . .
N9 N 0.04344(18) 0.44548(14) 0.39716(11) 0.0161(4) Uani 1 1 d . . .
N8 N -0.01916(18) 0.27981(14) 0.51867(12) 0.0161(4) Uani 1 1 d . . .
N3 N 0.14557(18) 0.14293(15) 0.02433(12) 0.0196(4) Uani 1 1 d . . .
N10 N 0.08803(18) 0.36323(14) 0.40109(12) 0.0173(4) Uani 1 1 d . . .
N5 N 0.13378(19) -0.06275(15) 0.00609(12) 0.0209(4) Uani 1 1 d . . .
N6 N 0.24326(18) -0.02486(15) 0.07134(12) 0.0196(4) Uani 1 1 d . . .
N2 N 0.13262(18) 0.03114(14) 0.18114(11) 0.0180(4) Uani 1 1 d . . .
N12 N 0.21186(18) 0.42677(14) 0.55580(12) 0.0166(4) Uani 1 1 d . . .
N4 N 0.25053(19) 0.16413(15) 0.09198(12) 0.0199(4) Uani 1 1 d . . .
C1 C -0.0869(2) -0.02679(19) 0.16780(15) 0.0234(5) Uani 1 1 d . . .
H1 H -0.1762 -0.0552 0.1398 0.028 Uiso 1 1 d R . .
C13 C -0.1972(2) 0.30323(17) 0.54801(14) 0.0200(4) Uani 1 1 d . . .
H13 H -0.2501 0.3406 0.5581 0.024 Uiso 1 1 d R . .
C3 C 0.1456(2) 0.23291(18) -0.00630(15) 0.0240(5) Uani 1 1 d . . .
H3 H 0.0835 0.2330 -0.0542 0.029 Uiso 1 1 d R . .
C8 C 0.4123(2) 0.04095(18) 0.27811(14) 0.0222(5) Uani 1 1 d . . .
H8 H 0.3352 -0.0064 0.2933 0.027 Uiso 1 1 d R . .
C14 C -0.0978(2) 0.17903(17) 0.52767(14) 0.0199(4) Uani 1 1 d . . .
H14 H -0.0727 0.1212 0.5205 0.024 Uiso 1 1 d R . .
C18 C 0.3306(2) 0.44307(18) 0.60603(15) 0.0226(5) Uani 1 1 d . . .
H18 H 0.3700 0.3928 0.6068 0.027 Uiso 1 1 d R . .
C24 C 0.3027(2) 0.26946(18) 0.44382(15) 0.0215(5) Uani 1 1 d . . .
H24 H 0.3166 0.3250 0.4091 0.026 Uiso 1 1 d R . .
C5 C 0.1381(2) -0.1411(2) -0.04415(15) 0.0256(5) Uani 1 1 d . . .
H5 H 0.0717 -0.1754 -0.0923 0.031 Uiso 1 1 d R . .
C22 C 0.3651(2) 0.12823(19) 0.49877(16) 0.0253(5) Uani 1 1 d . . .
H22 H 0.4171 0.0873 0.4997 0.030 Uiso 1 1 d R . .
C17 C 0.2631(2) 0.58775(18) 0.62184(14) 0.0207(5) Uani 1 1 d . . .
H17 H 0.2519 0.6507 0.6359 0.025 Uiso 1 1 d R . .
C15 C 0.0143(2) 0.46413(17) 0.31606(14) 0.0200(4) Uani 1 1 d . . .
H15 H -0.0147 0.5189 0.3017 0.024 Uiso 1 1 d R . .
C20 C 0.1887(2) 0.16639(18) 0.54518(15) 0.0221(5) Uani 1 1 d . . .
H20 H 0.1255 0.1519 0.5799 0.026 Uiso 1 1 d R . .
C12 C 0.5200(2) 0.1607(2) 0.18333(15) 0.0261(5) Uani 1 1 d . . .
H12 H 0.5162 0.1958 0.1343 0.031 Uiso 1 1 d R . .
C11 C 0.6440(2) 0.1753(2) 0.23235(16) 0.0294(5) Uani 1 1 d . . .
H11 H 0.7216 0.2195 0.2157 0.035 Uiso 1 1 d R . .
C19 C 0.2002(2) 0.24709(17) 0.49090(14) 0.0184(4) Uani 1 1 d . . .
C16 C 0.0851(2) 0.31974(18) 0.32357(14) 0.0219(5) Uani 1 1 d . . .
H16 H 0.1086 0.2611 0.3162 0.026 Uiso 1 1 d R . .
C21 C 0.2686(2) 0.10670(19) 0.54846(16) 0.0259(5) Uani 1 1 d . . .
H21 H 0.2575 0.0525 0.5844 0.031 Uiso 1 1 d R . .
C4 C 0.3218(2) 0.26945(18) 0.11367(15) 0.0263(5) Uani 1 1 d . . .
H4 H 0.3935 0.2960 0.1601 0.032 Uiso 1 1 d R . .
C2 C 0.1219(2) 0.04271(18) 0.26312(14) 0.0213(5) Uani 1 1 d . . .
H2 H 0.1959 0.0701 0.3080 0.026 Uiso 1 1 d R . .
C10 C 0.6527(3) 0.1241(2) 0.30569(16) 0.0281(5) Uani 1 1 d . . .
H10 H 0.7356 0.1351 0.3395 0.034 Uiso 1 1 d R . .
C23 C 0.3837(2) 0.21080(19) 0.44737(15) 0.0239(5) Uani 1 1 d . . .
H23 H 0.4504 0.2271 0.4152 0.029 Uiso 1 1 d R . .
C9 C 0.5360(3) 0.0565(2) 0.32830(15) 0.0268(5) Uani 1 1 d . . .
H9 H 0.5404 0.0211 0.3772 0.032 Uiso 1 1 d R . .
C6 C 0.3270(2) -0.0760(2) 0.06884(16) 0.0281(5) Uani 1 1 d . . .
H6 H 0.4059 -0.0591 0.1092 0.034 Uiso 1 1 d R . .
B1 B 0.2602(3) 0.0675(2) 0.14001(16) 0.0191(5) Uani 1 1 d . . .
B2 B 0.1205(2) 0.32564(19) 0.49111(16) 0.0166(5) Uani 1 1 d . . .
C32 C 0.8464(3) 0.5545(2) 0.14229(18) 0.0402(7) Uani 1 1 d . . .
C33 C 0.9560(4) 0.5586(3) 0.1121(2) 0.0488(8) Uani 1 1 d . . .
H33 H 0.9486 0.5041 0.0718 0.059 Uiso 1 1 d R . .
C30 C 0.5092(3) 0.7915(3) 0.2448(2) 0.0514(9) Uani 1 1 d . . .
H30 H 0.5083 0.8353 0.2908 0.062 Uiso 1 1 d R . .
C37 C 0.8578(3) 0.6372(3) 0.20159(19) 0.0447(7) Uani 1 1 d . . .
H37 H 0.7835 0.6366 0.2223 0.054 Uiso 1 1 d R . .
C26 C 0.4527(3) 0.6179(3) 0.1747(2) 0.0515(9) Uani 1 1 d . . .
H26 H 0.4147 0.5437 0.1729 0.062 Uiso 1 1 d R . .
C28 C 0.5670(3) 0.7740(3) 0.1086(2) 0.0572(9) Uani 1 1 d . . .
H28 H 0.6041 0.8040 0.0627 0.069 Uiso 1 1 d R . .
C36 C 0.9825(4) 0.7213(3) 0.2297(2) 0.0533(9) Uani 1 1 d . . .
H36 H 0.9918 0.7765 0.2699 0.064 Uiso 1 1 d R . .
C25 C 0.4511(3) 0.6810(3) 0.2445(2) 0.0487(8) Uani 1 1 d . . .
C31 C 0.3851(3) 0.6307(3) 0.3147(2) 0.0629(10) Uani 1 1 d . . .
H31A H 0.2955 0.6289 0.3048 0.075 Uiso 1 1 d R . .
H31B H 0.4341 0.6717 0.3687 0.075 Uiso 1 1 d R . .
H31C H 0.3825 0.5591 0.3159 0.075 Uiso 1 1 d R . .
C29 C 0.5673(3) 0.8377(3) 0.1787(3) 0.0627(10) Uani 1 1 d . . .
H29 H 0.6073 0.9118 0.1811 0.075 Uiso 1 1 d R . .
C38 C 0.7140(4) 0.4610(3) 0.1146(2) 0.0588(10) Uani 1 1 d . . .
H38A H 0.7128 0.4245 0.0614 0.071 Uiso 1 1 d R . .
H38B H 0.6426 0.4867 0.1069 0.071 Uiso 1 1 d R . .
H38C H 0.7025 0.4125 0.1579 0.071 Uiso 1 1 d R . .
C35 C 1.0913(4) 0.7209(3) 0.1971(2) 0.0573(10) Uani 1 1 d . . .
H35 H 1.1745 0.7761 0.2152 0.069 Uiso 1 1 d R . .
C34 C 1.0765(4) 0.6401(3) 0.1390(2) 0.0574(9) Uani 1 1 d . . .
H34 H 1.1499 0.6405 0.1171 0.069 Uiso 1 1 d R . .
C27 C 0.5092(4) 0.6619(3) 0.1091(2) 0.0620(10) Uani 1 1 d . . .
H27 H 0.5094 0.6176 0.0631 0.074 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 1.941(2) . ?
Fe1 N5 1.941(2) 2 ?
Fe1 N3 1.9719(18) 2 ?
Fe1 N3 1.9719(18) . ?
Fe1 N1 1.9794(18) . ?
Fe1 N1 1.9794(18) 2 ?
Fe2 N11 1.9492(18) . ?
Fe2 N11 1.9493(18) 2_566 ?
Fe2 N7 1.9726(18) . ?
Fe2 N7 1.9726(18) 2_566 ?
Fe2 N9 1.9734(18) 2_566 ?
Fe2 N9 1.9734(18) . ?
P5 C16 1.724(2) . ?
P5 C15 1.745(2) . ?
P6 C18 1.724(2) . ?
P6 C17 1.745(2) . ?
P4 C14 1.724(2) . ?
P4 C13 1.742(2) . ?
P1 C2 1.725(2) . ?
P1 C1 1.741(2) . ?
P3 C6 1.722(3) . ?
P3 C5 1.744(3) . ?
P2 C4 1.723(3) . ?
P2 C3 1.744(2) . ?
C7 C8 1.398(3) . ?
C7 C12 1.404(3) . ?
C7 B1 1.604(3) . ?
N7 C13 1.325(3) . ?
N7 N8 1.369(2) . ?
N11 C17 1.324(3) . ?
N11 N12 1.362(2) . ?
N1 C1 1.325(3) . ?
N1 N2 1.368(3) . ?
N9 C15 1.330(3) . ?
N9 N10 1.371(2) . ?
N8 C14 1.345(3) . ?
N8 B2 1.573(3) . ?
N3 C3 1.326(3) . ?
N3 N4 1.369(3) . ?
N10 C16 1.338(3) . ?
N10 B2 1.563(3) . ?
N5 C5 1.326(3) . ?
N5 N6 1.364(3) . ?
N6 C6 1.345(3) . ?
N6 B1 1.567(3) . ?
N2 C2 1.338(3) . ?
N2 B1 1.569(3) . ?
N12 C18 1.342(3) . ?
N12 B2 1.571(3) . ?
N4 C4 1.345(3) . ?
N4 B1 1.563(3) . ?
C1 H1 0.9300 . ?
C13 H13 0.9300 . ?
C3 H3 0.9299 . ?
C8 C9 1.389(3) . ?
C8 H8 0.9300 . ?
C14 H14 0.9301 . ?
C18 H18 0.9300 . ?
C24 C23 1.391(3) . ?
C24 C19 1.405(3) . ?
C24 H24 0.9300 . ?
C5 H5 0.9300 . ?
C22 C21 1.381(4) . ?
C22 C23 1.381(3) . ?
C22 H22 0.9300 . ?
C17 H17 0.9296 . ?
C15 H15 0.9299 . ?
C20 C21 1.392(3) . ?
C20 C19 1.397(3) . ?
C20 H20 0.9300 . ?
C12 C11 1.386(3) . ?
C12 H12 0.9301 . ?
C11 C10 1.383(4) . ?
C11 H11 0.9300 . ?
C19 B2 1.608(3) . ?
C16 H16 0.9301 . ?
C21 H21 0.9300 . ?
C4 H4 0.9299 . ?
C2 H2 0.9299 . ?
C10 C9 1.386(4) . ?
C10 H10 0.9300 . ?
C23 H23 0.9300 . ?
C9 H9 0.9302 . ?
C6 H6 0.9300 . ?
C32 C33 1.355(5) . ?
C32 C37 1.392(4) . ?
C32 C38 1.511(4) . ?
C33 C34 1.357(5) . ?
C33 H33 0.9299 . ?
C30 C29 1.374(6) . ?
C30 C25 1.390(5) . ?
C30 H30 0.9300 . ?
C37 C36 1.403(5) . ?
C37 H37 0.9300 . ?
C26 C27 1.350(5) . ?
C26 C25 1.384(4) . ?
C26 H26 0.9300 . ?
C28 C29 1.384(5) . ?
C28 C27 1.410(5) . ?
C28 H28 0.9300 . ?
C36 C35 1.385(5) . ?
C36 H36 0.9303 . ?
C25 C31 1.482(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C29 H29 0.9300 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9599 . ?
C38 H38C 0.9601 . ?
C35 C34 1.349(5) . ?
C35 H35 0.9300 . ?
C34 H34 0.9300 . ?
C27 H27 0.9299 . ?

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
N5 Fe1 N5 180.0 . 2 ?
N5 Fe1 N3 91.11(8) . 2 ?
N5 Fe1 N3 88.89(8) 2 2 ?
N5 Fe1 N3 88.89(8) . . ?
N5 Fe1 N3 91.11(8) 2 . ?
N3 Fe1 N3 180.0 2 . ?
N5 Fe1 N1 88.61(8) . . ?
N5 Fe1 N1 91.39(8) 2 . ?
N3 Fe1 N1 91.18(7) 2 . ?
N3 Fe1 N1 88.82(7) . . ?
N5 Fe1 N1 91.39(8) . 2 ?
N5 Fe1 N1 88.61(8) 2 2 ?
N3 Fe1 N1 88.82(7) 2 2 ?
N3 Fe1 N1 91.18(7) . 2 ?
N1 Fe1 N1 180.0 . 2 ?
N11 Fe2 N11 179.997(1) . 2_566 ?
N11 Fe2 N7 88.67(7) . . ?
N11 Fe2 N7 91.33(7) 2_566 . ?
N11 Fe2 N7 91.33(7) . 2_566 ?
N11 Fe2 N7 88.67(7) 2_566 2_566 ?
N7 Fe2 N7 180.0 . 2_566 ?
N11 Fe2 N9 91.26(7) . 2_566 ?
N11 Fe2 N9 88.75(7) 2_566 2_566 ?
N7 Fe2 N9 91.18(7) . 2_566 ?
N7 Fe2 N9 88.82(7) 2_566 2_566 ?
N11 Fe2 N9 88.74(7) . . ?
N11 Fe2 N9 91.25(7) 2_566 . ?
N7 Fe2 N9 88.82(7) . . ?
N7 Fe2 N9 91.18(7) 2_566 . ?
N9 Fe2 N9 180.00(5) 2_566 . ?
C16 P5 C15 85.48(11) . . ?
C18 P6 C17 85.57(11) . . ?
C14 P4 C13 85.74(11) . . ?
C2 P1 C1 85.56(11) . . ?
C6 P3 C5 85.69(12) . . ?
C4 P2 C3 85.86(11) . . ?
C8 C7 C12 116.1(2) . . ?
C8 C7 B1 123.0(2) . . ?
C12 C7 B1 120.0(2) . . ?
C13 N7 N8 110.56(17) . . ?
C13 N7 Fe2 127.02(15) . . ?
N8 N7 Fe2 121.96(13) . . ?
C17 N11 N12 110.87(18) . . ?
C17 N11 Fe2 130.06(15) . . ?
N12 N11 Fe2 119.05(13) . . ?
C1 N1 N2 110.30(18) . . ?
C1 N1 Fe1 127.29(16) . . ?
N2 N1 Fe1 121.35(14) . . ?
C15 N9 N10 110.29(17) . . ?
C15 N9 Fe2 128.55(15) . . ?
N10 N9 Fe2 120.08(13) . . ?
C14 N8 N7 112.90(18) . . ?
C14 N8 B2 130.93(18) . . ?
N7 N8 B2 115.88(16) . . ?
C3 N3 N4 110.55(18) . . ?
C3 N3 Fe1 127.58(15) . . ?
N4 N3 Fe1 120.47(14) . . ?
C16 N10 N9 112.94(18) . . ?
C16 N10 B2 128.92(18) . . ?
N9 N10 B2 117.81(17) . . ?
C5 N5 N6 110.82(19) . . ?
C5 N5 Fe1 130.39(16) . . ?
N6 N5 Fe1 118.78(14) . . ?
C6 N6 N5 112.81(19) . . ?
C6 N6 B1 126.77(19) . . ?
N5 N6 B1 120.41(18) . . ?
C2 N2 N1 113.14(18) . . ?
C2 N2 B1 129.95(19) . . ?
N1 N2 B1 116.35(17) . . ?
C18 N12 N11 112.88(18) . . ?
C18 N12 B2 127.13(18) . . ?
N11 N12 B2 119.98(17) . . ?
C4 N4 N3 113.05(19) . . ?
C4 N4 B1 129.02(19) . . ?
N3 N4 B1 117.38(17) . . ?
N1 C1 P1 116.29(17) . . ?
N1 C1 H1 121.8 . . ?
P1 C1 H1 121.9 . . ?
N7 C13 P4 116.18(16) . . ?
N7 C13 H13 121.8 . . ?
P4 C13 H13 122.0 . . ?
N3 C3 P2 115.98(17) . . ?
N3 C3 H3 122.0 . . ?
P2 C3 H3 122.1 . . ?
C9 C8 C7 122.1(2) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 118.8 . . ?
N8 C14 P4 114.54(16) . . ?
N8 C14 H14 122.7 . . ?
P4 C14 H14 122.8 . . ?
N12 C18 P6 114.72(17) . . ?
N12 C18 H18 122.6 . . ?
P6 C18 H18 122.7 . . ?
C23 C24 C19 122.0(2) . . ?
C23 C24 H24 119.0 . . ?
C19 C24 H24 119.0 . . ?
N5 C5 P3 115.94(18) . . ?
N5 C5 H5 122.1 . . ?
P3 C5 H5 122.0 . . ?
C21 C22 C23 119.6(2) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.0 . . ?
N11 C17 P6 115.96(17) . . ?
N11 C17 H17 122.0 . . ?
P6 C17 H17 122.0 . . ?
N9 C15 P5 116.19(16) . . ?
N9 C15 H15 121.9 . . ?
P5 C15 H15 122.0 . . ?
C21 C20 C19 121.9(2) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.0 . . ?
C11 C12 C7 122.1(2) . . ?
C11 C12 H12 119.1 . . ?
C7 C12 H12 118.8 . . ?
C10 C11 C12 120.3(2) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.8 . . ?
C20 C19 C24 116.3(2) . . ?
C20 C19 B2 123.9(2) . . ?
C24 C19 B2 119.08(19) . . ?
N10 C16 P5 115.02(16) . . ?
N10 C16 H16 122.5 . . ?
P5 C16 H16 122.5 . . ?
C22 C21 C20 120.1(2) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 120.0 . . ?
N4 C4 P2 114.45(17) . . ?
N4 C4 H4 122.7 . . ?
P2 C4 H4 122.8 . . ?
N2 C2 P1 114.62(17) . . ?
N2 C2 H2 122.7 . . ?
P1 C2 H2 122.7 . . ?
C11 C10 C9 119.1(2) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.4 . . ?
C22 C23 C24 119.9(2) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.1 . . ?
C10 C9 C8 120.3(2) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 119.7 . . ?
N6 C6 P3 114.73(18) . . ?
N6 C6 H6 122.7 . . ?
P3 C6 H6 122.6 . . ?
N4 B1 N6 108.27(18) . . ?
N4 B1 N2 102.96(18) . . ?
N6 B1 N2 107.89(17) . . ?
N4 B1 C7 114.13(18) . . ?
N6 B1 C7 107.53(19) . . ?
N2 B1 C7 115.72(18) . . ?
N10 B2 N12 108.58(17) . . ?
N10 B2 N8 103.61(17) . . ?
N12 B2 N8 107.17(17) . . ?
N10 B2 C19 113.17(18) . . ?
N12 B2 C19 107.20(17) . . ?
N8 B2 C19 116.76(17) . . ?
C33 C32 C37 118.9(3) . . ?
C33 C32 C38 121.3(3) . . ?
C37 C32 C38 119.8(3) . . ?
C32 C33 C34 121.7(3) . . ?
C32 C33 H33 119.3 . . ?
C34 C33 H33 119.0 . . ?
C29 C30 C25 121.8(3) . . ?
C29 C30 H30 119.0 . . ?
C25 C30 H30 119.2 . . ?
C32 C37 C36 119.4(3) . . ?
C32 C37 H37 120.2 . . ?
C36 C37 H37 120.3 . . ?
C27 C26 C25 121.2(3) . . ?
C27 C26 H26 119.1 . . ?
C25 C26 H26 119.7 . . ?
C29 C28 C27 118.0(4) . . ?
C29 C28 H28 121.1 . . ?
C27 C28 H28 120.9 . . ?
C35 C36 C37 119.2(3) . . ?
C35 C36 H36 120.6 . . ?
C37 C36 H36 120.3 . . ?
C26 C25 C30 117.9(4) . . ?
C26 C25 C31 120.2(3) . . ?
C30 C25 C31 122.0(3) . . ?
C25 C31 H31A 109.2 . . ?
C25 C31 H31B 109.6 . . ?
H31A C31 H31B 109.5 . . ?
C25 C31 H31C 109.7 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C29 C28 120.0(4) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C32 C38 H38A 109.6 . . ?
C32 C38 H38B 109.4 . . ?
H38A C38 H38B 109.5 . . ?
C32 C38 H38C 109.3 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C34 C35 C36 119.9(3) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.0 . . ?
C35 C34 C33 120.9(4) . . ?
C35 C34 H34 119.4 . . ?
C33 C34 H34 119.6 . . ?
C26 C27 C28 121.2(3) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 H27 119.4 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.071
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1406794'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 B2 Cd N12 P6, 1.5(C7 H8)'
_chemical_formula_sum            'C34.50 H34 B2 Cd N12 P6'
_chemical_formula_weight         936.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   14.0480(7)
_cell_length_b                   14.0970(3)
_cell_length_c                   14.1551(12)
_cell_angle_alpha                66.977(3)
_cell_angle_beta                 61.712(4)
_cell_angle_gamma                61.256(3)
_cell_volume                     2115.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    48277
_cell_measurement_theta_min      1
_cell_measurement_theta_max      30.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_F_000             946
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.785
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.158
-1 -1 0 0.180
0 -1 -1 0.043
0 1 1 0.091
1 0 1 0.123
-1 0 -1 0.094


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            48084
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.899
_diffrn_reflns_theta_max         30.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             12693
_reflns_number_gt                10573
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0292P)²+1.9455P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12693
_refine_ls_number_parameters     472
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0821
_refine_ls_wR_factor_gt          0.0714
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.108
_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
Cd1 Cd 1.0000 0.0000 0.0000 0.02178(5) Uani 1 2 d S . P . .
Cd2 Cd 0.5000 0.5000 0.5000 0.02122(5) Uani 1 2 d S . P . .
P6 P 0.19878(5) 0.81921(5) 0.64435(5) 0.03188(12) Uani 1 1 d . . . . .
P5 P 0.33325(5) 0.44062(5) 0.32167(4) 0.03261(12) Uani 1 1 d . . . . .
P3 P 1.02541(5) 0.29671(4) -0.32484(4) 0.02834(11) Uani 1 1 d . . . . .
P1 P 0.58860(5) 0.13740(5) 0.20164(6) 0.04022(14) Uani 1 1 d . . . . .
P4 P 0.35487(5) 0.21481(4) 0.78161(5) 0.03372(12) Uani 1 1 d . . . . .
P2 P 1.12595(5) 0.19353(5) 0.08372(5) 0.03474(12) Uani 1 1 d . . . . .
N8 N 0.28716(13) 0.41659(13) 0.67312(12) 0.0204(3) Uani 1 1 d . . . . .
N4 N 0.94594(13) 0.22067(12) 0.05325(12) 0.0191(3) Uani 1 1 d . . . . .
N10 N 0.27211(13) 0.51569(13) 0.48999(12) 0.0205(3) Uani 1 1 d . . . . .
N9 N 0.37043(14) 0.53673(15) 0.41897(13) 0.0259(3) Uani 1 1 d . . . . .
N3 N 0.98799(15) 0.11056(12) 0.09637(13) 0.0242(3) Uani 1 1 d . . . . .
N7 N 0.40472(14) 0.38498(13) 0.63834(13) 0.0232(3) Uani 1 1 d . . . . .
C7 C 0.76287(15) 0.39459(14) 0.02087(14) 0.0186(3) Uani 1 1 d . . . . .
N2 N 0.76568(13) 0.19765(12) 0.07334(12) 0.0199(3) Uani 1 1 d . . . . .
N6 N 0.91131(13) 0.25857(12) -0.11569(12) 0.0191(3) Uani 1 1 d . . . . .
N12 N 0.23682(13) 0.63034(13) 0.61702(12) 0.0205(3) Uani 1 1 d . . . . .
N1 N 0.80312(15) 0.09190(13) 0.06422(15) 0.0273(3) Uani 1 1 d . . . . .
B2 B 0.21722(17) 0.53072(17) 0.61206(16) 0.0196(3) Uani 1 1 d . . . . .
C20 C 0.02054(17) 0.55157(16) 0.77718(15) 0.0250(4) Uani 1 1 d . . . . .
H20 H 0.0625 0.5166 0.8240 0.030 Uiso 1 1 d R U . . .
C6 C 0.92273(16) 0.34019(15) -0.20534(14) 0.0220(3) Uani 1 1 d . . . . .
H6 H 0.8784 0.4144 -0.2031 0.026 Uiso 1 1 d R U . . .
N5 N 0.98584(15) 0.15648(13) -0.13797(13) 0.0271(3) Uani 1 1 d . . . . .
C12 C 0.75584(16) 0.44254(15) 0.09487(14) 0.0214(3) Uani 1 1 d . . . . .
H12 H 0.8032 0.4018 0.1368 0.026 Uiso 1 1 d R U . . .
C2 C 0.65509(17) 0.23266(16) 0.14249(16) 0.0269(4) Uani 1 1 d . . . . .
H2 H 0.6175 0.3033 0.1570 0.032 Uiso 1 1 d R U . . .
C14 C 0.24877(18) 0.33566(16) 0.74630(16) 0.0268(4) Uani 1 1 d . . . . .
H14 H 0.1710 0.3439 0.7757 0.032 Uiso 1 1 d R U . . .
C8 C 0.68493(16) 0.45763(15) -0.03537(15) 0.0232(3) Uani 1 1 d . . . . .
H8 H 0.6835 0.4263 -0.0814 0.028 Uiso 1 1 d R U . . .
B1 B 0.84497(17) 0.26901(15) 0.00876(15) 0.0178(3) Uani 1 1 d . . . . .
C19 C 0.08008(16) 0.55976(16) 0.66386(15) 0.0223(3) Uani 1 1 d . . . . .
C18 C 0.15247(17) 0.72614(16) 0.64391(15) 0.0253(4) Uani 1 1 d . . . . .
H18 H 0.0746 0.7414 0.6611 0.030 Uiso 1 1 d R U . . .
C13 C 0.45142(18) 0.28220(16) 0.68835(16) 0.0275(4) Uani 1 1 d . . . . .
H13 H 0.5308 0.2481 0.6748 0.033 Uiso 1 1 d R U . . .
C4 C 1.00952(16) 0.27469(16) 0.03984(16) 0.0255(4) Uani 1 1 d . . . . .
H4 H 0.9922 0.3500 0.0094 0.031 Uiso 1 1 d R U . . .
C3 C 1.08085(18) 0.08506(17) 0.11739(18) 0.0305(4) Uani 1 1 d . . . . .
H3 H 1.1198 0.0132 0.1483 0.037 Uiso 1 1 d R U . . .
N11 N 0.34410(14) 0.62691(14) 0.59441(14) 0.0263(3) Uani 1 1 d . . . . .
C11 C 0.68051(17) 0.54996(16) 0.10660(16) 0.0265(4) Uani 1 1 d . . . . .
H11 H 0.6779 0.5799 0.1562 0.032 Uiso 1 1 d R U . . .
C10 C 0.60770(17) 0.61197(16) 0.04654(17) 0.0292(4) Uani 1 1 d . . . . .
H10 H 0.5594 0.6848 0.0524 0.035 Uiso 1 1 d R U . . .
C5 C 1.04984(19) 0.16323(17) -0.24353(16) 0.0309(4) Uani 1 1 d . . . . .
H5 H 1.1039 0.1006 -0.2722 0.037 Uiso 1 1 d R U . . .
C16 C 0.24276(17) 0.46382(17) 0.45203(15) 0.0264(4) Uani 1 1 d . . . . .
H16 H 0.1783 0.4431 0.4920 0.032 Uiso 1 1 d R U . . .
C15 C 0.41091(18) 0.5032(2) 0.32732(15) 0.0306(4) Uani 1 1 d . . . . .
H15 H 0.4770 0.5127 0.2693 0.037 Uiso 1 1 d R U . . .
C24 C 0.01191(17) 0.61277(18) 0.59841(16) 0.0288(4) Uani 1 1 d . . . . .
H24 H 0.0486 0.6205 0.5227 0.035 Uiso 1 1 d R U . . .
C22 C -0.16468(18) 0.64534(18) 0.75470(19) 0.0328(4) Uani 1 1 d . . . . .
H22 H -0.2453 0.6742 0.7846 0.039 Uiso 1 1 d R U . . .
C17 C 0.33733(19) 0.71934(17) 0.60520(17) 0.0299(4) Uani 1 1 d . . . . .
H17 H 0.4029 0.7304 0.5924 0.036 Uiso 1 1 d R U . . .
C9 C 0.60843(17) 0.56432(16) -0.02296(17) 0.0280(4) Uani 1 1 d . . . . .
H9 H 0.5580 0.6040 -0.0619 0.034 Uiso 1 1 d R U . . .
C21 C -0.10030(18) 0.59387(17) 0.82190(17) 0.0300(4) Uani 1 1 d . . . . .
H21 H -0.1377 0.5868 0.8975 0.036 Uiso 1 1 d R U . . .
C23 C -0.10902(18) 0.65465(19) 0.64299(19) 0.0331(4) Uani 1 1 d . . . . .
H23 H -0.1519 0.6889 0.5971 0.040 Uiso 1 1 d R U . . .
C28 C 0.2394(4) 0.7942(3) 0.2561(4) 0.0796(12) Uani 1 1 d . . . . .
H28 H 0.2096 0.7414 0.2713 0.096 Uiso 1 1 d R U . . .
C1 C 0.7206(2) 0.05040(18) 0.1253(2) 0.0370(5) Uani 1 1 d . . . . .
H1 H 0.7317 -0.0209 0.1275 0.044 Uiso 1 1 d R U . . .
C30 C 0.2456(4) 0.9297(4) 0.3110(4) 0.0859(13) Uani 1 1 d . . . . .
H30 H 0.2198 0.9684 0.3641 0.103 Uiso 1 1 d R U . . .
C29 C 0.2045(4) 0.8481(4) 0.3331(4) 0.0921(14) Uani 1 1 d . . . . .
H29 H 0.1551 0.8275 0.4032 0.111 Uiso 1 1 d R U . . .
C31 C 0.3676(5) 1.0434(4) 0.1872(6) 0.124(2) Uani 1 1 d . U . . .
H31A H 0.3914 1.0327 0.2452 0.149 Uiso 1 1 d R U . . .
H31B H 0.3102 1.1163 0.1777 0.149 Uiso 1 1 d R U . . .
H31C H 0.4337 1.0353 0.1202 0.149 Uiso 1 1 d R U . . .
C25 C 0.3223(3) 0.9557(3) 0.2101(4) 0.0671(10) Uani 1 1 d . . . . .
C26 C 0.3573(3) 0.9005(3) 0.1317(3) 0.0686(9) Uani 1 1 d . . . . .
H26 H 0.4087 0.9187 0.0620 0.082 Uiso 1 1 d R U . . .
C27 C 0.3151(3) 0.8199(3) 0.1547(4) 0.0751(11) Uani 1 1 d . . . . .
H27 H 0.3389 0.7823 0.1014 0.090 Uiso 1 1 d 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
Cd1 N1 2.2904(17) 2_755 ?
Cd1 N1 2.2905(17) . ?
Cd1 N5 2.3013(16) . ?
Cd1 N5 2.3013(16) 2_755 ?
Cd1 N3 2.3474(15) 2_755 ?
Cd1 N3 2.3474(15) . ?
Cd2 N11 2.2606(17) 2_666 ?
Cd2 N11 2.2606(17) . ?
Cd2 N7 2.3183(16) . ?
Cd2 N7 2.3183(16) 2_666 ?
Cd2 N9 2.3461(16) 2_666 ?
Cd2 N9 2.3461(16) . ?
P6 C18 1.725(2) . ?
P6 C17 1.741(2) . ?
P5 C16 1.725(2) . ?
P5 C15 1.743(2) . ?
P3 C6 1.7221(19) . ?
P3 C5 1.744(2) . ?
P1 C2 1.721(2) . ?
P1 C1 1.749(3) . ?
P4 C14 1.724(2) . ?
P4 C13 1.745(2) . ?
P2 C4 1.725(2) . ?
P2 C3 1.744(2) . ?
N8 C14 1.343(2) . ?
N8 N7 1.364(2) . ?
N8 B2 1.580(3) . ?
N4 C4 1.339(2) . ?
N4 N3 1.360(2) . ?
N4 B1 1.567(2) . ?
N10 C16 1.342(2) . ?
N10 N9 1.361(2) . ?
N10 B2 1.578(2) . ?
N9 C15 1.323(3) . ?
N3 C3 1.324(3) . ?
N7 C13 1.325(2) . ?
C7 C12 1.398(2) . ?
C7 C8 1.400(2) . ?
C7 B1 1.606(2) . ?
N2 C2 1.347(2) . ?
N2 N1 1.359(2) . ?
N2 B1 1.575(2) . ?
N6 C6 1.343(2) . ?
N6 N5 1.364(2) . ?
N6 B1 1.584(2) . ?
N12 C18 1.345(2) . ?
N12 N11 1.364(2) . ?
N12 B2 1.588(2) . ?
N1 C1 1.319(3) . ?
B2 C19 1.598(3) . ?
C20 C21 1.393(3) . ?
C20 C19 1.401(2) . ?
C20 H20 0.9300 . ?
C6 H6 0.9300 . ?
N5 C5 1.322(2) . ?
C12 C11 1.389(3) . ?
C12 H12 0.9300 . ?
C2 H2 0.9300 . ?
C14 H14 0.9301 . ?
C8 C9 1.386(3) . ?
C8 H8 0.9300 . ?
C19 C24 1.395(3) . ?
C18 H18 0.9301 . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C3 H3 0.9299 . ?
N11 C17 1.324(2) . ?
C11 C10 1.384(3) . ?
C11 H11 0.9300 . ?
C10 C9 1.386(3) . ?
C10 H10 0.9301 . ?
C5 H5 0.9300 . ?
C16 H16 0.9300 . ?
C15 H15 0.9300 . ?
C24 C23 1.394(3) . ?
C24 H24 0.9301 . ?
C22 C23 1.376(3) . ?
C22 C21 1.376(3) . ?
C22 H22 0.9299 . ?
C17 H17 0.9299 . ?
C9 H9 0.9300 . ?
C21 H21 0.9300 . ?
C23 H23 0.9299 . ?
C28 C29 1.338(6) . ?
C28 C27 1.356(6) . ?
C28 H28 0.9300 . ?
C1 H1 0.9300 . ?
C30 C25 1.360(6) . ?
C30 C29 1.394(7) . ?
C30 H30 0.9301 . ?
C29 H29 0.9301 . ?
C31 C25 1.512(6) . ?
C31 H31A 0.9601 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C25 C26 1.368(5) . ?
C26 C27 1.386(5) . ?
C26 H26 0.9301 . ?
C27 H27 0.9302 . ?

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
N1 Cd1 N1 180.0 2_755 . ?
N1 Cd1 N5 99.21(6) 2_755 . ?
N1 Cd1 N5 80.79(6) . . ?
N1 Cd1 N5 80.79(6) 2_755 2_755 ?
N1 Cd1 N5 99.21(6) . 2_755 ?
N5 Cd1 N5 180.0 . 2_755 ?
N1 Cd1 N3 80.01(6) 2_755 2_755 ?
N1 Cd1 N3 99.99(6) . 2_755 ?
N5 Cd1 N3 95.24(6) . 2_755 ?
N5 Cd1 N3 84.76(6) 2_755 2_755 ?
N1 Cd1 N3 99.99(6) 2_755 . ?
N1 Cd1 N3 80.01(6) . . ?
N5 Cd1 N3 84.76(6) . . ?
N5 Cd1 N3 95.24(6) 2_755 . ?
N3 Cd1 N3 180.0 2_755 . ?
N11 Cd2 N11 180.0 2_666 . ?
N11 Cd2 N7 99.29(6) 2_666 . ?
N11 Cd2 N7 80.71(6) . . ?
N11 Cd2 N7 80.71(6) 2_666 2_666 ?
N11 Cd2 N7 99.29(6) . 2_666 ?
N7 Cd2 N7 180.0 . 2_666 ?
N11 Cd2 N9 81.60(6) 2_666 2_666 ?
N11 Cd2 N9 98.40(6) . 2_666 ?
N7 Cd2 N9 96.32(5) . 2_666 ?
N7 Cd2 N9 83.68(5) 2_666 2_666 ?
N11 Cd2 N9 98.40(6) 2_666 . ?
N11 Cd2 N9 81.60(6) . . ?
N7 Cd2 N9 83.68(5) . . ?
N7 Cd2 N9 96.32(5) 2_666 . ?
N9 Cd2 N9 180.0 2_666 . ?
C18 P6 C17 85.23(9) . . ?
C16 P5 C15 85.53(9) . . ?
C6 P3 C5 85.72(9) . . ?
C2 P1 C1 85.12(10) . . ?
C14 P4 C13 85.56(10) . . ?
C4 P2 C3 85.30(9) . . ?
C14 N8 N7 112.70(16) . . ?
C14 N8 B2 127.88(16) . . ?
N7 N8 B2 118.60(14) . . ?
C4 N4 N3 113.23(15) . . ?
C4 N4 B1 125.97(15) . . ?
N3 N4 B1 120.12(14) . . ?
C16 N10 N9 113.26(15) . . ?
C16 N10 B2 125.04(15) . . ?
N9 N10 B2 120.59(14) . . ?
C15 N9 N10 110.55(16) . . ?
C15 N9 Cd2 119.37(13) . . ?
N10 N9 Cd2 114.89(11) . . ?
C3 N3 N4 110.42(16) . . ?
C3 N3 Cd1 117.64(13) . . ?
N4 N3 Cd1 112.87(11) . . ?
C13 N7 N8 110.94(16) . . ?
C13 N7 Cd2 127.74(13) . . ?
N8 N7 Cd2 121.17(11) . . ?
C12 C7 C8 116.58(16) . . ?
C12 C7 B1 122.94(15) . . ?
C8 C7 B1 120.14(15) . . ?
C2 N2 N1 112.38(15) . . ?
C2 N2 B1 125.01(15) . . ?
N1 N2 B1 122.60(14) . . ?
C6 N6 N5 112.51(15) . . ?
C6 N6 B1 127.89(14) . . ?
N5 N6 B1 118.19(13) . . ?
C18 N12 N11 112.13(15) . . ?
C18 N12 B2 125.25(15) . . ?
N11 N12 B2 122.62(15) . . ?
C1 N1 N2 111.11(17) . . ?
C1 N1 Cd1 128.67(14) . . ?
N2 N1 Cd1 116.57(11) . . ?
N10 B2 N8 103.08(14) . . ?
N10 B2 N12 110.28(14) . . ?
N8 B2 N12 111.06(14) . . ?
N10 B2 C19 112.94(14) . . ?
N8 B2 C19 113.43(14) . . ?
N12 B2 C19 106.14(15) . . ?
C21 C20 C19 121.68(19) . . ?
C21 C20 H20 119.0 . . ?
C19 C20 H20 119.3 . . ?
N6 C6 P3 114.82(13) . . ?
N6 C6 H6 122.5 . . ?
P3 C6 H6 122.6 . . ?
C5 N5 N6 111.29(15) . . ?
C5 N5 Cd1 127.23(13) . . ?
N6 N5 Cd1 121.31(11) . . ?
C11 C12 C7 121.58(17) . . ?
C11 C12 H12 119.1 . . ?
C7 C12 H12 119.3 . . ?
N2 C2 P1 115.20(14) . . ?
N2 C2 H2 122.3 . . ?
P1 C2 H2 122.5 . . ?
N8 C14 P4 114.84(15) . . ?
N8 C14 H14 122.8 . . ?
P4 C14 H14 122.4 . . ?
C9 C8 C7 122.04(17) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 118.9 . . ?
N4 B1 N2 110.12(13) . . ?
N4 B1 N6 103.18(13) . . ?
N2 B1 N6 111.11(13) . . ?
N4 B1 C7 113.10(14) . . ?
N2 B1 C7 107.35(14) . . ?
N6 B1 C7 112.01(13) . . ?
C24 C19 C20 116.41(17) . . ?
C24 C19 B2 121.65(16) . . ?
C20 C19 B2 120.95(16) . . ?
N12 C18 P6 115.28(14) . . ?
N12 C18 H18 122.6 . . ?
P6 C18 H18 122.1 . . ?
N7 C13 P4 115.93(15) . . ?
N7 C13 H13 122.1 . . ?
P4 C13 H13 122.0 . . ?
N4 C4 P2 114.68(14) . . ?
N4 C4 H4 122.6 . . ?
P2 C4 H4 122.7 . . ?
N3 C3 P2 116.34(15) . . ?
N3 C3 H3 121.6 . . ?
P2 C3 H3 122.0 . . ?
C17 N11 N12 111.06(16) . . ?
C17 N11 Cd2 128.38(14) . . ?
N12 N11 Cd2 117.62(11) . . ?
C10 C11 C12 120.45(18) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C10 C9 119.12(17) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.5 . . ?
N5 C5 P3 115.65(15) . . ?
N5 C5 H5 121.8 . . ?
P3 C5 H5 122.5 . . ?
N10 C16 P5 114.43(14) . . ?
N10 C16 H16 122.9 . . ?
P5 C16 H16 122.6 . . ?
N9 C15 P5 116.20(14) . . ?
N9 C15 H15 121.7 . . ?
P5 C15 H15 122.1 . . ?
C23 C24 C19 122.02(19) . . ?
C23 C24 H24 119.3 . . ?
C19 C24 H24 118.7 . . ?
C23 C22 C21 119.61(19) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.1 . . ?
N11 C17 P6 116.29(15) . . ?
N11 C17 H17 121.9 . . ?
P6 C17 H17 121.8 . . ?
C10 C9 C8 120.08(18) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 119.8 . . ?
C22 C21 C20 120.25(19) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.9 . . ?
C22 C23 C24 120.0(2) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 119.8 . . ?
C29 C28 C27 119.6(4) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.3 . . ?
N1 C1 P1 116.18(16) . . ?
N1 C1 H1 122.0 . . ?
P1 C1 H1 121.8 . . ?
C25 C30 C29 120.1(4) . . ?
C25 C30 H30 119.0 . . ?
C29 C30 H30 120.9 . . ?
C28 C29 C30 120.9(4) . . ?
C28 C29 H29 118.8 . . ?
C30 C29 H29 120.2 . . ?
C25 C31 H31A 111.1 . . ?
C25 C31 H31B 111.2 . . ?
H31A C31 H31B 109.5 . . ?
C25 C31 H31C 106.1 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C25 C26 118.6(4) . . ?
C30 C25 C31 119.8(5) . . ?
C26 C25 C31 121.6(5) . . ?
C25 C26 C27 120.7(4) . . ?
C25 C26 H26 119.1 . . ?
C27 C26 H26 120.2 . . ?
C28 C27 C26 120.1(4) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 120.7 . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.056 0.000 0.500 275 82 ' '
_platon_squeeze_details          ?


_refine_diff_density_max         0.535
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.077


####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1406795'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 B2 Co N12 P6, 2(C7 H8)'
_chemical_formula_sum            'C38 H38 B2 Co N12 P6'
_chemical_formula_weight         929.17

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'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   11.1320(5)
_cell_length_b                   13.7490(10)
_cell_length_c                   15.6951(14)
_cell_angle_alpha                90.726(6)
_cell_angle_beta                 99.272(4)
_cell_angle_gamma                112.266(5)
_cell_volume                     2186.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    40073
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_F_000             954
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.26
_exptl_absorpt_coefficient_mu    0.657
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.139
0 1 0 0.152
-1 0 0 0.142
1 0 0 0.164
0 0 1 0.101
0 0 -1 0.129
1 -1 0 0.180
-1 1 0 0.186
0 1 -1 0.146
0 -1 1 0.096
0 -1 -1 0.144


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            39918
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.197
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             9824
_reflns_number_gt                8256
_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       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0454P)²+13.9183P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9824
_refine_ls_number_parameters     535
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0673
_refine_ls_wR_factor_ref         0.1864
_refine_ls_wR_factor_gt          0.1750
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.000
_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 1.0000 0.0000 0.0000 0.01572(17) Uani 1 2 d S . P . .
Co2 Co 1.0000 0.5000 0.5000 0.01840(18) Uani 1 2 d S . P . .
P4 P 1.02125(12) 0.49252(10) 0.20553(8) 0.0280(3) Uani 1 1 d . . . . .
P3 P 0.96851(13) 0.12859(10) 0.26770(8) 0.0291(3) Uani 1 1 d . . . . .
P1 P 1.23834(11) 0.34780(9) -0.05097(8) 0.0246(2) Uani 1 1 d . . . . .
P2 P 0.59378(12) -0.05293(10) -0.17000(9) 0.0301(3) Uani 1 1 d . . . . .
P6 P 0.70407(15) 0.66019(13) 0.51211(9) 0.0394(3) Uani 1 1 d . . . . .
P5 P 0.73778(15) 0.14612(10) 0.43613(9) 0.0370(3) Uani 1 1 d . . . . .
C19 C 0.5956(4) 0.4014(3) 0.2925(3) 0.0214(8) Uani 1 1 d . . . . .
N8 N 0.8581(3) 0.4700(3) 0.3107(2) 0.0199(7) Uani 1 1 d . . . . .
N5 N 0.9483(4) 0.0561(3) 0.1087(2) 0.0200(7) Uani 1 1 d . . . . .
N2 N 1.0115(3) 0.2254(3) -0.0181(2) 0.0175(7) Uani 1 1 d . . . . .
N3 N 0.8181(4) -0.0073(3) -0.0651(2) 0.0209(7) Uani 1 1 d . . . . .
N4 N 0.7833(3) 0.0762(3) -0.0546(2) 0.0185(7) Uani 1 1 d . . . . .
N6 N 0.9054(3) 0.1369(3) 0.1026(2) 0.0185(7) Uani 1 1 d . . . . .
N9 N 0.8455(4) 0.3502(3) 0.4721(2) 0.0237(8) Uani 1 1 d . . . . .
N11 N 0.8534(4) 0.5567(3) 0.4931(2) 0.0248(8) Uani 1 1 d . . . . .
C2 C 1.0876(4) 0.3272(3) -0.0223(3) 0.0223(8) Uani 1 1 d . . . . .
H2 H 1.0613 0.3819 -0.0108 0.027 Uiso 1 1 d R U . . .
N12 N 0.7480(4) 0.5185(3) 0.4268(2) 0.0223(7) Uani 1 1 d . . . . .
N10 N 0.7463(3) 0.3328(3) 0.4026(2) 0.0210(7) Uani 1 1 d . . . . .
C4 C 0.6682(4) 0.0641(4) -0.1059(3) 0.0256(9) Uani 1 1 d . . . . .
H4 H 0.6318 0.1149 -0.1066 0.031 Uiso 1 1 d R U . . .
C12 C 0.8025(4) 0.3297(4) -0.0443(3) 0.0245(9) Uani 1 1 d . . . . .
H12 H 0.8672 0.3466 -0.0787 0.029 Uiso 1 1 d R U . . .
C14 C 0.8632(4) 0.4532(3) 0.2272(3) 0.0232(9) Uani 1 1 d . . . . .
H14 H 0.7882 0.4227 0.1848 0.028 Uiso 1 1 d R U . . .
N7 N 0.9790(4) 0.5120(3) 0.3625(2) 0.0243(8) Uani 1 1 d . . . . .
N1 N 1.0716(4) 0.1588(3) -0.0334(2) 0.0204(7) Uani 1 1 d . . . . .
C8 C 0.6900(4) 0.2262(3) 0.0597(3) 0.0236(9) Uani 1 1 d . . . . .
H8 H 0.6780 0.1722 0.0967 0.028 Uiso 1 1 d R U . . .
C3 C 0.7284(5) -0.0805(4) -0.1225(3) 0.0263(9) Uani 1 1 d . . . . .
H3 H 0.7365 -0.1435 -0.1362 0.032 Uiso 1 1 d R U . . .
C7 C 0.7917(4) 0.2494(3) 0.0116(3) 0.0206(8) Uani 1 1 d . . . . .
C10 C 0.6238(5) 0.3623(4) 0.0010(3) 0.0262(9) Uani 1 1 d . . . . .
H10 H 0.5710 0.4011 -0.0009 0.031 Uiso 1 1 d R U . . .
C13 C 1.0728(5) 0.5298(4) 0.3156(3) 0.0288(10) Uani 1 1 d . . . . .
H13 H 1.1618 0.5607 0.3402 0.035 Uiso 1 1 d R U . . .
C5 C 0.9830(5) 0.0420(4) 0.1910(3) 0.0242(9) Uani 1 1 d . . . . .
H5 H 1.0128 -0.0110 0.2069 0.029 Uiso 1 1 d R U . . .
B2 B 0.7346(5) 0.4299(4) 0.3564(3) 0.0209(9) Uani 1 1 d . . . . .
C20 C 0.4787(5) 0.3302(4) 0.3148(3) 0.0285(10) Uani 1 1 d . . . . .
H20 H 0.4837 0.2919 0.3628 0.034 Uiso 1 1 d R U . . .
C15 C 0.8501(5) 0.2597(4) 0.4968(3) 0.0298(10) Uani 1 1 d . . . . .
H15 H 0.9104 0.2573 0.5443 0.036 Uiso 1 1 d R U . . .
C21 C 0.3565(5) 0.3145(4) 0.2670(3) 0.0344(11) Uani 1 1 d . . . . .
H21 H 0.2808 0.2680 0.2845 0.041 Uiso 1 1 d R U . . .
C16 C 0.6830(5) 0.2299(4) 0.3750(3) 0.0287(10) Uani 1 1 d . . . . .
H16 H 0.6155 0.2058 0.3270 0.034 Uiso 1 1 d R U . . .
C23 C 0.4583(5) 0.4390(4) 0.1705(3) 0.0299(10) Uani 1 1 d . . . . .
H23 H 0.4523 0.4744 0.1209 0.036 Uiso 1 1 d R U . . .
C11 C 0.7210(5) 0.3857(4) -0.0496(3) 0.0281(10) Uani 1 1 d . . . . .
H11 H 0.7313 0.4383 -0.0878 0.034 Uiso 1 1 d R U . . .
C9 C 0.6070(5) 0.2806(4) 0.0545(3) 0.0270(9) Uani 1 1 d . . . . .
H9 H 0.5401 0.2622 0.0871 0.032 Uiso 1 1 d R U . . .
C22 C 0.3448(5) 0.3669(4) 0.1943(3) 0.0327(11) Uani 1 1 d . . . . .
H22 H 0.2622 0.3549 0.1616 0.039 Uiso 1 1 d R U . . .
C17 C 0.8437(5) 0.6307(4) 0.5424(3) 0.0328(11) Uani 1 1 d . . . . .
H17 H 0.9074 0.6651 0.5907 0.039 Uiso 1 1 d R U . . .
C1 C 1.1887(4) 0.2120(3) -0.0522(3) 0.0238(9) Uani 1 1 d . . . . .
H1 H 1.2424 0.1781 -0.0653 0.029 Uiso 1 1 d R U . . .
C6 C 0.9131(5) 0.1842(4) 0.1800(3) 0.0246(9) Uani 1 1 d . . . . .
H6 H 0.8908 0.2423 0.1858 0.030 Uiso 1 1 d R U . . .
C24 C 0.5811(5) 0.4570(4) 0.2200(3) 0.0255(9) Uani 1 1 d . . . . .
H24 H 0.6558 0.5080 0.2049 0.031 Uiso 1 1 d R U . . .
C18 C 0.6618(5) 0.5647(4) 0.4286(3) 0.0323(11) Uani 1 1 d . . . . .
H18 H 0.5849 0.5465 0.3876 0.039 Uiso 1 1 d R U . . .
B1 B 0.8727(5) 0.1748(4) 0.0104(3) 0.0185(9) Uani 1 1 d . . . . .
C34 C -0.0758(9) 0.8580(8) 0.3650(5) 0.069(2) Uani 1 1 d . . . . .
H34 H -0.1488 0.8559 0.3877 0.083 Uiso 1 1 d R U . . .
C28 C 0.4214(8) 0.7041(10) 0.3932(6) 0.092(3) Uani 1 1 d . U . . .
H28 H 0.3782 0.6681 0.4362 0.110 Uiso 1 1 d R U . . .
C36 C 0.0179(8) 0.7813(5) 0.2734(4) 0.0560(18) Uani 1 1 d . . . . .
H36 H 0.0087 0.7277 0.2331 0.067 Uiso 1 1 d R U . . .
C26 C 0.4915(6) 0.7029(5) 0.2585(4) 0.0498(16) Uani 1 1 d . U . . .
H26 H 0.4985 0.6660 0.2107 0.060 Uiso 1 1 d R U . . .
C30 C 0.5378(7) 0.8670(7) 0.3349(6) 0.076(3) Uani 1 1 d . U . . .
H30 H 0.5743 0.9403 0.3398 0.091 Uiso 1 1 d R U . . .
C29 C 0.4759(10) 0.8144(9) 0.3972(7) 0.092(3) Uani 1 1 d . U . . .
H29 H 0.4708 0.8515 0.4455 0.110 Uiso 1 1 d R U . . .
C25 C 0.5467(6) 0.8101(6) 0.2648(5) 0.0561(18) Uani 1 1 d . . . . .
C32 C 0.1519(7) 0.9440(5) 0.3619(4) 0.0498(16) Uani 1 1 d . . . . .
C37 C 0.1418(7) 0.8659(6) 0.3022(4) 0.0558(18) Uani 1 1 d . . . . .
H37 H 0.2157 0.8683 0.2803 0.067 Uiso 1 1 d R U . . .
C35 C -0.0887(7) 0.7814(6) 0.3080(5) 0.062(2) Uani 1 1 d . . . . .
H35 H -0.1709 0.7272 0.2904 0.075 Uiso 1 1 d R U . . .
C38 C 0.2795(9) 1.0355(6) 0.3899(5) 0.082(3) Uani 1 1 d . . . . .
H38A H 0.3082 1.0713 0.3403 0.098 Uiso 1 1 d R U . . .
H38B H 0.3444 1.0104 0.4175 0.098 Uiso 1 1 d R U . . .
H38C H 0.2684 1.0834 0.4300 0.098 Uiso 1 1 d R U . . .
C27 C 0.4274(7) 0.6472(8) 0.3208(6) 0.076(2) Uani 1 1 d . U . . .
H27 H 0.3895 0.5739 0.3144 0.091 Uiso 1 1 d R U . . .
C33 C 0.0417(9) 0.9383(7) 0.3917(4) 0.063(2) Uani 1 1 d . . . . .
H33 H 0.0470 0.9917 0.4310 0.076 Uiso 1 1 d R U . . .
C31 C 0.6186(8) 0.8694(8) 0.1960(6) 0.081(3) Uani 1 1 d . U . . .
H31A H 0.6315 0.9424 0.2029 0.097 Uiso 1 1 d R U . . .
H31B H 0.5667 0.8395 0.1400 0.097 Uiso 1 1 d R U . . .
H31C H 0.7027 0.8637 0.2008 0.097 Uiso 1 1 d 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 N3 2.081(4) 2_755 ?
Co1 N3 2.082(4) . ?
Co1 N5 2.112(3) . ?
Co1 N5 2.112(3) 2_755 ?
Co1 N1 2.127(3) 2_755 ?
Co1 N1 2.127(3) . ?
Co2 N11 2.047(4) . ?
Co2 N11 2.047(4) 2_766 ?
Co2 N9 2.108(4) . ?
Co2 N9 2.108(4) 2_766 ?
Co2 N7 2.148(4) . ?
Co2 N7 2.148(4) 2_766 ?
P4 C14 1.727(5) . ?
P4 C13 1.736(5) . ?
P3 C6 1.723(5) . ?
P3 C5 1.751(5) . ?
P1 C2 1.727(5) . ?
P1 C1 1.734(5) . ?
P2 C4 1.722(5) . ?
P2 C3 1.739(5) . ?
P6 C18 1.718(5) . ?
P6 C17 1.747(5) . ?
P5 C16 1.729(5) . ?
P5 C15 1.734(5) . ?
C19 C20 1.401(6) . ?
C19 C24 1.402(6) . ?
C19 B2 1.607(6) . ?
N8 C14 1.342(5) . ?
N8 N7 1.361(5) . ?
N8 B2 1.569(6) . ?
N5 C5 1.326(5) . ?
N5 N6 1.364(5) . ?
N2 C2 1.343(5) . ?
N2 N1 1.361(5) . ?
N2 B1 1.577(6) . ?
N3 C3 1.321(6) . ?
N3 N4 1.360(5) . ?
N4 C4 1.349(6) . ?
N4 B1 1.576(6) . ?
N6 C6 1.345(5) . ?
N6 B1 1.578(6) . ?
N9 C15 1.324(6) . ?
N9 N10 1.368(5) . ?
N11 C17 1.317(6) . ?
N11 N12 1.365(5) . ?
C2 H2 0.9299 . ?
N12 C18 1.341(6) . ?
N12 B2 1.581(6) . ?
N10 C16 1.347(6) . ?
N10 B2 1.566(6) . ?
C4 H4 0.9300 . ?
C12 C11 1.389(6) . ?
C12 C7 1.400(6) . ?
C12 H12 0.9299 . ?
C14 H14 0.9300 . ?
N7 C13 1.322(6) . ?
N1 C1 1.315(5) . ?
C8 C9 1.387(6) . ?
C8 C7 1.400(6) . ?
C8 H8 0.9300 . ?
C3 H3 0.9300 . ?
C7 B1 1.603(6) . ?
C10 C9 1.384(7) . ?
C10 C11 1.387(7) . ?
C10 H10 0.9299 . ?
C13 H13 0.9300 . ?
C5 H5 0.9301 . ?
C20 C21 1.381(7) . ?
C20 H20 0.9300 . ?
C15 H15 0.9299 . ?
C21 C22 1.373(7) . ?
C21 H21 0.9300 . ?
C16 H16 0.9300 . ?
C23 C24 1.389(6) . ?
C23 C22 1.390(7) . ?
C23 H23 0.9300 . ?
C11 H11 0.9300 . ?
C9 H9 0.9299 . ?
C22 H22 0.9300 . ?
C17 H17 0.9300 . ?
C1 H1 0.9301 . ?
C6 H6 0.9300 . ?
C24 H24 0.9300 . ?
C18 H18 0.9301 . ?
C34 C35 1.323(12) . ?
C34 C33 1.351(12) . ?
C34 H34 0.9299 . ?
C28 C27 1.396(13) . ?
C28 C29 1.400(15) . ?
C28 H28 0.9299 . ?
C36 C35 1.382(11) . ?
C36 C37 1.425(10) . ?
C36 H36 0.9300 . ?
C26 C25 1.360(10) . ?
C26 C27 1.372(11) . ?
C26 H26 0.9299 . ?
C30 C29 1.346(14) . ?
C30 C25 1.380(9) . ?
C30 H30 0.9299 . ?
C29 H29 0.9301 . ?
C25 C31 1.510(12) . ?
C32 C33 1.358(11) . ?
C32 C37 1.375(10) . ?
C32 C38 1.492(10) . ?
C37 H37 0.9300 . ?
C35 H35 0.9301 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9599 . ?
C38 H38C 0.9601 . ?
C27 H27 0.9300 . ?
C33 H33 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9599 . ?

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 Co1 N3 180.0 2_755 . ?
N3 Co1 N5 95.09(14) 2_755 . ?
N3 Co1 N5 84.91(14) . . ?
N3 Co1 N5 84.91(14) 2_755 2_755 ?
N3 Co1 N5 95.09(14) . 2_755 ?
N5 Co1 N5 180.0 . 2_755 ?
N3 Co1 N1 84.85(14) 2_755 2_755 ?
N3 Co1 N1 95.15(14) . 2_755 ?
N5 Co1 N1 93.39(13) . 2_755 ?
N5 Co1 N1 86.61(13) 2_755 2_755 ?
N3 Co1 N1 95.15(14) 2_755 . ?
N3 Co1 N1 84.85(14) . . ?
N5 Co1 N1 86.61(13) . . ?
N5 Co1 N1 93.39(13) 2_755 . ?
N1 Co1 N1 180.0 2_755 . ?
N11 Co2 N11 180.0(2) . 2_766 ?
N11 Co2 N9 85.48(15) . . ?
N11 Co2 N9 94.52(15) 2_766 . ?
N11 Co2 N9 94.53(15) . 2_766 ?
N11 Co2 N9 85.48(15) 2_766 2_766 ?
N9 Co2 N9 180.0 . 2_766 ?
N11 Co2 N7 85.26(15) . . ?
N11 Co2 N7 94.74(15) 2_766 . ?
N9 Co2 N7 86.69(14) . . ?
N9 Co2 N7 93.31(14) 2_766 . ?
N11 Co2 N7 94.74(15) . 2_766 ?
N11 Co2 N7 85.26(15) 2_766 2_766 ?
N9 Co2 N7 93.31(14) . 2_766 ?
N9 Co2 N7 86.69(14) 2_766 2_766 ?
N7 Co2 N7 180.0 . 2_766 ?
C14 P4 C13 85.6(2) . . ?
C6 P3 C5 85.7(2) . . ?
C2 P1 C1 85.3(2) . . ?
C4 P2 C3 85.5(2) . . ?
C18 P6 C17 85.3(2) . . ?
C16 P5 C15 85.6(2) . . ?
C20 C19 C24 116.2(4) . . ?
C20 C19 B2 120.6(4) . . ?
C24 C19 B2 122.5(4) . . ?
C14 N8 N7 113.4(4) . . ?
C14 N8 B2 128.3(4) . . ?
N7 N8 B2 117.3(3) . . ?
C5 N5 N6 110.6(3) . . ?
C5 N5 Co1 126.9(3) . . ?
N6 N5 Co1 120.2(3) . . ?
C2 N2 N1 113.0(3) . . ?
C2 N2 B1 129.9(3) . . ?
N1 N2 B1 116.8(3) . . ?
C3 N3 N4 111.1(4) . . ?
C3 N3 Co1 129.8(3) . . ?
N4 N3 Co1 119.0(3) . . ?
C4 N4 N3 112.4(3) . . ?
C4 N4 B1 125.9(3) . . ?
N3 N4 B1 121.6(3) . . ?
C6 N6 N5 113.2(3) . . ?
C6 N6 B1 127.2(4) . . ?
N5 N6 B1 119.0(3) . . ?
C15 N9 N10 110.5(4) . . ?
C15 N9 Co2 126.2(3) . . ?
N10 N9 Co2 120.0(3) . . ?
C17 N11 N12 110.7(4) . . ?
C17 N11 Co2 130.3(3) . . ?
N12 N11 Co2 119.0(3) . . ?
N2 C2 P1 114.4(3) . . ?
N2 C2 H2 122.8 . . ?
P1 C2 H2 122.9 . . ?
C18 N12 N11 112.7(4) . . ?
C18 N12 B2 125.5(4) . . ?
N11 N12 B2 121.8(4) . . ?
C16 N10 N9 112.7(4) . . ?
C16 N10 B2 127.8(4) . . ?
N9 N10 B2 118.6(3) . . ?
N4 C4 P2 114.8(3) . . ?
N4 C4 H4 122.6 . . ?
P2 C4 H4 122.7 . . ?
C11 C12 C7 122.4(4) . . ?
C11 C12 H12 118.8 . . ?
C7 C12 H12 118.8 . . ?
N8 C14 P4 114.1(3) . . ?
N8 C14 H14 122.9 . . ?
P4 C14 H14 122.9 . . ?
C13 N7 N8 110.2(4) . . ?
C13 N7 Co2 126.4(3) . . ?
N8 N7 Co2 120.7(3) . . ?
C1 N1 N2 110.4(3) . . ?
C1 N1 Co1 126.2(3) . . ?
N2 N1 Co1 121.9(3) . . ?
C9 C8 C7 122.5(4) . . ?
C9 C8 H8 118.8 . . ?
C7 C8 H8 118.6 . . ?
N3 C3 P2 116.2(3) . . ?
N3 C3 H3 121.8 . . ?
P2 C3 H3 121.9 . . ?
C8 C7 C12 115.7(4) . . ?
C8 C7 B1 120.5(4) . . ?
C12 C7 B1 123.0(4) . . ?
C9 C10 C11 119.1(4) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.4 . . ?
N7 C13 P4 116.6(3) . . ?
N7 C13 H13 121.9 . . ?
P4 C13 H13 121.6 . . ?
N5 C5 P3 116.0(3) . . ?
N5 C5 H5 121.9 . . ?
P3 C5 H5 122.1 . . ?
N8 B2 N10 103.5(3) . . ?
N8 B2 N12 108.9(3) . . ?
N10 B2 N12 109.5(3) . . ?
N8 B2 C19 114.6(3) . . ?
N10 B2 C19 112.9(4) . . ?
N12 B2 C19 107.4(4) . . ?
C21 C20 C19 121.8(4) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
N9 C15 P5 116.7(3) . . ?
N9 C15 H15 121.6 . . ?
P5 C15 H15 121.7 . . ?
C22 C21 C20 121.0(5) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.6 . . ?
N10 C16 P5 114.5(3) . . ?
N10 C16 H16 122.9 . . ?
P5 C16 H16 122.7 . . ?
C24 C23 C22 120.0(4) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 120.1 . . ?
C10 C11 C12 120.1(4) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 119.6 . . ?
C10 C9 C8 120.1(4) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 119.7 . . ?
C21 C22 C23 118.9(4) . . ?
C21 C22 H22 120.6 . . ?
C23 C22 H22 120.5 . . ?
N11 C17 P6 116.2(4) . . ?
N11 C17 H17 121.9 . . ?
P6 C17 H17 121.9 . . ?
N1 C1 P1 116.9(3) . . ?
N1 C1 H1 121.3 . . ?
P1 C1 H1 121.8 . . ?
N6 C6 P3 114.5(3) . . ?
N6 C6 H6 122.8 . . ?
P3 C6 H6 122.7 . . ?
C23 C24 C19 122.0(4) . . ?
C23 C24 H24 119.0 . . ?
C19 C24 H24 119.0 . . ?
N12 C18 P6 115.0(4) . . ?
N12 C18 H18 122.4 . . ?
P6 C18 H18 122.6 . . ?
N4 B1 N2 108.4(3) . . ?
N4 B1 N6 109.6(3) . . ?
N2 B1 N6 103.6(3) . . ?
N4 B1 C7 106.6(3) . . ?
N2 B1 C7 116.1(3) . . ?
N6 B1 C7 112.4(3) . . ?
C35 C34 C33 121.3(8) . . ?
C35 C34 H34 119.4 . . ?
C33 C34 H34 119.3 . . ?
C27 C28 C29 118.8(9) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 H28 121.7 . . ?
C35 C36 C37 117.5(7) . . ?
C35 C36 H36 121.0 . . ?
C37 C36 H36 121.5 . . ?
C25 C26 C27 122.3(7) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 H26 118.8 . . ?
C29 C30 C25 118.7(9) . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 121.3 . . ?
C30 C29 C28 122.0(9) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 118.1 . . ?
C26 C25 C30 120.3(8) . . ?
C26 C25 C31 121.2(7) . . ?
C30 C25 C31 118.5(8) . . ?
C33 C32 C37 118.5(7) . . ?
C33 C32 C38 120.7(8) . . ?
C37 C32 C38 120.7(8) . . ?
C32 C37 C36 120.0(7) . . ?
C32 C37 H37 120.2 . . ?
C36 C37 H37 119.9 . . ?
C34 C35 C36 121.0(7) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C32 C38 H38A 109.5 . . ?
C32 C38 H38B 109.1 . . ?
H38A C38 H38B 109.5 . . ?
C32 C38 H38C 109.8 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C26 C27 C28 117.8(9) . . ?
C26 C27 H27 120.4 . . ?
C28 C27 H27 121.7 . . ?
C34 C33 C32 121.7(7) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.2 . . ?
C25 C31 H31A 109.8 . . ?
C25 C31 H31B 108.9 . . ?
H31A C31 H31B 109.5 . . ?
C25 C31 H31C 109.7 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

_refine_diff_density_max         2.057
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.112



####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1406796'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 B2 N12 Ni P6, 2(C7 H8)'
_chemical_formula_sum            'C38 H38 B2 N12 Ni P6'
_chemical_formula_weight         928.95

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'
P P 0.1023 0.0942 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   11.0910(5)
_cell_length_b                   13.6971(10)
_cell_length_c                   15.7350(9)
_cell_angle_alpha                90.977(6)
_cell_angle_beta                 99.368(4)
_cell_angle_gamma                112.091(5)
_cell_volume                     2177.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    36813
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_F_000             956
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    0.711
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.115
0 0 1 0.163
0 -1 0 0.083
0 1 0 0.046
-1 0 0 0.067
1 0 0 0.102
0 -1 1 0.093
-1 0 1 0.066
1 0 -1 0.086


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            36709
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.197
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             9891
_reflns_number_gt                7606
_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       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0237P)²+3.4153P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9891
_refine_ls_number_parameters     535
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1045
_refine_ls_wR_factor_gt          0.0910
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.004
_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
Ni1 Ni 0.0000 0.0000 0.0000 0.01924(11) Uani 1 2 d S . P . .
Ni2 Ni 0.0000 0.5000 0.5000 0.01578(11) Uani 1 2 d S . P . .
P1 P -0.02639(8) 0.00648(7) 0.29062(5) 0.02846(17) Uani 1 1 d . . . . .
P5 P 0.03178(8) 0.37384(6) 0.23353(5) 0.02800(17) Uani 1 1 d . . . . .
P4 P -0.24096(7) 0.15562(6) 0.55158(5) 0.02459(16) Uani 1 1 d . . . . .
P6 P 0.40548(8) 0.55594(6) 0.66955(5) 0.02903(18) Uani 1 1 d . . . . .
P3 P 0.29231(9) -0.16406(8) -0.01265(6) 0.0387(2) Uani 1 1 d . . . . .
P2 P 0.26254(9) 0.35349(6) 0.06059(6) 0.0360(2) Uani 1 1 d . . . . .
C7 C 0.4028(3) 0.0975(2) 0.20671(17) 0.0215(6) Uani 1 1 d . . . . .
N9 N 0.0503(2) 0.44505(17) 0.39233(14) 0.0196(5) Uani 1 1 d . . . . .
N2 N 0.1391(2) 0.03046(17) 0.18692(14) 0.0188(5) Uani 1 1 d . . . . .
N7 N -0.0734(2) 0.34402(17) 0.53194(14) 0.0198(5) Uani 1 1 d . . . . .
N8 N -0.0133(2) 0.27630(17) 0.51837(14) 0.0181(4) Uani 1 1 d . . . . .
N11 N 0.1793(2) 0.50836(17) 0.56555(14) 0.0205(5) Uani 1 1 d . . . . .
N12 N 0.2154(2) 0.42516(17) 0.55510(14) 0.0179(4) Uani 1 1 d . . . . .
N10 N 0.0932(2) 0.36363(17) 0.39835(14) 0.0182(4) Uani 1 1 d . . . . .
N3 N 0.1524(2) 0.14852(18) 0.02643(14) 0.0222(5) Uani 1 1 d . . . . .
C2 C 0.1324(3) 0.0454(2) 0.27007(17) 0.0234(6) Uani 1 1 d . . . . .
H2 H 0.2070 0.0742 0.3132 0.028 Uiso 1 1 d R U . . .
N6 N 0.2501(2) -0.01970(18) 0.07254(14) 0.0217(5) Uani 1 1 d . . . . .
N4 N 0.2524(2) 0.16668(18) 0.09561(14) 0.0219(5) Uani 1 1 d . . . . .
C14 C -0.0899(3) 0.1748(2) 0.52402(17) 0.0214(6) Uani 1 1 d . . . . .
H14 H -0.0635 0.1194 0.5139 0.026 Uiso 1 1 d R U . . .
C8 C 0.4156(3) 0.0419(2) 0.27903(18) 0.0242(6) Uani 1 1 d . . . . .
H8 H 0.3400 -0.0076 0.2944 0.029 Uiso 1 1 d R U . . .
C18 C 0.3314(3) 0.4382(2) 0.60533(18) 0.0243(6) Uani 1 1 d . . . . .
H18 H 0.3689 0.3879 0.6054 0.029 Uiso 1 1 d R U . . .
N5 N 0.1440(2) -0.05883(19) 0.00663(15) 0.0245(5) Uani 1 1 d . . . . .
N1 N 0.0180(2) -0.01045(19) 0.13421(14) 0.0232(5) Uani 1 1 d . . . . .
C20 C 0.1957(3) 0.1701(2) 0.54490(18) 0.0231(6) Uani 1 1 d . . . . .
H20 H 0.1327 0.1548 0.5804 0.028 Uiso 1 1 d R U . . .
C24 C 0.3081(3) 0.2727(2) 0.44090(18) 0.0232(6) Uani 1 1 d . . . . .
H24 H 0.3214 0.3274 0.4047 0.028 Uiso 1 1 d R U . . .
C15 C 0.0170(3) 0.4600(2) 0.31054(17) 0.0222(6) Uani 1 1 d . . . . .
H15 H -0.0129 0.5133 0.2948 0.027 Uiso 1 1 d R U . . .
C17 C 0.2688(3) 0.5823(2) 0.62273(18) 0.0238(6) Uani 1 1 d . . . . .
H17 H 0.2594 0.6448 0.6371 0.029 Uiso 1 1 d R U . . .
C13 C -0.1919(3) 0.2923(2) 0.55071(18) 0.0230(6) Uani 1 1 d . . . . .
H13 H -0.2456 0.3270 0.5630 0.028 Uiso 1 1 d R U . . .
C22 C 0.3731(3) 0.1359(2) 0.49859(19) 0.0261(6) Uani 1 1 d . . . . .
H22 H 0.4266 0.0972 0.5006 0.031 Uiso 1 1 d R U . . .
C23 C 0.3894(3) 0.2167(2) 0.44554(19) 0.0250(6) Uani 1 1 d . . . . .
H23 H 0.4553 0.2336 0.4122 0.030 Uiso 1 1 d R U . . .
C21 C 0.2764(3) 0.1126(2) 0.5488(2) 0.0276(6) Uani 1 1 d . . . . .
H21 H 0.2653 0.0586 0.5855 0.033 Uiso 1 1 d R U . . .
C3 C 0.1481(3) 0.2388(2) 0.00036(19) 0.0287(6) Uani 1 1 d . . . . .
H3 H 0.0875 0.2407 -0.0473 0.034 Uiso 1 1 d R U . . .
C19 C 0.2061(3) 0.2500(2) 0.48912(17) 0.0193(5) Uani 1 1 d . . . . .
C11 C 0.6427(3) 0.1831(3) 0.2329(2) 0.0321(7) Uani 1 1 d . . . . .
H11 H 0.7188 0.2303 0.2164 0.038 Uiso 1 1 d R U . . .
C28 C 1.0889(4) 0.7191(4) 0.1935(3) 0.0634(13) Uani 1 1 d . . . . .
H28 H 1.1716 0.7733 0.2107 0.076 Uiso 1 1 d R U . . .
C4 C 0.3168(3) 0.2700(2) 0.12229(19) 0.0284(6) Uani 1 1 d . . . . .
H4 H 0.3852 0.2945 0.1700 0.034 Uiso 1 1 d R U . . .
C16 C 0.0863(3) 0.3170(2) 0.32089(17) 0.0236(6) Uani 1 1 d . . . . .
H16 H 0.1090 0.2588 0.3148 0.028 Uiso 1 1 d R U . . .
C9 C 0.5392(3) 0.0589(2) 0.32856(19) 0.0290(6) Uani 1 1 d . . . . .
H9 H 0.5447 0.0224 0.3774 0.035 Uiso 1 1 d R U . . .
C12 C 0.5203(3) 0.1674(2) 0.18474(18) 0.0277(6) Uani 1 1 d . . . . .
H12 H 0.5158 0.2045 0.1362 0.033 Uiso 1 1 d R U . . .
C5 C 0.1525(3) -0.1340(3) -0.04267(19) 0.0316(7) Uani 1 1 d . . . . .
H5 H 0.0877 -0.1692 -0.0904 0.038 Uiso 1 1 d R U . . .
C1 C -0.0770(3) -0.0284(2) 0.17971(19) 0.0283(6) Uani 1 1 d . . . . .
H1 H -0.1660 -0.0584 0.1541 0.034 Uiso 1 1 d R U . . .
C10 C 0.6531(3) 0.1297(3) 0.3056(2) 0.0318(7) Uani 1 1 d . . . . .
H10 H 0.7356 0.1409 0.3385 0.038 Uiso 1 1 d R U . . .
B1 B 0.2639(3) 0.0696(2) 0.14215(19) 0.0202(6) Uani 1 1 d . . . . .
C6 C 0.3361(3) -0.0674(3) 0.07048(19) 0.0306(7) Uani 1 1 d . . . . .
H6 H 0.4135 -0.0494 0.1112 0.037 Uiso 1 1 d R U . . .
B2 B 0.1257(3) 0.3257(2) 0.48996(19) 0.0180(6) Uani 1 1 d . . . . .
C25 C 0.8482(4) 0.5556(3) 0.1392(2) 0.0467(10) Uani 1 1 d . . . . .
C32 C 0.4519(4) 0.6864(4) 0.2378(3) 0.0569(12) Uani 1 1 d . . . . .
C33 C 0.5081(4) 0.7952(3) 0.2417(3) 0.0532(11) Uani 1 1 d . . . . .
H33 H 0.5023 0.8342 0.2888 0.064 Uiso 1 1 d R U . . .
C27 C 0.9819(5) 0.7196(3) 0.2274(2) 0.0569(12) Uani 1 1 d . . . . .
H27 H 0.9912 0.7737 0.2676 0.068 Uiso 1 1 d R U . . .
C35 C 0.5756(4) 0.7884(6) 0.1062(4) 0.089(2) Uani 1 1 d . . . . .
H35 H 0.6157 0.8219 0.0614 0.107 Uiso 1 1 d R U . . .
C29 C 1.0751(5) 0.6404(5) 0.1355(3) 0.0672(13) Uani 1 1 d . . . . .
H29 H 1.1481 0.6410 0.1134 0.081 Uiso 1 1 d R U . . .
C26 C 0.8581(4) 0.6354(3) 0.1990(2) 0.0505(10) Uani 1 1 d . . . . .
H26 H 0.7838 0.6332 0.2204 0.061 Uiso 1 1 d R U . . .
C31 C 0.7183(5) 0.4632(4) 0.1108(3) 0.0763(15) Uani 1 1 d . . . . .
H31A H 0.7173 0.4318 0.0556 0.092 Uiso 1 1 d R U . . .
H31B H 0.6469 0.4874 0.1064 0.092 Uiso 1 1 d R U . . .
H31C H 0.7081 0.4117 0.1525 0.092 Uiso 1 1 d R U . . .
C30 C 0.9576(5) 0.5614(4) 0.1093(3) 0.0585(12) Uani 1 1 d . . . . .
H30 H 0.9511 0.5085 0.0688 0.070 Uiso 1 1 d R U . . .
C37 C 0.4594(4) 0.6290(4) 0.1683(4) 0.0745(16) Uani 1 1 d . . . . .
H37 H 0.4208 0.5555 0.1644 0.089 Uiso 1 1 d R U . . .
C34 C 0.5708(4) 0.8474(5) 0.1784(4) 0.0754(15) Uani 1 1 d . . . . .
H34 H 0.6095 0.9208 0.1834 0.090 Uiso 1 1 d R U . . .
C38 C 0.3826(4) 0.6309(5) 0.3071(4) 0.0799(16) Uani 1 1 d . . . . .
H38A H 0.2988 0.6379 0.3023 0.096 Uiso 1 1 d R U . . .
H38B H 0.4356 0.6618 0.3626 0.096 Uiso 1 1 d R U . . .
H38C H 0.3684 0.5574 0.3010 0.096 Uiso 1 1 d R U . . .
C36 C 0.5196(6) 0.6767(5) 0.1053(4) 0.0880(17) Uani 1 1 d . U . . .
H36 H 0.5247 0.6362 0.0589 0.106 Uiso 1 1 d 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
Ni1 N5 2.032(2) 2 ?
Ni1 N5 2.032(2) . ?
Ni1 N3 2.079(2) 2 ?
Ni1 N3 2.079(2) . ?
Ni1 N1 2.101(2) . ?
Ni1 N1 2.101(2) 2 ?
Ni2 N11 2.046(2) . ?
Ni2 N11 2.046(2) 2_566 ?
Ni2 N9 2.080(2) . ?
Ni2 N9 2.080(2) 2_566 ?
Ni2 N7 2.084(2) 2_566 ?
Ni2 N7 2.084(2) . ?
P1 C2 1.725(3) . ?
P1 C1 1.744(3) . ?
P5 C16 1.727(3) . ?
P5 C15 1.747(3) . ?
P4 C14 1.724(3) . ?
P4 C13 1.743(3) . ?
P6 C18 1.724(3) . ?
P6 C17 1.740(3) . ?
P3 C6 1.717(3) . ?
P3 C5 1.745(3) . ?
P2 C4 1.726(3) . ?
P2 C3 1.742(3) . ?
C7 C8 1.398(4) . ?
C7 C12 1.398(4) . ?
C7 B1 1.608(4) . ?
N9 C15 1.321(3) . ?
N9 N10 1.366(3) . ?
N2 C2 1.339(3) . ?
N2 N1 1.364(3) . ?
N2 B1 1.573(4) . ?
N7 C13 1.322(3) . ?
N7 N8 1.362(3) . ?
N8 C14 1.343(3) . ?
N8 B2 1.576(4) . ?
N11 C17 1.320(3) . ?
N11 N12 1.358(3) . ?
N12 C18 1.343(3) . ?
N12 B2 1.580(4) . ?
N10 C16 1.344(3) . ?
N10 B2 1.573(4) . ?
N3 C3 1.324(4) . ?
N3 N4 1.367(3) . ?
C2 H2 0.9300 . ?
N6 C6 1.348(4) . ?
N6 N5 1.362(3) . ?
N6 B1 1.574(4) . ?
N4 C4 1.346(4) . ?
N4 B1 1.566(4) . ?
C14 H14 0.9301 . ?
C8 C9 1.395(4) . ?
C8 H8 0.9300 . ?
C18 H18 0.9300 . ?
N5 C5 1.319(4) . ?
N1 C1 1.318(4) . ?
C20 C21 1.393(4) . ?
C20 C19 1.397(4) . ?
C20 H20 0.9301 . ?
C24 C23 1.382(4) . ?
C24 C19 1.405(4) . ?
C24 H24 0.9301 . ?
C15 H15 0.9299 . ?
C17 H17 0.9300 . ?
C13 H13 0.9299 . ?
C22 C23 1.373(4) . ?
C22 C21 1.379(4) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C21 H21 0.9300 . ?
C3 H3 0.9300 . ?
C19 B2 1.604(4) . ?
C11 C12 1.380(4) . ?
C11 C10 1.381(4) . ?
C11 H11 0.9300 . ?
C28 C29 1.347(7) . ?
C28 C27 1.381(7) . ?
C28 H28 0.9301 . ?
C4 H4 0.9300 . ?
C16 H16 0.9299 . ?
C9 C10 1.381(5) . ?
C9 H9 0.9300 . ?
C12 H12 0.9300 . ?
C5 H5 0.9301 . ?
C1 H1 0.9300 . ?
C10 H10 0.9300 . ?
C6 H6 0.9300 . ?
C25 C30 1.347(6) . ?
C25 C26 1.391(6) . ?
C25 C31 1.509(6) . ?
C32 C37 1.368(6) . ?
C32 C33 1.378(6) . ?
C32 C38 1.490(7) . ?
C33 C34 1.365(7) . ?
C33 H33 0.9301 . ?
C27 C26 1.416(6) . ?
C27 H27 0.9300 . ?
C35 C34 1.402(8) . ?
C35 C36 1.418(9) . ?
C35 H35 0.9300 . ?
C29 C30 1.337(7) . ?
C29 H29 0.9299 . ?
C26 H26 0.9301 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C30 H30 0.9301 . ?
C37 C36 1.328(8) . ?
C37 H37 0.9299 . ?
C34 H34 0.9299 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9599 . ?
C38 H38C 0.9599 . ?
C36 H36 0.9301 . ?

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
N5 Ni1 N5 180.0 2 . ?
N5 Ni1 N3 86.48(9) 2 2 ?
N5 Ni1 N3 93.52(9) . 2 ?
N5 Ni1 N3 93.52(9) 2 . ?
N5 Ni1 N3 86.48(9) . . ?
N3 Ni1 N3 180.0 2 . ?
N5 Ni1 N1 93.73(9) 2 . ?
N5 Ni1 N1 86.27(9) . . ?
N3 Ni1 N1 92.57(9) 2 . ?
N3 Ni1 N1 87.43(9) . . ?
N5 Ni1 N1 86.28(9) 2 2 ?
N5 Ni1 N1 93.73(9) . 2 ?
N3 Ni1 N1 87.43(9) 2 2 ?
N3 Ni1 N1 92.57(9) . 2 ?
N1 Ni1 N1 180.0 . 2 ?
N11 Ni2 N11 180.0 . 2_566 ?
N11 Ni2 N9 86.15(9) . . ?
N11 Ni2 N9 93.85(9) 2_566 . ?
N11 Ni2 N9 93.85(9) . 2_566 ?
N11 Ni2 N9 86.16(9) 2_566 2_566 ?
N9 Ni2 N9 180.0 . 2_566 ?
N11 Ni2 N7 94.00(9) . 2_566 ?
N11 Ni2 N7 86.00(9) 2_566 2_566 ?
N9 Ni2 N7 92.57(8) . 2_566 ?
N9 Ni2 N7 87.43(8) 2_566 2_566 ?
N11 Ni2 N7 86.00(9) . . ?
N11 Ni2 N7 94.00(9) 2_566 . ?
N9 Ni2 N7 87.43(8) . . ?
N9 Ni2 N7 92.57(8) 2_566 . ?
N7 Ni2 N7 180.0 2_566 . ?
C2 P1 C1 85.52(14) . . ?
C16 P5 C15 85.50(13) . . ?
C14 P4 C13 85.59(13) . . ?
C18 P6 C17 85.44(13) . . ?
C6 P3 C5 85.42(14) . . ?
C4 P2 C3 85.72(14) . . ?
C8 C7 C12 116.5(2) . . ?
C8 C7 B1 122.3(2) . . ?
C12 C7 B1 120.4(2) . . ?
C15 N9 N10 110.7(2) . . ?
C15 N9 Ni2 127.58(18) . . ?
N10 N9 Ni2 119.60(16) . . ?
C2 N2 N1 113.3(2) . . ?
C2 N2 B1 128.8(2) . . ?
N1 N2 B1 117.2(2) . . ?
C13 N7 N8 110.8(2) . . ?
C13 N7 Ni2 126.08(18) . . ?
N8 N7 Ni2 121.91(16) . . ?
C14 N8 N7 113.0(2) . . ?
C14 N8 B2 130.1(2) . . ?
N7 N8 B2 116.6(2) . . ?
C17 N11 N12 111.0(2) . . ?
C17 N11 Ni2 130.13(19) . . ?
N12 N11 Ni2 118.76(16) . . ?
C18 N12 N11 112.7(2) . . ?
C18 N12 B2 125.9(2) . . ?
N11 N12 B2 121.4(2) . . ?
C16 N10 N9 113.0(2) . . ?
C16 N10 B2 127.5(2) . . ?
N9 N10 B2 119.0(2) . . ?
C3 N3 N4 110.8(2) . . ?
C3 N3 Ni1 126.46(19) . . ?
N4 N3 Ni1 119.81(17) . . ?
N2 C2 P1 114.4(2) . . ?
N2 C2 H2 122.9 . . ?
P1 C2 H2 122.7 . . ?
C6 N6 N5 112.1(2) . . ?
C6 N6 B1 126.0(2) . . ?
N5 N6 B1 121.9(2) . . ?
C4 N4 N3 112.8(2) . . ?
C4 N4 B1 128.0(2) . . ?
N3 N4 B1 118.4(2) . . ?
N8 C14 P4 114.5(2) . . ?
N8 C14 H14 122.7 . . ?
P4 C14 H14 122.8 . . ?
C9 C8 C7 121.5(3) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.2 . . ?
N12 C18 P6 114.7(2) . . ?
N12 C18 H18 122.7 . . ?
P6 C18 H18 122.7 . . ?
C5 N5 N6 111.2(2) . . ?
C5 N5 Ni1 130.4(2) . . ?
N6 N5 Ni1 118.32(17) . . ?
C1 N1 N2 110.5(2) . . ?
C1 N1 Ni1 126.51(19) . . ?
N2 N1 Ni1 120.68(17) . . ?
C21 C20 C19 122.0(3) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 118.9 . . ?
C23 C24 C19 122.2(3) . . ?
C23 C24 H24 118.9 . . ?
C19 C24 H24 118.9 . . ?
N9 C15 P5 116.2(2) . . ?
N9 C15 H15 121.9 . . ?
P5 C15 H15 121.8 . . ?
N11 C17 P6 116.1(2) . . ?
N11 C17 H17 121.9 . . ?
P6 C17 H17 121.9 . . ?
N7 C13 P4 116.1(2) . . ?
N7 C13 H13 121.9 . . ?
P4 C13 H13 122.1 . . ?
C23 C22 C21 119.3(3) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 120.5(3) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.7 . . ?
C22 C21 C20 120.1(3) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 119.9 . . ?
N3 C3 P2 116.1(2) . . ?
N3 C3 H3 121.9 . . ?
P2 C3 H3 122.0 . . ?
C20 C19 C24 115.8(2) . . ?
C20 C19 B2 123.3(2) . . ?
C24 C19 B2 120.2(2) . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.8 . . ?
C29 C28 C27 120.5(4) . . ?
C29 C28 H28 119.4 . . ?
C27 C28 H28 120.1 . . ?
N4 C4 P2 114.5(2) . . ?
N4 C4 H4 122.8 . . ?
P2 C4 H4 122.7 . . ?
N10 C16 P5 114.6(2) . . ?
N10 C16 H16 122.7 . . ?
P5 C16 H16 122.7 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.7 . . ?
C11 C12 C7 122.0(3) . . ?
C11 C12 H12 119.0 . . ?
C7 C12 H12 119.0 . . ?
N5 C5 P3 116.0(2) . . ?
N5 C5 H5 122.1 . . ?
P3 C5 H5 121.9 . . ?
N1 C1 P1 116.3(2) . . ?
N1 C1 H1 121.9 . . ?
P1 C1 H1 121.8 . . ?
C9 C10 C11 118.9(3) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.6 . . ?
N4 B1 N2 103.1(2) . . ?
N4 B1 N6 109.4(2) . . ?
N2 B1 N6 108.8(2) . . ?
N4 B1 C7 113.4(2) . . ?
N2 B1 C7 114.7(2) . . ?
N6 B1 C7 107.4(2) . . ?
N6 C6 P3 115.2(2) . . ?
N6 C6 H6 122.4 . . ?
P3 C6 H6 122.4 . . ?
N10 B2 N8 103.7(2) . . ?
N10 B2 N12 109.3(2) . . ?
N8 B2 N12 108.0(2) . . ?
N10 B2 C19 112.7(2) . . ?
N8 B2 C19 116.2(2) . . ?
N12 B2 C19 106.9(2) . . ?
C30 C25 C26 118.6(4) . . ?
C30 C25 C31 121.1(4) . . ?
C26 C25 C31 120.3(4) . . ?
C37 C32 C33 118.9(5) . . ?
C37 C32 C38 119.8(5) . . ?
C33 C32 C38 121.3(4) . . ?
C34 C33 C32 122.1(4) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 118.8 . . ?
C28 C27 C26 118.0(4) . . ?
C28 C27 H27 120.7 . . ?
C26 C27 H27 121.3 . . ?
C34 C35 C36 117.4(5) . . ?
C34 C35 H35 120.8 . . ?
C36 C35 H35 121.8 . . ?
C30 C29 C28 120.9(5) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.5 . . ?
C25 C26 C27 119.6(4) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.3 . . ?
C25 C31 H31A 109.5 . . ?
C25 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C25 C31 H31C 109.4 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C30 C25 122.4(4) . . ?
C29 C30 H30 118.8 . . ?
C25 C30 H30 118.7 . . ?
C36 C37 C32 120.9(5) . . ?
C36 C37 H37 119.2 . . ?
C32 C37 H37 119.8 . . ?
C33 C34 C35 118.9(5) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.9 . . ?
C32 C38 H38A 109.3 . . ?
C32 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C32 C38 H38C 109.6 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C36 C35 121.6(5) . . ?
C37 C36 H36 119.6 . . ?
C35 C36 H36 118.7 . . ?

_refine_diff_density_max         0.780
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.083


####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1406797'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 B2 Co N12 P6, C6 H6, B F4, 2(C H Cl3)'
_chemical_formula_sum            'C32 H30 B3 Cl6 Co F4 N12 P6'
_chemical_formula_weight         1148.56

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'
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'
Cl Cl 0.1484 0.1585 '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                   11.2374(5)
_cell_length_b                   17.1902(3)
_cell_length_c                   24.3814(6)
_cell_angle_alpha                90
_cell_angle_beta                 97.463(5)
_cell_angle_gamma                90
_cell_volume                     4669.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    21639
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_F_000             2304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.975
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.164
0 0 1 0.191
0 1 0 0.070
0 -1 0 0.037
1 0 -1 0.040
-1 0 1 0.017
1 1 -1 0.060
-1 1 1 0.036
1 -1 -1 0.044
-1 -1 1 0.028


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            21548
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.178
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5342
_reflns_number_gt                4274
_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       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.1085P)²+74.7900P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5342
_refine_ls_number_parameters     292
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0866
_refine_ls_wR_factor_ref         0.2439
_refine_ls_wR_factor_gt          0.2217
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.144
_refine_ls_shift/su_max          0.000
_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 0.7500 0.2500 0.0000 0.0148(2) Uani 1 2 d S . P . .
P1 P 0.43970(13) 0.11272(10) 0.04804(6) 0.0292(4) Uani 1 1 d . . . . .
P2 P 0.77994(15) 0.45557(8) 0.11409(6) 0.0274(3) Uani 1 1 d . . . . .
P3 P 1.07962(13) 0.13791(10) 0.08868(6) 0.0285(4) Uani 1 1 d . . . . .
Cl3 Cl 0.1922(3) 0.47212(16) 0.08754(9) 0.0719(7) Uani 1 1 d . . . . .
Cl2 Cl 0.2890(3) 0.31769(12) 0.08399(11) 0.0794(8) Uani 1 1 d . . . . .
N2 N 0.6386(4) 0.1822(2) 0.08626(16) 0.0174(8) Uani 1 1 d . . . . .
N6 N 0.8653(4) 0.1847(2) 0.10215(16) 0.0170(8) Uani 1 1 d . . . . .
Cl1 Cl 0.4247(3) 0.4553(2) 0.06179(18) 0.1071(12) Uani 1 1 d . U . . .
N5 N 0.8723(4) 0.1939(3) 0.04722(16) 0.0180(8) Uani 1 1 d . . . . .
N4 N 0.7537(4) 0.3056(2) 0.11155(16) 0.0169(8) Uani 1 1 d . . . . .
N1 N 0.6298(4) 0.1910(3) 0.03034(16) 0.0188(8) Uani 1 1 d . . . . .
N3 N 0.7448(4) 0.3272(2) 0.05707(17) 0.0183(8) Uani 1 1 d . . . . .
C12 C 0.6692(5) 0.2411(3) 0.2189(2) 0.0228(10) Uani 1 1 d . . . . .
H12 H 0.6365 0.2874 0.2040 0.027 Uiso 1 1 d R U . . .
C3 C 0.7541(5) 0.4043(3) 0.0521(2) 0.0226(10) Uani 1 1 d . . . . .
H3 H 0.7474 0.4288 0.0178 0.027 Uiso 1 1 d R U . . .
C2 C 0.5457(5) 0.1424(3) 0.1016(2) 0.0248(11) Uani 1 1 d . . . . .
H2 H 0.5385 0.1320 0.1384 0.030 Uiso 1 1 d R U . . .
B1 B 0.7502(5) 0.2159(3) 0.1248(2) 0.0182(10) Uani 1 1 d . . . . .
C8 C 0.7768(5) 0.1236(3) 0.2104(2) 0.0250(11) Uani 1 1 d . . . . .
H8 H 0.8178 0.0896 0.1898 0.030 Uiso 1 1 d R U . . .
C5 C 0.9773(5) 0.1710(3) 0.0340(2) 0.0216(10) Uani 1 1 d . . . . .
H5 H 0.9954 0.1724 -0.0021 0.026 Uiso 1 1 d R U . . .
C4 C 0.7747(5) 0.3658(3) 0.1460(2) 0.0229(10) Uani 1 1 d . . . . .
H4 H 0.7858 0.3599 0.1843 0.028 Uiso 1 1 d R U . . .
C7 C 0.7363(4) 0.1946(3) 0.1872(2) 0.0196(10) Uani 1 1 d . . . . .
C1 C 0.5304(5) 0.1579(3) 0.0048(2) 0.0228(10) Uani 1 1 d . . . . .
H1 H 0.5109 0.1584 -0.0335 0.027 Uiso 1 1 d R U . . .
C10 C 0.6944(5) 0.1502(4) 0.2941(2) 0.0305(13) Uani 1 1 d . . . . .
H10 H 0.6819 0.1362 0.3298 0.037 Uiso 1 1 d R U . . .
C6 C 0.9679(5) 0.1571(3) 0.1295(2) 0.0232(11) Uani 1 1 d . . . . .
H6 H 0.9783 0.1486 0.1675 0.028 Uiso 1 1 d R U . . .
C11 C 0.6497(5) 0.2202(4) 0.2717(2) 0.0281(12) Uani 1 1 d . . . . .
H11 H 0.6069 0.2530 0.2923 0.034 Uiso 1 1 d R U . . .
C9 C 0.7575(5) 0.1020(4) 0.2636(2) 0.0292(12) Uani 1 1 d . . . . .
H9 H 0.7871 0.0549 0.2784 0.035 Uiso 1 1 d R U . . .
C13 C 0.3217(7) 0.4136(5) 0.1031(3) 0.0487(18) Uani 1 1 d . . . . .
H13 H 0.3515 0.4167 0.1426 0.058 Uiso 1 1 d R U . . .
F2 F 0.3867(8) 0.4160(5) 0.2376(4) 0.117(3) Uani 1 1 d . U . . .
C14 C 0.0000 0.4601(7) 0.2500 0.062(3) Uani 1 2 d DS T P . .
H14 H 0.0000 0.5142 0.2500 0.074 Uiso 1 2 d R U P . .
F1 F 0.5022(8) 0.5017(5) 0.2108(4) 0.125(3) Uani 1 1 d . U . . .
C15 C 0.0680(7) 0.4202(5) 0.2177(3) 0.065(3) Uani 1 1 d D . . . .
H15 H 0.1141 0.4487 0.1959 0.078 Uiso 1 1 d R U . . .
C17 C 0.0000 0.3009(8) 0.2500 0.063(3) Uani 1 2 d DS TU P . .
H17 H 0.0000 0.2468 0.2500 0.076 Uiso 1 2 d R U P . .
B2 B 0.5000 0.4460(7) 0.2500 0.047(3) Uani 1 2 d S T P . .
C16 C 0.0704(7) 0.3406(5) 0.2174(3) 0.082(4) Uani 1 1 d D . . . .
H16 H 0.1181 0.3148 0.1948 0.098 Uiso 1 1 d 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 N1 1.913(4) 7_655 ?
Co1 N1 1.913(4) . ?
Co1 N3 1.930(4) 7_655 ?
Co1 N3 1.930(4) . ?
Co1 N5 1.932(4) . ?
Co1 N5 1.932(4) 7_655 ?
P1 C2 1.726(6) . ?
P1 C1 1.742(5) . ?
P2 C4 1.733(6) . ?
P2 C3 1.741(5) . ?
P3 C6 1.732(6) . ?
P3 C5 1.739(5) . ?
Cl3 C13 1.769(9) . ?
Cl2 C13 1.739(8) . ?
N2 C2 1.340(7) . ?
N2 N1 1.362(6) . ?
N2 B1 1.576(7) . ?
N6 C6 1.342(6) . ?
N6 N5 1.361(5) . ?
N6 B1 1.565(7) . ?
Cl1 C13 1.780(9) . ?
N5 C5 1.322(7) . ?
N4 C4 1.336(7) . ?
N4 N3 1.371(5) . ?
N4 B1 1.577(7) . ?
N1 C1 1.334(7) . ?
N3 C3 1.335(7) . ?
C12 C11 1.382(7) . ?
C12 C7 1.399(7) . ?
C12 H12 0.9300 . ?
C3 H3 0.9301 . ?
C2 H2 0.9301 . ?
B1 C7 1.593(7) . ?
C8 C9 1.391(7) . ?
C8 C7 1.397(7) . ?
C8 H8 0.9300 . ?
C5 H5 0.9299 . ?
C4 H4 0.9300 . ?
C1 H1 0.9299 . ?
C10 C9 1.372(9) . ?
C10 C11 1.388(9) . ?
C10 H10 0.9302 . ?
C6 H6 0.9301 . ?
C11 H11 0.9301 . ?
C9 H9 0.9301 . ?
C13 H13 0.9799 . ?
F2 B2 1.371(9) . ?
C14 C15 1.352(8) . ?
C14 C15 1.352(8) 2 ?
C14 H14 0.9300 . ?
F1 B2 1.355(12) . ?
C15 C16 1.368(8) . ?
C15 H15 0.9300 . ?
C17 C16 1.374(8) 2 ?
C17 C16 1.374(8) . ?
C17 H17 0.9300 . ?
B2 F1 1.355(12) 2_655 ?
B2 F2 1.371(9) 2_655 ?
C16 H16 0.9299 . ?

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
N1 Co1 N1 180.0 7_655 . ?
N1 Co1 N3 89.83(18) 7_655 7_655 ?
N1 Co1 N3 90.17(18) . 7_655 ?
N1 Co1 N3 90.17(18) 7_655 . ?
N1 Co1 N3 89.83(18) . . ?
N3 Co1 N3 180.0(2) 7_655 . ?
N1 Co1 N5 90.66(18) 7_655 . ?
N1 Co1 N5 89.34(18) . . ?
N3 Co1 N5 90.04(18) 7_655 . ?
N3 Co1 N5 89.96(18) . . ?
N1 Co1 N5 89.34(18) 7_655 7_655 ?
N1 Co1 N5 90.66(18) . 7_655 ?
N3 Co1 N5 89.96(18) 7_655 7_655 ?
N3 Co1 N5 90.04(18) . 7_655 ?
N5 Co1 N5 180.0 . 7_655 ?
C2 P1 C1 85.7(3) . . ?
C4 P2 C3 85.8(2) . . ?
C6 P3 C5 85.5(2) . . ?
C2 N2 N1 112.2(4) . . ?
C2 N2 B1 127.5(4) . . ?
N1 N2 B1 120.2(4) . . ?
C6 N6 N5 112.0(4) . . ?
C6 N6 B1 130.0(4) . . ?
N5 N6 B1 117.5(4) . . ?
C5 N5 N6 111.8(4) . . ?
C5 N5 Co1 126.3(3) . . ?
N6 N5 Co1 121.1(3) . . ?
C4 N4 N3 112.6(4) . . ?
C4 N4 B1 129.6(4) . . ?
N3 N4 B1 117.6(4) . . ?
C1 N1 N2 111.6(4) . . ?
C1 N1 Co1 129.5(3) . . ?
N2 N1 Co1 118.9(3) . . ?
C3 N3 N4 111.2(4) . . ?
C3 N3 Co1 127.4(4) . . ?
N4 N3 Co1 120.4(3) . . ?
C11 C12 C7 121.8(5) . . ?
C11 C12 H12 119.0 . . ?
C7 C12 H12 119.2 . . ?
N3 C3 P2 115.4(4) . . ?
N3 C3 H3 122.2 . . ?
P2 C3 H3 122.3 . . ?
N2 C2 P1 115.2(4) . . ?
N2 C2 H2 122.5 . . ?
P1 C2 H2 122.3 . . ?
N6 B1 N2 107.1(4) . . ?
N6 B1 N4 102.7(4) . . ?
N2 B1 N4 106.1(4) . . ?
N6 B1 C7 116.5(4) . . ?
N2 B1 C7 108.4(4) . . ?
N4 B1 C7 115.3(4) . . ?
C9 C8 C7 121.9(5) . . ?
C9 C8 H8 118.8 . . ?
C7 C8 H8 119.2 . . ?
N5 C5 P3 115.7(4) . . ?
N5 C5 H5 122.3 . . ?
P3 C5 H5 122.0 . . ?
N4 C4 P2 114.9(4) . . ?
N4 C4 H4 122.4 . . ?
P2 C4 H4 122.7 . . ?
C8 C7 C12 116.5(5) . . ?
C8 C7 B1 121.4(5) . . ?
C12 C7 B1 121.6(4) . . ?
N1 C1 P1 115.3(4) . . ?
N1 C1 H1 122.6 . . ?
P1 C1 H1 122.1 . . ?
C9 C10 C11 119.7(5) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.0 . . ?
N6 C6 P3 114.9(4) . . ?
N6 C6 H6 122.6 . . ?
P3 C6 H6 122.4 . . ?
C12 C11 C10 120.0(5) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C10 C9 C8 119.9(5) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 120.2 . . ?
Cl2 C13 Cl3 110.1(4) . . ?
Cl2 C13 Cl1 111.1(4) . . ?
Cl3 C13 Cl1 103.1(5) . . ?
Cl2 C13 H13 110.4 . . ?
Cl3 C13 H13 110.2 . . ?
Cl1 C13 H13 111.7 . . ?
C15 C14 C15 119.1(12) . 2 ?
C15 C14 H14 120.5 . . ?
C15 C14 H14 120.5 2 . ?
C14 C15 C16 121.6(9) . . ?
C14 C15 H15 117.7 . . ?
C16 C15 H15 120.7 . . ?
C16 C17 C16 120.4(12) 2 . ?
C16 C17 H17 119.8 2 . ?
C16 C17 H17 119.8 . . ?
F1 B2 F1 90.0(11) 2_655 . ?
F1 B2 F2 102.2(6) 2_655 2_655 ?
F1 B2 F2 108.7(6) . 2_655 ?
F1 B2 F2 108.7(6) 2_655 . ?
F1 B2 F2 102.2(6) . . ?
F2 B2 F2 135.8(13) 2_655 . ?
C15 C16 C17 118.7(9) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 121.7 . . ?

_refine_diff_density_max         3.931
_refine_diff_density_min         -2.021
_refine_diff_density_rms         0.166

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1406798'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H11 B N6 P3 Tl'
_chemical_formula_sum            'C12 H11 B N6 P3 Tl'
_chemical_formula_weight         547.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   9.1440(4)
_cell_length_b                   10.3091(8)
_cell_length_c                   17.5949(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1658.61(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    11619
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024
_exptl_absorpt_coefficient_mu    10.032
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 1 0.127
0 0 -1 0.086
-1 0 0 0.095
1 0 1 0.031
0 -1 0 0.066
0 1 0 0.026


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.304
_exptl_absorpt_correction_T_max  0.444
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11561
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         27.49
_reflns_number_total             1997
_reflns_number_gt                1771
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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     
'calc w=1/[σ²(Fo²)+(0.0187P)²+2.2071P] 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         1997
_refine_ls_number_parameters     118
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0464
_refine_ls_wR_factor_gt          0.0437
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl1 Tl 0.596060(19) 0.2500 0.244360(9) 0.02248(7) Uani 1 2 d S . .
P1 P 0.18848(10) -0.06715(8) 0.34163(5) 0.02513(18) Uani 1 1 d . . .
P2 P 0.37279(15) 0.2500 0.65688(7) 0.0290(3) Uani 1 2 d S . .
N4 N 0.3683(4) 0.2500 0.51013(19) 0.0180(7) Uani 1 2 d S . .
N1 N 0.3990(3) 0.0985(3) 0.31397(14) 0.0197(5) Uani 1 1 d . . .
C5 C 0.5895(5) 0.2500 0.4184(2) 0.0148(8) Uani 1 2 d S . .
N2 N 0.3476(3) 0.1277(3) 0.38467(13) 0.0162(5) Uani 1 1 d . . .
C3 C 0.2102(6) 0.2500 0.6040(3) 0.0274(10) Uani 1 2 d S . .
H3 H 0.1192 0.2500 0.6276 0.033 Uiso 1 2 d SR . .
C6 C 0.6700(3) 0.3664(3) 0.41858(17) 0.0205(6) Uani 1 1 d . . .
H6 H 0.6204 0.4451 0.4172 0.025 Uiso 1 1 d R . .
C2 C 0.2383(3) 0.0495(3) 0.40696(17) 0.0195(6) Uani 1 1 d . . .
H2 H 0.1929 0.0580 0.4540 0.023 Uiso 1 1 d R . .
C7 C 0.8213(3) 0.3659(4) 0.42075(17) 0.0237(7) Uani 1 1 d . . .
H7 H 0.8718 0.4442 0.4213 0.028 Uiso 1 1 d R . .
N3 N 0.2239(4) 0.2500 0.5291(2) 0.0246(8) Uani 1 2 d S . .
C4 C 0.4600(5) 0.2500 0.5702(2) 0.0212(9) Uani 1 2 d S . .
H4 H 0.5613 0.2500 0.5652 0.025 Uiso 1 2 d SR . .
B1 B 0.4155(5) 0.2500 0.4253(3) 0.0165(9) Uani 1 2 d S . .
C1 C 0.3265(3) -0.0004(3) 0.28489(18) 0.0223(7) Uani 1 1 d . . .
H1 H 0.3476 -0.0326 0.2368 0.027 Uiso 1 1 d R . .
C8 C 0.8978(5) 0.2500 0.4224(2) 0.0245(10) Uani 1 2 d S . .
H8 H 0.9995 0.2500 0.4242 0.029 Uiso 1 2 d SR . .


_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
Tl1 N1 2.681(3) . ?
Tl1 N1 2.681(3) 8_565 ?
P1 C2 1.725(3) . ?
P1 C1 1.750(3) . ?
P2 C4 1.721(4) . ?
P2 C3 1.754(5) . ?
N4 C4 1.350(6) . ?
N4 N3 1.363(5) . ?
N4 B1 1.553(5) . ?
N1 C1 1.319(4) . ?
N1 N2 1.363(3) . ?
C5 C6 1.407(4) . ?
C5 C6 1.407(4) 8_565 ?
C5 B1 1.596(6) . ?
N2 C2 1.342(4) . ?
N2 B1 1.577(4) . ?
C3 N3 1.323(6) . ?
C3 H3 0.9300 . ?
C6 C7 1.384(4) . ?
C6 H6 0.9299 . ?
C2 H2 0.9300 . ?
C7 C8 1.385(4) . ?
C7 H7 0.9300 . ?
C4 H4 0.9299 . ?
B1 N2 1.577(4) 8_565 ?
C1 H1 0.9300 . ?
C8 C7 1.385(4) 8_565 ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Tl1 N1 71.26(11) . 8_565 ?
C2 P1 C1 85.14(15) . . ?
C4 P2 C3 85.6(2) . . ?
C4 N4 N3 114.2(3) . . ?
C4 N4 B1 125.4(4) . . ?
N3 N4 B1 120.3(3) . . ?
C1 N1 N2 110.6(3) . . ?
C1 N1 Tl1 127.6(2) . . ?
N2 N1 Tl1 121.31(19) . . ?
C6 C5 C6 116.9(4) . 8_565 ?
C6 C5 B1 121.41(19) . . ?
C6 C5 B1 121.41(19) 8_565 . ?
C2 N2 N1 113.0(3) . . ?
C2 N2 B1 129.8(3) . . ?
N1 N2 B1 117.1(3) . . ?
N3 C3 P2 116.6(4) . . ?
N3 C3 H3 121.9 . . ?
P2 C3 H3 121.4 . . ?
C7 C6 C5 121.3(3) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.2 . . ?
N2 C2 P1 114.9(2) . . ?
N2 C2 H2 122.4 . . ?
P1 C2 H2 122.7 . . ?
C6 C7 C8 120.6(3) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.8 . . ?
C3 N3 N4 109.6(4) . . ?
N4 C4 P2 114.0(3) . . ?
N4 C4 H4 123.0 . . ?
P2 C4 H4 123.1 . . ?
N4 B1 N2 109.0(2) . . ?
N4 B1 N2 109.1(2) . 8_565 ?
N2 B1 N2 106.1(3) . 8_565 ?
N4 B1 C5 110.5(3) . . ?
N2 B1 C5 111.0(2) . . ?
N2 B1 C5 111.0(2) 8_565 . ?
N1 C1 P1 116.4(2) . . ?
N1 C1 H1 121.7 . . ?
P1 C1 H1 121.9 . . ?
C7 C8 C7 119.3(4) 8_565 . ?
C7 C8 H8 120.4 8_565 . ?
C7 C8 H8 120.4 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.125
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1406799'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H11 B Cl3 N6 P3 Ti'
_chemical_formula_sum            'C12 H11 B Cl3 N6 P3 Ti'
_chemical_formula_weight         497.24

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'
P P 0.1023 0.0942 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/m'
_symmetry_space_group_name_Hall  '-P 2yb'

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

_cell_length_a                   8.2810(4)
_cell_length_b                   10.2920(3)
_cell_length_c                   11.4621(10)
_cell_angle_alpha                90
_cell_angle_beta                 102.607(5)
_cell_angle_gamma                90
_cell_volume                     953.34(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    9626
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_absorpt_coefficient_mu    1.131
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-18 0 0 0.122
4 0 0 0.145
0 1 -1 0.094
0 -1 1 0.034
0 -1 -1 0.090
0 1 1 0.025
1 -1 -1 0.135
1 1 -1 0.138


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9590
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2295
_reflns_number_gt                2101
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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     
'calc w=1/[σ²(Fo²)+(0.0209P)²+0.6280P] 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         2295
_refine_ls_number_parameters     133
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0572
_refine_ls_wR_factor_gt          0.0546
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.77224(4) 0.2500 0.40141(3) 0.01374(9) Uani 1 2 d S . .
P2 P 0.97268(5) -0.06997(4) 0.17729(4) 0.02528(10) Uani 1 1 d . . .
Cl1 Cl 1.04482(5) 0.2500 0.48616(4) 0.02063(11) Uani 1 2 d S . .
Cl2 Cl 0.69550(4) 0.08532(4) 0.50350(3) 0.02247(9) Uani 1 1 d . . .
P1 P 0.21511(6) 0.2500 0.19684(5) 0.02230(12) Uani 1 2 d S . .
N2 N 0.51373(19) 0.2500 0.15898(14) 0.0143(3) Uani 1 2 d S . .
N1 N 0.53488(19) 0.2500 0.27989(14) 0.0165(3) Uani 1 2 d S . .
C2 C 0.3532(2) 0.2500 0.10298(17) 0.0181(4) Uani 1 2 d S . .
H2 H 0.3191 0.2500 0.0201 0.022 Uiso 1 2 d SR . .
N4 N 0.77711(13) 0.13030(11) 0.14701(9) 0.0144(2) Uani 1 1 d . . .
N3 N 0.81897(13) 0.11274(11) 0.26818(9) 0.0153(2) Uani 1 1 d . . .
C1 C 0.3896(2) 0.2500 0.31270(18) 0.0215(4) Uani 1 2 d S . .
H1 H 0.3824 0.2500 0.3926 0.026 Uiso 1 2 d SR . .
C5 C 0.5982(2) 0.2500 -0.04482(17) 0.0175(4) Uani 1 2 d S . .
C6 C 0.55770(17) 0.36553(16) -0.10976(13) 0.0226(3) Uani 1 1 d . . .
H6 H 0.5763 0.4445 -0.0696 0.027 Uiso 1 1 d R . .
C4 C 0.85056(17) 0.04393(14) 0.08849(13) 0.0201(3) Uani 1 1 d . . .
H4 H 0.8369 0.0451 0.0058 0.024 Uiso 1 1 d R . .
B1 B 0.6664(2) 0.2500 0.09698(18) 0.0145(4) Uani 1 2 d S . .
C7 C 0.49076(19) 0.36608(18) -0.23190(13) 0.0291(4) Uani 1 1 d . . .
H7 H 0.4682 0.4445 -0.2726 0.035 Uiso 1 1 d R . .
C3 C 0.91799(17) 0.01053(14) 0.29624(13) 0.0201(3) Uani 1 1 d . . .
H3 H 0.9557 -0.0164 0.3749 0.024 Uiso 1 1 d R . .
C8 C 0.4589(3) 0.2500 -0.29320(19) 0.0314(5) Uani 1 2 d S . .
H8 H 0.4151 0.2500 -0.3751 0.038 Uiso 1 2 d SR . .


_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
Ti1 N1 2.1467(16) . ?
Ti1 N3 2.1761(11) . ?
Ti1 N3 2.1761(11) 4_565 ?
Ti1 Cl2 2.2295(4) . ?
Ti1 Cl2 2.2295(4) 4_565 ?
Ti1 Cl1 2.2543(6) . ?
P2 C4 1.7273(15) . ?
P2 C3 1.7378(15) . ?
P1 C2 1.733(2) . ?
P1 C1 1.736(2) . ?
N2 C2 1.344(2) . ?
N2 N1 1.358(2) . ?
N2 B1 1.579(2) . ?
N1 C1 1.337(2) . ?
C2 H2 0.9299 . ?
N4 C4 1.3371(17) . ?
N4 N3 1.3680(15) . ?
N4 B1 1.5679(16) . ?
N3 C3 1.3294(18) . ?
C1 H1 0.9301 . ?
C5 C6 1.4040(18) 4_565 ?
C5 C6 1.4040(18) . ?
C5 B1 1.600(3) . ?
C6 C7 1.389(2) . ?
C6 H6 0.9300 . ?
C4 H4 0.9300 . ?
B1 N4 1.5679(16) 4_565 ?
C7 C8 1.382(2) . ?
C7 H7 0.9300 . ?
C3 H3 0.9300 . ?
C8 C7 1.382(2) 4_565 ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ti1 N3 79.78(4) . . ?
N1 Ti1 N3 79.78(4) . 4_565 ?
N3 Ti1 N3 80.96(6) . 4_565 ?
N1 Ti1 Cl2 90.86(3) . . ?
N3 Ti1 Cl2 89.40(3) . . ?
N3 Ti1 Cl2 167.58(3) 4_565 . ?
N1 Ti1 Cl2 90.86(3) . 4_565 ?
N3 Ti1 Cl2 167.57(3) . 4_565 ?
N3 Ti1 Cl2 89.40(3) 4_565 4_565 ?
Cl2 Ti1 Cl2 98.97(2) . 4_565 ?
N1 Ti1 Cl1 165.58(5) . . ?
N3 Ti1 Cl1 89.29(3) . . ?
N3 Ti1 Cl1 89.29(3) 4_565 . ?
Cl2 Ti1 Cl1 98.461(16) . . ?
Cl2 Ti1 Cl1 98.462(16) 4_565 . ?
C4 P2 C3 85.37(7) . . ?
C2 P1 C1 85.58(9) . . ?
C2 N2 N1 112.41(15) . . ?
C2 N2 B1 126.17(16) . . ?
N1 N2 B1 121.42(14) . . ?
C1 N1 N2 111.31(15) . . ?
C1 N1 Ti1 124.78(13) . . ?
N2 N1 Ti1 123.91(12) . . ?
N2 C2 P1 114.92(14) . . ?
N2 C2 H2 122.5 . . ?
P1 C2 H2 122.6 . . ?
C4 N4 N3 112.29(11) . . ?
C4 N4 B1 129.25(12) . . ?
N3 N4 B1 118.26(12) . . ?
C3 N3 N4 110.87(11) . . ?
C3 N3 Ti1 122.60(9) . . ?
N4 N3 Ti1 125.61(9) . . ?
N1 C1 P1 115.77(15) . . ?
N1 C1 H1 122.1 . . ?
P1 C1 H1 122.1 . . ?
C6 C5 C6 115.74(18) 4_565 . ?
C6 C5 B1 121.94(9) 4_565 . ?
C6 C5 B1 121.94(9) . . ?
C7 C6 C5 122.31(15) . . ?
C7 C6 H6 118.8 . . ?
C5 C6 H6 118.9 . . ?
N4 C4 P2 115.31(10) . . ?
N4 C4 H4 122.4 . . ?
P2 C4 H4 122.3 . . ?
N4 B1 N4 103.58(14) . 4_565 ?
N4 B1 N2 107.29(10) . . ?
N4 B1 N2 107.29(10) 4_565 . ?
N4 B1 C5 114.84(10) . . ?
N4 B1 C5 114.84(10) 4_565 . ?
N2 B1 C5 108.52(15) . . ?
C8 C7 C6 119.93(16) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.1 . . ?
N3 C3 P2 116.11(10) . . ?
N3 C3 H3 122.0 . . ?
P2 C3 H3 121.9 . . ?
C7 C8 C7 119.65(19) 4_565 . ?
C7 C8 H8 120.2 4_565 . ?
C7 C8 H8 120.2 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.061
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1416914'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H11 B Mn N6 O3 P3'
_chemical_formula_sum            'C15 H11 B Mn N6 O3 P3'
_chemical_formula_weight         481.96

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'
O O 0.0106 0.0060 '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'
B B 0.0013 0.0007 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.9620(9)
_cell_length_b                   10.4820(7)
_cell_length_c                   24.6311(14)
_cell_angle_alpha                90
_cell_angle_beta                 112.579(5)
_cell_angle_gamma                90
_cell_volume                     4043.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    29452
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_F_000             1936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_exptl_absorpt_coefficient_mu    0.920
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.147
0 0 -1 0.213
1 0 0 0.158
-2 0 -1 0.119
0 -1 0 0.098
0 1 -1 0.098
0 -1 -1 0.103
0 1 1 0.159
-1 0 1 0.178
1 0 -1 0.251


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            29387
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.139
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             8927
_reflns_number_gt                6447
_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       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0220P)²+6.9083P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8927
_refine_ls_number_parameters     541
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1062
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_restrained_S_all      1.170
_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
Mn2 Mn 0.48172(3) 0.28866(5) 0.15964(2) 0.02911(12) Uani 1 1 d . . . . .
Mn1 Mn -0.00029(3) 0.70615(4) 0.16705(2) 0.02545(11) Uani 1 1 d . . . . .
P2 P 0.11257(5) 0.63811(8) 0.02629(3) 0.02611(17) Uani 1 1 d . . . . .
P4 P 0.61300(5) 0.36239(8) 0.02951(3) 0.02797(17) Uani 1 1 d . . . . .
P3 P -0.15415(5) 1.07402(9) 0.09576(4) 0.03291(19) Uani 1 1 d . . . . .
P6 P 0.34248(5) -0.08945(9) 0.08764(4) 0.0358(2) Uani 1 1 d . . . . .
P1 P 0.24583(7) 0.88566(9) 0.30145(4) 0.0433(2) Uani 1 1 d . . . . .
P5 P 0.72321(7) 0.12356(9) 0.30486(4) 0.0452(3) Uani 1 1 d . . . . .
O4 O 0.33915(16) 0.4393(2) 0.07661(12) 0.0473(6) Uani 1 1 d . U . . .
O1 O 0.09269(19) 0.4687(2) 0.21809(12) 0.0551(7) Uani 1 1 d . U . . .
N12 N 0.48718(14) 0.0282(2) 0.11583(9) 0.0193(5) Uani 1 1 d . . . . .
N7 N 0.54084(14) 0.2895(2) 0.10090(9) 0.0213(5) Uani 1 1 d . . . . .
N6 N -0.00711(14) 0.9664(2) 0.11949(9) 0.0193(5) Uani 1 1 d . . . . .
N2 N 0.13855(14) 0.9036(2) 0.19339(9) 0.0207(5) Uani 1 1 d . . . . .
N4 N 0.08867(13) 0.8139(2) 0.09253(9) 0.0165(4) Uani 1 1 d . . . . .
N5 N -0.05442(14) 0.8765(2) 0.13355(10) 0.0238(5) Uani 1 1 d . . . . .
N3 N 0.04944(13) 0.7089(2) 0.10302(9) 0.0198(5) Uani 1 1 d . . . . .
N10 N 0.62650(15) 0.0997(2) 0.19458(10) 0.0243(5) Uani 1 1 d . . . . .
C107 C 0.62323(16) -0.0609(3) 0.10869(11) 0.0189(5) Uani 1 1 d . . . . .
C112 C 0.61005(17) -0.0807(3) 0.04926(12) 0.0233(6) Uani 1 1 d . . . . .
H112 H 0.5841 -0.0167 0.0222 0.028 Uiso 1 1 d R U . . .
N8 N 0.58477(13) 0.1863(2) 0.09366(9) 0.0187(5) Uani 1 1 d . . . . .
C6 C -0.05041(17) 1.0749(3) 0.09965(12) 0.0236(6) Uani 1 1 d . . . . .
H6 H -0.0264 1.1454 0.0889 0.028 Uiso 1 1 d R U . . .
C7 C 0.12230(16) 1.0639(2) 0.10499(11) 0.0180(5) Uani 1 1 d . . . . .
N1 N 0.10242(16) 0.8159(2) 0.21776(10) 0.0269(5) Uani 1 1 d . . . . .
C111 C 0.63408(19) -0.1919(3) 0.02966(13) 0.0293(6) Uani 1 1 d . . . . .
H111 H 0.6253 -0.2007 -0.0098 0.035 Uiso 1 1 d R U . . .
N11 N 0.43451(15) 0.1158(2) 0.12524(10) 0.0251(5) Uani 1 1 d . . . . .
C109 C 0.68291(19) -0.2761(3) 0.12667(14) 0.0300(7) Uani 1 1 d . . . . .
H109 H 0.7070 -0.3422 0.1530 0.036 Uiso 1 1 d R U . . .
C3 C 0.05554(17) 0.6113(3) 0.07079(12) 0.0234(6) Uani 1 1 d . . . . .
H3 H 0.0308 0.5327 0.0718 0.028 Uiso 1 1 d R U . . .
N9 N 0.58399(17) 0.1846(2) 0.21539(10) 0.0300(6) Uani 1 1 d . . . . .
C113 C 0.3933(2) 0.3792(3) 0.10823(15) 0.0332(7) Uani 1 1 d . U . . .
C103 C 0.6266(2) 0.2036(3) 0.27246(13) 0.0404(8) Uani 1 1 d . . . . .
H103 H 0.6058 0.2571 0.2940 0.048 Uiso 1 1 d R U . . .
C102 C 0.62705(16) 0.2108(3) 0.05875(12) 0.0226(6) Uani 1 1 d . . . . .
H102 H 0.6615 0.1506 0.0509 0.027 Uiso 1 1 d R U . . .
C104 C 0.7012(2) 0.0619(3) 0.23555(13) 0.0312(7) Uani 1 1 d . . . . .
H104 H 0.7381 0.0069 0.2273 0.037 Uiso 1 1 d R U . . .
B1 B 0.08816(18) 0.9392(3) 0.12719(13) 0.0186(6) Uani 1 1 d . . . . .
C11 C 0.12690(19) 1.1935(3) 0.02391(13) 0.0290(6) Uani 1 1 d . . . . .
H11 H 0.1166 1.2010 -0.0159 0.035 Uiso 1 1 d R U . . .
C9 C 0.17632(19) 1.2820(3) 0.11999(14) 0.0304(7) Uani 1 1 d . . . . .
H9 H 0.1989 1.3502 0.1454 0.036 Uiso 1 1 d R U . . .
C108 C 0.65886(18) -0.1647(3) 0.14604(13) 0.0250(6) Uani 1 1 d . . . . .
H108 H 0.6664 -0.1580 0.1854 0.030 Uiso 1 1 d R U . . .
C105 C 0.35712(19) 0.0676(3) 0.11234(14) 0.0323(7) Uani 1 1 d . . . . .
H105 H 0.3133 0.1149 0.1164 0.039 Uiso 1 1 d R U . . .
C8 C 0.15603(17) 1.1693(3) 0.14148(13) 0.0244(6) Uani 1 1 d . . . . .
H8 H 0.1648 1.1640 0.1811 0.029 Uiso 1 1 d R U . . .
C106 C 0.44844(17) -0.0839(3) 0.09679(12) 0.0244(6) Uani 1 1 d . . . . .
H106 H 0.4765 -0.1535 0.0890 0.029 Uiso 1 1 d R U . . .
C5 C -0.13214(19) 0.9191(3) 0.12336(14) 0.0325(7) Uani 1 1 d . . . . .
H5 H -0.1726 0.8697 0.1307 0.039 Uiso 1 1 d R U . . .
C101 C 0.54917(18) 0.3872(3) 0.06937(12) 0.0251(6) Uani 1 1 d . . . . .
H101 H 0.5223 0.4649 0.0686 0.030 Uiso 1 1 d R U . . .
O2 O -0.14710(16) 0.5518(3) 0.09095(13) 0.0507(7) Uani 1 1 d . U . . .
C12 C 0.10627(17) 1.0820(3) 0.04524(12) 0.0237(6) Uani 1 1 d . . . . .
H12 H 0.0805 1.0165 0.0189 0.028 Uiso 1 1 d R U . . .
C2 C 0.21464(19) 0.9456(3) 0.23116(13) 0.0300(7) Uani 1 1 d . . . . .
H2 H 0.2479 1.0027 0.2202 0.036 Uiso 1 1 d R U . . .
C14 C -0.0908(2) 0.6132(3) 0.12007(15) 0.0319(7) Uani 1 1 d . U . . .
C13 C 0.0567(2) 0.5605(3) 0.19792(14) 0.0356(7) Uani 1 1 d . U . . .
C1 C 0.1513(2) 0.8004(3) 0.27419(13) 0.0384(8) Uani 1 1 d . . . . .
H1 H 0.1355 0.7458 0.2980 0.046 Uiso 1 1 d R U . . .
C4 C 0.12618(16) 0.7902(3) 0.05435(11) 0.0216(5) Uani 1 1 d . . . . .
H4 H 0.1572 0.8517 0.0439 0.026 Uiso 1 1 d R U . . .
B2 B 0.58355(18) 0.0613(3) 0.12820(13) 0.0196(6) Uani 1 1 d . . . . .
C10 C 0.16311(19) 1.2939(3) 0.06144(14) 0.0318(7) Uani 1 1 d . . . . .
H10 H 0.1785 1.3684 0.0475 0.038 Uiso 1 1 d R U . . .
C15 C -0.0443(2) 0.7021(3) 0.22298(16) 0.0420(8) Uani 1 1 d . U . . .
O3 O -0.0730(2) 0.6917(3) 0.25793(14) 0.0696(9) Uani 1 1 d . U . . .
C110 C 0.67129(19) -0.2904(3) 0.06840(14) 0.0310(7) Uani 1 1 d . . . . .
H110 H 0.6883 -0.3648 0.0554 0.037 Uiso 1 1 d R U . . .
O6 O 0.3761(5) 0.2777(8) 0.2329(3) 0.051(2) Uani 0.6 1 d . . P A 1
O5 O 0.5643(2) 0.5301(3) 0.21384(15) 0.0804(11) Uani 1 1 d . U . . .
C114 C 0.5320(3) 0.4362(4) 0.19228(16) 0.0489(10) Uani 1 1 d . U . . .
C115 C 0.4169(6) 0.2797(13) 0.2051(4) 0.029(2) Uani 0.6 1 d . U P A 1
O6X O 0.4144(8) 0.3071(13) 0.2516(5) 0.054(3) Uani 0.4 1 d D . P A 2
C15X C 0.4464(8) 0.297(2) 0.2182(6) 0.039(4) Uani 0.4 1 d D U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn2 C15X 1.765(14) . ?
Mn2 C114 1.800(4) . ?
Mn2 C113 1.815(3) . ?
Mn2 C115 1.848(9) . ?
Mn2 N11 2.030(3) . ?
Mn2 N7 2.053(2) . ?
Mn2 N9 2.063(3) . ?
Mn1 C15 1.802(3) . ?
Mn1 C14 1.811(3) . ?
Mn1 C13 1.811(4) . ?
Mn1 N5 2.032(3) . ?
Mn1 N3 2.055(2) . ?
Mn1 N1 2.061(2) . ?
P2 C4 1.717(3) . ?
P2 C3 1.741(3) . ?
P4 C102 1.723(3) . ?
P4 C101 1.738(3) . ?
P3 C6 1.725(3) . ?
P3 C5 1.745(3) . ?
P6 C106 1.724(3) . ?
P6 C105 1.740(4) . ?
P1 C2 1.723(3) . ?
P1 C1 1.731(4) . ?
P5 C104 1.727(3) . ?
P5 C103 1.738(4) . ?
O4 C113 1.140(4) . ?
O1 C13 1.146(4) . ?
N12 C106 1.340(4) . ?
N12 N11 1.362(3) . ?
N12 B2 1.582(4) . ?
N7 C101 1.325(4) . ?
N7 N8 1.364(3) . ?
N6 C6 1.340(4) . ?
N6 N5 1.366(3) . ?
N6 B1 1.579(4) . ?
N2 C2 1.343(4) . ?
N2 N1 1.365(3) . ?
N2 B1 1.568(3) . ?
N4 C4 1.345(3) . ?
N4 N3 1.362(3) . ?
N4 B1 1.568(4) . ?
N5 C5 1.321(4) . ?
N3 C3 1.322(4) . ?
N10 C104 1.341(4) . ?
N10 N9 1.363(3) . ?
N10 B2 1.566(4) . ?
C107 C108 1.403(4) . ?
C107 C112 1.409(4) . ?
C107 B2 1.604(4) . ?
C112 C111 1.382(4) . ?
C112 H112 0.9300 . ?
N8 C102 1.339(3) . ?
N8 B2 1.567(4) . ?
C6 H6 0.9299 . ?
C7 C8 1.401(4) . ?
C7 C12 1.403(4) . ?
C7 B1 1.608(4) . ?
N1 C1 1.327(4) . ?
C111 C110 1.383(4) . ?
C111 H111 0.9302 . ?
N11 C105 1.326(4) . ?
C109 C110 1.380(4) . ?
C109 C108 1.382(4) . ?
C109 H109 0.9301 . ?
C3 H3 0.9300 . ?
N9 C103 1.326(4) . ?
C103 H103 0.9300 . ?
C102 H102 0.9300 . ?
C104 H104 0.9300 . ?
C11 C10 1.380(4) . ?
C11 C12 1.380(4) . ?
C11 H11 0.9301 . ?
C9 C10 1.377(4) . ?
C9 C8 1.391(4) . ?
C9 H9 0.9299 . ?
C108 H108 0.9301 . ?
C105 H105 0.9300 . ?
C8 H8 0.9302 . ?
C106 H106 0.9299 . ?
C5 H5 0.9299 . ?
C101 H101 0.9300 . ?
O2 C14 1.146(4) . ?
C12 H12 0.9301 . ?
C2 H2 0.9300 . ?
C1 H1 0.9301 . ?
C4 H4 0.9299 . ?
C10 H10 0.9299 . ?
C15 O3 1.145(4) . ?
C110 H110 0.9300 . ?
O6 C115 1.145(9) . ?
O5 C114 1.152(5) . ?
O6X C15X 1.150(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15X Mn2 C114 80.9(6) . . ?
C15X Mn2 C113 95.4(6) . . ?
C114 Mn2 C113 89.16(16) . . ?
C114 Mn2 C115 93.6(4) . . ?
C113 Mn2 C115 85.7(4) . . ?
C15X Mn2 N11 100.6(7) . . ?
C114 Mn2 N11 175.37(14) . . ?
C113 Mn2 N11 95.03(13) . . ?
C115 Mn2 N11 88.6(4) . . ?
C15X Mn2 N7 170.9(4) . . ?
C114 Mn2 N7 91.99(15) . . ?
C113 Mn2 N7 90.11(11) . . ?
C115 Mn2 N7 172.9(3) . . ?
N11 Mn2 N7 86.04(9) . . ?
C15X Mn2 N9 86.9(6) . . ?
C114 Mn2 N9 91.36(14) . . ?
C113 Mn2 N9 177.67(12) . . ?
C115 Mn2 N9 96.5(4) . . ?
N11 Mn2 N9 84.37(10) . . ?
N7 Mn2 N9 87.60(9) . . ?
C15 Mn1 C14 88.71(15) . . ?
C15 Mn1 C13 88.29(16) . . ?
C14 Mn1 C13 89.96(15) . . ?
C15 Mn1 N5 94.35(13) . . ?
C14 Mn1 N5 94.21(12) . . ?
C13 Mn1 N5 175.10(12) . . ?
C15 Mn1 N3 179.40(13) . . ?
C14 Mn1 N3 90.80(11) . . ?
C13 Mn1 N3 91.36(12) . . ?
N5 Mn1 N3 86.03(9) . . ?
C15 Mn1 N1 92.97(14) . . ?
C14 Mn1 N1 177.83(12) . . ?
C13 Mn1 N1 91.46(13) . . ?
N5 Mn1 N1 84.30(10) . . ?
N3 Mn1 N1 87.52(9) . . ?
C4 P2 C3 85.27(13) . . ?
C102 P4 C101 85.28(14) . . ?
C6 P3 C5 85.56(14) . . ?
C106 P6 C105 85.44(14) . . ?
C2 P1 C1 85.25(15) . . ?
C104 P5 C103 85.33(15) . . ?
C106 N12 N11 112.6(2) . . ?
C106 N12 B2 126.2(2) . . ?
N11 N12 B2 121.1(2) . . ?
C101 N7 N8 110.5(2) . . ?
C101 N7 Mn2 127.41(19) . . ?
N8 N7 Mn2 121.87(17) . . ?
C6 N6 N5 112.7(2) . . ?
C6 N6 B1 126.1(2) . . ?
N5 N6 B1 121.2(2) . . ?
C2 N2 N1 113.0(2) . . ?
C2 N2 B1 129.6(2) . . ?
N1 N2 B1 117.4(2) . . ?
C4 N4 N3 112.3(2) . . ?
C4 N4 B1 129.7(2) . . ?
N3 N4 B1 118.0(2) . . ?
C5 N5 N6 111.0(2) . . ?
C5 N5 Mn1 129.5(2) . . ?
N6 N5 Mn1 119.44(17) . . ?
C3 N3 N4 110.8(2) . . ?
C3 N3 Mn1 126.87(19) . . ?
N4 N3 Mn1 122.10(16) . . ?
C104 N10 N9 113.1(2) . . ?
C104 N10 B2 129.5(3) . . ?
N9 N10 B2 117.4(2) . . ?
C108 C107 C112 115.1(3) . . ?
C108 C107 B2 123.2(2) . . ?
C112 C107 B2 120.8(2) . . ?
C111 C112 C107 122.5(3) . . ?
C111 C112 H112 118.7 . . ?
C107 C112 H112 118.8 . . ?
C102 N8 N7 112.7(2) . . ?
C102 N8 B2 129.1(2) . . ?
N7 N8 B2 118.1(2) . . ?
N6 C6 P3 114.8(2) . . ?
N6 C6 H6 122.7 . . ?
P3 C6 H6 122.5 . . ?
C8 C7 C12 115.7(2) . . ?
C8 C7 B1 122.3(2) . . ?
C12 C7 B1 121.1(2) . . ?
C1 N1 N2 109.7(3) . . ?
C1 N1 Mn1 127.5(2) . . ?
N2 N1 Mn1 121.82(17) . . ?
C112 C111 C110 120.4(3) . . ?
C112 C111 H111 119.9 . . ?
C110 C111 H111 119.7 . . ?
C105 N11 N12 110.9(2) . . ?
C105 N11 Mn2 129.4(2) . . ?
N12 N11 Mn2 119.57(18) . . ?
C110 C109 C108 120.5(3) . . ?
C110 C109 H109 119.6 . . ?
C108 C109 H109 119.8 . . ?
N3 C3 P2 116.4(2) . . ?
N3 C3 H3 121.9 . . ?
P2 C3 H3 121.7 . . ?
C103 N9 N10 110.2(3) . . ?
C103 N9 Mn2 127.1(2) . . ?
N10 N9 Mn2 121.72(17) . . ?
O4 C113 Mn2 177.9(3) . . ?
N9 C103 P5 116.6(3) . . ?
N9 C103 H103 121.6 . . ?
P5 C103 H103 121.8 . . ?
N8 C102 P4 115.0(2) . . ?
N8 C102 H102 122.6 . . ?
P4 C102 H102 122.4 . . ?
N10 C104 P5 114.6(2) . . ?
N10 C104 H104 122.7 . . ?
P5 C104 H104 122.7 . . ?
N2 B1 N4 104.6(2) . . ?
N2 B1 N6 107.0(2) . . ?
N4 B1 N6 107.8(2) . . ?
N2 B1 C7 115.1(2) . . ?
N4 B1 C7 114.7(2) . . ?
N6 B1 C7 107.3(2) . . ?
C10 C11 C12 120.2(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 120.0 . . ?
C10 C9 C8 120.7(3) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.7 . . ?
C109 C108 C107 122.6(3) . . ?
C109 C108 H108 118.8 . . ?
C107 C108 H108 118.6 . . ?
N11 C105 P6 116.1(2) . . ?
N11 C105 H105 122.0 . . ?
P6 C105 H105 121.9 . . ?
C9 C8 C7 121.7(3) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
N12 C106 P6 115.0(2) . . ?
N12 C106 H106 122.6 . . ?
P6 C106 H106 122.4 . . ?
N5 C5 P3 115.9(2) . . ?
N5 C5 H5 122.1 . . ?
P3 C5 H5 122.0 . . ?
N7 C101 P4 116.5(2) . . ?
N7 C101 H101 121.7 . . ?
P4 C101 H101 121.8 . . ?
C11 C12 C7 122.6(3) . . ?
C11 C12 H12 118.7 . . ?
C7 C12 H12 118.8 . . ?
N2 C2 P1 114.8(2) . . ?
N2 C2 H2 122.6 . . ?
P1 C2 H2 122.6 . . ?
O2 C14 Mn1 178.4(3) . . ?
O1 C13 Mn1 179.2(3) . . ?
N1 C1 P1 117.1(3) . . ?
N1 C1 H1 121.4 . . ?
P1 C1 H1 121.4 . . ?
N4 C4 P2 115.2(2) . . ?
N4 C4 H4 122.4 . . ?
P2 C4 H4 122.3 . . ?
N10 B2 N8 104.7(2) . . ?
N10 B2 N12 106.8(2) . . ?
N8 B2 N12 107.9(2) . . ?
N10 B2 C107 116.0(2) . . ?
N8 B2 C107 114.2(2) . . ?
N12 B2 C107 106.8(2) . . ?
C9 C10 C11 118.9(3) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.6 . . ?
O3 C15 Mn1 175.8(3) . . ?
C109 C110 C111 118.8(3) . . ?
C109 C110 H110 120.7 . . ?
C111 C110 H110 120.5 . . ?
O5 C114 Mn2 179.1(4) . . ?
O6 C115 Mn2 178.0(12) . . ?
O6X C15X Mn2 172.1(14) . . ?

_refine_diff_density_max         0.664
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.073

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1416915'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H23 B N7 P3 Pd'
_chemical_formula_sum            'C21 H23 B N7 P3 Pd'
_chemical_formula_weight         583.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   9.4040(16)
_cell_length_b                   15.931(4)
_cell_length_c                   16.528(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.27(2)
_cell_angle_gamma                90
_cell_volume                     2436.5(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    38818
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    0.983
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.208
-1 0 0 0.138
0 0 -1 0.089
0 0 1 0.058
0 -1 0 0.084
0 1 0 0.145


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38654
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.55
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5531
_reflns_number_gt                4734
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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     
'calc w=1/[σ²(Fo²)+(0.0173P)²+3.0810P] 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         5531
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0641
_refine_ls_wR_factor_gt          0.0545
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.142
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.410311(17) 0.159254(10) 0.011885(10) 0.01576(5) Uani 1 1 d . . .
P1 P -0.05354(6) 0.19123(4) -0.15294(4) 0.02549(13) Uani 1 1 d . . .
P2 P 0.64394(7) 0.32984(4) -0.14705(4) 0.02800(14) Uani 1 1 d . . .
P3 P 0.15913(8) 0.58398(4) -0.06872(5) 0.03743(17) Uani 1 1 d . . .
N2 N 0.20412(19) 0.18906(11) -0.06197(11) 0.0187(4) Uani 1 1 d . . .
N4 N 0.49047(19) 0.24632(11) -0.05763(11) 0.0179(4) Uani 1 1 d . . .
N3 N 0.16814(18) 0.27133(11) -0.07467(11) 0.0177(4) Uani 1 1 d . . .
N5 N 0.42328(19) 0.32193(11) -0.07309(11) 0.0172(4) Uani 1 1 d . . .
N6 N 0.22599(19) 0.42727(11) -0.06551(11) 0.0198(4) Uani 1 1 d . . .
C1 C 0.6028(2) 0.13545(14) 0.08026(14) 0.0211(4) Uani 1 1 d . . .
C2 C 0.6084(2) 0.06159(14) 0.12637(14) 0.0226(5) Uani 1 1 d . . .
N1 N 0.3468(2) 0.06765(12) 0.08981(12) 0.0217(4) Uani 1 1 d . . .
C11 C 0.0369(2) 0.28309(15) -0.11980(14) 0.0228(5) Uani 1 1 d . . .
H11 H -0.0024 0.3361 -0.1321 0.027 Uiso 1 1 d R . .
C13 C 0.4916(2) 0.37245(15) -0.11783(14) 0.0237(5) Uani 1 1 d . . .
H13 H 0.4599 0.4266 -0.1321 0.028 Uiso 1 1 d R . .
C16 C 0.3138(2) 0.33337(13) 0.06165(13) 0.0181(4) Uani 1 1 d . . .
C10 C 0.0990(2) 0.14017(14) -0.10059(14) 0.0223(5) Uani 1 1 d . . .
H10 H 0.1064 0.0819 -0.0992 0.027 Uiso 1 1 d R . .
C3 C 0.7344(3) 0.03800(15) 0.17943(15) 0.0286(5) Uani 1 1 d . . .
H3 H 0.7364 -0.0114 0.2096 0.034 Uiso 1 1 d R . .
C19 C 0.3578(3) 0.33325(16) 0.23438(15) 0.0339(6) Uani 1 1 d . . .
H19 H 0.3724 0.3319 0.2915 0.041 Uiso 1 1 d R . .
N7 N 0.1884(2) 0.44365(13) -0.14765(13) 0.0292(5) Uani 1 1 d . . .
C7 C 0.4732(3) 0.01064(14) 0.11436(15) 0.0254(5) Uani 1 1 d . . .
H7A H 0.4759 -0.0313 0.0721 0.030 Uiso 1 1 d R . .
H7B H 0.4649 -0.0180 0.1651 0.030 Uiso 1 1 d R . .
C8 C 0.3165(3) 0.11213(16) 0.16393(15) 0.0301(5) Uani 1 1 d . . .
H8A H 0.2991 0.0717 0.2041 0.036 Uiso 1 1 d R . .
H8B H 0.2327 0.1470 0.1490 0.036 Uiso 1 1 d R . .
H8C H 0.3979 0.1463 0.1866 0.036 Uiso 1 1 d R . .
C9 C 0.2186(3) 0.01588(16) 0.05665(17) 0.0310(5) Uani 1 1 d . . .
H9A H 0.2031 -0.0247 0.0972 0.037 Uiso 1 1 d R . .
H9B H 0.2346 -0.0126 0.0079 0.037 Uiso 1 1 d R . .
H9C H 0.1352 0.0513 0.0436 0.037 Uiso 1 1 d R . .
C21 C 0.2009(3) 0.31862(15) 0.10416(15) 0.0248(5) Uani 1 1 d . . .
H21 H 0.1090 0.3082 0.0745 0.030 Uiso 1 1 d R . .
C17 C 0.4501(3) 0.34871(15) 0.10887(14) 0.0247(5) Uani 1 1 d . . .
H17 H 0.5279 0.3597 0.0828 0.030 Uiso 1 1 d R . .
C14 C 0.2170(2) 0.49375(14) -0.01658(16) 0.0250(5) Uani 1 1 d . . .
H14 H 0.2399 0.4910 0.0405 0.030 Uiso 1 1 d R . .
C15 C 0.1506(3) 0.52313(16) -0.15816(18) 0.0339(6) Uani 1 1 d . . .
H15 H 0.1209 0.5459 -0.2102 0.041 Uiso 1 1 d R . .
C5 C 0.8518(3) 0.16192(16) 0.14223(17) 0.0322(6) Uani 1 1 d . . .
H5 H 0.9335 0.1958 0.1477 0.039 Uiso 1 1 d R . .
C12 C 0.6058(2) 0.24138(15) -0.09303(14) 0.0226(5) Uani 1 1 d . . .
H12 H 0.6634 0.1936 -0.0890 0.027 Uiso 1 1 d R . .
C18 C 0.4711(3) 0.34848(17) 0.19494(15) 0.0315(6) Uani 1 1 d . . .
H18 H 0.5626 0.3584 0.2254 0.038 Uiso 1 1 d R . .
C6 C 0.7256(3) 0.18630(15) 0.09011(15) 0.0264(5) Uani 1 1 d . . .
H6 H 0.7235 0.2367 0.0615 0.032 Uiso 1 1 d R . .
C20 C 0.2217(3) 0.31955(16) 0.18925(16) 0.0324(6) Uani 1 1 d . . .
H20 H 0.1436 0.3111 0.2158 0.039 Uiso 1 1 d R . .
B1 B 0.2826(3) 0.33929(15) -0.03654(15) 0.0169(4) Uani 1 1 d . . .
C4 C 0.8569(3) 0.08792(17) 0.18650(16) 0.0326(6) Uani 1 1 d . . .
H4 H 0.9418 0.0718 0.2208 0.039 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 1.992(2) . ?
Pd1 N4 2.0300(19) . ?
Pd1 N1 2.102(2) . ?
Pd1 N2 2.1521(19) . ?
P1 C11 1.732(2) . ?
P1 C10 1.739(2) . ?
P2 C13 1.730(2) . ?
P2 C12 1.740(2) . ?
P3 C14 1.714(3) . ?
P3 C15 1.758(3) . ?
N2 C10 1.329(3) . ?
N2 N3 1.361(3) . ?
N4 C12 1.323(3) . ?
N4 N5 1.363(2) . ?
N3 C11 1.336(3) . ?
N3 B1 1.577(3) . ?
N5 C13 1.333(3) . ?
N5 B1 1.573(3) . ?
N6 C14 1.344(3) . ?
N6 N7 1.366(3) . ?
N6 B1 1.545(3) . ?
C1 C6 1.396(3) . ?
C1 C2 1.398(3) . ?
C2 C3 1.394(3) . ?
C2 C7 1.492(3) . ?
N1 C9 1.483(3) . ?
N1 C8 1.486(3) . ?
N1 C7 1.494(3) . ?
C11 H11 0.9299 . ?
C13 H13 0.9299 . ?
C16 C21 1.394(3) . ?
C16 C17 1.398(3) . ?
C16 B1 1.600(3) . ?
C10 H10 0.9301 . ?
C3 C4 1.388(4) . ?
C3 H3 0.9301 . ?
C19 C18 1.366(4) . ?
C19 C20 1.379(4) . ?
C19 H19 0.9300 . ?
N7 C15 1.318(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9601 . ?
C8 H8B 0.9599 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9599 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C21 C20 1.385(3) . ?
C21 H21 0.9300 . ?
C17 C18 1.401(3) . ?
C17 H17 0.9301 . ?
C14 H14 0.9299 . ?
C15 H15 0.9300 . ?
C5 C4 1.384(4) . ?
C5 C6 1.392(3) . ?
C5 H5 0.9300 . ?
C12 H12 0.9299 . ?
C18 H18 0.9300 . ?
C6 H6 0.9300 . ?
C20 H20 0.9300 . ?
C4 H4 0.9299 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 N4 93.41(9) . . ?
C1 Pd1 N1 81.32(9) . . ?
N4 Pd1 N1 174.73(7) . . ?
C1 Pd1 N2 178.21(8) . . ?
N4 Pd1 N2 85.19(7) . . ?
N1 Pd1 N2 100.08(8) . . ?
C11 P1 C10 85.57(11) . . ?
C13 P2 C12 85.28(11) . . ?
C14 P3 C15 85.59(12) . . ?
C10 N2 N3 110.31(18) . . ?
C10 N2 Pd1 131.38(15) . . ?
N3 N2 Pd1 118.31(13) . . ?
C12 N4 N5 111.02(18) . . ?
C12 N4 Pd1 128.75(15) . . ?
N5 N4 Pd1 120.22(13) . . ?
C11 N3 N2 113.62(18) . . ?
C11 N3 B1 128.58(18) . . ?
N2 N3 B1 117.80(16) . . ?
C13 N5 N4 112.59(18) . . ?
C13 N5 B1 128.93(19) . . ?
N4 N5 B1 118.47(17) . . ?
C14 N6 N7 114.49(19) . . ?
C14 N6 B1 125.69(19) . . ?
N7 N6 B1 119.69(18) . . ?
C6 C1 C2 118.3(2) . . ?
C6 C1 Pd1 127.21(17) . . ?
C2 C1 Pd1 114.32(17) . . ?
C3 C2 C1 121.0(2) . . ?
C3 C2 C7 123.1(2) . . ?
C1 C2 C7 115.9(2) . . ?
C9 N1 C8 107.89(19) . . ?
C9 N1 C7 108.51(18) . . ?
C8 N1 C7 109.04(18) . . ?
C9 N1 Pd1 117.44(15) . . ?
C8 N1 Pd1 106.93(14) . . ?
C7 N1 Pd1 106.81(14) . . ?
N3 C11 P1 114.25(17) . . ?
N3 C11 H11 122.8 . . ?
P1 C11 H11 123.0 . . ?
N5 C13 P2 115.04(17) . . ?
N5 C13 H13 122.4 . . ?
P2 C13 H13 122.6 . . ?
C21 C16 C17 116.9(2) . . ?
C21 C16 B1 120.19(19) . . ?
C17 C16 B1 122.7(2) . . ?
N2 C10 P1 116.22(17) . . ?
N2 C10 H10 121.8 . . ?
P1 C10 H10 122.0 . . ?
C4 C3 C2 119.9(2) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.0 . . ?
C18 C19 C20 119.8(2) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.0 . . ?
C15 N7 N6 109.3(2) . . ?
C2 C7 N1 108.88(18) . . ?
C2 C7 H7A 109.8 . . ?
N1 C7 H7A 110.2 . . ?
C2 C7 H7B 109.8 . . ?
N1 C7 H7B 109.7 . . ?
H7A C7 H7B 108.3 . . ?
N1 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.6 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 H9A 109.3 . . ?
N1 C9 H9B 109.6 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C20 C21 C16 121.9(2) . . ?
C20 C21 H21 119.1 . . ?
C16 C21 H21 119.0 . . ?
C16 C17 C18 121.1(2) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.4 . . ?
N6 C14 P3 113.99(18) . . ?
N6 C14 H14 123.0 . . ?
P3 C14 H14 123.0 . . ?
N7 C15 P3 116.6(2) . . ?
N7 C15 H15 121.7 . . ?
P3 C15 H15 121.6 . . ?
C4 C5 C6 120.7(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.7 . . ?
N4 C12 P2 116.05(17) . . ?
N4 C12 H12 122.0 . . ?
P2 C12 H12 121.9 . . ?
C19 C18 C17 120.2(2) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.9 . . ?
C5 C6 C1 120.4(2) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 120.0 . . ?
C19 C20 C21 120.0(2) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 119.9 . . ?
N6 B1 N5 107.91(17) . . ?
N6 B1 N3 109.01(17) . . ?
N5 B1 N3 106.66(17) . . ?
N6 B1 C16 111.02(18) . . ?
N5 B1 C16 111.37(17) . . ?
N3 B1 C16 110.71(18) . . ?
C5 C4 C3 119.6(2) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.078
