# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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. 
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data_raz-01-094c
_database_code_depnum_ccdc_archive 'CCDC 1448199'
_audit_update_record             
;
2016-01-19 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;
_audit_creation_date             2015-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2014-3
_chemical_name_common            tri(dmp-BIAN)Al
_chemical_name_systematic        
"tri(N,N'-bis(3,5-dimethylphenylimino)acenaphthenesemiquinone) aluminum"
_chemical_formula_moiety         'C84 H72 Al1 N6'
_chemical_formula_sum            'C84 H72 Al N6'
_chemical_formula_weight         1192.45
_chemical_melting_point          n/a

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   13.1342(3)
_cell_length_b                   13.1342(3)
_cell_length_c                   72.139(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10777.3(5)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    10704
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      23.8500
_cell_measurement_theta_min      3.0790
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5054.000
_exptl_crystal_size_max          0.2055
_exptl_crystal_size_mid          0.1798
_exptl_crystal_size_min          0.1183
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.897
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            99797
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.883
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.2358
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0193221000
_diffrn_orient_matrix_UB_12      0.0220110000
_diffrn_orient_matrix_UB_13      -0.0090735000
_diffrn_orient_matrix_UB_21      0.0590518000
_diffrn_orient_matrix_UB_22      0.0301957000
_diffrn_orient_matrix_UB_23      0.0031604000
_diffrn_orient_matrix_UB_31      0.0053313000
_diffrn_orient_matrix_UB_32      -0.0498920000
_diffrn_orient_matrix_UB_33      -0.0020941000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1802
_reflns_number_total             2120
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0487
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0862P)²+8.6745P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1499
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C9(H9), C3(H3), C11(H11), C5(H5), C4(H4)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C)

All atoms are refined anisotropically and protons are generated 
in calculated positions and refined using the riding model. A 
421.5 Ang^3 solvent accessible void is present in the unit cell (~3.9%)
that corresponds to a total of 130 electrons. Attempts to model the disordered
THF molecules resulted in an unstable refinement of the model. The solvent mask
routine in OLEX 2 was used to remove this void for the final refinement.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.6667 0.3333 0.0833 0.0208(3) Uani 1 6 d S T P . .
N1 N 0.51776(12) 0.26703(12) 0.06838(2) 0.0244(4) Uani 1 1 d . . . . .
C1 C 0.44260(14) 0.29696(14) 0.07521(2) 0.0243(4) Uani 1 1 d . . . . .
C13 C 0.45748(15) 0.07434(15) 0.05544(2) 0.0302(4) Uani 1 1 d . . . . .
H13 H 0.4575 0.0479 0.0674 0.036 Uiso 1 1 calc R . . . .
C8 C 0.48439(14) 0.18954(15) 0.05273(2) 0.0257(4) Uani 1 1 d . . . . .
C9 C 0.48305(17) 0.22912(17) 0.03496(2) 0.0345(5) Uani 1 1 d . . . . .
H9 H 0.5007 0.3064 0.0331 0.041 Uiso 1 1 calc R . . . .
C2 C 0.32339(15) 0.27096(15) 0.07023(3) 0.0304(4) Uani 1 1 d . . . . .
C7 C 0.29526(19) 0.3333 0.0833 0.0341(6) Uani 1 2 d S T P . .
C3 C 0.24189(17) 0.20478(17) 0.05698(3) 0.0406(5) Uani 1 1 d . . . . .
H3 H 0.2579 0.1632 0.0481 0.049 Uiso 1 1 calc R . . . .
C11 C 0.42989(19) 0.03903(18) 0.02289(3) 0.0442(5) Uani 1 1 d . . . . .
H11 H 0.4120 -0.0113 0.0128 0.053 Uiso 1 1 calc R . . . .
C10 C 0.45538(19) 0.15387(19) 0.01984(3) 0.0428(5) Uani 1 1 d . . . . .
C12 C 0.43038(18) -0.00249(16) 0.04058(3) 0.0379(5) Uani 1 1 d . . . . .
C6 C 0.1885(2) 0.3333 0.0833 0.0484(8) Uani 1 2 d S T P . .
C5 C 0.10599(19) 0.2631(2) 0.06965(4) 0.0615(8) Uani 1 1 d . . . . .
H5 H 0.0331 0.2586 0.0691 0.074 Uiso 1 1 calc R . . . .
C4 C 0.13252(18) 0.2018(2) 0.05719(4) 0.0565(7) Uani 1 1 d . . . . .
H4 H 0.0762 0.1560 0.0484 0.068 Uiso 1 1 calc R . . . .
C15 C 0.4031(3) -0.12698(19) 0.04398(3) 0.0616(7) Uani 1 1 d . . . . .
H15A H 0.4737 -0.1266 0.0476 0.092 Uiso 1 1 calc GR . . . .
H15B H 0.3724 -0.1722 0.0328 0.092 Uiso 1 1 calc GR . . . .
H15C H 0.3459 -0.1613 0.0537 0.092 Uiso 1 1 calc GR . . . .
C14 C 0.4536(3) 0.1967(2) 0.00049(3) 0.0694(8) Uani 1 1 d . . . . .
H14A H 0.3919 0.2155 -0.0005 0.104 Uiso 1 1 calc GR . . . .
H14B H 0.4400 0.1363 -0.0083 0.104 Uiso 1 1 calc GR . . . .
H14C H 0.5278 0.2656 -0.0021 0.104 Uiso 1 1 calc GR . . . .


_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
Al1 N1 2.0111(13) . ?
Al1 N1 2.0112(13) 2_655 ?
Al1 N1 2.0112(13) 3_665 ?
Al1 N1 2.0111(13) 18_654 ?
Al1 N1 2.0111(13) 16_544 ?
Al1 N1 2.0111(13) 17_554 ?
N1 C1 1.327(2) . ?
N1 C8 1.434(2) . ?
C1 C1 1.434(3) 17_554 ?
C1 C2 1.470(2) . ?
C13 C8 1.385(3) . ?
C13 C12 1.391(3) . ?
C8 C9 1.387(2) . ?
C9 C10 1.392(3) . ?
C2 C7 1.416(2) . ?
C2 C3 1.373(3) . ?
C7 C2 1.415(2) 17_554 ?
C7 C6 1.403(4) . ?
C3 C4 1.418(3) . ?
C11 C10 1.389(3) . ?
C11 C12 1.389(3) . ?
C10 C14 1.510(3) . ?
C12 C15 1.509(3) . ?
C6 C5 1.414(3) . ?
C6 C5 1.414(3) 17_554 ?
C5 C4 1.362(4) . ?

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 Al1 N1 93.91(5) . 2_655 ?
N1 Al1 N1 93.91(5) . 3_665 ?
N1 Al1 N1 93.91(5) 2_655 3_665 ?
N1 Al1 N1 173.90(8) . 18_654 ?
N1 Al1 N1 90.70(8) 2_655 18_654 ?
N1 Al1 N1 81.78(8) 3_665 18_654 ?
N1 Al1 N1 90.70(8) . 16_544 ?
N1 Al1 N1 81.78(8) 2_655 16_544 ?
N1 Al1 N1 173.90(8) 3_665 16_544 ?
N1 Al1 N1 93.91(5) 18_654 16_544 ?
N1 Al1 N1 81.78(8) . 17_554 ?
N1 Al1 N1 173.90(8) 2_655 17_554 ?
N1 Al1 N1 90.70(8) 3_665 17_554 ?
N1 Al1 N1 93.91(5) 18_654 17_554 ?
N1 Al1 N1 93.91(5) 16_544 17_554 ?
C1 N1 Al1 112.27(11) . . ?
C1 N1 C8 119.62(14) . . ?
C8 N1 Al1 128.00(11) . . ?
N1 C1 C1 116.84(9) . 17_554 ?
N1 C1 C2 134.75(16) . . ?
C1 C1 C2 108.40(10) 17_554 . ?
C8 C13 C12 121.12(17) . . ?
C13 C8 N1 119.02(15) . . ?
C13 C8 C9 119.71(16) . . ?
C9 C8 N1 121.22(15) . . ?
C8 C9 C10 120.38(18) . . ?
C7 C2 C1 104.96(16) . . ?
C3 C2 C1 136.05(18) . . ?
C3 C2 C7 118.99(18) . . ?
C2 C7 C2 113.2(2) . 17_554 ?
C6 C7 C2 123.39(11) . . ?
C6 C7 C2 123.40(11) . 17_554 ?
C2 C3 C4 118.0(2) . . ?
C12 C11 C10 121.70(18) . . ?
C9 C10 C14 120.5(2) . . ?
C11 C10 C9 118.85(18) . . ?
C11 C10 C14 120.69(19) . . ?
C13 C12 C15 119.79(18) . . ?
C11 C12 C13 118.23(18) . . ?
C11 C12 C15 121.98(18) . . ?
C7 C6 C5 116.09(14) . 17_554 ?
C7 C6 C5 116.09(14) . . ?
C5 C6 C5 127.8(3) . 17_554 ?
C4 C5 C6 120.5(2) . . ?
C5 C4 C3 123.1(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Al1 N1 C1 C1 0.4(2) . . . 17_554 ?
Al1 N1 C1 C2 -178.08(16) . . . . ?
Al1 N1 C8 C13 69.66(19) . . . . ?
Al1 N1 C8 C9 -107.83(17) . . . . ?
N1 C1 C2 C7 -179.15(17) . . . . ?
N1 C1 C2 C3 1.5(4) . . . . ?
N1 C8 C9 C10 177.17(17) . . . . ?
C1 N1 C8 C13 -106.07(18) . . . . ?
C1 N1 C8 C9 76.4(2) . . . . ?
C1 C1 C2 C7 2.2(2) 17_554 . . . ?
C1 C1 C2 C3 -177.1(2) 17_554 . . . ?
C1 C2 C7 C2 -0.83(8) . . . 17_554 ?
C1 C2 C7 C6 179.16(8) . . . . ?
C1 C2 C3 C4 178.9(2) . . . . ?
C13 C8 C9 C10 -0.3(3) . . . . ?
C8 N1 C1 C1 176.80(17) . . . 17_554 ?
C8 N1 C1 C2 -1.7(3) . . . . ?
C8 C13 C12 C11 -0.6(3) . . . . ?
C8 C13 C12 C15 179.2(2) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C8 C9 C10 C14 179.9(2) . . . . ?
C2 C7 C6 C5 2.10(15) 17_554 . . 17_554 ?
C2 C7 C6 C5 -177.89(15) . . . 17_554 ?
C2 C7 C6 C5 -177.91(15) 17_554 . . . ?
C2 C7 C6 C5 2.10(15) . . . . ?
C2 C3 C4 C5 1.3(4) . . . . ?
C7 C2 C3 C4 -0.3(3) . . . . ?
C7 C6 C5 C4 -1.2(3) . . . . ?
C3 C2 C7 C2 178.65(19) . . . 17_554 ?
C3 C2 C7 C6 -1.36(19) . . . . ?
C10 C11 C12 C13 -0.1(3) . . . . ?
C10 C11 C12 C15 -179.8(2) . . . . ?
C12 C13 C8 N1 -176.74(16) . . . . ?
C12 C13 C8 C9 0.8(3) . . . . ?
C12 C11 C10 C9 0.6(3) . . . . ?
C12 C11 C10 C14 -179.7(2) . . . . ?
C6 C5 C4 C3 -0.5(4) . . . . ?
C5 C6 C5 C4 178.8(3) 17_554 . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 67.5 21.6 ?
2 0.000 0.000 0.091 1.4 0.0 ?
3 0.000 0.000 0.409 1.4 0.0 ?
4 0.000 0.000 0.500 67.5 21.6 ?
5 0.000 0.000 0.591 1.4 0.0 ?
6 0.000 0.000 0.909 1.4 0.0 ?
7 0.333 0.667 0.667 67.5 21.6 ?
8 0.333 0.667 0.167 67.5 21.6 ?
9 0.333 0.667 0.576 1.4 0.0 ?
10 0.333 0.667 0.076 1.4 0.0 ?
11 0.333 0.667 0.257 1.4 0.0 ?
12 0.333 0.667 0.757 1.4 0.0 ?
13 0.667 0.333 0.333 67.5 21.6 ?
14 0.667 0.333 0.833 67.5 21.6 ?
15 0.667 0.333 0.243 1.4 0.0 ?
16 0.667 0.333 0.743 1.4 0.0 ?
17 0.667 0.333 0.924 1.4 0.0 ?
18 0.667 0.333 0.424 1.4 0.0 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
15 2 10 0.0886 14.6723 2.1631 10.1055 0.2394 0.9637 -0.0509
3 -8 -91 0.0692 3.0149 -8.0023 -91.0474 0.7082 -0.3513 0.6060
18 -7 -20 0.0653 18.0078 -7.0066 -19.9190 0.3745 0.7889 0.4873
-18 5 20 0.0646 -17.6753 5.3394 19.9150 -0.4047 -0.8196 -0.4023
3 -17 -13 0.0850 2.6607 -16.8382 -13.0497 -0.2008 -0.3926 0.8816
-11 -8 4 0.0829 -10.6766 -7.6657 3.9057 -0.4105 -0.8496 0.3174
13 -17 -24 0.0974 13.3340 -17.1745 -23.9874 0.0973 0.1930 0.9782
-8 18 -23 0.0733 -8.3218 18.1737 -22.9963 0.4479 -0.0153 -0.9029
7 -4 -94 0.0513 6.6862 -3.8356 -94.0101 0.8978 -0.0181 0.4239
-5 7 95 0.0650 -5.3508 6.6692 95.0293 -0.8188 0.1857 -0.5603
-16 0 -7 0.0804 -15.6722 -0.1624 -7.1033 -0.2419 -0.9528 -0.0606
2 15 22 0.0794 1.6715 14.6697 22.0731 0.1549 0.6114 -0.7692
-9 17 -44 0.0689 -8.6519 16.8402 -44.0119 0.6028 -0.1415 -0.7942
-8 -2 83 0.0592 -8.0215 -2.4989 82.9740 -0.9629 -0.2869 -0.0918
-15 17 15 0.0871 -15.0000 16.5082 14.9708 -0.0623 -0.3400 -0.9349
2 -1 100 0.0633 1.9806 -0.5013 100.0520 -0.8806 0.4180 -0.1739


_exptl_crystal_recrystallization_method 'Slow diffusion of THF'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_raz01193e
_database_code_depnum_ccdc_archive 'CCDC 1448200'
_audit_update_record             
;
2016-01-19 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;
_audit_creation_date             2015-12-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2014-3
_chemical_name_common            'tris(dmp-BIAN)Al tri-PF6'
_chemical_name_systematic        
"tri(N,N'-bis(3,5-dimethylphenylimino)acenaphthenequinone) aluminum tri(hexafluorophosphate)"
_chemical_formula_moiety         'C84 H72 Al N6, 3(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C88 H78 Al F18 N8 P3'
_chemical_formula_weight         1709.47
_chemical_melting_point          n/a

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.5661(3)
_cell_length_b                   21.2001(5)
_cell_length_c                   23.1498(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.3886(17)
_cell_angle_gamma                90
_cell_volume                     8127.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    32155
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.4210
_cell_measurement_theta_min      3.0480
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.3083
_exptl_crystal_size_mid          0.2519
_exptl_crystal_size_min          0.2013
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.897
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            238601
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.641
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2358
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0365293000
_diffrn_orient_matrix_UB_12      0.0129595000
_diffrn_orient_matrix_UB_13      -0.0100732000
_diffrn_orient_matrix_UB_21      -0.0173620000
_diffrn_orient_matrix_UB_22      0.0305871000
_diffrn_orient_matrix_UB_23      0.0004734000
_diffrn_orient_matrix_UB_31      0.0141087000
_diffrn_orient_matrix_UB_32      0.0040137000
_diffrn_orient_matrix_UB_33      0.0289338000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11256
_reflns_number_total             14349
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         14349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0493
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0487P)²+10.5205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1298
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(F17A)=Sof(F18A)=Sof(F15A)=Sof(F16A)=1-FVAR(1)
 Sof(F15)=Sof(F16)=Sof(F17)=Sof(F18)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16),
 C18(H18), C22(H22), C24(H24), C26(H26), C32(H32), C33(H33), C34(H34), C36(H36),
  C37(H37), C38(H38), C42(H42), C44(H44), C46(H46), C50(H50), C52(H52),
 C54(H54), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C70(H70),
  C72(H72), C74(H74), C78(H78), C80(H80), C82(H82)
3.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C83(H83A,H83B,H83C),
 C84(H84A,H84B,H84C), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.55851(13) 0.66295(11) 0.31343(9) 0.0218(5) Uani 1 1 d . . . . .
C2 C 0.48023(13) 0.63195(11) 0.29343(9) 0.0210(5) Uani 1 1 d . . . . .
C3 C 0.47513(13) 0.57127(11) 0.32259(9) 0.0235(5) Uani 1 1 d . . . . .
C4 C 0.41934(14) 0.52337(11) 0.32411(10) 0.0289(5) Uani 1 1 d . . . . .
H4 H 0.3725 0.5249 0.3012 0.035 Uiso 1 1 calc R . . . .
C5 C 0.43495(16) 0.47193(12) 0.36119(11) 0.0338(6) Uani 1 1 d . . . . .
H5 H 0.3980 0.4389 0.3619 0.041 Uiso 1 1 calc R . . . .
C6 C 0.50260(15) 0.46871(12) 0.39629(11) 0.0332(6) Uani 1 1 d . . . . .
H6 H 0.5102 0.4341 0.4204 0.040 Uiso 1 1 calc R . . . .
C7 C 0.56119(15) 0.51757(12) 0.39628(10) 0.0281(5) Uani 1 1 d . . . . .
C8 C 0.63339(15) 0.52179(12) 0.43021(11) 0.0329(6) Uani 1 1 d . . . . .
H8 H 0.6458 0.4901 0.4567 0.039 Uiso 1 1 calc R . . . .
C9 C 0.68522(15) 0.57163(13) 0.42471(11) 0.0338(6) Uani 1 1 d . . . . .
H9 H 0.7325 0.5724 0.4472 0.041 Uiso 1 1 calc R . . . .
C10 C 0.66929(15) 0.62155(12) 0.38620(10) 0.0300(5) Uani 1 1 d . . . . .
H10 H 0.7054 0.6549 0.3828 0.036 Uiso 1 1 calc R . . . .
C11 C 0.59870(14) 0.61976(11) 0.35360(9) 0.0236(5) Uani 1 1 d . . . . .
C12 C 0.54598(14) 0.56764(11) 0.35830(9) 0.0240(5) Uani 1 1 d . . . . .
C13 C 0.64477(13) 0.75313(11) 0.31255(10) 0.0247(5) Uani 1 1 d . . . . .
C14 C 0.71564(14) 0.74414(12) 0.28309(10) 0.0295(5) Uani 1 1 d . . . . .
H14 H 0.7186 0.7134 0.2545 0.035 Uiso 1 1 calc R . . . .
C15 C 0.78279(15) 0.78184(13) 0.29685(11) 0.0349(6) Uani 1 1 d . . . . .
C16 C 0.77580(15) 0.82780(13) 0.33907(11) 0.0362(6) Uani 1 1 d . . . . .
H16 H 0.8195 0.8543 0.3469 0.043 Uiso 1 1 calc R . . . .
C17 C 0.70579(16) 0.83557(13) 0.36992(11) 0.0340(6) Uani 1 1 d . . . . .
C18 C 0.63954(14) 0.79715(12) 0.35659(10) 0.0278(5) Uani 1 1 d . . . . .
H18 H 0.5922 0.8010 0.3771 0.033 Uiso 1 1 calc R . . . .
C19 C 0.86012(16) 0.77284(17) 0.26495(14) 0.0513(8) Uani 1 1 d . . . . .
H19A H 0.8823 0.7321 0.2740 0.077 Uiso 1 1 calc GR . . . .
H19B H 0.8980 0.8050 0.2764 0.077 Uiso 1 1 calc GR . . . .
H19C H 0.8492 0.7757 0.2241 0.077 Uiso 1 1 calc GR . . . .
C20 C 0.70068(19) 0.88444(15) 0.41703(13) 0.0506(8) Uani 1 1 d . . . . .
H20A H 0.6714 0.9205 0.4027 0.076 Uiso 1 1 calc GR . . . .
H20B H 0.7542 0.8970 0.4291 0.076 Uiso 1 1 calc GR . . . .
H20C H 0.6732 0.8669 0.4493 0.076 Uiso 1 1 calc GR . . . .
C21 C 0.36066(13) 0.63948(10) 0.23371(10) 0.0220(5) Uani 1 1 d . . . . .
C22 C 0.35689(14) 0.62510(11) 0.17538(10) 0.0256(5) Uani 1 1 d . . . . .
H22 H 0.4033 0.6264 0.1536 0.031 Uiso 1 1 calc R . . . .
C23 C 0.28320(15) 0.60863(11) 0.14946(10) 0.0302(6) Uani 1 1 d . . . . .
C24 C 0.21537(15) 0.60617(12) 0.18366(11) 0.0316(6) Uani 1 1 d . . . . .
H24 H 0.1656 0.5968 0.1663 0.038 Uiso 1 1 calc R . . . .
C25 C 0.21942(14) 0.61721(11) 0.24264(11) 0.0298(5) Uani 1 1 d . . . . .
C26 C 0.29370(14) 0.63443(11) 0.26801(10) 0.0257(5) Uani 1 1 d . . . . .
H26 H 0.2980 0.6424 0.3075 0.031 Uiso 1 1 calc R . . . .
C27 C 0.27746(19) 0.59347(16) 0.08611(12) 0.0488(8) Uani 1 1 d . . . . .
H27A H 0.2638 0.5498 0.0811 0.073 Uiso 1 1 calc GR . . . .
H27B H 0.3285 0.6017 0.0688 0.073 Uiso 1 1 calc GR . . . .
H27C H 0.2365 0.6192 0.0679 0.073 Uiso 1 1 calc GR . . . .
C28 C 0.14611(16) 0.61035(15) 0.27919(13) 0.0446(7) Uani 1 1 d . . . . .
H28A H 0.1550 0.6320 0.3152 0.067 Uiso 1 1 calc GR . . . .
H28B H 0.1364 0.5665 0.2865 0.067 Uiso 1 1 calc GR . . . .
H28C H 0.1001 0.6283 0.2592 0.067 Uiso 1 1 calc GR . . . .
C29 C 0.47734(13) 0.73524(11) 0.12751(9) 0.0226(5) Uani 1 1 d . . . . .
C30 C 0.39715(13) 0.76537(10) 0.14029(9) 0.0215(5) Uani 1 1 d . . . . .
C31 C 0.35299(13) 0.77223(11) 0.08577(9) 0.0234(5) Uani 1 1 d . . . . .
C32 C 0.27979(14) 0.79746(12) 0.06868(10) 0.0280(5) Uani 1 1 d . . . . .
H32 H 0.2460 0.8160 0.0953 0.034 Uiso 1 1 calc R . . . .
C33 C 0.25751(15) 0.79433(12) 0.00962(11) 0.0327(6) Uani 1 1 d . . . . .
H33 H 0.2084 0.8117 -0.0024 0.039 Uiso 1 1 calc R . . . .
C34 C 0.30506(16) 0.76678(13) -0.03068(11) 0.0351(6) Uani 1 1 d . . . . .
H34 H 0.2875 0.7656 -0.0691 0.042 Uiso 1 1 calc R . . . .
C35 C 0.38073(15) 0.73999(12) -0.01470(10) 0.0297(5) Uani 1 1 d . . . . .
C36 C 0.43542(16) 0.70793(14) -0.05041(11) 0.0367(6) Uani 1 1 d . . . . .
H36 H 0.4229 0.7031 -0.0895 0.044 Uiso 1 1 calc R . . . .
C37 C 0.50667(16) 0.68389(14) -0.02829(11) 0.0369(6) Uani 1 1 d . . . . .
H37 H 0.5406 0.6622 -0.0528 0.044 Uiso 1 1 calc R . . . .
C38 C 0.53022(15) 0.69099(13) 0.03022(11) 0.0326(6) Uani 1 1 d . . . . .
H38 H 0.5795 0.6755 0.0441 0.039 Uiso 1 1 calc R . . . .
C39 C 0.47785(14) 0.72158(11) 0.06622(10) 0.0257(5) Uani 1 1 d . . . . .
C40 C 0.40329(14) 0.74463(11) 0.04389(10) 0.0250(5) Uani 1 1 d . . . . .
C41 C 0.60763(13) 0.70379(12) 0.15912(9) 0.0252(5) Uani 1 1 d . . . . .
C42 C 0.62892(14) 0.64320(12) 0.17564(10) 0.0300(5) Uani 1 1 d . . . . .
H42 H 0.5919 0.6172 0.1936 0.036 Uiso 1 1 calc R . . . .
C43 C 0.70693(16) 0.62162(13) 0.16492(12) 0.0388(6) Uani 1 1 d . . . . .
C44 C 0.75984(16) 0.66169(15) 0.13743(12) 0.0426(7) Uani 1 1 d . . . . .
H44 H 0.8117 0.6473 0.1302 0.051 Uiso 1 1 calc R . . . .
C45 C 0.73877(15) 0.72231(14) 0.12025(11) 0.0377(6) Uani 1 1 d . . . . .
C46 C 0.66105(14) 0.74317(13) 0.13180(10) 0.0310(6) Uani 1 1 d . . . . .
H46 H 0.6451 0.7837 0.1211 0.037 Uiso 1 1 calc R . . . .
C47 C 0.7322(2) 0.55639(15) 0.18389(17) 0.0611(9) Uani 1 1 d . . . . .
H47A H 0.7596 0.5588 0.2209 0.092 Uiso 1 1 calc GR . . . .
H47B H 0.7679 0.5387 0.1561 0.092 Uiso 1 1 calc GR . . . .
H47C H 0.6853 0.5301 0.1868 0.092 Uiso 1 1 calc GR . . . .
C48 C 0.79645(18) 0.76414(18) 0.08871(14) 0.0565(9) Uani 1 1 d . . . . .
H48A H 0.8001 0.7502 0.0494 0.085 Uiso 1 1 calc GR . . . .
H48B H 0.8488 0.7621 0.1073 0.085 Uiso 1 1 calc GR . . . .
H48C H 0.7772 0.8068 0.0893 0.085 Uiso 1 1 calc GR . . . .
C49 C 0.31071(13) 0.80862(11) 0.21044(9) 0.0221(5) Uani 1 1 d . . . . .
C50 C 0.23818(14) 0.77626(11) 0.20461(9) 0.0246(5) Uani 1 1 d . . . . .
H50 H 0.2368 0.7362 0.1882 0.029 Uiso 1 1 calc R . . . .
C51 C 0.16760(14) 0.80417(12) 0.22349(10) 0.0281(5) Uani 1 1 d . . . . .
C52 C 0.17218(15) 0.86342(12) 0.24903(11) 0.0324(6) Uani 1 1 d . . . . .
H52 H 0.1254 0.8817 0.2629 0.039 Uiso 1 1 calc R . . . .
C53 C 0.24464(15) 0.89621(12) 0.25447(11) 0.0319(6) Uani 1 1 d . . . . .
C54 C 0.31394(14) 0.86843(11) 0.23400(10) 0.0264(5) Uani 1 1 d . . . . .
H54 H 0.3628 0.8901 0.2361 0.032 Uiso 1 1 calc R . . . .
C55 C 0.08732(15) 0.77140(15) 0.21617(13) 0.0413(7) Uani 1 1 d . . . . .
H55A H 0.0532 0.7952 0.1902 0.062 Uiso 1 1 calc GR . . . .
H55B H 0.0622 0.7682 0.2530 0.062 Uiso 1 1 calc GR . . . .
H55C H 0.0954 0.7299 0.2007 0.062 Uiso 1 1 calc GR . . . .
C56 C 0.25002(19) 0.96023(14) 0.28191(15) 0.0531(8) Uani 1 1 d . . . . .
H56A H 0.2872 0.9588 0.3144 0.080 Uiso 1 1 calc GR . . . .
H56B H 0.1977 0.9726 0.2947 0.080 Uiso 1 1 calc GR . . . .
H56C H 0.2687 0.9902 0.2542 0.080 Uiso 1 1 calc GR . . . .
C57 C 0.50220(13) 0.87561(11) 0.28707(10) 0.0235(5) Uani 1 1 d . . . . .
C58 C 0.45054(13) 0.84315(11) 0.33091(9) 0.0230(5) Uani 1 1 d . . . . .
C59 C 0.43484(14) 0.88827(11) 0.37645(10) 0.0269(5) Uani 1 1 d . . . . .
C60 C 0.39430(15) 0.88670(13) 0.42757(10) 0.0318(6) Uani 1 1 d . . . . .
H60 H 0.3690 0.8501 0.4399 0.038 Uiso 1 1 calc R . . . .
C61 C 0.39240(16) 0.94259(13) 0.46084(12) 0.0384(6) Uani 1 1 d . . . . .
H61 H 0.3662 0.9419 0.4959 0.046 Uiso 1 1 calc R . . . .
C62 C 0.42761(16) 0.99771(14) 0.44345(12) 0.0391(6) Uani 1 1 d . . . . .
H62 H 0.4239 1.0335 0.4664 0.047 Uiso 1 1 calc R . . . .
C63 C 0.46962(15) 1.00081(12) 0.39079(12) 0.0335(6) Uani 1 1 d . . . . .
C64 C 0.50760(16) 1.05430(13) 0.36686(13) 0.0398(7) Uani 1 1 d . . . . .
H64 H 0.5073 1.0925 0.3867 0.048 Uiso 1 1 calc R . . . .
C65 C 0.54498(16) 1.05021(13) 0.31446(13) 0.0399(7) Uani 1 1 d . . . . .
H65 H 0.5685 1.0863 0.2994 0.048 Uiso 1 1 calc R . . . .
C66 C 0.54901(15) 0.99372(12) 0.28290(12) 0.0334(6) Uani 1 1 d . . . . .
H66 H 0.5752 0.9921 0.2478 0.040 Uiso 1 1 calc R . . . .
C67 C 0.51291(14) 0.94066(11) 0.30560(10) 0.0276(5) Uani 1 1 d . . . . .
C68 C 0.47270(14) 0.94515(12) 0.35885(10) 0.0280(5) Uani 1 1 d . . . . .
C69 C 0.57236(14) 0.87122(11) 0.19991(10) 0.0253(5) Uani 1 1 d . . . . .
C70 C 0.65256(14) 0.88458(12) 0.21305(11) 0.0305(6) Uani 1 1 d . . . . .
H70 H 0.6741 0.8755 0.2496 0.037 Uiso 1 1 calc R . . . .
C71 C 0.70059(15) 0.91158(13) 0.17135(12) 0.0357(6) Uani 1 1 d . . . . .
C72 C 0.66651(16) 0.92323(13) 0.11689(11) 0.0367(6) Uani 1 1 d . . . . .
H72 H 0.6986 0.9406 0.0886 0.044 Uiso 1 1 calc R . . . .
C73 C 0.58599(15) 0.90980(13) 0.10328(11) 0.0323(6) Uani 1 1 d . . . . .
C74 C 0.53824(14) 0.88439(11) 0.14600(10) 0.0279(5) Uani 1 1 d . . . . .
H74 H 0.4838 0.8763 0.1385 0.033 Uiso 1 1 calc R . . . .
C75 C 0.78732(17) 0.92824(17) 0.18565(14) 0.0523(8) Uani 1 1 d . . . . .
H75A H 0.8220 0.9071 0.1592 0.079 Uiso 1 1 calc GR . . . .
H75B H 0.8006 0.9151 0.2244 0.079 Uiso 1 1 calc GR . . . .
H75C H 0.7945 0.9730 0.1824 0.079 Uiso 1 1 calc GR . . . .
C76 C 0.55067(18) 0.92026(16) 0.04356(12) 0.0484(8) Uani 1 1 d . . . . .
H76A H 0.5839 0.9494 0.0231 0.073 Uiso 1 1 calc GR . . . .
H76B H 0.4972 0.9373 0.0463 0.073 Uiso 1 1 calc GR . . . .
H76C H 0.5484 0.8808 0.0232 0.073 Uiso 1 1 calc GR . . . .
C77 C 0.37864(14) 0.75256(11) 0.35901(9) 0.0230(5) Uani 1 1 d . . . . .
C78 C 0.41260(15) 0.70881(11) 0.39664(9) 0.0255(5) Uani 1 1 d . . . . .
H78 H 0.4682 0.7029 0.3983 0.031 Uiso 1 1 calc R . . . .
C79 C 0.36302(16) 0.67366(12) 0.43202(10) 0.0313(6) Uani 1 1 d . . . . .
C80 C 0.28046(16) 0.68451(13) 0.42908(11) 0.0351(6) Uani 1 1 d . . . . .
H80 H 0.2469 0.6605 0.4520 0.042 Uiso 1 1 calc R . . . .
C81 C 0.24636(15) 0.73011(13) 0.39306(11) 0.0335(6) Uani 1 1 d . . . . .
C82 C 0.29662(14) 0.76398(12) 0.35688(10) 0.0282(5) Uani 1 1 d . . . . .
H82 H 0.2751 0.7940 0.3316 0.034 Uiso 1 1 calc R . . . .
C83 C 0.3989(2) 0.62503(13) 0.47235(12) 0.0449(7) Uani 1 1 d . . . . .
H83A H 0.3732 0.6275 0.5090 0.067 Uiso 1 1 calc GR . . . .
H83B H 0.4557 0.6328 0.4776 0.067 Uiso 1 1 calc GR . . . .
H83C H 0.3908 0.5838 0.4562 0.067 Uiso 1 1 calc GR . . . .
C84 C 0.15718(17) 0.74357(17) 0.39302(15) 0.0535(8) Uani 1 1 d . . . . .
H84A H 0.1458 0.7732 0.4231 0.080 Uiso 1 1 calc GR . . . .
H84B H 0.1282 0.7051 0.3996 0.080 Uiso 1 1 calc GR . . . .
H84C H 0.1406 0.7609 0.3563 0.080 Uiso 1 1 calc GR . . . .
N1 N 0.57243(11) 0.71869(9) 0.29466(8) 0.0221(4) Uani 1 1 d . . . . .
N2 N 0.43623(11) 0.66417(9) 0.25752(8) 0.0212(4) Uani 1 1 d . . . . .
N3 N 0.52729(11) 0.72730(9) 0.17049(8) 0.0227(4) Uani 1 1 d . . . . .
N4 N 0.38555(11) 0.77954(9) 0.19362(8) 0.0213(4) Uani 1 1 d . . . . .
N5 N 0.52313(11) 0.84242(9) 0.24360(8) 0.0234(4) Uani 1 1 d . . . . .
N6 N 0.43056(11) 0.78580(9) 0.31956(8) 0.0215(4) Uani 1 1 d . . . . .
Al1 Al 0.47935(4) 0.75290(3) 0.24583(3) 0.02085(15) Uani 1 1 d . . . . .
F13 F 0.51857(14) 0.52942(10) 0.13488(11) 0.0841(7) Uani 1 1 d . . . . .
F14 F 0.49604(18) 0.38488(12) 0.16492(14) 0.1155(10) Uani 1 1 d . . . . .
F15 F 0.4395(4) 0.4780(2) 0.1957(3) 0.084(2) Uani 0.591(12) 1 d . . P A 1
F16 F 0.5661(5) 0.4732(7) 0.2087(3) 0.192(5) Uani 0.591(12) 1 d . . P A 1
F17 F 0.5842(4) 0.4393(4) 0.1198(4) 0.105(3) Uani 0.591(12) 1 d . . P A 1
F18 F 0.4502(6) 0.4477(3) 0.1050(4) 0.125(4) Uani 0.591(12) 1 d . . P A 1
P3 P 0.50794(5) 0.45786(4) 0.15244(4) 0.0586(2) Uani 1 1 d . . . . .
F7 F 0.12683(13) 0.71257(15) 0.07172(10) 0.0965(9) Uani 1 1 d . . . . .
F8 F 0.08054(12) 0.74118(11) -0.01745(8) 0.0675(6) Uani 1 1 d . . . . .
F9 F 0.04191(15) 0.64935(10) 0.02225(9) 0.0773(6) Uani 1 1 d . . . . .
F10 F 0.04110(19) 0.79216(10) 0.06160(9) 0.0953(9) Uani 1 1 d . . . . .
F11 F 0.00005(11) 0.70144(9) 0.10138(7) 0.0551(5) Uani 1 1 d . . . . .
F12 F -0.04509(11) 0.72888(11) 0.01283(8) 0.0669(6) Uani 1 1 d . . . . .
P2 P 0.04128(5) 0.72134(4) 0.04218(3) 0.04126(18) Uani 1 1 d . . . . .
F1 F 0.34729(10) 0.95022(9) 0.02438(8) 0.0563(5) Uani 1 1 d . . . . .
F2 F 0.37742(11) 1.03088(11) 0.08440(8) 0.0661(6) Uani 1 1 d . . . . .
F3 F 0.34165(15) 0.93641(13) 0.11980(9) 0.0901(8) Uani 1 1 d . . . . .
F4 F 0.26452(12) 1.03200(9) 0.02904(9) 0.0658(5) Uani 1 1 d . . . . .
F5 F 0.25701(12) 1.02027(11) 0.12559(9) 0.0759(7) Uani 1 1 d . . . . .
F6 F 0.22733(11) 0.93917(9) 0.06570(8) 0.0580(5) Uani 1 1 d . . . . .
P1 P 0.30261(4) 0.98508(4) 0.07585(3) 0.03621(17) Uani 1 1 d . . . . .
C1S C 0.6024(2) 0.10115(18) 0.14755(16) 0.0617(9) Uani 1 1 d . . . . .
C2S C 0.5546(3) 0.0977(2) 0.09492(18) 0.0866(13) Uani 1 1 d . . . . .
H2SA H 0.5877 0.0836 0.0640 0.130 Uiso 1 1 calc GR . . . .
H2SB H 0.5331 0.1386 0.0858 0.130 Uiso 1 1 calc GR . . . .
H2SC H 0.5110 0.0685 0.0998 0.130 Uiso 1 1 calc GR . . . .
N1S N 0.6410(3) 0.1043(2) 0.18807(17) 0.0973(12) Uani 1 1 d . . . . .
C3S C 0.6815(3) 0.5837(2) -0.00106(16) 0.0678(11) Uani 1 1 d . . . . .
C4S C 0.6359(3) 0.5312(2) 0.0183(2) 0.1014(17) Uani 1 1 d . . . . .
H4SA H 0.5979 0.5187 -0.0115 0.152 Uiso 1 1 calc GR . . . .
H4SB H 0.6075 0.5428 0.0523 0.152 Uiso 1 1 calc GR . . . .
H4SC H 0.6717 0.4967 0.0271 0.152 Uiso 1 1 calc GR . . . .
N2S N 0.7156(2) 0.6264(2) -0.01577(19) 0.0974(13) Uani 1 1 d . . . . .
F17A F 0.5249(11) 0.4421(4) 0.0822(5) 0.134(7) Uani 0.409(12) 1 d . . P A 2
F18A F 0.4132(6) 0.4637(7) 0.1298(6) 0.124(4) Uani 0.409(12) 1 d . . P A 2
F15A F 0.4849(11) 0.4729(7) 0.2080(4) 0.163(6) Uani 0.409(12) 1 d . . P A 2
F16A F 0.5956(5) 0.4523(5) 0.1668(11) 0.159(8) Uani 0.409(12) 1 d . . 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
C1 C2 1.516(3) . ?
C1 C11 1.455(3) . ?
C1 N1 1.282(3) . ?
C2 C3 1.456(3) . ?
C2 N2 1.288(3) . ?
C3 C4 1.374(3) . ?
C3 C12 1.421(3) . ?
C4 C5 1.408(3) . ?
C5 C6 1.370(4) . ?
C6 C7 1.419(4) . ?
C7 C8 1.418(3) . ?
C7 C12 1.397(3) . ?
C8 C9 1.369(4) . ?
C9 C10 1.405(3) . ?
C10 C11 1.377(3) . ?
C11 C12 1.414(3) . ?
C13 C14 1.385(3) . ?
C13 C18 1.386(3) . ?
C13 N1 1.455(3) . ?
C14 C15 1.400(3) . ?
C15 C16 1.387(4) . ?
C15 C19 1.506(4) . ?
C16 C17 1.386(4) . ?
C17 C18 1.395(3) . ?
C17 C20 1.508(4) . ?
C21 C22 1.384(3) . ?
C21 C26 1.384(3) . ?
C21 N2 1.453(3) . ?
C22 C23 1.392(3) . ?
C23 C24 1.391(4) . ?
C23 C27 1.502(4) . ?
C24 C25 1.385(4) . ?
C25 C26 1.399(3) . ?
C25 C28 1.504(4) . ?
C29 C30 1.510(3) . ?
C29 C39 1.448(3) . ?
C29 N3 1.290(3) . ?
C30 C31 1.451(3) . ?
C30 N4 1.290(3) . ?
C31 C32 1.375(3) . ?
C31 C40 1.420(3) . ?
C32 C33 1.409(3) . ?
C33 C34 1.367(4) . ?
C34 C35 1.417(4) . ?
C35 C36 1.415(4) . ?
C35 C40 1.402(3) . ?
C36 C37 1.373(4) . ?
C37 C38 1.409(3) . ?
C38 C39 1.380(3) . ?
C39 C40 1.414(3) . ?
C41 C42 1.383(3) . ?
C41 C46 1.381(3) . ?
C41 N3 1.451(3) . ?
C42 C43 1.399(4) . ?
C43 C44 1.386(4) . ?
C43 C47 1.507(4) . ?
C44 C45 1.387(4) . ?
C45 C46 1.393(4) . ?
C45 C48 1.505(4) . ?
C49 C50 1.387(3) . ?
C49 C54 1.381(3) . ?
C49 N4 1.446(3) . ?
C50 C51 1.390(3) . ?
C51 C52 1.390(4) . ?
C51 C55 1.506(3) . ?
C52 C53 1.390(4) . ?
C53 C54 1.384(4) . ?
C53 C56 1.500(4) . ?
C57 C58 1.509(3) . ?
C57 C67 1.454(3) . ?
C57 N5 1.282(3) . ?
C58 C59 1.452(3) . ?
C58 N6 1.286(3) . ?
C59 C60 1.375(3) . ?
C59 C68 1.423(3) . ?
C60 C61 1.414(4) . ?
C61 C62 1.371(4) . ?
C62 C63 1.420(4) . ?
C63 C64 1.416(4) . ?
C63 C68 1.394(4) . ?
C64 C65 1.378(4) . ?
C65 C66 1.405(4) . ?
C66 C67 1.384(3) . ?
C67 C68 1.419(3) . ?
C69 C70 1.385(3) . ?
C69 C74 1.386(3) . ?
C69 N5 1.449(3) . ?
C70 C71 1.389(3) . ?
C71 C72 1.391(4) . ?
C71 C75 1.508(4) . ?
C72 C73 1.393(4) . ?
C73 C74 1.390(3) . ?
C73 C76 1.505(3) . ?
C77 C78 1.383(3) . ?
C77 C82 1.380(3) . ?
C77 N6 1.452(3) . ?
C78 C79 1.391(3) . ?
C79 C80 1.387(4) . ?
C79 C83 1.504(4) . ?
C80 C81 1.388(4) . ?
C81 C82 1.394(3) . ?
C81 C84 1.505(4) . ?
N1 Al1 2.0242(19) . ?
N2 Al1 2.033(2) . ?
N3 Al1 2.0085(19) . ?
N4 Al1 2.0257(19) . ?
N5 Al1 2.033(2) . ?
N6 Al1 2.0297(19) . ?
F13 P3 1.582(2) . ?
F14 P3 1.587(3) . ?
F15 P3 1.590(5) . ?
F16 P3 1.634(6) . ?
F17 P3 1.540(5) . ?
F18 P3 1.456(5) . ?
P3 F17A 1.690(8) . ?
P3 F18A 1.648(9) . ?
P3 F15A 1.389(10) . ?
P3 F16A 1.486(8) . ?
F7 P2 1.570(2) . ?
F8 P2 1.5966(19) . ?
F9 P2 1.594(2) . ?
F10 P2 1.567(2) . ?
F11 P2 1.6023(18) . ?
F12 P2 1.5772(19) . ?
F1 P1 1.5990(18) . ?
F2 P1 1.5831(18) . ?
F3 P1 1.577(2) . ?
F4 P1 1.5902(19) . ?
F5 P1 1.5796(19) . ?
F6 P1 1.5948(18) . ?
C1S C2S 1.440(5) . ?
C1S N1S 1.124(5) . ?
C3S C4S 1.423(7) . ?
C3S N2S 1.124(5) . ?

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
C11 C1 C2 107.29(19) . . ?
N1 C1 C2 117.11(19) . . ?
N1 C1 C11 135.5(2) . . ?
C3 C2 C1 107.47(18) . . ?
N2 C2 C1 115.7(2) . . ?
N2 C2 C3 136.8(2) . . ?
C4 C3 C2 135.3(2) . . ?
C4 C3 C12 119.4(2) . . ?
C12 C3 C2 105.13(19) . . ?
C3 C4 C5 118.3(2) . . ?
C6 C5 C4 122.4(2) . . ?
C5 C6 C7 120.9(2) . . ?
C8 C7 C6 127.9(2) . . ?
C12 C7 C6 116.2(2) . . ?
C12 C7 C8 115.9(2) . . ?
C9 C8 C7 121.3(2) . . ?
C8 C9 C10 122.1(2) . . ?
C11 C10 C9 118.1(2) . . ?
C10 C11 C1 134.6(2) . . ?
C10 C11 C12 119.8(2) . . ?
C12 C11 C1 105.49(19) . . ?
C7 C12 C3 122.7(2) . . ?
C7 C12 C11 122.7(2) . . ?
C11 C12 C3 114.6(2) . . ?
C14 C13 C18 121.6(2) . . ?
C14 C13 N1 119.5(2) . . ?
C18 C13 N1 118.8(2) . . ?
C13 C14 C15 119.2(2) . . ?
C14 C15 C19 119.8(3) . . ?
C16 C15 C14 118.8(2) . . ?
C16 C15 C19 121.4(2) . . ?
C17 C16 C15 122.1(2) . . ?
C16 C17 C18 118.7(2) . . ?
C16 C17 C20 121.1(2) . . ?
C18 C17 C20 120.2(3) . . ?
C13 C18 C17 119.5(2) . . ?
C22 C21 N2 117.9(2) . . ?
C26 C21 C22 121.7(2) . . ?
C26 C21 N2 120.4(2) . . ?
C21 C22 C23 119.6(2) . . ?
C22 C23 C27 120.6(2) . . ?
C24 C23 C22 118.4(2) . . ?
C24 C23 C27 121.0(2) . . ?
C25 C24 C23 122.3(2) . . ?
C24 C25 C26 118.6(2) . . ?
C24 C25 C28 121.2(2) . . ?
C26 C25 C28 120.2(2) . . ?
C21 C26 C25 119.2(2) . . ?
C39 C29 C30 107.61(18) . . ?
N3 C29 C30 117.1(2) . . ?
N3 C29 C39 135.3(2) . . ?
C31 C30 C29 107.43(18) . . ?
N4 C30 C29 116.01(19) . . ?
N4 C30 C31 136.5(2) . . ?
C32 C31 C30 135.4(2) . . ?
C32 C31 C40 119.5(2) . . ?
C40 C31 C30 105.11(19) . . ?
C31 C32 C33 118.0(2) . . ?
C34 C33 C32 122.7(2) . . ?
C33 C34 C35 120.9(2) . . ?
C36 C35 C34 127.9(2) . . ?
C40 C35 C34 116.0(2) . . ?
C40 C35 C36 116.1(2) . . ?
C37 C36 C35 121.1(2) . . ?
C36 C37 C38 122.3(2) . . ?
C39 C38 C37 117.9(2) . . ?
C38 C39 C29 134.8(2) . . ?
C38 C39 C40 119.9(2) . . ?
C40 C39 C29 105.3(2) . . ?
C35 C40 C31 122.9(2) . . ?
C35 C40 C39 122.7(2) . . ?
C39 C40 C31 114.5(2) . . ?
C42 C41 N3 119.8(2) . . ?
C46 C41 C42 121.7(2) . . ?
C46 C41 N3 118.4(2) . . ?
C41 C42 C43 119.0(2) . . ?
C42 C43 C47 120.0(3) . . ?
C44 C43 C42 118.6(3) . . ?
C44 C43 C47 121.4(3) . . ?
C43 C44 C45 122.8(2) . . ?
C44 C45 C46 117.8(3) . . ?
C44 C45 C48 121.8(3) . . ?
C46 C45 C48 120.4(3) . . ?
C41 C46 C45 120.1(2) . . ?
C50 C49 N4 120.6(2) . . ?
C54 C49 C50 121.2(2) . . ?
C54 C49 N4 118.2(2) . . ?
C49 C50 C51 119.5(2) . . ?
C50 C51 C55 121.0(2) . . ?
C52 C51 C50 118.7(2) . . ?
C52 C51 C55 120.2(2) . . ?
C51 C52 C53 121.9(2) . . ?
C52 C53 C56 122.2(2) . . ?
C54 C53 C52 118.5(2) . . ?
C54 C53 C56 119.2(2) . . ?
C49 C54 C53 120.1(2) . . ?
C67 C57 C58 107.5(2) . . ?
N5 C57 C58 116.5(2) . . ?
N5 C57 C67 135.9(2) . . ?
C59 C58 C57 107.6(2) . . ?
N6 C58 C57 116.2(2) . . ?
N6 C58 C59 136.2(2) . . ?
C60 C59 C58 135.1(2) . . ?
C60 C59 C68 119.6(2) . . ?
C68 C59 C58 105.2(2) . . ?
C59 C60 C61 117.8(2) . . ?
C62 C61 C60 122.6(3) . . ?
C61 C62 C63 120.8(2) . . ?
C64 C63 C62 127.2(2) . . ?
C68 C63 C62 116.2(2) . . ?
C68 C63 C64 116.6(2) . . ?
C65 C64 C63 120.5(2) . . ?
C64 C65 C66 122.6(3) . . ?
C67 C66 C65 118.0(2) . . ?
C66 C67 C57 135.2(2) . . ?
C66 C67 C68 119.5(2) . . ?
C68 C67 C57 105.3(2) . . ?
C63 C68 C59 122.9(2) . . ?
C63 C68 C67 122.8(2) . . ?
C67 C68 C59 114.3(2) . . ?
C70 C69 C74 121.6(2) . . ?
C70 C69 N5 119.1(2) . . ?
C74 C69 N5 119.3(2) . . ?
C69 C70 C71 119.6(2) . . ?
C70 C71 C72 118.4(2) . . ?
C70 C71 C75 120.2(2) . . ?
C72 C71 C75 121.4(2) . . ?
C71 C72 C73 122.3(2) . . ?
C72 C73 C76 121.8(2) . . ?
C74 C73 C72 118.5(2) . . ?
C74 C73 C76 119.7(2) . . ?
C69 C74 C73 119.5(2) . . ?
C78 C77 N6 118.9(2) . . ?
C82 C77 C78 121.7(2) . . ?
C82 C77 N6 119.3(2) . . ?
C77 C78 C79 119.6(2) . . ?
C78 C79 C83 120.2(2) . . ?
C80 C79 C78 118.6(2) . . ?
C80 C79 C83 121.3(2) . . ?
C79 C80 C81 122.1(2) . . ?
C80 C81 C82 118.6(2) . . ?
C80 C81 C84 121.2(2) . . ?
C82 C81 C84 120.2(3) . . ?
C77 C82 C81 119.3(2) . . ?
C1 N1 C13 121.33(19) . . ?
C1 N1 Al1 112.25(15) . . ?
C13 N1 Al1 126.17(15) . . ?
C2 N2 C21 121.50(19) . . ?
C2 N2 Al1 112.43(15) . . ?
C21 N2 Al1 125.82(14) . . ?
C29 N3 C41 118.61(19) . . ?
C29 N3 Al1 112.02(15) . . ?
C41 N3 Al1 129.35(14) . . ?
C30 N4 C49 120.38(18) . . ?
C30 N4 Al1 112.10(15) . . ?
C49 N4 Al1 127.47(14) . . ?
C57 N5 C69 118.9(2) . . ?
C57 N5 Al1 112.89(15) . . ?
C69 N5 Al1 128.18(15) . . ?
C58 N6 C77 118.94(19) . . ?
C58 N6 Al1 113.03(15) . . ?
C77 N6 Al1 128.03(15) . . ?
N1 Al1 N2 81.92(8) . . ?
N1 Al1 N4 174.94(8) . . ?
N1 Al1 N5 94.66(8) . . ?
N1 Al1 N6 88.11(8) . . ?
N2 Al1 N5 173.80(8) . . ?
N3 Al1 N1 94.37(8) . . ?
N3 Al1 N2 90.76(8) . . ?
N3 Al1 N4 82.59(8) . . ?
N3 Al1 N5 94.67(8) . . ?
N3 Al1 N6 175.51(8) . . ?
N4 Al1 N2 94.05(8) . . ?
N4 Al1 N5 89.63(8) . . ?
N4 Al1 N6 95.19(8) . . ?
N6 Al1 N2 93.30(8) . . ?
N6 Al1 N5 81.38(8) . . ?
F13 P3 F14 175.57(18) . . ?
F13 P3 F15 89.4(2) . . ?
F13 P3 F16 86.9(5) . . ?
F13 P3 F17A 85.4(3) . . ?
F13 P3 F18A 87.5(5) . . ?
F14 P3 F15 93.0(2) . . ?
F14 P3 F16 97.1(5) . . ?
F14 P3 F17A 90.4(3) . . ?
F14 P3 F18A 90.6(5) . . ?
F15 P3 F16 81.9(4) . . ?
F17 P3 F13 91.2(3) . . ?
F17 P3 F14 87.0(3) . . ?
F17 P3 F15 170.0(5) . . ?
F17 P3 F16 88.1(4) . . ?
F18 P3 F13 91.3(3) . . ?
F18 P3 F14 84.9(3) . . ?
F18 P3 F15 92.8(4) . . ?
F18 P3 F16 174.5(5) . . ?
F18 P3 F17 97.1(5) . . ?
F18A P3 F17A 83.5(7) . . ?
F15A P3 F13 93.0(6) . . ?
F15A P3 F14 91.0(6) . . ?
F15A P3 F17A 173.2(9) . . ?
F15A P3 F18A 89.8(7) . . ?
F15A P3 F16A 95.7(10) . . ?
F16A P3 F13 91.1(5) . . ?
F16A P3 F14 90.4(5) . . ?
F16A P3 F17A 90.9(8) . . ?
F16A P3 F18A 174.3(10) . . ?
F7 P2 F8 91.46(12) . . ?
F7 P2 F9 90.03(15) . . ?
F7 P2 F11 89.73(12) . . ?
F7 P2 F12 178.95(15) . . ?
F8 P2 F11 178.80(11) . . ?
F9 P2 F8 89.78(12) . . ?
F9 P2 F11 90.08(11) . . ?
F10 P2 F7 89.80(16) . . ?
F10 P2 F8 89.96(12) . . ?
F10 P2 F9 179.69(16) . . ?
F10 P2 F11 90.18(12) . . ?
F10 P2 F12 91.06(14) . . ?
F12 P2 F8 89.14(11) . . ?
F12 P2 F9 89.11(13) . . ?
F12 P2 F11 89.67(10) . . ?
F2 P1 F1 90.09(10) . . ?
F2 P1 F4 89.89(12) . . ?
F2 P1 F6 178.71(11) . . ?
F3 P1 F1 89.32(13) . . ?
F3 P1 F2 90.74(13) . . ?
F3 P1 F4 177.22(14) . . ?
F3 P1 F5 91.99(14) . . ?
F3 P1 F6 90.16(13) . . ?
F4 P1 F1 87.97(11) . . ?
F4 P1 F6 89.17(11) . . ?
F5 P1 F1 178.61(13) . . ?
F5 P1 F2 90.34(11) . . ?
F5 P1 F4 90.72(13) . . ?
F5 P1 F6 90.55(10) . . ?
F6 P1 F1 89.00(10) . . ?
N1S C1S C2S 178.7(5) . . ?
N2S C3S C4S 177.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 177.5(3) . . . . ?
C1 C2 C3 C12 0.9(2) . . . . ?
C1 C2 N2 C21 178.42(18) . . . . ?
C1 C2 N2 Al1 -7.1(2) . . . . ?
C1 C11 C12 C3 2.5(3) . . . . ?
C1 C11 C12 C7 -175.7(2) . . . . ?
C2 C1 C11 C10 -178.6(3) . . . . ?
C2 C1 C11 C12 -1.8(2) . . . . ?
C2 C1 N1 C13 178.31(19) . . . . ?
C2 C1 N1 Al1 3.7(2) . . . . ?
C2 C3 C4 C5 -176.6(2) . . . . ?
C2 C3 C12 C7 176.0(2) . . . . ?
C2 C3 C12 C11 -2.1(3) . . . . ?
C3 C2 N2 C21 -2.9(4) . . . . ?
C3 C2 N2 Al1 171.6(2) . . . . ?
C3 C4 C5 C6 1.3(4) . . . . ?
C4 C3 C12 C7 -1.3(4) . . . . ?
C4 C3 C12 C11 -179.4(2) . . . . ?
C4 C5 C6 C7 -0.7(4) . . . . ?
C5 C6 C7 C8 179.1(3) . . . . ?
C5 C6 C7 C12 -0.8(4) . . . . ?
C6 C7 C8 C9 178.8(3) . . . . ?
C6 C7 C12 C3 1.8(3) . . . . ?
C6 C7 C12 C11 179.8(2) . . . . ?
C7 C8 C9 C10 1.1(4) . . . . ?
C8 C7 C12 C3 -178.2(2) . . . . ?
C8 C7 C12 C11 -0.2(3) . . . . ?
C8 C9 C10 C11 0.5(4) . . . . ?
C9 C10 C11 C1 174.6(2) . . . . ?
C9 C10 C11 C12 -1.9(4) . . . . ?
C10 C11 C12 C3 179.9(2) . . . . ?
C10 C11 C12 C7 1.8(4) . . . . ?
C11 C1 C2 C3 0.6(2) . . . . ?
C11 C1 C2 N2 179.60(19) . . . . ?
C11 C1 N1 C13 2.1(4) . . . . ?
C11 C1 N1 Al1 -172.5(2) . . . . ?
C12 C3 C4 C5 -0.3(3) . . . . ?
C12 C7 C8 C9 -1.3(4) . . . . ?
C13 C14 C15 C16 -1.0(4) . . . . ?
C13 C14 C15 C19 -179.7(2) . . . . ?
C14 C13 C18 C17 3.1(4) . . . . ?
C14 C13 N1 C1 85.8(3) . . . . ?
C14 C13 N1 Al1 -100.4(2) . . . . ?
C14 C15 C16 C17 3.1(4) . . . . ?
C15 C16 C17 C18 -2.1(4) . . . . ?
C15 C16 C17 C20 177.9(3) . . . . ?
C16 C17 C18 C13 -1.0(4) . . . . ?
C18 C13 C14 C15 -2.1(4) . . . . ?
C18 C13 N1 C1 -98.1(3) . . . . ?
C18 C13 N1 Al1 75.7(2) . . . . ?
C19 C15 C16 C17 -178.2(3) . . . . ?
C20 C17 C18 C13 179.0(2) . . . . ?
C21 C22 C23 C24 -1.0(3) . . . . ?
C21 C22 C23 C27 179.4(2) . . . . ?
C22 C21 C26 C25 -3.0(3) . . . . ?
C22 C21 N2 C2 -111.8(2) . . . . ?
C22 C21 N2 Al1 74.5(2) . . . . ?
C22 C23 C24 C25 -2.4(4) . . . . ?
C23 C24 C25 C26 3.2(4) . . . . ?
C23 C24 C25 C28 -176.2(2) . . . . ?
C24 C25 C26 C21 -0.4(3) . . . . ?
C26 C21 C22 C23 3.8(3) . . . . ?
C26 C21 N2 C2 72.1(3) . . . . ?
C26 C21 N2 Al1 -101.7(2) . . . . ?
C27 C23 C24 C25 177.1(3) . . . . ?
C28 C25 C26 C21 179.0(2) . . . . ?
C29 C30 C31 C32 -177.4(3) . . . . ?
C29 C30 C31 C40 2.7(2) . . . . ?
C29 C30 N4 C49 179.97(19) . . . . ?
C29 C30 N4 Al1 -2.5(2) . . . . ?
C29 C39 C40 C31 -0.4(3) . . . . ?
C29 C39 C40 C35 -179.8(2) . . . . ?
C30 C29 C39 C38 -174.6(3) . . . . ?
C30 C29 C39 C40 2.1(2) . . . . ?
C30 C29 N3 C41 -174.51(19) . . . . ?
C30 C29 N3 Al1 4.0(2) . . . . ?
C30 C31 C32 C33 -179.5(3) . . . . ?
C30 C31 C40 C35 177.9(2) . . . . ?
C30 C31 C40 C39 -1.5(3) . . . . ?
C31 C30 N4 C49 2.2(4) . . . . ?
C31 C30 N4 Al1 179.8(2) . . . . ?
C31 C32 C33 C34 0.8(4) . . . . ?
C32 C31 C40 C35 -2.0(4) . . . . ?
C32 C31 C40 C39 178.6(2) . . . . ?
C32 C33 C34 C35 -0.5(4) . . . . ?
C33 C34 C35 C36 177.5(3) . . . . ?
C33 C34 C35 C40 -1.0(4) . . . . ?
C34 C35 C36 C37 -179.4(3) . . . . ?
C34 C35 C40 C31 2.2(4) . . . . ?
C34 C35 C40 C39 -178.4(2) . . . . ?
C35 C36 C37 C38 -1.6(4) . . . . ?
C36 C35 C40 C31 -176.4(2) . . . . ?
C36 C35 C40 C39 3.0(4) . . . . ?
C36 C37 C38 C39 2.1(4) . . . . ?
C37 C38 C39 C29 176.2(3) . . . . ?
C37 C38 C39 C40 0.0(4) . . . . ?
C38 C39 C40 C31 176.9(2) . . . . ?
C38 C39 C40 C35 -2.5(4) . . . . ?
C39 C29 C30 C31 -3.0(2) . . . . ?
C39 C29 C30 N4 178.6(2) . . . . ?
C39 C29 N3 C41 6.0(4) . . . . ?
C39 C29 N3 Al1 -175.5(2) . . . . ?
C40 C31 C32 C33 0.4(3) . . . . ?
C40 C35 C36 C37 -0.9(4) . . . . ?
C41 C42 C43 C44 -0.8(4) . . . . ?
C41 C42 C43 C47 178.4(3) . . . . ?
C42 C41 C46 C45 -0.1(4) . . . . ?
C42 C41 N3 C29 -109.2(3) . . . . ?
C42 C41 N3 Al1 72.6(3) . . . . ?
C42 C43 C44 C45 0.2(4) . . . . ?
C43 C44 C45 C46 0.4(4) . . . . ?
C43 C44 C45 C48 -178.0(3) . . . . ?
C44 C45 C46 C41 -0.5(4) . . . . ?
C46 C41 C42 C43 0.7(4) . . . . ?
C46 C41 N3 C29 70.8(3) . . . . ?
C46 C41 N3 Al1 -107.4(2) . . . . ?
C47 C43 C44 C45 -179.0(3) . . . . ?
C48 C45 C46 C41 177.9(3) . . . . ?
C49 C50 C51 C52 -1.5(3) . . . . ?
C49 C50 C51 C55 178.0(2) . . . . ?
C50 C49 C54 C53 2.6(3) . . . . ?
C50 C49 N4 C30 64.7(3) . . . . ?
C50 C49 N4 Al1 -112.4(2) . . . . ?
C50 C51 C52 C53 2.1(4) . . . . ?
C51 C52 C53 C54 -0.4(4) . . . . ?
C51 C52 C53 C56 179.9(3) . . . . ?
C52 C53 C54 C49 -2.0(4) . . . . ?
C54 C49 C50 C51 -0.8(3) . . . . ?
C54 C49 N4 C30 -117.2(2) . . . . ?
C54 C49 N4 Al1 65.6(3) . . . . ?
C55 C51 C52 C53 -177.4(2) . . . . ?
C56 C53 C54 C49 177.7(2) . . . . ?
C57 C58 C59 C60 -178.2(3) . . . . ?
C57 C58 C59 C68 2.2(2) . . . . ?
C57 C58 N6 C77 -177.95(18) . . . . ?
C57 C58 N6 Al1 2.6(2) . . . . ?
C57 C67 C68 C59 -1.1(3) . . . . ?
C57 C67 C68 C63 179.7(2) . . . . ?
C58 C57 C67 C66 -175.6(3) . . . . ?
C58 C57 C67 C68 2.5(2) . . . . ?
C58 C57 N5 C69 179.63(18) . . . . ?
C58 C57 N5 Al1 0.2(2) . . . . ?
C58 C59 C60 C61 -179.7(3) . . . . ?
C58 C59 C68 C63 178.4(2) . . . . ?
C58 C59 C68 C67 -0.7(3) . . . . ?
C59 C58 N6 C77 0.5(4) . . . . ?
C59 C58 N6 Al1 -179.0(2) . . . . ?
C59 C60 C61 C62 1.4(4) . . . . ?
C60 C59 C68 C63 -1.2(4) . . . . ?
C60 C59 C68 C67 179.7(2) . . . . ?
C60 C61 C62 C63 -1.2(4) . . . . ?
C61 C62 C63 C64 178.8(3) . . . . ?
C61 C62 C63 C68 -0.2(4) . . . . ?
C62 C63 C64 C65 -178.8(3) . . . . ?
C62 C63 C68 C59 1.4(3) . . . . ?
C62 C63 C68 C67 -179.5(2) . . . . ?
C63 C64 C65 C66 -1.3(4) . . . . ?
C64 C63 C68 C59 -177.7(2) . . . . ?
C64 C63 C68 C67 1.3(4) . . . . ?
C64 C65 C66 C67 0.8(4) . . . . ?
C65 C66 C67 C57 178.6(3) . . . . ?
C65 C66 C67 C68 0.8(3) . . . . ?
C66 C67 C68 C59 177.3(2) . . . . ?
C66 C67 C68 C63 -1.9(4) . . . . ?
C67 C57 C58 C59 -3.0(2) . . . . ?
C67 C57 C58 N6 175.87(19) . . . . ?
C67 C57 N5 C69 2.7(4) . . . . ?
C67 C57 N5 Al1 -176.8(2) . . . . ?
C68 C59 C60 C61 -0.2(3) . . . . ?
C68 C63 C64 C65 0.2(4) . . . . ?
C69 C70 C71 C72 -1.3(4) . . . . ?
C69 C70 C71 C75 178.1(3) . . . . ?
C70 C69 C74 C73 2.1(4) . . . . ?
C70 C69 N5 C57 71.4(3) . . . . ?
C70 C69 N5 Al1 -109.2(2) . . . . ?
C70 C71 C72 C73 1.1(4) . . . . ?
C71 C72 C73 C74 0.6(4) . . . . ?
C71 C72 C73 C76 -177.6(3) . . . . ?
C72 C73 C74 C69 -2.2(4) . . . . ?
C74 C69 C70 C71 -0.3(4) . . . . ?
C74 C69 N5 C57 -108.9(3) . . . . ?
C74 C69 N5 Al1 70.5(3) . . . . ?
C75 C71 C72 C73 -178.2(3) . . . . ?
C76 C73 C74 C69 176.0(3) . . . . ?
C77 C78 C79 C80 -1.1(3) . . . . ?
C77 C78 C79 C83 178.8(2) . . . . ?
C78 C77 C82 C81 -0.7(4) . . . . ?
C78 C77 N6 C58 -103.0(2) . . . . ?
C78 C77 N6 Al1 76.3(2) . . . . ?
C78 C79 C80 C81 -1.5(4) . . . . ?
C79 C80 C81 C82 3.0(4) . . . . ?
C79 C80 C81 C84 -176.5(3) . . . . ?
C80 C81 C82 C77 -1.8(4) . . . . ?
C82 C77 C78 C79 2.2(3) . . . . ?
C82 C77 N6 C58 78.9(3) . . . . ?
C82 C77 N6 Al1 -101.8(2) . . . . ?
C83 C79 C80 C81 178.6(2) . . . . ?
C84 C81 C82 C77 177.7(2) . . . . ?
N1 C1 C2 C3 -176.65(19) . . . . ?
N1 C1 C2 N2 2.4(3) . . . . ?
N1 C1 C11 C10 -2.1(5) . . . . ?
N1 C1 C11 C12 174.7(3) . . . . ?
N1 C13 C14 C15 173.9(2) . . . . ?
N1 C13 C18 C17 -172.9(2) . . . . ?
N2 C2 C3 C4 -1.2(5) . . . . ?
N2 C2 C3 C12 -177.9(3) . . . . ?
N2 C21 C22 C23 -172.3(2) . . . . ?
N2 C21 C26 C25 172.9(2) . . . . ?
N3 C29 C30 C31 177.3(2) . . . . ?
N3 C29 C30 N4 -1.1(3) . . . . ?
N3 C29 C39 C38 5.0(5) . . . . ?
N3 C29 C39 C40 -178.4(3) . . . . ?
N3 C41 C42 C43 -179.3(2) . . . . ?
N3 C41 C46 C45 179.9(2) . . . . ?
N4 C30 C31 C32 0.5(5) . . . . ?
N4 C30 C31 C40 -179.4(3) . . . . ?
N4 C49 C50 C51 177.1(2) . . . . ?
N4 C49 C54 C53 -175.4(2) . . . . ?
N5 C57 C58 C59 179.20(19) . . . . ?
N5 C57 C58 N6 -1.9(3) . . . . ?
N5 C57 C67 C66 1.6(5) . . . . ?
N5 C57 C67 C68 179.6(3) . . . . ?
N5 C69 C70 C71 179.3(2) . . . . ?
N5 C69 C74 C73 -177.6(2) . . . . ?
N6 C58 C59 C60 3.2(5) . . . . ?
N6 C58 C59 C68 -176.3(3) . . . . ?
N6 C77 C78 C79 -175.8(2) . . . . ?
N6 C77 C82 C81 177.3(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6 -7 -30 0.1269 -6.0341 -7.0882 -29.9727 -0.0104 -0.1262 -0.9808
-1 -28 -11 0.1378 -1.1231 -28.0357 -10.9302 -0.2943 -0.8432 -0.4446
-22 1 13 0.0988 -21.9698 1.1614 13.0412 -0.9189 0.4231 0.0720
7 3 31 0.1131 7.0162 3.0875 30.9805 -0.0158 -0.0127 1.0078
8 -5 30 0.1333 7.9805 -4.9206 29.9981 -0.0744 -0.2749 0.9608
5 -25 16 0.1283 4.8928 -24.9590 16.0521 -0.3064 -0.8408 0.4333
19 -13 -11 0.1005 18.9218 -13.1373 -11.0059 0.6318 -0.7356 -0.1042
22 2 -13 0.1002 21.9827 1.8383 -13.0486 0.9583 -0.3316 -0.0600
-4 29 2 0.1423 -3.8706 29.0250 1.9371 0.2152 0.9559 0.1179
20 4 16 0.1255 20.0028 3.9630 15.9519 0.6214 -0.2185 0.7597
17 0 -22 0.1072 16.9760 -0.1722 -22.0344 0.8398 -0.3104 -0.3987
-19 16 10 0.0988 -18.9092 16.1330 9.9986 -0.5824 0.8265 0.0873
18 17 -9 0.0970 18.0525 16.8726 -9.0772 0.9695 0.1984 0.0598
-17 -16 14 0.1006 -17.0475 -15.8579 14.0730 -0.9700 -0.1824 0.1030
-7 11 -28 0.1504 -6.9550 10.9229 -28.0146 0.1697 0.4416 -0.8649

_exptl_crystal_recrystallization_method 
'Slow diffusion of diethyl ether into a saturated MeCN solution of the complex'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_raz-01-078
_database_code_depnum_ccdc_archive 'CCDC 1448201'
_audit_update_record             
;
2016-01-19 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;
_audit_creation_date             2015-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2014-3
_chemical_name_common            tri(dmp-BIAN)Cr
_chemical_name_systematic        
"tri(N,N'-bis(3,5-dimethylphenylimino)acenaphthenesemiquinone) chromium"
_chemical_formula_moiety         'C84 H72 Cr1 N6'
_chemical_formula_sum            'C84 H72 Cr N6'
_chemical_formula_weight         1217.47
_chemical_melting_point          n/a

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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   13.1548(2)
_cell_length_b                   13.1548(2)
_cell_length_c                   71.8546(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10768.4(4)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    17297
_cell_measurement_temperature    150.05(10)
_cell_measurement_theta_max      28.6770
_cell_measurement_theta_min      2.8860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             3852
_exptl_crystal_size_max          0.2731
_exptl_crystal_size_mid          0.1665
_exptl_crystal_size_min          0.1041
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 0.897
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            54503
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.888
_diffrn_ambient_temperature      150.05(10)
_diffrn_detector_area_resol_mean 10.2358
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0248840000
_diffrn_orient_matrix_UB_12      0.0528495000
_diffrn_orient_matrix_UB_13      0.0052121000
_diffrn_orient_matrix_UB_21      -0.0556185000
_diffrn_orient_matrix_UB_22      -0.0175844000
_diffrn_orient_matrix_UB_23      0.0040203000
_diffrn_orient_matrix_UB_31      0.0127652000
_diffrn_orient_matrix_UB_32      -0.0278135000
_diffrn_orient_matrix_UB_33      0.0073595000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1963
_reflns_number_total             2119
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0405
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0764P)²+17.4878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1279
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C13(H13)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)

All atoms are refined anisotropically and protons are generated 
in calculated positions and refined using the riding model. A 
446.6 Ang^3 solvent accessible void is present in the unit cell (~4.1%)
that corresponds to a total of 126 electrons. Attempts to model the disordered
THF molecules resulted in an unstable refinement of the model. The solvent mask
routine in OLEX 2 was used to remove this void for the final refinement.

;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.85758(14) 0.55990(14) 0.07518(2) 0.0224(4) Uani 1 1 d . . . . .
C2 C 0.95070(15) 0.67878(14) 0.07009(2) 0.0286(4) Uani 1 1 d . . . . .
C3 C 0.96663(17) 0.76003(17) 0.05664(3) 0.0388(5) Uani 1 1 d . . . . .
H3 H 0.9095 0.7437 0.0477 0.047 Uiso 1 1 calc R . . . .
C4 C 1.0729(2) 0.86943(19) 0.05690(4) 0.0540(6) Uani 1 1 d . . . . .
H4 H 1.0835 0.9256 0.0481 0.065 Uiso 1 1 calc R . . . .
C5 C 1.1596(2) 0.89581(19) 0.06943(4) 0.0587(7) Uani 1 1 d . . . . .
H5 H 1.2280 0.9685 0.0689 0.070 Uiso 1 1 calc R . . . .
C6 C 1.1474(2) 0.8141(2) 0.0833 0.0468(8) Uani 1 2 d S T P . .
C7 C 1.04067(18) 0.70734(18) 0.0833 0.0319(6) Uani 1 2 d S T P . .
C8 C 0.70716(14) 0.51574(13) 0.05272(2) 0.0241(4) Uani 1 1 d . . . . .
C9 C 0.61820(15) 0.54149(14) 0.05551(2) 0.0277(4) Uani 1 1 d . . . . .
H9 H 0.5917 0.5411 0.0675 0.033 Uiso 1 1 calc R . . . .
C10 C 0.56800(18) 0.56792(17) 0.04066(3) 0.0357(4) Uani 1 1 d . . . . .
C11 C 0.61009(19) 0.56857(19) 0.02284(3) 0.0423(5) Uani 1 1 d . . . . .
H11 H 0.5770 0.5856 0.0127 0.051 Uiso 1 1 calc R . . . .
C12 C 0.69970(19) 0.54459(19) 0.01977(3) 0.0404(5) Uani 1 1 d . . . . .
C13 C 0.74835(16) 0.51744(17) 0.03491(2) 0.0317(4) Uani 1 1 d . . . . .
H13 H 0.8083 0.5005 0.0330 0.038 Uiso 1 1 calc R . . . .
C14 C 0.4702(2) 0.5942(3) 0.04409(3) 0.0566(6) Uani 1 1 d . . . . .
H14A H 0.3997 0.5229 0.0473 0.085 Uiso 1 1 calc GR . . . .
H14B H 0.4571 0.6271 0.0330 0.085 Uiso 1 1 calc GR . . . .
H14C H 0.4916 0.6492 0.0541 0.085 Uiso 1 1 calc GR . . . .
C15 C 0.7446(3) 0.5460(3) 0.00030(3) 0.0661(8) Uani 1 1 d . . . . .
H15A H 0.8238 0.6098 -0.0008 0.099 Uiso 1 1 calc GR . . . .
H15B H 0.6958 0.5560 -0.0086 0.099 Uiso 1 1 calc GR . . . .
H15C H 0.7427 0.4732 -0.0020 0.099 Uiso 1 1 calc GR . . . .
N1 N 0.75243(12) 0.48445(12) 0.06848(2) 0.0214(3) Uani 1 1 d . . . . .
Cr1 Cr 0.6667 0.3333 0.0833 0.0177(2) Uani 1 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C1 1.425(3) 16_544 ?
C1 C2 1.471(2) . ?
C1 N1 1.326(2) . ?
C2 C3 1.377(3) . ?
C2 C7 1.415(2) . ?
C3 C4 1.419(3) . ?
C4 C5 1.355(4) . ?
C5 C6 1.417(3) . ?
C6 C5 1.417(3) 16_544 ?
C6 C7 1.404(4) . ?
C7 C2 1.415(2) 16_544 ?
C8 C9 1.386(2) . ?
C8 C13 1.385(2) . ?
C8 N1 1.432(2) . ?
C9 C10 1.388(2) . ?
C10 C11 1.393(3) . ?
C10 C14 1.510(3) . ?
C11 C12 1.382(3) . ?
C12 C13 1.396(3) . ?
C12 C15 1.515(3) . ?
N1 Cr1 2.0300(13) . ?
Cr1 N1 2.0300(13) 2_655 ?
Cr1 N1 2.0299(13) 3_665 ?
Cr1 N1 2.0299(13) 16_544 ?
Cr1 N1 2.0299(13) 17_554 ?
Cr1 N1 2.0298(13) 18_654 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C1 C2 108.54(9) 16_544 . ?
N1 C1 C1 116.36(8) . 16_544 ?
N1 C1 C2 135.07(15) . . ?
C3 C2 C1 136.24(17) . . ?
C3 C2 C7 118.90(18) . . ?
C7 C2 C1 104.85(15) . . ?
C2 C3 C4 117.9(2) . . ?
C5 C4 C3 123.0(2) . . ?
C4 C5 C6 120.9(2) . . ?
C5 C6 C5 128.3(3) . 16_544 ?
C7 C6 C5 115.84(14) . . ?
C7 C6 C5 115.84(14) . 16_544 ?
C2 C7 C2 113.1(2) . 16_544 ?
C6 C7 C2 123.43(11) . . ?
C6 C7 C2 123.44(11) . 16_544 ?
C9 C8 N1 118.61(14) . . ?
C13 C8 C9 120.07(15) . . ?
C13 C8 N1 121.30(15) . . ?
C8 C9 C10 121.04(16) . . ?
C9 C10 C11 118.09(17) . . ?
C9 C10 C14 119.90(17) . . ?
C11 C10 C14 122.01(17) . . ?
C12 C11 C10 121.81(17) . . ?
C11 C12 C13 119.09(17) . . ?
C11 C12 C15 121.11(18) . . ?
C13 C12 C15 119.80(19) . . ?
C8 C13 C12 119.89(17) . . ?
C1 N1 C8 120.01(13) . . ?
C1 N1 Cr1 113.77(10) . . ?
C8 N1 Cr1 126.14(10) . . ?
N1 Cr1 N1 94.90(5) 3_665 2_655 ?
N1 Cr1 N1 94.90(5) 3_665 . ?
N1 Cr1 N1 94.90(5) 2_655 . ?
N1 Cr1 N1 90.92(7) 3_665 16_544 ?
N1 Cr1 N1 172.41(7) 2_655 16_544 ?
N1 Cr1 N1 79.74(7) . 16_544 ?
N1 Cr1 N1 79.73(7) 3_665 17_554 ?
N1 Cr1 N1 90.92(7) 2_655 17_554 ?
N1 Cr1 N1 172.41(7) . 17_554 ?
N1 Cr1 N1 94.90(5) 16_544 17_554 ?
N1 Cr1 N1 172.41(7) 3_665 18_654 ?
N1 Cr1 N1 79.73(7) 2_655 18_654 ?
N1 Cr1 N1 90.92(7) . 18_654 ?
N1 Cr1 N1 94.91(5) 16_544 18_654 ?
N1 Cr1 N1 94.91(5) 17_554 18_654 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1 C2 C3 -177.3(2) 16_544 . . . ?
C1 C1 C2 C7 2.1(2) 16_544 . . . ?
C1 C1 N1 C8 176.73(16) 16_544 . . . ?
C1 C1 N1 Cr1 -0.2(2) 16_544 . . . ?
C1 C2 C3 C4 178.7(2) . . . . ?
C1 C2 C7 C2 -0.78(7) . . . 16_544 ?
C1 C2 C7 C6 179.21(7) . . . . ?
C2 C1 N1 C8 -1.3(3) . . . . ?
C2 C1 N1 Cr1 -178.23(15) . . . . ?
C2 C3 C4 C5 1.7(4) . . . . ?
C3 C2 C7 C2 178.74(19) . . . 16_544 ?
C3 C2 C7 C6 -1.27(19) . . . . ?
C3 C4 C5 C6 -0.8(4) . . . . ?
C4 C5 C6 C5 178.9(3) . . . 16_544 ?
C4 C5 C6 C7 -1.1(3) . . . . ?
C5 C6 C7 C2 -177.90(15) 16_544 . . . ?
C5 C6 C7 C2 2.09(15) 16_544 . . 16_544 ?
C5 C6 C7 C2 2.10(15) . . . . ?
C5 C6 C7 C2 -177.91(15) . . . 16_544 ?
C7 C2 C3 C4 -0.6(3) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C8 C9 C10 C14 179.2(2) . . . . ?
C9 C8 C13 C12 -0.3(3) . . . . ?
C9 C8 N1 C1 -106.60(18) . . . . ?
C9 C8 N1 Cr1 69.96(18) . . . . ?
C9 C10 C11 C12 -0.4(3) . . . . ?
C10 C11 C12 C13 0.9(3) . . . . ?
C10 C11 C12 C15 -179.8(2) . . . . ?
C11 C12 C13 C8 -0.5(3) . . . . ?
C13 C8 C9 C10 0.8(3) . . . . ?
C13 C8 N1 C1 75.2(2) . . . . ?
C13 C8 N1 Cr1 -108.28(16) . . . . ?
C14 C10 C11 C12 179.9(2) . . . . ?
C15 C12 C13 C8 -179.8(2) . . . . ?
N1 C1 C2 C3 0.8(4) . . . . ?
N1 C1 C2 C7 -179.77(16) . . . . ?
N1 C8 C9 C10 -177.50(16) . . . . ?
N1 C8 C13 C12 177.90(17) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 71.0 20.8 ?
2 0.000 0.000 0.090 1.7 0.1 ?
3 0.000 0.000 0.410 1.7 0.1 ?
4 0.000 0.000 0.500 71.0 20.8 ?
5 0.000 0.000 0.590 1.7 0.1 ?
6 0.000 0.000 0.910 1.7 0.1 ?
7 0.333 0.667 0.667 71.0 20.8 ?
8 0.333 0.667 0.167 71.0 20.8 ?
9 0.333 0.667 0.577 1.7 0.1 ?
10 0.333 0.667 0.077 1.7 0.1 ?
11 0.333 0.667 0.257 1.7 0.1 ?
12 0.333 0.667 0.757 1.7 0.1 ?
13 0.667 0.333 0.333 71.0 20.8 ?
14 0.667 0.333 0.833 71.0 20.8 ?
15 0.667 0.333 0.243 1.7 0.1 ?
16 0.667 0.333 0.743 1.7 0.1 ?
17 0.667 0.333 0.923 1.7 0.1 ?
18 0.667 0.333 0.423 1.7 0.1 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4 4 98 0.0755 -3.9810 3.9988 97.8563 0.6223 0.5445 0.5581
14 -17 19 0.1016 13.9772 -16.9781 18.9760 -0.4506 -0.4026 0.7903
10 8 -22 0.0775 9.9865 7.9857 -21.9779 0.5560 -0.7842 -0.2564
3 -3 -100 0.0689 2.9824 -3.0001 -99.8536 -0.6048 -0.5146 -0.6134
-16 1 -30 0.0491 -15.9816 1.0009 -29.9489 -0.5009 0.7509 -0.4523
-14 9 -68 0.0889 -13.9862 8.9877 -67.8994 -0.2269 0.3469 -0.9282
16 -1 30 0.0550 15.9816 -1.0009 29.9489 0.5009 -0.7509 0.4523
-9 -9 31 0.0861 -8.9871 -8.9841 30.9649 -0.5370 0.7823 0.3630
1 -1 101 0.0850 1.0108 -0.9950 100.8526 0.4982 0.3667 0.7828
9 -12 74 0.1082 8.9927 -11.9821 73.8950 -0.0243 0.0076 0.9919
12 -16 -42 0.0964 11.9727 -15.9814 -41.9345 -0.7652 -0.5535 0.2887
-2 13 -69 0.1063 -2.0012 12.9794 -68.9065 0.2770 -0.3940 -0.8937
-14 17 -21 0.1265 -13.9775 16.9780 -20.9731 0.4402 0.3945 -0.8050

_exptl_crystal_recrystallization_method 'Slow evaporation of THF'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_raz01194c
_database_code_depnum_ccdc_archive 'CCDC 1448202'
_audit_update_record             
;
2016-01-19 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;
_audit_creation_date             2015-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2014-3
_chemical_name_common            'tris(dmp-BIAN)Cr tri-PF6'
_chemical_name_systematic        
"tri(N,N'-bis(3,5-dimethylphenylimino)acenaphthenequinone) chromium tri(hexafluorophosphate)"
_chemical_formula_moiety         'C84 H72 Cr N6, 3(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C88 H78 Cr F18 N8 P3'
_chemical_formula_weight         1734.49
_chemical_melting_point          n/a

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'
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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.5848(3)
_cell_length_b                   21.1661(4)
_cell_length_c                   23.1949(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.3501(17)
_cell_angle_gamma                90
_cell_volume                     8140.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    32069
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.5230
_cell_measurement_theta_min      2.9840
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3572
_exptl_crystal_size_max          0.2877
_exptl_crystal_size_mid          0.2116
_exptl_crystal_size_min          0.1607
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.897
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            241245
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.763
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2358
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0131398000
_diffrn_orient_matrix_UB_12      0.0311932000
_diffrn_orient_matrix_UB_13      -0.0062510000
_diffrn_orient_matrix_UB_21      0.0388512000
_diffrn_orient_matrix_UB_22      0.0075436000
_diffrn_orient_matrix_UB_23      -0.0101614000
_diffrn_orient_matrix_UB_31      -0.0121863000
_diffrn_orient_matrix_UB_32      -0.0096341000
_diffrn_orient_matrix_UB_33      -0.0281657000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11548
_reflns_number_total             14357
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         14357
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0464
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0497P)²+11.2528P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1235
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16),
 C18(H18), C22(H22), C24(H24), C26(H26), C32(H32), C33(H33), C34(H34), C36(H36),
  C37(H37), C38(H38), C42(H42), C44(H44), C46(H46), C50(H50), C52(H52),
 C54(H54), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C70(H70),
  C72(H72), C74(H74), C78(H78), C80(H80), C82(H82)
3.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C83(H83A,H83B,H83C),
 C84(H84A,H84B,H84C), C4S(H4SA,H4SB,H4SC), C2S(H2SA,H2SB,H2SC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.10378(13) 0.26604(11) 0.86208(10) 0.0205(5) Uani 1 1 d . . . . .
C2 C 0.02384(14) 0.23608(11) 0.87484(10) 0.0222(5) Uani 1 1 d . . . . .
C3 C 0.02333(14) 0.22258(12) 0.93629(10) 0.0255(5) Uani 1 1 d . . . . .
C4 C -0.02885(15) 0.19235(13) 0.97233(11) 0.0310(6) Uani 1 1 d . . . . .
H4 H -0.0782 0.1771 0.9585 0.037 Uiso 1 1 calc R . . . .
C5 C -0.00550(16) 0.18513(14) 1.03072(11) 0.0354(6) Uani 1 1 d . . . . .
H5 H -0.0396 0.1636 1.0552 0.042 Uiso 1 1 calc R . . . .
C6 C 0.06592(16) 0.20886(14) 1.05265(11) 0.0354(6) Uani 1 1 d . . . . .
H6 H 0.0786 0.2039 1.0917 0.043 Uiso 1 1 calc R . . . .
C7 C 0.12057(15) 0.24071(12) 1.01681(10) 0.0289(6) Uani 1 1 d . . . . .
C8 C 0.19652(16) 0.26707(13) 1.03255(11) 0.0334(6) Uani 1 1 d . . . . .
H8 H 0.2143 0.2658 1.0709 0.040 Uiso 1 1 calc R . . . .
C9 C 0.24407(15) 0.29442(13) 0.99212(11) 0.0309(6) Uani 1 1 d . . . . .
H9 H 0.2933 0.3117 1.0040 0.037 Uiso 1 1 calc R . . . .
C10 C 0.22154(14) 0.29753(12) 0.93323(10) 0.0259(5) Uani 1 1 d . . . . .
H10 H 0.2553 0.3159 0.9065 0.031 Uiso 1 1 calc R . . . .
C11 C 0.14819(14) 0.27261(11) 0.91639(10) 0.0230(5) Uani 1 1 d . . . . .
C12 C 0.09802(14) 0.24527(11) 0.95844(10) 0.0236(5) Uani 1 1 d . . . . .
C13 C 0.19030(13) 0.30917(11) 0.79132(9) 0.0207(5) Uani 1 1 d . . . . .
C14 C 0.26239(14) 0.27644(12) 0.79710(10) 0.0233(5) Uani 1 1 d . . . . .
H14 H 0.2638 0.2366 0.8141 0.028 Uiso 1 1 calc R . . . .
C15 C 0.33274(14) 0.30389(12) 0.77719(10) 0.0272(5) Uani 1 1 d . . . . .
C16 C 0.32832(16) 0.36269(13) 0.75083(11) 0.0316(6) Uani 1 1 d . . . . .
H16 H 0.3750 0.3806 0.7366 0.038 Uiso 1 1 calc R . . . .
C17 C 0.25601(16) 0.39567(12) 0.74516(11) 0.0302(6) Uani 1 1 d . . . . .
C18 C 0.18687(15) 0.36849(11) 0.76663(10) 0.0251(5) Uani 1 1 d . . . . .
H18 H 0.1382 0.3902 0.7644 0.030 Uiso 1 1 calc R . . . .
C19 C 0.41302(15) 0.27088(15) 0.78437(13) 0.0397(7) Uani 1 1 d . . . . .
H19A H 0.4471 0.2944 0.8106 0.060 Uiso 1 1 calc GR . . . .
H19B H 0.4383 0.2680 0.7476 0.060 Uiso 1 1 calc GR . . . .
H19C H 0.4048 0.2292 0.7994 0.060 Uiso 1 1 calc GR . . . .
C20 C 0.2509(2) 0.45882(15) 0.71600(16) 0.0532(9) Uani 1 1 d . . . . .
H20A H 0.2211 0.4548 0.6802 0.080 Uiso 1 1 calc GR . . . .
H20B H 0.3043 0.4738 0.7086 0.080 Uiso 1 1 calc GR . . . .
H20C H 0.2240 0.4882 0.7405 0.080 Uiso 1 1 calc GR . . . .
C21 C -0.10679(14) 0.20488(12) 0.84380(10) 0.0248(5) Uani 1 1 d . . . . .
C22 C -0.12924(15) 0.14432(12) 0.82739(11) 0.0293(6) Uani 1 1 d . . . . .
H22 H -0.0928 0.1178 0.8095 0.035 Uiso 1 1 calc R . . . .
C23 C -0.20736(16) 0.12372(14) 0.83817(13) 0.0383(7) Uani 1 1 d . . . . .
C24 C -0.25986(16) 0.16476(15) 0.86506(13) 0.0408(7) Uani 1 1 d . . . . .
H24 H -0.3120 0.1511 0.8722 0.049 Uiso 1 1 calc R . . . .
C25 C -0.23768(16) 0.22524(14) 0.88170(12) 0.0360(6) Uani 1 1 d . . . . .
C26 C -0.15991(15) 0.24544(13) 0.87037(10) 0.0297(6) Uani 1 1 d . . . . .
H26 H -0.1436 0.2860 0.8806 0.036 Uiso 1 1 calc R . . . .
C27 C -0.2338(2) 0.05850(16) 0.81942(19) 0.0611(10) Uani 1 1 d . . . . .
H27A H -0.2606 0.0610 0.7823 0.092 Uiso 1 1 calc GR . . . .
H27B H -0.2701 0.0415 0.8470 0.092 Uiso 1 1 calc GR . . . .
H27C H -0.1874 0.0315 0.8170 0.092 Uiso 1 1 calc GR . . . .
C28 C -0.29538(19) 0.26811(18) 0.91232(15) 0.0548(9) Uani 1 1 d . . . . .
H28A H -0.3014 0.2537 0.9512 0.082 Uiso 1 1 calc GR . . . .
H28B H -0.3469 0.2674 0.8926 0.082 Uiso 1 1 calc GR . . . .
H28C H -0.2746 0.3104 0.9126 0.082 Uiso 1 1 calc GR . . . .
C29 C 0.01928(13) 0.13031(11) 0.70719(9) 0.0203(5) Uani 1 1 d . . . . .
C30 C -0.05864(13) 0.16136(11) 0.68702(9) 0.0212(5) Uani 1 1 d . . . . .
C31 C -0.09872(14) 0.11824(11) 0.64687(10) 0.0228(5) Uani 1 1 d . . . . .
C32 C -0.16903(15) 0.12008(12) 0.61432(10) 0.0284(5) Uani 1 1 d . . . . .
H32 H -0.2052 0.1533 0.6179 0.034 Uiso 1 1 calc R . . . .
C33 C -0.18474(16) 0.07028(13) 0.57544(11) 0.0328(6) Uani 1 1 d . . . . .
H33 H -0.2318 0.0713 0.5528 0.039 Uiso 1 1 calc R . . . .
C34 C -0.13276(16) 0.02026(13) 0.56989(11) 0.0317(6) Uani 1 1 d . . . . .
H34 H -0.1450 -0.0114 0.5433 0.038 Uiso 1 1 calc R . . . .
C35 C -0.06099(15) 0.01597(12) 0.60376(10) 0.0271(5) Uani 1 1 d . . . . .
C36 C -0.00216(16) -0.03281(12) 0.60360(11) 0.0318(6) Uani 1 1 d . . . . .
H36 H -0.0096 -0.0674 0.5793 0.038 Uiso 1 1 calc R . . . .
C37 C 0.06530(16) -0.02967(12) 0.63872(11) 0.0320(6) Uani 1 1 d . . . . .
H37 H 0.1023 -0.0626 0.6379 0.038 Uiso 1 1 calc R . . . .
C38 C 0.08052(15) 0.02183(12) 0.67602(11) 0.0275(5) Uani 1 1 d . . . . .
H38 H 0.1272 0.0233 0.6990 0.033 Uiso 1 1 calc R . . . .
C39 C 0.02474(14) 0.06977(11) 0.67758(10) 0.0223(5) Uani 1 1 d . . . . .
C40 C -0.04590(14) 0.06602(11) 0.64203(10) 0.0228(5) Uani 1 1 d . . . . .
C41 C 0.13865(13) 0.13828(11) 0.76713(10) 0.0215(5) Uani 1 1 d . . . . .
C42 C 0.14305(15) 0.12458(11) 0.82565(10) 0.0247(5) Uani 1 1 d . . . . .
H42 H 0.0968 0.1260 0.8476 0.030 Uiso 1 1 calc R . . . .
C43 C 0.21682(16) 0.10875(12) 0.85128(11) 0.0292(6) Uani 1 1 d . . . . .
C44 C 0.28422(15) 0.10611(12) 0.81697(12) 0.0310(6) Uani 1 1 d . . . . .
H44 H 0.3341 0.0969 0.8342 0.037 Uiso 1 1 calc R . . . .
C45 C 0.27983(14) 0.11670(12) 0.75793(12) 0.0290(6) Uani 1 1 d . . . . .
C46 C 0.20542(14) 0.13339(11) 0.73285(11) 0.0250(5) Uani 1 1 d . . . . .
H46 H 0.2009 0.1411 0.6934 0.030 Uiso 1 1 calc R . . . .
C47 C 0.2232(2) 0.09446(16) 0.91479(12) 0.0475(8) Uani 1 1 d . . . . .
H47A H 0.2389 0.0512 0.9202 0.071 Uiso 1 1 calc GR . . . .
H47B H 0.1719 0.1015 0.9320 0.071 Uiso 1 1 calc GR . . . .
H47C H 0.2630 0.1216 0.9326 0.071 Uiso 1 1 calc GR . . . .
C48 C 0.35305(16) 0.10971(16) 0.72122(14) 0.0437(7) Uani 1 1 d . . . . .
H48A H 0.3628 0.0657 0.7141 0.066 Uiso 1 1 calc GR . . . .
H48B H 0.3990 0.1278 0.7410 0.066 Uiso 1 1 calc GR . . . .
H48C H 0.3439 0.1312 0.6852 0.066 Uiso 1 1 calc GR . . . .
C49 C -0.14467(14) 0.25225(11) 0.68775(10) 0.0231(5) Uani 1 1 d . . . . .
C50 C -0.21494(14) 0.24398(13) 0.71771(11) 0.0292(6) Uani 1 1 d . . . . .
H50 H -0.2179 0.2133 0.7463 0.035 Uiso 1 1 calc R . . . .
C51 C -0.28161(15) 0.28235(14) 0.70441(11) 0.0337(6) Uani 1 1 d . . . . .
C52 C -0.27461(16) 0.32808(13) 0.66226(11) 0.0346(6) Uani 1 1 d . . . . .
H52 H -0.3179 0.3550 0.6547 0.041 Uiso 1 1 calc R . . . .
C53 C -0.20484(16) 0.33518(13) 0.63079(11) 0.0322(6) Uani 1 1 d . . . . .
C54 C -0.13931(15) 0.29626(12) 0.64369(10) 0.0271(5) Uani 1 1 d . . . . .
H54 H -0.0922 0.2997 0.6229 0.033 Uiso 1 1 calc R . . . .
C55 C -0.35874(17) 0.27406(17) 0.73681(14) 0.0490(8) Uani 1 1 d . . . . .
H55A H -0.3829 0.2342 0.7266 0.074 Uiso 1 1 calc GR . . . .
H55B H -0.3954 0.3077 0.7269 0.074 Uiso 1 1 calc GR . . . .
H55C H -0.3470 0.2750 0.7775 0.074 Uiso 1 1 calc GR . . . .
C56 C -0.1995(2) 0.38384(15) 0.58339(14) 0.0491(8) Uani 1 1 d . . . . .
H56A H -0.1716 0.4205 0.5978 0.074 Uiso 1 1 calc GR . . . .
H56B H -0.2529 0.3956 0.5705 0.074 Uiso 1 1 calc GR . . . .
H56C H -0.1707 0.3664 0.5517 0.074 Uiso 1 1 calc GR . . . .
C57 C 0.04976(13) 0.34443(11) 0.66855(10) 0.0219(5) Uani 1 1 d . . . . .
C58 C -0.00104(14) 0.37737(11) 0.71216(10) 0.0231(5) Uani 1 1 d . . . . .
C59 C -0.01203(14) 0.44237(12) 0.69318(11) 0.0263(5) Uani 1 1 d . . . . .
C60 C -0.04802(15) 0.49570(12) 0.71561(12) 0.0323(6) Uani 1 1 d . . . . .
H60 H -0.0741 0.4942 0.7506 0.039 Uiso 1 1 calc R . . . .
C61 C -0.04396(17) 0.55219(13) 0.68385(13) 0.0390(7) Uani 1 1 d . . . . .
H61 H -0.0674 0.5884 0.6987 0.047 Uiso 1 1 calc R . . . .
C62 C -0.00663(16) 0.55580(13) 0.63171(13) 0.0379(7) Uani 1 1 d . . . . .
H62 H -0.0062 0.5940 0.6119 0.046 Uiso 1 1 calc R . . . .
C63 C 0.03120(15) 0.50222(12) 0.60776(12) 0.0323(6) Uani 1 1 d . . . . .
C64 C 0.07323(16) 0.49875(14) 0.55527(12) 0.0374(6) Uani 1 1 d . . . . .
H64 H 0.0770 0.5344 0.5321 0.045 Uiso 1 1 calc R . . . .
C65 C 0.10840(17) 0.44332(14) 0.53840(12) 0.0375(6) Uani 1 1 d . . . . .
H65 H 0.1348 0.4424 0.5035 0.045 Uiso 1 1 calc R . . . .
C66 C 0.10624(15) 0.38744(13) 0.57181(11) 0.0307(6) Uani 1 1 d . . . . .
H66 H 0.1313 0.3506 0.5596 0.037 Uiso 1 1 calc R . . . .
C67 C 0.06581(14) 0.38935(12) 0.62291(10) 0.0255(5) Uani 1 1 d . . . . .
C68 C 0.02816(14) 0.44648(12) 0.64004(11) 0.0261(5) Uani 1 1 d . . . . .
C69 C 0.12118(14) 0.25274(11) 0.64086(9) 0.0222(5) Uani 1 1 d . . . . .
C70 C 0.08718(15) 0.20853(11) 0.60393(10) 0.0244(5) Uani 1 1 d . . . . .
H70 H 0.0315 0.2030 0.6022 0.029 Uiso 1 1 calc R . . . .
C71 C 0.13641(17) 0.17233(12) 0.56932(10) 0.0299(6) Uani 1 1 d . . . . .
C72 C 0.21906(17) 0.18303(13) 0.57218(11) 0.0336(6) Uani 1 1 d . . . . .
H72 H 0.2526 0.1586 0.5496 0.040 Uiso 1 1 calc R . . . .
C73 C 0.25324(16) 0.22906(13) 0.60769(11) 0.0324(6) Uani 1 1 d . . . . .
C74 C 0.20318(15) 0.26392(12) 0.64313(10) 0.0271(5) Uani 1 1 d . . . . .
H74 H 0.2248 0.2943 0.6680 0.033 Uiso 1 1 calc R . . . .
C75 C 0.1009(2) 0.12336(14) 0.52956(12) 0.0435(7) Uani 1 1 d . . . . .
H75A H 0.1105 0.0821 0.5455 0.065 Uiso 1 1 calc GR . . . .
H75B H 0.1256 0.1264 0.4926 0.065 Uiso 1 1 calc GR . . . .
H75C H 0.0439 0.1302 0.5251 0.065 Uiso 1 1 calc GR . . . .
C76 C 0.34247(18) 0.24235(17) 0.60779(15) 0.0526(8) Uani 1 1 d . . . . .
H76A H 0.3531 0.2759 0.5812 0.079 Uiso 1 1 calc GR . . . .
H76B H 0.3708 0.2050 0.5964 0.079 Uiso 1 1 calc GR . . . .
H76C H 0.3603 0.2546 0.6458 0.079 Uiso 1 1 calc GR . . . .
C77 C -0.07104(14) 0.37374(11) 0.79976(10) 0.0241(5) Uani 1 1 d . . . . .
C78 C -0.15111(15) 0.38711(12) 0.78645(11) 0.0293(6) Uani 1 1 d . . . . .
H78 H -0.1725 0.3780 0.7500 0.035 Uiso 1 1 calc R . . . .
C79 C -0.19919(15) 0.41413(13) 0.82796(12) 0.0338(6) Uani 1 1 d . . . . .
C80 C -0.16578(16) 0.42549(13) 0.88254(12) 0.0345(6) Uani 1 1 d . . . . .
H80 H -0.1981 0.4428 0.9107 0.041 Uiso 1 1 calc R . . . .
C81 C -0.08537(16) 0.41179(13) 0.89635(11) 0.0314(6) Uani 1 1 d . . . . .
C82 C -0.03735(15) 0.38651(12) 0.85368(10) 0.0264(5) Uani 1 1 d . . . . .
H82 H 0.0169 0.3783 0.8613 0.032 Uiso 1 1 calc R . . . .
C83 C -0.28589(17) 0.43101(17) 0.81352(14) 0.0502(8) Uani 1 1 d . . . . .
H83A H -0.2927 0.4759 0.8162 0.075 Uiso 1 1 calc GR . . . .
H83B H -0.3207 0.4104 0.8402 0.075 Uiso 1 1 calc GR . . . .
H83C H -0.2993 0.4174 0.7750 0.075 Uiso 1 1 calc GR . . . .
C84 C -0.05062(18) 0.42182(17) 0.95623(12) 0.0461(8) Uani 1 1 d . . . . .
H84A H -0.0828 0.4521 0.9762 0.069 Uiso 1 1 calc GR . . . .
H84B H 0.0036 0.4372 0.9538 0.069 Uiso 1 1 calc GR . . . .
H84C H -0.0506 0.3825 0.9769 0.069 Uiso 1 1 calc GR . . . .
N1 N 0.11577(11) 0.28055(9) 0.80889(8) 0.0199(4) Uani 1 1 d . . . . .
N2 N -0.02652(11) 0.22766(9) 0.83240(8) 0.0215(4) Uani 1 1 d . . . . .
N3 N 0.06310(11) 0.16205(9) 0.74349(8) 0.0203(4) Uani 1 1 d . . . . .
N4 N -0.07288(11) 0.21750(9) 0.70532(8) 0.0210(4) Uani 1 1 d . . . . .
N5 N 0.06951(11) 0.28681(9) 0.67952(8) 0.0208(4) Uani 1 1 d . . . . .
N6 N -0.02183(11) 0.34490(9) 0.75645(8) 0.0221(4) Uani 1 1 d . . . . .
Cr1 Cr 0.02097(2) 0.25325(2) 0.75504(2) 0.01896(10) Uani 1 1 d . . . . .
F13 F 0.0675(5) 0.0198(7) 0.2092(3) 0.185(5) Uani 0.617(12) 1 d . . P A 1
F13A F 0.0349(14) 0.0603(4) 0.0863(6) 0.153(8) Uani 0.383(12) 1 d . . P A 2
F14 F -0.0598(3) 0.0213(2) 0.1962(3) 0.077(2) Uani 0.617(12) 1 d . . P A 1
F14A F 0.0955(5) 0.0482(5) 0.1730(12) 0.159(9) Uani 0.383(12) 1 d . . P A 2
F15 F -0.0471(5) 0.0559(4) 0.1077(4) 0.131(4) Uani 0.617(12) 1 d . . P A 1
F15A F -0.0191(14) 0.0270(9) 0.2086(5) 0.183(9) Uani 0.383(12) 1 d . . P A 2
F16 F 0.0862(4) 0.0590(4) 0.1219(4) 0.102(3) Uani 0.617(12) 1 d . . P A 1
F16A F -0.0824(8) 0.0399(8) 0.1255(8) 0.129(6) Uani 0.383(12) 1 d . . P A 2
F17 F 0.01808(15) -0.02931(10) 0.13405(11) 0.0810(7) Uani 1 1 d . . . . .
F18 F -0.00018(19) 0.11417(14) 0.16922(17) 0.1296(13) Uani 1 1 d . . . . .
P3 P 0.00985(5) 0.04175(5) 0.15434(5) 0.0575(2) Uani 1 1 d . . . . .
F1 F 0.25662(12) 0.02075(11) 0.62483(9) 0.0720(7) Uani 1 1 d . . . . .
F2 F 0.34047(15) -0.06436(13) 0.61943(9) 0.0850(7) Uani 1 1 d . . . . .
F3 F 0.34729(10) -0.05054(9) 0.52434(8) 0.0528(5) Uani 1 1 d . . . . .
F4 F 0.26573(12) 0.03215(9) 0.52842(9) 0.0623(5) Uani 1 1 d . . . . .
F5 F 0.22681(11) -0.06056(9) 0.56495(8) 0.0559(5) Uani 1 1 d . . . . .
F6 F 0.37780(11) 0.02998(11) 0.58422(8) 0.0631(6) Uani 1 1 d . . . . .
P1 P 0.30258(4) -0.01523(4) 0.57544(3) 0.03483(17) Uani 1 1 d . . . . .
F7 F -0.00201(11) 0.70328(9) 0.60075(7) 0.0517(5) Uani 1 1 d . . . . .
F8 F -0.04685(12) 0.73025(11) 0.51214(8) 0.0662(6) Uani 1 1 d . . . . .
F9 F 0.07862(12) 0.74284(11) 0.48219(8) 0.0672(6) Uani 1 1 d . . . . .
F10 F 0.12461(13) 0.71459(16) 0.57122(10) 0.0967(9) Uani 1 1 d . . . . .
F11 F 0.04052(15) 0.65104(10) 0.52188(9) 0.0755(6) Uani 1 1 d . . . . .
F12 F 0.0385(2) 0.79403(10) 0.56084(10) 0.0984(9) Uani 1 1 d . . . . .
P2 P 0.03914(5) 0.72319(4) 0.54173(3) 0.03968(18) Uani 1 1 d . . . . .
C3S C -0.1791(3) 0.0832(2) 0.00227(17) 0.0691(11) Uani 1 1 d . . . . .
C4S C -0.1324(4) 0.0308(2) -0.0164(2) 0.1063(19) Uani 1 1 d . . . . .
H4SA H -0.1062 0.0416 -0.0515 0.159 Uiso 1 1 calc GR . . . .
H4SB H -0.1671 -0.0049 -0.0229 0.159 Uiso 1 1 calc GR . . . .
H4SC H -0.0925 0.0206 0.0128 0.159 Uiso 1 1 calc GR . . . .
N2S N -0.2140(2) 0.1255(2) 0.0168(2) 0.0971(13) Uani 1 1 d . . . . .
C1S C -0.3980(2) 0.10213(18) 0.64820(16) 0.0605(9) Uani 1 1 d . . . . .
C2S C -0.4453(3) 0.0983(2) 0.59524(18) 0.0816(13) Uani 1 1 d . . . . .
H2SA H -0.4117 0.0841 0.5647 0.122 Uiso 1 1 calc GR . . . .
H2SB H -0.4667 0.1393 0.5858 0.122 Uiso 1 1 calc GR . . . .
H2SC H -0.4888 0.0690 0.6000 0.122 Uiso 1 1 calc GR . . . .
N1S N -0.3598(3) 0.1053(2) 0.68900(17) 0.0961(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.505(3) . ?
C1 C11 1.451(3) . ?
C1 N1 1.291(3) . ?
C2 C3 1.454(3) . ?
C2 N2 1.288(3) . ?
C3 C4 1.375(3) . ?
C3 C12 1.414(3) . ?
C4 C5 1.408(4) . ?
C5 C6 1.373(4) . ?
C6 C7 1.415(4) . ?
C7 C8 1.418(4) . ?
C7 C12 1.399(3) . ?
C8 C9 1.368(4) . ?
C9 C10 1.409(3) . ?
C10 C11 1.374(3) . ?
C11 C12 1.420(3) . ?
C13 C14 1.386(3) . ?
C13 C18 1.381(3) . ?
C13 N1 1.444(3) . ?
C14 C15 1.392(3) . ?
C15 C16 1.388(4) . ?
C15 C19 1.509(4) . ?
C16 C17 1.391(4) . ?
C17 C18 1.386(4) . ?
C17 C20 1.500(4) . ?
C21 C22 1.386(4) . ?
C21 C26 1.385(4) . ?
C21 N2 1.446(3) . ?
C22 C23 1.395(4) . ?
C23 C24 1.388(4) . ?
C23 C27 1.509(4) . ?
C24 C25 1.384(4) . ?
C25 C26 1.390(4) . ?
C25 C28 1.509(4) . ?
C29 C30 1.514(3) . ?
C29 C39 1.458(3) . ?
C29 N3 1.288(3) . ?
C30 C31 1.454(3) . ?
C30 N4 1.286(3) . ?
C31 C32 1.375(3) . ?
C31 C40 1.416(3) . ?
C32 C33 1.408(4) . ?
C33 C34 1.373(4) . ?
C34 C35 1.414(4) . ?
C35 C36 1.421(4) . ?
C35 C40 1.401(3) . ?
C36 C37 1.370(4) . ?
C37 C38 1.411(4) . ?
C38 C39 1.374(3) . ?
C39 C40 1.419(3) . ?
C41 C42 1.388(3) . ?
C41 C46 1.382(3) . ?
C41 N3 1.446(3) . ?
C42 C43 1.389(3) . ?
C43 C44 1.389(4) . ?
C43 C47 1.505(4) . ?
C44 C45 1.388(4) . ?
C45 C46 1.397(3) . ?
C45 C48 1.507(4) . ?
C49 C50 1.382(4) . ?
C49 C54 1.387(4) . ?
C49 N4 1.450(3) . ?
C50 C51 1.400(4) . ?
C51 C52 1.383(4) . ?
C51 C55 1.509(4) . ?
C52 C53 1.391(4) . ?
C53 C54 1.391(3) . ?
C53 C56 1.511(4) . ?
C57 C58 1.503(3) . ?
C57 C67 1.452(3) . ?
C57 N5 1.287(3) . ?
C58 C59 1.455(3) . ?
C58 N6 1.290(3) . ?
C59 C60 1.384(4) . ?
C59 C68 1.418(4) . ?
C60 C61 1.407(4) . ?
C61 C62 1.374(4) . ?
C62 C63 1.416(4) . ?
C63 C64 1.419(4) . ?
C63 C68 1.399(4) . ?
C64 C65 1.371(4) . ?
C65 C66 1.415(4) . ?
C66 C67 1.376(3) . ?
C67 C68 1.422(3) . ?
C69 C70 1.380(3) . ?
C69 C74 1.380(3) . ?
C69 N5 1.447(3) . ?
C70 C71 1.389(3) . ?
C71 C72 1.389(4) . ?
C71 C75 1.499(4) . ?
C72 C73 1.388(4) . ?
C73 C74 1.393(4) . ?
C73 C76 1.506(4) . ?
C77 C78 1.386(3) . ?
C77 C82 1.384(3) . ?
C77 N6 1.445(3) . ?
C78 C79 1.388(4) . ?
C79 C80 1.391(4) . ?
C79 C83 1.512(4) . ?
C80 C81 1.395(4) . ?
C81 C82 1.392(3) . ?
C81 C84 1.506(4) . ?
N1 Cr1 2.0673(18) . ?
N2 Cr1 2.0494(19) . ?
N3 Cr1 2.0725(19) . ?
N4 Cr1 2.0592(19) . ?
N5 Cr1 2.0706(19) . ?
N6 Cr1 2.066(2) . ?
F13 P3 1.640(7) . ?
F13A P3 1.689(9) . ?
F14 P3 1.586(5) . ?
F14A P3 1.481(9) . ?
F15 P3 1.451(6) . ?
F15A P3 1.393(12) . ?
F16 P3 1.533(5) . ?
F16A P3 1.656(12) . ?
F17 P3 1.583(2) . ?
F18 P3 1.581(3) . ?
F1 P1 1.5857(19) . ?
F2 P1 1.577(2) . ?
F3 P1 1.5983(18) . ?
F4 P1 1.593(2) . ?
F5 P1 1.5951(19) . ?
F6 P1 1.5817(19) . ?
F7 P2 1.6004(18) . ?
F8 P2 1.575(2) . ?
F9 P2 1.5974(19) . ?
F10 P2 1.570(2) . ?
F11 P2 1.595(2) . ?
F12 P2 1.564(2) . ?
C3S C4S 1.425(7) . ?
C3S N2S 1.122(6) . ?
C1S C2S 1.444(5) . ?
C1S N1S 1.128(5) . ?

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
C11 C1 C2 107.52(19) . . ?
N1 C1 C2 116.4(2) . . ?
N1 C1 C11 136.1(2) . . ?
C3 C2 C1 107.52(19) . . ?
N2 C2 C1 117.8(2) . . ?
N2 C2 C3 134.7(2) . . ?
C4 C3 C2 134.9(2) . . ?
C4 C3 C12 119.7(2) . . ?
C12 C3 C2 105.3(2) . . ?
C3 C4 C5 118.2(2) . . ?
C6 C5 C4 122.1(2) . . ?
C5 C6 C7 121.0(2) . . ?
C6 C7 C8 127.9(2) . . ?
C12 C7 C6 116.2(2) . . ?
C12 C7 C8 115.9(2) . . ?
C9 C8 C7 120.9(2) . . ?
C8 C9 C10 122.7(2) . . ?
C11 C10 C9 118.1(2) . . ?
C10 C11 C1 135.4(2) . . ?
C10 C11 C12 119.4(2) . . ?
C12 C11 C1 105.3(2) . . ?
C3 C12 C11 114.3(2) . . ?
C7 C12 C3 122.7(2) . . ?
C7 C12 C11 123.0(2) . . ?
C14 C13 N1 120.4(2) . . ?
C18 C13 C14 121.5(2) . . ?
C18 C13 N1 118.1(2) . . ?
C13 C14 C15 119.2(2) . . ?
C14 C15 C19 121.0(2) . . ?
C16 C15 C14 119.0(2) . . ?
C16 C15 C19 120.1(2) . . ?
C15 C16 C17 121.9(2) . . ?
C16 C17 C20 122.0(2) . . ?
C18 C17 C16 118.5(2) . . ?
C18 C17 C20 119.6(2) . . ?
C13 C18 C17 120.0(2) . . ?
C22 C21 N2 120.0(2) . . ?
C26 C21 C22 121.7(2) . . ?
C26 C21 N2 118.2(2) . . ?
C21 C22 C23 119.0(2) . . ?
C22 C23 C27 119.9(3) . . ?
C24 C23 C22 118.7(3) . . ?
C24 C23 C27 121.4(3) . . ?
C25 C24 C23 122.6(2) . . ?
C24 C25 C26 118.3(3) . . ?
C24 C25 C28 121.3(3) . . ?
C26 C25 C28 120.4(3) . . ?
C21 C26 C25 119.8(3) . . ?
C39 C29 C30 107.34(19) . . ?
N3 C29 C30 116.1(2) . . ?
N3 C29 C39 136.5(2) . . ?
C31 C30 C29 107.43(19) . . ?
N4 C30 C29 117.5(2) . . ?
N4 C30 C31 135.0(2) . . ?
C32 C31 C30 134.7(2) . . ?
C32 C31 C40 119.8(2) . . ?
C40 C31 C30 105.4(2) . . ?
C31 C32 C33 118.2(2) . . ?
C34 C33 C32 122.0(2) . . ?
C33 C34 C35 121.3(2) . . ?
C34 C35 C36 127.9(2) . . ?
C40 C35 C34 116.1(2) . . ?
C40 C35 C36 116.0(2) . . ?
C37 C36 C35 121.0(2) . . ?
C36 C37 C38 122.3(2) . . ?
C39 C38 C37 118.4(2) . . ?
C38 C39 C29 135.3(2) . . ?
C38 C39 C40 119.4(2) . . ?
C40 C39 C29 105.3(2) . . ?
C31 C40 C39 114.5(2) . . ?
C35 C40 C31 122.6(2) . . ?
C35 C40 C39 122.9(2) . . ?
C42 C41 N3 117.9(2) . . ?
C46 C41 C42 121.5(2) . . ?
C46 C41 N3 120.4(2) . . ?
C41 C42 C43 119.6(2) . . ?
C42 C43 C47 120.6(2) . . ?
C44 C43 C42 118.5(2) . . ?
C44 C43 C47 120.9(2) . . ?
C45 C44 C43 122.3(2) . . ?
C44 C45 C46 118.5(2) . . ?
C44 C45 C48 121.2(2) . . ?
C46 C45 C48 120.3(2) . . ?
C41 C46 C45 119.4(2) . . ?
C50 C49 C54 121.7(2) . . ?
C50 C49 N4 119.4(2) . . ?
C54 C49 N4 118.8(2) . . ?
C49 C50 C51 119.1(2) . . ?
C50 C51 C55 119.8(3) . . ?
C52 C51 C50 118.9(2) . . ?
C52 C51 C55 121.3(2) . . ?
C51 C52 C53 122.1(2) . . ?
C52 C53 C54 118.6(2) . . ?
C52 C53 C56 121.3(2) . . ?
C54 C53 C56 120.1(3) . . ?
C49 C54 C53 119.5(2) . . ?
C67 C57 C58 107.6(2) . . ?
N5 C57 C58 116.8(2) . . ?
N5 C57 C67 135.6(2) . . ?
C59 C58 C57 107.7(2) . . ?
N6 C58 C57 117.0(2) . . ?
N6 C58 C59 135.3(2) . . ?
C60 C59 C58 135.2(2) . . ?
C60 C59 C68 119.5(2) . . ?
C68 C59 C58 105.2(2) . . ?
C59 C60 C61 118.0(3) . . ?
C62 C61 C60 122.4(3) . . ?
C61 C62 C63 120.9(3) . . ?
C62 C63 C64 127.5(3) . . ?
C68 C63 C62 116.3(2) . . ?
C68 C63 C64 116.1(2) . . ?
C65 C64 C63 120.7(2) . . ?
C64 C65 C66 122.9(3) . . ?
C67 C66 C65 117.8(2) . . ?
C66 C67 C57 135.2(2) . . ?
C66 C67 C68 119.5(2) . . ?
C68 C67 C57 105.3(2) . . ?
C59 C68 C67 114.2(2) . . ?
C63 C68 C59 122.7(2) . . ?
C63 C68 C67 123.1(2) . . ?
C70 C69 C74 121.8(2) . . ?
C70 C69 N5 118.9(2) . . ?
C74 C69 N5 119.2(2) . . ?
C69 C70 C71 119.7(2) . . ?
C70 C71 C72 118.4(2) . . ?
C70 C71 C75 120.6(3) . . ?
C72 C71 C75 121.0(2) . . ?
C73 C72 C71 122.1(2) . . ?
C72 C73 C74 118.8(2) . . ?
C72 C73 C76 121.3(3) . . ?
C74 C73 C76 119.9(3) . . ?
C69 C74 C73 119.1(2) . . ?
C78 C77 N6 119.1(2) . . ?
C82 C77 C78 121.7(2) . . ?
C82 C77 N6 119.2(2) . . ?
C77 C78 C79 119.5(2) . . ?
C78 C79 C80 118.7(2) . . ?
C78 C79 C83 120.2(2) . . ?
C80 C79 C83 121.1(2) . . ?
C79 C80 C81 122.1(2) . . ?
C80 C81 C84 121.7(2) . . ?
C82 C81 C80 118.5(2) . . ?
C82 C81 C84 119.8(2) . . ?
C77 C82 C81 119.5(2) . . ?
C1 N1 C13 121.44(19) . . ?
C1 N1 Cr1 112.25(15) . . ?
C13 N1 Cr1 126.22(14) . . ?
C2 N2 C21 119.30(19) . . ?
C2 N2 Cr1 112.14(15) . . ?
C21 N2 Cr1 128.51(14) . . ?
C29 N3 C41 122.47(19) . . ?
C29 N3 Cr1 112.55(15) . . ?
C41 N3 Cr1 124.52(14) . . ?
C30 N4 C49 122.15(19) . . ?
C30 N4 Cr1 112.47(15) . . ?
C49 N4 Cr1 125.17(15) . . ?
C57 N5 C69 120.09(19) . . ?
C57 N5 Cr1 112.97(15) . . ?
C69 N5 Cr1 126.93(15) . . ?
C58 N6 C77 119.7(2) . . ?
C58 N6 Cr1 112.91(15) . . ?
C77 N6 Cr1 127.42(15) . . ?
N1 Cr1 N3 94.85(7) . . ?
N1 Cr1 N5 96.30(7) . . ?
N2 Cr1 N1 81.23(7) . . ?
N2 Cr1 N3 90.27(8) . . ?
N2 Cr1 N4 95.29(8) . . ?
N2 Cr1 N5 175.17(8) . . ?
N2 Cr1 N6 95.45(8) . . ?
N4 Cr1 N1 174.36(8) . . ?
N4 Cr1 N3 80.68(7) . . ?
N4 Cr1 N5 87.49(7) . . ?
N4 Cr1 N6 95.65(7) . . ?
N5 Cr1 N3 94.09(7) . . ?
N6 Cr1 N1 89.12(7) . . ?
N6 Cr1 N3 173.48(7) . . ?
N6 Cr1 N5 80.32(8) . . ?
F14 P3 F13 82.4(4) . . ?
F14A P3 F13A 89.8(9) . . ?
F14A P3 F16A 172.2(10) . . ?
F14A P3 F17 94.9(5) . . ?
F14A P3 F18 87.2(5) . . ?
F15 P3 F13 173.8(5) . . ?
F15 P3 F14 92.4(4) . . ?
F15 P3 F16 96.6(5) . . ?
F15 P3 F17 91.9(4) . . ?
F15 P3 F18 83.8(4) . . ?
F15A P3 F13A 174.1(10) . . ?
F15A P3 F14A 96.0(12) . . ?
F15A P3 F16A 91.4(9) . . ?
F15A P3 F17 95.1(8) . . ?
F15A P3 F18 88.9(8) . . ?
F16 P3 F13 88.6(4) . . ?
F16 P3 F14 171.0(5) . . ?
F16 P3 F17 90.2(3) . . ?
F16 P3 F18 88.2(3) . . ?
F16A P3 F13A 82.7(8) . . ?
F17 P3 F13 84.7(5) . . ?
F17 P3 F13A 85.3(4) . . ?
F17 P3 F14 89.5(2) . . ?
F17 P3 F16A 86.7(5) . . ?
F18 P3 F13 99.7(5) . . ?
F18 P3 F13A 90.5(4) . . ?
F18 P3 F14 92.8(2) . . ?
F18 P3 F16A 90.6(5) . . ?
F18 P3 F17 175.2(2) . . ?
F1 P1 F3 178.39(13) . . ?
F1 P1 F4 90.52(13) . . ?
F1 P1 F5 90.50(10) . . ?
F2 P1 F1 92.30(14) . . ?
F2 P1 F3 89.24(13) . . ?
F2 P1 F4 177.11(14) . . ?
F2 P1 F5 90.14(13) . . ?
F2 P1 F6 90.83(13) . . ?
F4 P1 F3 87.93(11) . . ?
F4 P1 F5 89.21(11) . . ?
F5 P1 F3 89.04(10) . . ?
F6 P1 F1 90.42(11) . . ?
F6 P1 F3 90.01(10) . . ?
F6 P1 F4 89.77(12) . . ?
F6 P1 F5 178.63(11) . . ?
F8 P2 F7 89.87(11) . . ?
F8 P2 F9 89.08(11) . . ?
F8 P2 F11 89.09(13) . . ?
F9 P2 F7 178.91(11) . . ?
F10 P2 F7 89.76(12) . . ?
F10 P2 F8 178.79(16) . . ?
F10 P2 F9 91.29(12) . . ?
F10 P2 F11 89.76(16) . . ?
F11 P2 F7 90.25(11) . . ?
F11 P2 F9 89.46(12) . . ?
F12 P2 F7 90.25(12) . . ?
F12 P2 F8 91.18(15) . . ?
F12 P2 F9 90.05(13) . . ?
F12 P2 F10 89.98(18) . . ?
F12 P2 F11 179.44(16) . . ?
N2S C3S C4S 178.0(5) . . ?
N1S C1S C2S 178.7(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -174.8(3) . . . . ?
C1 C2 C3 C12 1.7(3) . . . . ?
C1 C2 N2 C21 -173.9(2) . . . . ?
C1 C2 N2 Cr1 3.9(3) . . . . ?
C1 C11 C12 C3 -1.4(3) . . . . ?
C1 C11 C12 C7 178.2(2) . . . . ?
C2 C1 C11 C10 -177.6(3) . . . . ?
C2 C1 C11 C12 2.4(2) . . . . ?
C2 C1 N1 C13 -179.62(19) . . . . ?
C2 C1 N1 Cr1 -3.0(2) . . . . ?
C2 C3 C4 C5 176.1(3) . . . . ?
C2 C3 C12 C7 -179.8(2) . . . . ?
C2 C3 C12 C11 -0.2(3) . . . . ?
C3 C2 N2 C21 6.8(4) . . . . ?
C3 C2 N2 Cr1 -175.5(2) . . . . ?
C3 C4 C5 C6 2.0(4) . . . . ?
C4 C3 C12 C7 -2.7(4) . . . . ?
C4 C3 C12 C11 176.9(2) . . . . ?
C4 C5 C6 C7 -1.5(4) . . . . ?
C5 C6 C7 C8 -179.2(3) . . . . ?
C5 C6 C7 C12 -1.1(4) . . . . ?
C6 C7 C8 C9 177.4(3) . . . . ?
C6 C7 C12 C3 3.2(4) . . . . ?
C6 C7 C12 C11 -176.4(2) . . . . ?
C7 C8 C9 C10 -0.7(4) . . . . ?
C8 C7 C12 C3 -178.5(2) . . . . ?
C8 C7 C12 C11 1.9(4) . . . . ?
C8 C9 C10 C11 0.9(4) . . . . ?
C9 C10 C11 C1 -179.7(3) . . . . ?
C9 C10 C11 C12 0.4(4) . . . . ?
C10 C11 C12 C3 178.6(2) . . . . ?
C10 C11 C12 C7 -1.8(4) . . . . ?
C11 C1 C2 C3 -2.6(3) . . . . ?
C11 C1 C2 N2 177.9(2) . . . . ?
C11 C1 N1 C13 2.5(4) . . . . ?
C11 C1 N1 Cr1 179.1(2) . . . . ?
C12 C3 C4 C5 0.0(4) . . . . ?
C12 C7 C8 C9 -0.7(4) . . . . ?
C13 C14 C15 C16 -1.5(3) . . . . ?
C13 C14 C15 C19 178.0(2) . . . . ?
C14 C13 C18 C17 2.2(3) . . . . ?
C14 C13 N1 C1 64.0(3) . . . . ?
C14 C13 N1 Cr1 -112.1(2) . . . . ?
C14 C15 C16 C17 1.8(4) . . . . ?
C15 C16 C17 C18 0.0(4) . . . . ?
C15 C16 C17 C20 -179.2(3) . . . . ?
C16 C17 C18 C13 -2.0(4) . . . . ?
C18 C13 C14 C15 -0.4(3) . . . . ?
C18 C13 N1 C1 -118.7(2) . . . . ?
C18 C13 N1 Cr1 65.2(3) . . . . ?
C19 C15 C16 C17 -177.7(2) . . . . ?
C20 C17 C18 C13 177.2(3) . . . . ?
C21 C22 C23 C24 0.0(4) . . . . ?
C21 C22 C23 C27 178.6(3) . . . . ?
C22 C21 C26 C25 0.7(4) . . . . ?
C22 C21 N2 C2 -110.0(3) . . . . ?
C22 C21 N2 Cr1 72.7(3) . . . . ?
C22 C23 C24 C25 -0.2(4) . . . . ?
C23 C24 C25 C26 0.6(4) . . . . ?
C23 C24 C25 C28 -178.3(3) . . . . ?
C24 C25 C26 C21 -0.9(4) . . . . ?
C26 C21 C22 C23 -0.2(4) . . . . ?
C26 C21 N2 C2 71.1(3) . . . . ?
C26 C21 N2 Cr1 -106.3(2) . . . . ?
C27 C23 C24 C25 -178.7(3) . . . . ?
C28 C25 C26 C21 178.0(3) . . . . ?
C29 C30 C31 C32 -178.8(3) . . . . ?
C29 C30 C31 C40 -2.1(2) . . . . ?
C29 C30 N4 C49 178.55(19) . . . . ?
C29 C30 N4 Cr1 3.6(2) . . . . ?
C29 C39 C40 C31 -1.7(3) . . . . ?
C29 C39 C40 C35 176.2(2) . . . . ?
C30 C29 C39 C38 177.6(3) . . . . ?
C30 C29 C39 C40 0.2(2) . . . . ?
C30 C29 N3 C41 179.27(19) . . . . ?
C30 C29 N3 Cr1 -8.2(2) . . . . ?
C30 C31 C32 C33 174.2(3) . . . . ?
C30 C31 C40 C35 -175.4(2) . . . . ?
C30 C31 C40 C39 2.4(3) . . . . ?
C31 C30 N4 C49 2.7(4) . . . . ?
C31 C30 N4 Cr1 -172.2(2) . . . . ?
C31 C32 C33 C34 0.8(4) . . . . ?
C32 C31 C40 C35 1.8(4) . . . . ?
C32 C31 C40 C39 179.7(2) . . . . ?
C32 C33 C34 C35 0.9(4) . . . . ?
C33 C34 C35 C36 179.1(3) . . . . ?
C33 C34 C35 C40 -1.2(4) . . . . ?
C34 C35 C36 C37 179.1(3) . . . . ?
C34 C35 C40 C31 -0.2(3) . . . . ?
C34 C35 C40 C39 -177.9(2) . . . . ?
C35 C36 C37 C38 -0.8(4) . . . . ?
C36 C35 C40 C31 179.6(2) . . . . ?
C36 C35 C40 C39 1.9(3) . . . . ?
C36 C37 C38 C39 1.1(4) . . . . ?
C37 C38 C39 C29 -177.0(3) . . . . ?
C37 C38 C39 C40 0.1(4) . . . . ?
C38 C39 C40 C31 -179.5(2) . . . . ?
C38 C39 C40 C35 -1.7(4) . . . . ?
C39 C29 C30 C31 1.2(2) . . . . ?
C39 C29 C30 N4 -175.7(2) . . . . ?
C39 C29 N3 C41 -2.2(4) . . . . ?
C39 C29 N3 Cr1 170.4(2) . . . . ?
C40 C31 C32 C33 -2.1(4) . . . . ?
C40 C35 C36 C37 -0.7(4) . . . . ?
C41 C42 C43 C44 -1.1(4) . . . . ?
C41 C42 C43 C47 179.3(2) . . . . ?
C42 C41 C46 C45 -2.6(4) . . . . ?
C42 C41 N3 C29 -113.3(3) . . . . ?
C42 C41 N3 Cr1 75.1(2) . . . . ?
C42 C43 C44 C45 -2.1(4) . . . . ?
C43 C44 C45 C46 3.0(4) . . . . ?
C43 C44 C45 C48 -176.3(3) . . . . ?
C44 C45 C46 C41 -0.6(4) . . . . ?
C46 C41 C42 C43 3.4(4) . . . . ?
C46 C41 N3 C29 70.7(3) . . . . ?
C46 C41 N3 Cr1 -100.9(2) . . . . ?
C47 C43 C44 C45 177.5(3) . . . . ?
C48 C45 C46 C41 178.7(2) . . . . ?
C49 C50 C51 C52 -1.0(4) . . . . ?
C49 C50 C51 C55 -179.9(2) . . . . ?
C50 C49 C54 C53 2.9(4) . . . . ?
C50 C49 N4 C30 86.2(3) . . . . ?
C50 C49 N4 Cr1 -99.5(2) . . . . ?
C50 C51 C52 C53 3.1(4) . . . . ?
C51 C52 C53 C54 -2.2(4) . . . . ?
C51 C52 C53 C56 177.7(3) . . . . ?
C52 C53 C54 C49 -0.8(4) . . . . ?
C54 C49 C50 C51 -2.0(4) . . . . ?
C54 C49 N4 C30 -98.2(3) . . . . ?
C54 C49 N4 Cr1 76.1(2) . . . . ?
C55 C51 C52 C53 -178.1(3) . . . . ?
C56 C53 C54 C49 179.3(2) . . . . ?
C57 C58 C59 C60 -175.8(3) . . . . ?
C57 C58 C59 C68 1.8(2) . . . . ?
C57 C58 N6 C77 -179.66(19) . . . . ?
C57 C58 N6 Cr1 -0.5(3) . . . . ?
C57 C67 C68 C59 -0.6(3) . . . . ?
C57 C67 C68 C63 178.7(2) . . . . ?
C58 C57 C67 C66 -178.4(3) . . . . ?
C58 C57 C67 C68 1.7(2) . . . . ?
C58 C57 N5 C69 -177.39(19) . . . . ?
C58 C57 N5 Cr1 2.2(2) . . . . ?
C58 C59 C60 C61 178.2(3) . . . . ?
C58 C59 C68 C63 179.9(2) . . . . ?
C58 C59 C68 C67 -0.8(3) . . . . ?
C59 C58 N6 C77 3.4(4) . . . . ?
C59 C58 N6 Cr1 -177.5(2) . . . . ?
C59 C60 C61 C62 0.7(4) . . . . ?
C60 C59 C68 C63 -2.0(4) . . . . ?
C60 C59 C68 C67 177.2(2) . . . . ?
C60 C61 C62 C63 -1.1(4) . . . . ?
C61 C62 C63 C64 -178.7(3) . . . . ?
C61 C62 C63 C68 0.0(4) . . . . ?
C62 C63 C64 C65 178.5(3) . . . . ?
C62 C63 C68 C59 1.6(4) . . . . ?
C62 C63 C68 C67 -177.6(2) . . . . ?
C63 C64 C65 C66 -1.0(4) . . . . ?
C64 C63 C68 C59 -179.6(2) . . . . ?
C64 C63 C68 C67 1.2(4) . . . . ?
C64 C65 C66 C67 1.0(4) . . . . ?
C65 C66 C67 C57 -179.8(3) . . . . ?
C65 C66 C67 C68 0.1(4) . . . . ?
C66 C67 C68 C59 179.5(2) . . . . ?
C66 C67 C68 C63 -1.2(4) . . . . ?
C67 C57 C58 C59 -2.2(2) . . . . ?
C67 C57 C58 N6 180.0(2) . . . . ?
C67 C57 N5 C69 1.0(4) . . . . ?
C67 C57 N5 Cr1 -179.4(2) . . . . ?
C68 C59 C60 C61 0.8(4) . . . . ?
C68 C63 C64 C65 -0.2(4) . . . . ?
C69 C70 C71 C72 -1.4(4) . . . . ?
C69 C70 C71 C75 179.1(2) . . . . ?
C70 C69 C74 C73 -0.8(4) . . . . ?
C70 C69 N5 C57 -103.7(3) . . . . ?
C70 C69 N5 Cr1 76.8(3) . . . . ?
C70 C71 C72 C73 -1.0(4) . . . . ?
C71 C72 C73 C74 2.5(4) . . . . ?
C71 C72 C73 C76 -176.6(3) . . . . ?
C72 C73 C74 C69 -1.6(4) . . . . ?
C74 C69 C70 C71 2.4(4) . . . . ?
C74 C69 N5 C57 78.3(3) . . . . ?
C74 C69 N5 Cr1 -101.2(2) . . . . ?
C75 C71 C72 C73 178.5(2) . . . . ?
C76 C73 C74 C69 177.5(2) . . . . ?
C77 C78 C79 C80 -1.7(4) . . . . ?
C77 C78 C79 C83 178.0(3) . . . . ?
C78 C77 C82 C81 1.8(4) . . . . ?
C78 C77 N6 C58 70.5(3) . . . . ?
C78 C77 N6 Cr1 -108.6(2) . . . . ?
C78 C79 C80 C81 1.3(4) . . . . ?
C79 C80 C81 C82 0.6(4) . . . . ?
C79 C80 C81 C84 -177.5(3) . . . . ?
C80 C81 C82 C77 -2.2(4) . . . . ?
C82 C77 C78 C79 0.1(4) . . . . ?
C82 C77 N6 C58 -110.4(3) . . . . ?
C82 C77 N6 Cr1 70.6(3) . . . . ?
C83 C79 C80 C81 -178.3(3) . . . . ?
C84 C81 C82 C77 176.0(3) . . . . ?
N1 C1 C2 C3 179.0(2) . . . . ?
N1 C1 C2 N2 -0.6(3) . . . . ?
N1 C1 C11 C10 0.4(5) . . . . ?
N1 C1 C11 C12 -179.6(3) . . . . ?
N1 C13 C14 C15 176.8(2) . . . . ?
N1 C13 C18 C17 -175.1(2) . . . . ?
N2 C2 C3 C4 4.7(5) . . . . ?
N2 C2 C3 C12 -178.9(3) . . . . ?
N2 C21 C22 C23 -179.2(2) . . . . ?
N2 C21 C26 C25 179.6(2) . . . . ?
N3 C29 C30 C31 -179.86(19) . . . . ?
N3 C29 C30 N4 3.2(3) . . . . ?
N3 C29 C39 C38 -1.1(5) . . . . ?
N3 C29 C39 C40 -178.4(3) . . . . ?
N3 C41 C42 C43 -172.5(2) . . . . ?
N3 C41 C46 C45 173.3(2) . . . . ?
N4 C30 C31 C32 -2.7(5) . . . . ?
N4 C30 C31 C40 174.0(3) . . . . ?
N4 C49 C50 C51 173.5(2) . . . . ?
N4 C49 C54 C53 -172.5(2) . . . . ?
N5 C57 C58 C59 176.6(2) . . . . ?
N5 C57 C58 N6 -1.2(3) . . . . ?
N5 C57 C67 C66 3.0(5) . . . . ?
N5 C57 C67 C68 -176.8(3) . . . . ?
N5 C69 C70 C71 -175.6(2) . . . . ?
N5 C69 C74 C73 177.2(2) . . . . ?
N6 C58 C59 C60 1.4(5) . . . . ?
N6 C58 C59 C68 179.0(3) . . . . ?
N6 C77 C78 C79 179.2(2) . . . . ?
N6 C77 C82 C81 -177.3(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-14 -20 15 0.1149 -13.9997 -19.9964 15.0010 -0.5336 -0.8472 -0.0593
-10 -24 -12 0.1229 -9.9993 -23.9962 -11.9990 -0.5421 -0.4476 0.6910
-7 -7 -30 0.1149 -6.9995 -6.9989 -29.9995 0.0612 -0.0199 0.9977
-1 -11 30 0.1160 -1.0001 -10.9981 30.0002 -0.5175 -0.4267 -0.7268
9 26 -9 0.0939 8.9995 25.9958 -9.0009 0.7489 0.6372 -0.1066
13 19 17 0.1660 12.9993 18.9968 16.9990 0.3155 0.4756 -0.8202
-3 -4 32 0.1268 -3.0003 -3.9990 32.0001 -0.2854 -0.4719 -0.8262
17 -5 22 0.1362 16.9997 -4.9999 21.9992 -0.5169 0.3992 -0.7786
-20 15 0 0.1072 -20.0001 14.9988 0.0007 0.7307 -0.6639 0.0992
-13 20 17 0.0737 -13.0005 19.9979 17.0002 0.6884 -0.5270 -0.5131
-4 -13 29 0.1201 -4.0001 -12.9977 29.0004 -0.5342 -0.5481 -0.6428
-10 -23 14 0.1034 -9.9997 -22.9962 14.0009 -0.6734 -0.7042 -0.0509
11 5 28 0.1460 10.9995 4.9990 27.9993 -0.1636 0.1805 -0.9708
15 -15 -18 0.0667 15.0004 -14.9987 -18.0004 -0.5524 0.6525 0.4687
4 6 32 0.1391 3.9995 5.9992 31.9996 -0.0654 -0.1245 -1.0078

_exptl_crystal_recrystallization_method 
'Slow diffusion of diethyl ether into a saturated MeCN solution of the complex'
_chemical_properties_physical    Moisture-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_raz-01-030t
_database_code_depnum_ccdc_archive 'CCDC 1448203'
_audit_update_record             
;
2016-01-19 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;
_audit_creation_date             2015-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2014-3
_chemical_name_common            tri(dmp-BIAN)Ga
_chemical_name_systematic        
"tri(N,N'-bis(3,5-dimethylphenylimino)acenaphthenesemiquinone) gallium"
_chemical_formula_moiety         'C84 H72 Ga1 N6'
_chemical_formula_sum            'C84 H72 Ga N6'
_chemical_formula_weight         1235.19
_chemical_melting_point          n/a

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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   13.1696(2)
_cell_length_b                   13.1696(2)
_cell_length_c                   72.1013(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10829.8(4)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    13510
_cell_measurement_temperature    151(2)
_cell_measurement_theta_max      28.7260
_cell_measurement_theta_min      3.0980
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3894
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.2909
_exptl_crystal_size_min          0.2537
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       98
_diffrn_reflns_limit_l_min       -95
_diffrn_reflns_number            35186
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.271
_diffrn_reflns_theta_min         3.094
_diffrn_ambient_temperature      151(2)
_diffrn_detector_area_resol_mean 10.2358
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0472173333
_diffrn_orient_matrix_UB_12      0.0412245667
_diffrn_orient_matrix_UB_13      0.0055372667
_diffrn_orient_matrix_UB_21      -0.0403906667
_diffrn_orient_matrix_UB_22      0.0029588667
_diffrn_orient_matrix_UB_23      0.0061715667
_diffrn_orient_matrix_UB_31      -0.0022634000
_diffrn_orient_matrix_UB_32      -0.0464512000
_diffrn_orient_matrix_UB_33      0.0053016000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2816
_reflns_number_total             3156
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3156
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0718P)²+7.3512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1192
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C13(H13)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)

All atoms are refined anisotropically and protons are generated 
in calculated positions and refined using the riding model. A 
450.2 Ang^3 solvent accessible void is present in the unit cell (~4.2%)
that corresponds to a total of 89 electrons. Attempts to model the disordered
THF molecules resulted in an unstable refinement of the model. The solvent mask
routine in OLEX 2 was used to remove this void for the final refinement.

;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.70309(10) 0.14336(11) 0.07519(2) 0.0250(3) Uani 1 1 d . . . . .
C2 C 0.72850(12) 0.05017(12) 0.07026(2) 0.0315(3) Uani 1 1 d . . . . .
C3 C 0.79466(14) 0.03496(14) 0.05692(3) 0.0417(4) Uani 1 1 d . . . . .
H3 H 0.8358 0.0923 0.0480 0.050 Uiso 1 1 calc R . . . .
C4 C 0.79780(18) -0.07157(17) 0.05719(3) 0.0589(5) Uani 1 1 d . . . . .
H4 H 0.8438 -0.0819 0.0485 0.071 Uiso 1 1 calc R . . . .
C5 C 0.7368(2) -0.15866(18) 0.06960(4) 0.0660(6) Uani 1 1 d . . . . .
H5 H 0.7410 -0.2270 0.0691 0.079 Uiso 1 1 calc R . . . .
C6 C 0.6667 -0.14671(18) 0.0833 0.0510(7) Uani 1 2 d S T P . .
C7 C 0.6667 -0.04014(15) 0.0833 0.0354(4) Uani 1 2 d S T P . .
C8 C 0.81018(11) 0.29233(11) 0.05253(2) 0.0266(3) Uani 1 1 d . . . . .
C9 C 0.77080(13) 0.25151(14) 0.03469(2) 0.0356(3) Uani 1 1 d . . . . .
H9 H 0.6941 0.1915 0.0328 0.043 Uiso 1 1 calc R . . . .
C10 C 0.84636(15) 0.30070(16) 0.01968(2) 0.0449(4) Uani 1 1 d . . . . .
C11 C 0.96006(15) 0.39065(16) 0.02270(2) 0.0468(4) Uani 1 1 d . . . . .
H11 H 1.0101 0.4240 0.0126 0.056 Uiso 1 1 calc R . . . .
C12 C 1.00106(13) 0.43221(15) 0.04044(2) 0.0398(3) Uani 1 1 d . . . . .
C13 C 0.92468(12) 0.38157(13) 0.05527(2) 0.0309(3) Uani 1 1 d . . . . .
H13 H 0.9508 0.4080 0.0672 0.037 Uiso 1 1 calc R . . . .
C14 C 0.8032(2) 0.2563(3) 0.00025(3) 0.0740(7) Uani 1 1 d . . . . .
H14A H 0.7810 0.1750 -0.0006 0.111 Uiso 1 1 calc GR . . . .
H14B H 0.8646 0.3006 -0.0085 0.111 Uiso 1 1 calc GR . . . .
H14C H 0.7366 0.2650 -0.0025 0.111 Uiso 1 1 calc GR . . . .
C15 C 1.12494(17) 0.5303(2) 0.04386(3) 0.0642(6) Uani 1 1 d . . . . .
H15A H 1.1237 0.5998 0.0475 0.096 Uiso 1 1 calc GR . . . .
H15B H 1.1701 0.5455 0.0327 0.096 Uiso 1 1 calc GR . . . .
H15C H 1.1597 0.5079 0.0536 0.096 Uiso 1 1 calc GR . . . .
N1 N 0.73377(9) 0.24739(9) 0.06814(2) 0.0248(2) Uani 1 1 d . . . . .
Ga1 Ga 0.6667 0.3333 0.0833 0.02075(12) Uani 1 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C1 1.438(2) 18_654 ?
C1 C2 1.4681(17) . ?
C1 N1 1.3210(17) . ?
C2 C3 1.378(2) . ?
C2 C7 1.4133(18) . ?
C3 C4 1.424(2) . ?
C4 C5 1.356(3) . ?
C5 C6 1.415(2) . ?
C6 C5 1.415(2) 18_654 ?
C6 C7 1.403(3) . ?
C7 C2 1.4132(18) 18_654 ?
C8 C9 1.3901(19) . ?
C8 C13 1.3864(19) . ?
C8 N1 1.4264(16) . ?
C9 C10 1.392(2) . ?
C10 C11 1.385(2) . ?
C10 C14 1.515(2) . ?
C11 C12 1.390(2) . ?
C12 C13 1.3890(19) . ?
C12 C15 1.511(2) . ?
N1 Ga1 2.0645(11) . ?
Ga1 N1 2.0646(11) 18_654 ?
Ga1 N1 2.0645(11) 16_544 ?
Ga1 N1 2.0645(11) 17_554 ?
Ga1 N1 2.0646(11) 2_655 ?
Ga1 N1 2.0646(11) 3_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C1 C2 108.15(8) 18_654 . ?
N1 C1 C1 117.85(7) . 18_654 ?
N1 C1 C2 133.99(12) . . ?
C3 C2 C1 135.68(14) . . ?
C3 C2 C7 118.91(14) . . ?
C7 C2 C1 105.41(12) . . ?
C2 C3 C4 117.73(16) . . ?
C5 C4 C3 123.04(18) . . ?
C4 C5 C6 120.74(18) . . ?
C5 C6 C5 128.1(2) . 18_654 ?
C7 C6 C5 115.94(12) . 18_654 ?
C7 C6 C5 115.93(12) . . ?
C2 C7 C2 112.79(17) . 18_654 ?
C6 C7 C2 123.60(9) . 18_654 ?
C6 C7 C2 123.60(9) . . ?
C9 C8 N1 121.34(12) . . ?
C13 C8 C9 119.81(12) . . ?
C13 C8 N1 118.80(11) . . ?
C8 C9 C10 119.85(14) . . ?
C9 C10 C14 119.77(17) . . ?
C11 C10 C9 119.44(14) . . ?
C11 C10 C14 120.79(16) . . ?
C10 C11 C12 121.48(14) . . ?
C11 C12 C15 121.85(14) . . ?
C13 C12 C11 118.30(14) . . ?
C13 C12 C15 119.85(15) . . ?
C8 C13 C12 121.11(13) . . ?
C1 N1 C8 121.37(11) . . ?
C1 N1 Ga1 111.81(8) . . ?
C8 N1 Ga1 126.72(8) . . ?
N1 Ga1 N1 173.11(6) . 16_544 ?
N1 Ga1 N1 94.46(4) 17_554 18_654 ?
N1 Ga1 N1 90.80(6) 3_665 18_654 ?
N1 Ga1 N1 90.80(6) 2_655 16_544 ?
N1 Ga1 N1 94.46(4) 18_654 16_544 ?
N1 Ga1 N1 94.46(4) 17_554 16_544 ?
N1 Ga1 N1 80.68(6) 3_665 16_544 ?
N1 Ga1 N1 173.11(6) 2_655 18_654 ?
N1 Ga1 N1 94.45(4) 2_655 3_665 ?
N1 Ga1 N1 94.45(4) . 3_665 ?
N1 Ga1 N1 94.45(4) . 2_655 ?
N1 Ga1 N1 90.79(6) . 17_554 ?
N1 Ga1 N1 80.67(6) . 18_654 ?
N1 Ga1 N1 173.11(6) 3_665 17_554 ?
N1 Ga1 N1 80.68(6) 2_655 17_554 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1 C2 C3 -177.26(17) 18_654 . . . ?
C1 C1 C2 C7 2.06(16) 18_654 . . . ?
C1 C1 N1 C8 177.09(13) 18_654 . . . ?
C1 C1 N1 Ga1 0.55(18) 18_654 . . . ?
C1 C2 C3 C4 178.66(17) . . . . ?
C1 C2 C7 C2 -0.77(6) . . . 18_654 ?
C1 C2 C7 C6 179.22(6) . . . . ?
C2 C1 N1 C8 -1.7(2) . . . . ?
C2 C1 N1 Ga1 -178.26(12) . . . . ?
C2 C3 C4 C5 1.7(3) . . . . ?
C3 C2 C7 C2 178.68(15) . . . 18_654 ?
C3 C2 C7 C6 -1.32(15) . . . . ?
C3 C4 C5 C6 -0.9(4) . . . . ?
C4 C5 C6 C5 179.0(3) . . . 18_654 ?
C4 C5 C6 C7 -1.0(3) . . . . ?
C5 C6 C7 C2 -177.90(14) . . . 18_654 ?
C5 C6 C7 C2 2.10(14) . . . . ?
C5 C6 C7 C2 -177.89(14) 18_654 . . . ?
C5 C6 C7 C2 2.11(14) 18_654 . . 18_654 ?
C7 C2 C3 C4 -0.6(2) . . . . ?
C8 C9 C10 C11 -0.5(3) . . . . ?
C8 C9 C10 C14 -179.88(19) . . . . ?
C9 C8 C13 C12 0.7(2) . . . . ?
C9 C8 N1 C1 75.92(18) . . . . ?
C9 C8 N1 Ga1 -108.09(14) . . . . ?
C9 C10 C11 C12 0.7(3) . . . . ?
C10 C11 C12 C13 -0.3(3) . . . . ?
C10 C11 C12 C15 180.0(2) . . . . ?
C11 C12 C13 C8 -0.4(2) . . . . ?
C13 C8 C9 C10 -0.2(2) . . . . ?
C13 C8 N1 C1 -106.50(15) . . . . ?
C13 C8 N1 Ga1 69.49(15) . . . . ?
C14 C10 C11 C12 -179.8(2) . . . . ?
C15 C12 C13 C8 179.30(18) . . . . ?
N1 C1 C2 C3 1.6(3) . . . . ?
N1 C1 C2 C7 -179.05(13) . . . . ?
N1 C8 C9 C10 177.33(14) . . . . ?
N1 C8 C13 C12 -176.95(13) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 71.7 14.3 ?
2 0.000 0.000 0.090 1.7 0.3 ?
3 0.000 0.000 0.410 1.7 0.3 ?
4 0.000 0.000 0.500 71.7 14.3 ?
5 0.000 0.000 0.590 1.7 0.3 ?
6 0.000 0.000 0.910 1.7 0.3 ?
7 0.333 0.667 0.667 71.7 14.3 ?
8 0.333 0.667 0.167 71.7 14.3 ?
9 0.333 0.667 0.076 1.7 0.3 ?
10 0.333 0.667 0.576 1.7 0.3 ?
11 0.333 0.667 0.257 1.7 0.3 ?
12 0.333 0.667 0.757 1.7 0.3 ?
13 0.667 0.333 0.333 71.7 14.3 ?
14 0.667 0.333 0.833 71.7 14.3 ?
15 0.667 0.333 0.243 1.7 0.3 ?
16 0.667 0.333 0.743 1.7 0.3 ?
17 0.667 0.333 0.924 1.7 0.3 ?
18 0.667 0.333 0.424 1.7 0.3 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 12 -67 0.1533 0.4999 11.9988 -66.9900 0.1473 -0.3981 -0.9136
9 -17 -46 0.1434 8.9994 -16.9988 -45.9969 -0.5305 -0.6977 0.5254
-3 -14 -28 0.1234 -3.0000 -13.9987 -28.0016 -0.8738 -0.0931 0.5086
-10 -2 -74 0.1272 -9.9996 -1.9997 -73.9959 -0.9643 -0.0587 -0.2768
6 -18 -25 0.1463 6.4995 -17.9986 -25.0001 -0.5735 -0.4701 0.6888
-7 18 23 0.1426 -6.9995 17.9986 23.0002 0.5388 0.4779 -0.6983
-4 18 15 0.1415 -4.4996 17.9985 15.0017 0.6126 0.3276 -0.7463
-15 1 39 0.1289 -15.4991 1.0003 38.9918 -0.4747 0.8696 0.1953
18 -12 5 0.1833 18.4989 -11.9994 5.0020 0.4065 -0.7518 0.5420
7 -16 55 0.1557 7.4996 -15.9987 54.9926 -0.0009 -0.0109 1.0177
-15 15 -29 0.1296 -15.4991 14.9990 -28.9979 -0.2741 0.4914 -0.8154
0 -13 61 0.1556 0.0001 -12.9987 60.9905 -0.1981 0.3379 0.9272
-4 3 98 0.1586 -3.9996 3.0000 97.9896 0.4774 0.7752 0.3892
-2 -4 -95 0.1173 -1.5001 -3.9998 -94.9919 -0.7617 -0.5375 -0.3144
3 -5 -98 0.1209 3.4996 -4.9998 -97.9903 -0.5835 -0.7609 -0.2952
-14 -1 44 0.1389 -13.9992 -0.9995 43.9911 -0.4586 0.8340 0.3113
-4 16 43 0.1484 -3.9996 15.9987 42.9985 0.7088 0.4743 -0.5061
-6 17 40 0.1427 -5.9995 16.9987 39.9985 0.6390 0.5395 -0.5640
-5 16 49 0.1451 -5.4995 15.9988 48.9974 0.6712 0.5719 -0.4709
4 1 95 0.1253 4.4999 0.9999 94.9919 0.7797 0.4075 0.4470
14 1 -33 0.1599 14.4991 0.9995 -32.9922 0.5431 -0.7863 -0.2542
-3 2 -99 0.1224 -2.5000 1.9997 -98.9902 -0.5837 -0.5040 -0.6120
16 -4 -41 0.1578 16.4990 -4.0001 -40.9920 0.3872 -0.9312 -0.0689

_exptl_crystal_recrystallization_method 'Slow evaporation of THF'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_raz01149b
_database_code_depnum_ccdc_archive 'CCDC 1448204'
_audit_update_record             
;
2016-01-19 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;
_audit_creation_date             2015-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2014-3
_chemical_name_common            'tris(dmp-BIAN)Ga tri-PF6'
_chemical_name_systematic        
"tri(N,N'-bis(3,5-dimethylphenylimino)acenaphthenequinone) gallium tri(hexafluorophosphate)"
_chemical_formula_moiety         'C84 H72 Ga N6, 3(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C88 H78 F18 Ga N8 P3'
_chemical_formula_weight         1752.21
_chemical_melting_point          n/a

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'
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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.6140(2)
_cell_length_b                   21.1569(3)
_cell_length_c                   23.2187(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.3726(12)
_cell_angle_gamma                90
_cell_volume                     8159.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    41633
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.4610
_cell_measurement_theta_min      2.8860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.2583
_exptl_crystal_size_mid          0.2182
_exptl_crystal_size_min          0.1781
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.897
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            228412
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.605
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2358
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0380276000
_diffrn_orient_matrix_UB_12      0.0108410000
_diffrn_orient_matrix_UB_13      -0.0091247000
_diffrn_orient_matrix_UB_21      -0.0010778000
_diffrn_orient_matrix_UB_22      0.0247294000
_diffrn_orient_matrix_UB_23      0.0206046000
_diffrn_orient_matrix_UB_31      0.0194150000
_diffrn_orient_matrix_UB_32      -0.0198670000
_diffrn_orient_matrix_UB_33      0.0206371000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11745
_reflns_number_total             14387
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         14387
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0479
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0557P)²+12.0573P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1275
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16),
 C18(H18), C22(H22), C24(H24), C26(H26), C32(H32), C33(H33), C34(H34), C36(H36),
  C37(H37), C38(H38), C42(H42), C44(H44), C46(H46), C50(H50), C52(H52),
 C54(H54), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C70(H70),
  C72(H72), C74(H74), C78(H78), C80(H80), C82(H82)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C83(H83A,H83B,H83C),
 C84(H84A,H84B,H84C), C4S(H4SA,H4SB,H4SC), C2S(H2SA,H2SB,H2SC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.00158(16) 0.87726(12) 0.21239(11) 0.0227(6) Uani 1 1 d . . . . .
C2 C 0.05013(15) 0.84413(12) 0.16877(11) 0.0216(6) Uani 1 1 d . . . . .
C3 C 0.06585(16) 0.88893(13) 0.12292(12) 0.0254(6) Uani 1 1 d . . . . .
C4 C 0.10650(17) 0.88684(15) 0.07201(12) 0.0305(6) Uani 1 1 d . . . . .
H4 H 0.1317 0.8500 0.0600 0.037 Uiso 1 1 calc R . . . .
C5 C 0.10870(19) 0.94250(16) 0.03859(13) 0.0379(7) Uani 1 1 d . . . . .
H5 H 0.1353 0.9415 0.0038 0.045 Uiso 1 1 calc R . . . .
C6 C 0.07333(19) 0.99801(15) 0.05509(14) 0.0379(7) Uani 1 1 d . . . . .
H6 H 0.0769 1.0335 0.0317 0.045 Uiso 1 1 calc R . . . .
C7 C 0.03139(17) 1.00175(14) 0.10749(14) 0.0336(7) Uani 1 1 d . . . . .
C8 C -0.00694(19) 1.05543(14) 0.13100(15) 0.0390(8) Uani 1 1 d . . . . .
H8 H -0.0068 1.0935 0.1109 0.047 Uiso 1 1 calc R . . . .
C9 C -0.04426(19) 1.05202(15) 0.18294(15) 0.0394(8) Uani 1 1 d . . . . .
H9 H -0.0678 1.0883 0.1976 0.047 Uiso 1 1 calc R . . . .
C10 C -0.04815(18) 0.99573(14) 0.21480(14) 0.0330(7) Uani 1 1 d . . . . .
H10 H -0.0743 0.9944 0.2498 0.040 Uiso 1 1 calc R . . . .
C11 C -0.01211(16) 0.94229(13) 0.19277(12) 0.0272(6) Uani 1 1 d . . . . .
C12 C 0.02817(16) 0.94616(13) 0.13978(12) 0.0264(6) Uani 1 1 d . . . . .
C13 C -0.07209(16) 0.87422(13) 0.29949(12) 0.0250(6) Uani 1 1 d . . . . .
C14 C -0.03830(17) 0.88669(13) 0.35333(12) 0.0267(6) Uani 1 1 d . . . . .
H14 H 0.0158 0.8782 0.3610 0.032 Uiso 1 1 calc R . . . .
C15 C -0.08604(18) 0.91210(14) 0.39593(12) 0.0314(7) Uani 1 1 d . . . . .
C16 C -0.16612(18) 0.92605(15) 0.38239(13) 0.0352(7) Uani 1 1 d . . . . .
H16 H -0.1982 0.9432 0.4107 0.042 Uiso 1 1 calc R . . . .
C17 C -0.19956(17) 0.91505(15) 0.32778(13) 0.0342(7) Uani 1 1 d . . . . .
C18 C -0.15204(17) 0.88781(14) 0.28632(13) 0.0301(6) Uani 1 1 d . . . . .
H18 H -0.1736 0.8787 0.2499 0.036 Uiso 1 1 calc R . . . .
C19 C -0.0510(2) 0.92184(19) 0.45597(13) 0.0463(9) Uani 1 1 d . . . . .
H19A H -0.0846 0.9504 0.4767 0.069 Uiso 1 1 calc GR . . . .
H19B H 0.0021 0.9393 0.4536 0.069 Uiso 1 1 calc GR . . . .
H19C H -0.0483 0.8820 0.4757 0.069 Uiso 1 1 calc GR . . . .
C20 C -0.2861(2) 0.9322(2) 0.31322(16) 0.0515(10) Uani 1 1 d . . . . .
H20A H -0.2992 0.9192 0.2745 0.077 Uiso 1 1 calc GR . . . .
H20B H -0.2930 0.9771 0.3165 0.077 Uiso 1 1 calc GR . . . .
H20C H -0.3211 0.9111 0.3394 0.077 Uiso 1 1 calc GR . . . .
C21 C 0.12214(16) 0.75275(12) 0.14133(11) 0.0220(5) Uani 1 1 d . . . . .
C22 C 0.20439(17) 0.76349(14) 0.14368(12) 0.0275(6) Uani 1 1 d . . . . .
H22 H 0.2262 0.7937 0.1686 0.033 Uiso 1 1 calc R . . . .
C23 C 0.25395(18) 0.72856(15) 0.10829(13) 0.0331(7) Uani 1 1 d . . . . .
C24 C 0.21969(19) 0.68274(15) 0.07273(13) 0.0351(7) Uani 1 1 d . . . . .
H24 H 0.2530 0.6581 0.0502 0.042 Uiso 1 1 calc R . . . .
C25 C 0.13698(19) 0.67237(13) 0.06967(12) 0.0305(7) Uani 1 1 d . . . . .
C26 C 0.08787(17) 0.70855(13) 0.10431(11) 0.0249(6) Uani 1 1 d . . . . .
H26 H 0.0323 0.7031 0.1026 0.030 Uiso 1 1 calc R . . . .
C27 C 0.3433(2) 0.7415(2) 0.10860(18) 0.0545(10) Uani 1 1 d . . . . .
H27A H 0.3535 0.7785 0.0859 0.082 Uiso 1 1 calc GR . . . .
H27B H 0.3708 0.7060 0.0927 0.082 Uiso 1 1 calc GR . . . .
H27C H 0.3623 0.7485 0.1475 0.082 Uiso 1 1 calc GR . . . .
C28 C 0.1012(2) 0.62351(15) 0.03001(14) 0.0433(8) Uani 1 1 d . . . . .
H28A H 0.1110 0.5822 0.0458 0.065 Uiso 1 1 calc GR . . . .
H28B H 0.1254 0.6267 -0.0070 0.065 Uiso 1 1 calc GR . . . .
H28C H 0.0442 0.6304 0.0259 0.065 Uiso 1 1 calc GR . . . .
C29 C -0.05877(15) 0.66079(13) 0.18738(11) 0.0219(6) Uani 1 1 d . . . . .
C30 C 0.01981(16) 0.62971(13) 0.20739(11) 0.0229(6) Uani 1 1 d . . . . .
C31 C 0.02515(16) 0.56920(13) 0.17719(11) 0.0228(6) Uani 1 1 d . . . . .
C32 C 0.08058(17) 0.52158(13) 0.17532(12) 0.0271(6) Uani 1 1 d . . . . .
H32 H 0.1271 0.5228 0.1984 0.033 Uiso 1 1 calc R . . . .
C33 C 0.06549(18) 0.47043(14) 0.13752(13) 0.0336(7) Uani 1 1 d . . . . .
H33 H 0.1027 0.4376 0.1364 0.040 Uiso 1 1 calc R . . . .
C34 C -0.00168(18) 0.46741(14) 0.10260(13) 0.0329(7) Uani 1 1 d . . . . .
H34 H -0.0090 0.4329 0.0782 0.040 Uiso 1 1 calc R . . . .
C35 C -0.06060(17) 0.51611(13) 0.10300(12) 0.0271(6) Uani 1 1 d . . . . .
C36 C -0.13211(18) 0.52091(14) 0.06922(12) 0.0319(7) Uani 1 1 d . . . . .
H36 H -0.1441 0.4897 0.0422 0.038 Uiso 1 1 calc R . . . .
C37 C -0.18416(18) 0.57051(15) 0.07531(13) 0.0336(7) Uani 1 1 d . . . . .
H37 H -0.2312 0.5715 0.0528 0.040 Uiso 1 1 calc R . . . .
C38 C -0.16865(17) 0.61989(14) 0.11446(12) 0.0303(6) Uani 1 1 d . . . . .
H38 H -0.2050 0.6530 0.1184 0.036 Uiso 1 1 calc R . . . .
C39 C -0.09819(16) 0.61804(13) 0.14688(11) 0.0236(6) Uani 1 1 d . . . . .
C40 C -0.04542(16) 0.56591(13) 0.14153(11) 0.0228(6) Uani 1 1 d . . . . .
C41 C -0.14522(16) 0.75149(13) 0.18861(11) 0.0239(6) Uani 1 1 d . . . . .
C42 C -0.13958(17) 0.79535(13) 0.14434(12) 0.0273(6) Uani 1 1 d . . . . .
H42 H -0.0926 0.7986 0.1236 0.033 Uiso 1 1 calc R . . . .
C43 C -0.20487(18) 0.83433(14) 0.13146(13) 0.0334(7) Uani 1 1 d . . . . .
C44 C -0.27448(18) 0.82760(15) 0.16279(13) 0.0356(7) Uani 1 1 d . . . . .
H44 H -0.3176 0.8546 0.1550 0.043 Uiso 1 1 calc R . . . .
C45 C -0.28177(17) 0.78208(16) 0.20519(13) 0.0340(7) Uani 1 1 d . . . . .
C46 C -0.21524(17) 0.74357(14) 0.21870(12) 0.0295(6) Uani 1 1 d . . . . .
H46 H -0.2182 0.7132 0.2475 0.035 Uiso 1 1 calc R . . . .
C47 C -0.1993(2) 0.88292(17) 0.08396(16) 0.0506(9) Uani 1 1 d . . . . .
H47A H -0.1707 0.9193 0.0982 0.076 Uiso 1 1 calc GR . . . .
H47B H -0.2525 0.8951 0.0714 0.076 Uiso 1 1 calc GR . . . .
H47C H -0.1712 0.8651 0.0522 0.076 Uiso 1 1 calc GR . . . .
C48 C -0.35880(19) 0.7740(2) 0.23739(16) 0.0507(9) Uani 1 1 d . . . . .
H48A H -0.3845 0.7353 0.2256 0.076 Uiso 1 1 calc GR . . . .
H48B H -0.3941 0.8089 0.2290 0.076 Uiso 1 1 calc GR . . . .
H48C H -0.3469 0.7725 0.2780 0.076 Uiso 1 1 calc GR . . . .
C49 C 0.13979(15) 0.63736(12) 0.26689(11) 0.0213(5) Uani 1 1 d . . . . .
C50 C 0.20666(16) 0.63228(13) 0.23293(12) 0.0252(6) Uani 1 1 d . . . . .
H50 H 0.2024 0.6400 0.1935 0.030 Uiso 1 1 calc R . . . .
C51 C 0.28055(17) 0.61551(13) 0.25830(13) 0.0301(6) Uani 1 1 d . . . . .
C52 C 0.28456(18) 0.60511(13) 0.31710(13) 0.0325(7) Uani 1 1 d . . . . .
H52 H 0.3342 0.5958 0.3344 0.039 Uiso 1 1 calc R . . . .
C53 C 0.21715(18) 0.60806(13) 0.35125(12) 0.0302(7) Uani 1 1 d . . . . .
C54 C 0.14363(17) 0.62400(12) 0.32536(12) 0.0251(6) Uani 1 1 d . . . . .
H54 H 0.0974 0.6257 0.3471 0.030 Uiso 1 1 calc R . . . .
C55 C 0.35402(19) 0.60847(18) 0.22179(16) 0.0464(9) Uani 1 1 d . . . . .
H55A H 0.3577 0.5657 0.2084 0.070 Uiso 1 1 calc GR . . . .
H55B H 0.4014 0.6187 0.2444 0.070 Uiso 1 1 calc GR . . . .
H55C H 0.3497 0.6365 0.1894 0.070 Uiso 1 1 calc GR . . . .
C56 C 0.2229(2) 0.59407(19) 0.41486(14) 0.0507(9) Uani 1 1 d . . . . .
H56A H 0.1719 0.6024 0.4320 0.076 Uiso 1 1 calc GR . . . .
H56B H 0.2635 0.6204 0.4326 0.076 Uiso 1 1 calc GR . . . .
H56C H 0.2369 0.5505 0.4206 0.076 Uiso 1 1 calc GR . . . .
C57 C 0.02357(16) 0.73591(13) 0.37569(11) 0.0228(6) Uani 1 1 d . . . . .
C58 C 0.10399(15) 0.76540(12) 0.36253(11) 0.0207(5) Uani 1 1 d . . . . .
C59 C 0.14843(16) 0.77194(13) 0.41715(11) 0.0227(6) Uani 1 1 d . . . . .
C60 C 0.22163(17) 0.79680(13) 0.43381(12) 0.0269(6) Uani 1 1 d . . . . .
H60 H 0.2554 0.8149 0.4071 0.032 Uiso 1 1 calc R . . . .
C61 C 0.24404(18) 0.79400(15) 0.49282(12) 0.0320(7) Uani 1 1 d . . . . .
H61 H 0.2932 0.8112 0.5047 0.038 Uiso 1 1 calc R . . . .
C62 C 0.19653(19) 0.76707(15) 0.53301(13) 0.0348(7) Uani 1 1 d . . . . .
H62 H 0.2141 0.7661 0.5713 0.042 Uiso 1 1 calc R . . . .
C63 C 0.12060(18) 0.74044(14) 0.51743(12) 0.0294(6) Uani 1 1 d . . . . .
C64 C 0.06590(19) 0.70916(16) 0.55313(13) 0.0367(7) Uani 1 1 d . . . . .
H64 H 0.0786 0.7044 0.5921 0.044 Uiso 1 1 calc R . . . .
C65 C -0.00578(19) 0.68552(16) 0.53151(13) 0.0374(7) Uani 1 1 d . . . . .
H65 H -0.0398 0.6642 0.5561 0.045 Uiso 1 1 calc R . . . .
C66 C -0.02911(18) 0.69261(15) 0.47300(12) 0.0315(7) Uani 1 1 d . . . . .
H66 H -0.0785 0.6775 0.4592 0.038 Uiso 1 1 calc R . . . .
C67 C 0.02334(16) 0.72250(13) 0.43701(11) 0.0255(6) Uani 1 1 d . . . . .
C68 C 0.09805(16) 0.74517(13) 0.45906(12) 0.0242(6) Uani 1 1 d . . . . .
C69 C -0.10763(16) 0.70571(13) 0.34497(11) 0.0243(6) Uani 1 1 d . . . . .
C70 C -0.16042(17) 0.74643(15) 0.37112(12) 0.0303(6) Uani 1 1 d . . . . .
H70 H -0.1440 0.7871 0.3811 0.036 Uiso 1 1 calc R . . . .
C71 C -0.23833(18) 0.72641(16) 0.38259(13) 0.0360(7) Uani 1 1 d . . . . .
C72 C -0.26031(18) 0.66574(17) 0.36634(14) 0.0410(8) Uani 1 1 d . . . . .
H72 H -0.3122 0.6520 0.3737 0.049 Uiso 1 1 calc R . . . .
C73 C -0.20809(19) 0.62449(16) 0.33950(15) 0.0390(8) Uani 1 1 d . . . . .
C74 C -0.12990(17) 0.64489(14) 0.32899(13) 0.0307(6) Uani 1 1 d . . . . .
H74 H -0.0933 0.6181 0.3115 0.037 Uiso 1 1 calc R . . . .
C75 C -0.2957(2) 0.7695(2) 0.41278(17) 0.0552(10) Uani 1 1 d . . . . .
H75A H -0.3009 0.7559 0.4520 0.083 Uiso 1 1 calc GR . . . .
H75B H -0.3474 0.7681 0.3935 0.083 Uiso 1 1 calc GR . . . .
H75C H -0.2753 0.8120 0.4122 0.083 Uiso 1 1 calc GR . . . .
C76 C -0.2344(2) 0.55916(18) 0.3216(2) 0.0641(12) Uani 1 1 d . . . . .
H76A H -0.2597 0.5609 0.2841 0.096 Uiso 1 1 calc GR . . . .
H76B H -0.2720 0.5431 0.3488 0.096 Uiso 1 1 calc GR . . . .
H76C H -0.1884 0.5318 0.3207 0.096 Uiso 1 1 calc GR . . . .
C77 C 0.19088(15) 0.80813(12) 0.29204(11) 0.0210(5) Uani 1 1 d . . . . .
C78 C 0.26343(16) 0.77574(13) 0.29785(11) 0.0238(6) Uani 1 1 d . . . . .
H78 H 0.2651 0.7360 0.3150 0.029 Uiso 1 1 calc R . . . .
C79 C 0.33336(17) 0.80315(14) 0.27779(12) 0.0277(6) Uani 1 1 d . . . . .
C80 C 0.32840(18) 0.86215(15) 0.25119(12) 0.0321(7) Uani 1 1 d . . . . .
H80 H 0.3748 0.8802 0.2367 0.038 Uiso 1 1 calc R . . . .
C81 C 0.25617(18) 0.89470(14) 0.24566(13) 0.0309(6) Uani 1 1 d . . . . .
C82 C 0.18748(16) 0.86733(13) 0.26720(11) 0.0244(6) Uani 1 1 d . . . . .
H82 H 0.1388 0.8890 0.2649 0.029 Uiso 1 1 calc R . . . .
C83 C 0.41351(18) 0.77041(17) 0.28500(15) 0.0413(8) Uani 1 1 d . . . . .
H83A H 0.4473 0.7940 0.3113 0.062 Uiso 1 1 calc GR . . . .
H83B H 0.4388 0.7677 0.2483 0.062 Uiso 1 1 calc GR . . . .
H83C H 0.4055 0.7286 0.3000 0.062 Uiso 1 1 calc GR . . . .
C84 C 0.2507(2) 0.95799(16) 0.21647(18) 0.0526(10) Uani 1 1 d . . . . .
H84A H 0.2131 0.9556 0.1845 0.079 Uiso 1 1 calc GR . . . .
H84B H 0.3027 0.9697 0.2029 0.079 Uiso 1 1 calc GR . . . .
H84C H 0.2328 0.9891 0.2434 0.079 Uiso 1 1 calc GR . . . .
N1 N -0.02296(13) 0.84542(10) 0.25620(9) 0.0221(5) Uani 1 1 d . . . . .
N2 N 0.07068(13) 0.78708(10) 0.17999(9) 0.0207(5) Uani 1 1 d . . . . .
N3 N -0.07360(13) 0.71635(10) 0.20621(9) 0.0213(5) Uani 1 1 d . . . . .
N4 N 0.06435(13) 0.66114(10) 0.24289(9) 0.0211(5) Uani 1 1 d . . . . .
N5 N -0.02707(13) 0.72821(11) 0.33362(9) 0.0218(5) Uani 1 1 d . . . . .
N6 N 0.11686(13) 0.77947(10) 0.30969(9) 0.0205(5) Uani 1 1 d . . . . .
Ga1 Ga 0.02114(2) 0.75286(2) 0.25580(2) 0.01936(9) Uani 1 1 d . . . . .
F7 F 0.37544(15) 0.71417(18) 0.42943(12) 0.0959(10) Uani 1 1 d . . . . .
F8 F 0.4618(2) 0.79387(11) 0.43964(11) 0.0959(10) Uani 1 1 d . . . . .
F9 F 0.54715(13) 0.73016(12) 0.48839(9) 0.0637(6) Uani 1 1 d . . . . .
F10 F 0.45994(17) 0.65067(11) 0.47881(11) 0.0730(7) Uani 1 1 d . . . . .
F11 F 0.50211(13) 0.70291(10) 0.39988(8) 0.0511(5) Uani 1 1 d . . . . .
F12 F 0.42154(14) 0.74269(12) 0.51844(9) 0.0672(7) Uani 1 1 d . . . . .
P2 P 0.46102(5) 0.72291(4) 0.45881(4) 0.0398(2) Uani 1 1 d . . . . .
F13 F -0.01726(17) 0.52939(11) 0.36603(13) 0.0803(8) Uani 1 1 d . . . . .
F14 F 0.0541(2) 0.47900(16) 0.30064(16) 0.1234(14) Uani 1 1 d . . . . .
F15 F -0.0017(2) 0.38716(17) 0.3281(2) 0.1487(18) Uani 1 1 d . . . . .
F16 F -0.0836(3) 0.44181(17) 0.3785(3) 0.186(3) Uani 1 1 d . . . . .
F17 F -0.0726(3) 0.4749(4) 0.2948(2) 0.260(4) Uani 1 1 d . . . . .
F18 F 0.0531(4) 0.4468(2) 0.3895(2) 0.204(3) Uani 1 1 d . . . . .
P3 P -0.01017(6) 0.45880(5) 0.34440(5) 0.0588(3) Uani 1 1 d . . . . .
F1 F 0.12183(13) 1.02967(12) 0.41599(9) 0.0644(7) Uani 1 1 d . . . . .
F2 F 0.24225(14) 1.01965(13) 0.37474(10) 0.0723(7) Uani 1 1 d . . . . .
F3 F 0.27214(12) 0.93841(10) 0.43469(10) 0.0563(6) Uani 1 1 d . . . . .
F4 F 0.15216(12) 0.94923(10) 0.47577(9) 0.0534(5) Uani 1 1 d . . . . .
F5 F 0.15809(17) 0.93495(15) 0.38071(11) 0.0865(9) Uani 1 1 d . . . . .
F6 F 0.23455(14) 1.03139(10) 0.47114(10) 0.0629(6) Uani 1 1 d . . . . .
P1 P 0.19677(5) 0.98416(4) 0.42437(3) 0.03504(19) Uani 1 1 d . . . . .
C3S C 0.1021(3) 0.8983(2) 0.6487(2) 0.0629(11) Uani 1 1 d . . . . .
C4S C 0.0542(3) 0.9018(3) 0.5959(2) 0.0837(15) Uani 1 1 d . . . . .
H4SA H 0.0883 0.9126 0.5646 0.125 Uiso 1 1 calc GR . . . .
H4SB H 0.0134 0.9336 0.5997 0.125 Uiso 1 1 calc GR . . . .
H4SC H 0.0293 0.8616 0.5884 0.125 Uiso 1 1 calc GR . . . .
N2S N 0.1398(3) 0.8950(3) 0.6893(2) 0.0997(15) Uani 1 1 d . . . . .
C1S C 0.1784(3) 0.4172(3) 0.4973(2) 0.0726(14) Uani 1 1 d . . . . .
C2S C 0.1314(4) 0.4691(3) 0.5156(3) 0.110(2) Uani 1 1 d . . . . .
H2SA H 0.0960 0.4824 0.4846 0.164 Uiso 1 1 calc GR . . . .
H2SB H 0.1662 0.5035 0.5267 0.164 Uiso 1 1 calc GR . . . .
H2SC H 0.1001 0.4566 0.5479 0.164 Uiso 1 1 calc GR . . . .
N1S N 0.2132(3) 0.3752(3) 0.4821(2) 0.1041(16) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.516(4) . ?
C1 C11 1.458(4) . ?
C1 N1 1.277(3) . ?
C2 C3 1.454(4) . ?
C2 N2 1.279(3) . ?
C3 C4 1.376(4) . ?
C3 C12 1.422(4) . ?
C4 C5 1.411(4) . ?
C5 C6 1.372(5) . ?
C6 C7 1.419(5) . ?
C7 C8 1.418(5) . ?
C7 C12 1.396(4) . ?
C8 C9 1.371(5) . ?
C9 C10 1.404(4) . ?
C10 C11 1.383(4) . ?
C11 C12 1.417(4) . ?
C13 C14 1.383(4) . ?
C13 C18 1.386(4) . ?
C13 N1 1.445(3) . ?
C14 C15 1.391(4) . ?
C15 C16 1.391(4) . ?
C15 C19 1.512(4) . ?
C16 C17 1.392(4) . ?
C17 C18 1.385(4) . ?
C17 C20 1.513(4) . ?
C21 C22 1.385(4) . ?
C21 C26 1.384(4) . ?
C21 N2 1.450(3) . ?
C22 C23 1.390(4) . ?
C23 C24 1.387(5) . ?
C23 C27 1.509(5) . ?
C24 C25 1.392(4) . ?
C25 C26 1.389(4) . ?
C25 C28 1.498(4) . ?
C29 C30 1.524(4) . ?
C29 C39 1.450(4) . ?
C29 N3 1.280(3) . ?
C30 C31 1.463(4) . ?
C30 N4 1.281(3) . ?
C31 C32 1.366(4) . ?
C31 C40 1.421(4) . ?
C32 C33 1.412(4) . ?
C33 C34 1.365(4) . ?
C34 C35 1.421(4) . ?
C35 C36 1.411(4) . ?
C35 C40 1.401(4) . ?
C36 C37 1.369(4) . ?
C37 C38 1.405(4) . ?
C38 C39 1.377(4) . ?
C39 C40 1.416(4) . ?
C41 C42 1.390(4) . ?
C41 C46 1.381(4) . ?
C41 N3 1.453(3) . ?
C42 C43 1.389(4) . ?
C43 C44 1.388(5) . ?
C43 C47 1.512(5) . ?
C44 C45 1.385(5) . ?
C45 C46 1.402(4) . ?
C45 C48 1.507(5) . ?
C49 C50 1.382(4) . ?
C49 C54 1.387(4) . ?
C49 N4 1.449(3) . ?
C50 C51 1.395(4) . ?
C51 C52 1.383(4) . ?
C51 C55 1.510(4) . ?
C52 C53 1.389(4) . ?
C53 C54 1.390(4) . ?
C53 C56 1.507(4) . ?
C57 C58 1.512(4) . ?
C57 C67 1.452(4) . ?
C57 N5 1.284(3) . ?
C58 C59 1.459(4) . ?
C58 N6 1.285(3) . ?
C59 C60 1.372(4) . ?
C59 C68 1.417(4) . ?
C60 C61 1.412(4) . ?
C61 C62 1.362(4) . ?
C62 C63 1.421(4) . ?
C63 C64 1.410(4) . ?
C63 C68 1.401(4) . ?
C64 C65 1.376(4) . ?
C65 C66 1.412(4) . ?
C66 C67 1.376(4) . ?
C67 C68 1.415(4) . ?
C69 C70 1.381(4) . ?
C69 C74 1.387(4) . ?
C69 N5 1.451(3) . ?
C70 C71 1.394(4) . ?
C71 C72 1.384(5) . ?
C71 C75 1.504(5) . ?
C72 C73 1.389(5) . ?
C73 C74 1.396(4) . ?
C73 C76 1.505(5) . ?
C77 C78 1.390(4) . ?
C77 C82 1.379(4) . ?
C77 N6 1.440(3) . ?
C78 C79 1.389(4) . ?
C79 C80 1.394(4) . ?
C79 C83 1.507(4) . ?
C80 C81 1.387(4) . ?
C81 C82 1.384(4) . ?
C81 C84 1.503(4) . ?
N1 Ga1 2.091(2) . ?
N2 Ga1 2.090(2) . ?
N3 Ga1 2.077(2) . ?
N4 Ga1 2.093(2) . ?
N5 Ga1 2.061(2) . ?
N6 Ga1 2.078(2) . ?
F7 P2 1.573(2) . ?
F8 P2 1.566(3) . ?
F9 P2 1.580(2) . ?
F10 P2 1.598(2) . ?
F11 P2 1.601(2) . ?
F12 P2 1.602(2) . ?
F13 P3 1.581(3) . ?
F14 P3 1.551(3) . ?
F15 P3 1.569(3) . ?
F16 P3 1.514(3) . ?
F17 P3 1.569(5) . ?
F18 P3 1.487(4) . ?
F1 P1 1.582(2) . ?
F2 P1 1.582(2) . ?
F3 P1 1.596(2) . ?
F4 P1 1.601(2) . ?
F5 P1 1.579(2) . ?
F6 P1 1.593(2) . ?
C3S C4S 1.447(6) . ?
C3S N2S 1.121(6) . ?
C1S C2S 1.420(8) . ?
C1S N1S 1.121(7) . ?

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
C11 C1 C2 107.0(2) . . ?
N1 C1 C2 117.5(2) . . ?
N1 C1 C11 135.4(3) . . ?
C3 C2 C1 107.6(2) . . ?
N2 C2 C1 116.9(2) . . ?
N2 C2 C3 135.4(3) . . ?
C4 C3 C2 135.1(3) . . ?
C4 C3 C12 119.5(3) . . ?
C12 C3 C2 105.4(2) . . ?
C3 C4 C5 117.7(3) . . ?
C6 C5 C4 122.9(3) . . ?
C5 C6 C7 120.6(3) . . ?
C8 C7 C6 127.5(3) . . ?
C12 C7 C6 116.1(3) . . ?
C12 C7 C8 116.4(3) . . ?
C9 C8 C7 120.9(3) . . ?
C8 C9 C10 122.4(3) . . ?
C11 C10 C9 118.2(3) . . ?
C10 C11 C1 134.9(3) . . ?
C10 C11 C12 119.4(3) . . ?
C12 C11 C1 105.7(2) . . ?
C7 C12 C3 123.1(3) . . ?
C7 C12 C11 122.7(3) . . ?
C11 C12 C3 114.2(2) . . ?
C14 C13 C18 121.7(3) . . ?
C14 C13 N1 119.0(2) . . ?
C18 C13 N1 119.2(2) . . ?
C13 C14 C15 119.4(3) . . ?
C14 C15 C16 118.7(3) . . ?
C14 C15 C19 119.7(3) . . ?
C16 C15 C19 121.6(3) . . ?
C15 C16 C17 121.9(3) . . ?
C16 C17 C20 121.3(3) . . ?
C18 C17 C16 118.8(3) . . ?
C18 C17 C20 119.9(3) . . ?
C17 C18 C13 119.5(3) . . ?
C22 C21 N2 119.3(2) . . ?
C26 C21 C22 121.8(2) . . ?
C26 C21 N2 118.9(2) . . ?
C21 C22 C23 119.2(3) . . ?
C22 C23 C27 119.8(3) . . ?
C24 C23 C22 118.9(3) . . ?
C24 C23 C27 121.3(3) . . ?
C23 C24 C25 122.1(3) . . ?
C24 C25 C28 121.1(3) . . ?
C26 C25 C24 118.5(3) . . ?
C26 C25 C28 120.4(3) . . ?
C21 C26 C25 119.6(3) . . ?
C39 C29 C30 107.4(2) . . ?
N3 C29 C30 117.6(2) . . ?
N3 C29 C39 135.0(2) . . ?
C31 C30 C29 107.0(2) . . ?
N4 C30 C29 116.7(2) . . ?
N4 C30 C31 136.2(2) . . ?
C32 C31 C30 135.1(3) . . ?
C32 C31 C40 119.5(2) . . ?
C40 C31 C30 105.3(2) . . ?
C31 C32 C33 118.4(3) . . ?
C34 C33 C32 122.4(3) . . ?
C33 C34 C35 121.0(3) . . ?
C36 C35 C34 128.2(3) . . ?
C40 C35 C34 115.8(3) . . ?
C40 C35 C36 115.9(3) . . ?
C37 C36 C35 121.5(3) . . ?
C36 C37 C38 122.0(3) . . ?
C39 C38 C37 118.2(3) . . ?
C38 C39 C29 134.6(3) . . ?
C38 C39 C40 119.6(2) . . ?
C40 C39 C29 105.8(2) . . ?
C35 C40 C31 122.8(3) . . ?
C35 C40 C39 122.6(2) . . ?
C39 C40 C31 114.5(2) . . ?
C42 C41 N3 118.7(2) . . ?
C46 C41 C42 121.8(3) . . ?
C46 C41 N3 119.3(2) . . ?
C43 C42 C41 119.3(3) . . ?
C42 C43 C47 120.0(3) . . ?
C44 C43 C42 118.8(3) . . ?
C44 C43 C47 121.2(3) . . ?
C45 C44 C43 122.1(3) . . ?
C44 C45 C46 118.8(3) . . ?
C44 C45 C48 121.4(3) . . ?
C46 C45 C48 119.8(3) . . ?
C41 C46 C45 119.0(3) . . ?
C50 C49 C54 121.6(2) . . ?
C50 C49 N4 120.5(2) . . ?
C54 C49 N4 117.8(2) . . ?
C49 C50 C51 119.4(3) . . ?
C50 C51 C55 120.2(3) . . ?
C52 C51 C50 118.6(3) . . ?
C52 C51 C55 121.2(3) . . ?
C51 C52 C53 122.4(3) . . ?
C52 C53 C54 118.4(3) . . ?
C52 C53 C56 121.2(3) . . ?
C54 C53 C56 120.4(3) . . ?
C49 C54 C53 119.5(3) . . ?
C67 C57 C58 107.6(2) . . ?
N5 C57 C58 117.7(2) . . ?
N5 C57 C67 134.7(3) . . ?
C59 C58 C57 107.1(2) . . ?
N6 C58 C57 117.2(2) . . ?
N6 C58 C59 135.7(2) . . ?
C60 C59 C58 135.1(3) . . ?
C60 C59 C68 119.6(2) . . ?
C68 C59 C58 105.3(2) . . ?
C59 C60 C61 117.9(3) . . ?
C62 C61 C60 122.6(3) . . ?
C61 C62 C63 121.1(3) . . ?
C64 C63 C62 128.1(3) . . ?
C68 C63 C62 115.7(3) . . ?
C68 C63 C64 116.2(3) . . ?
C65 C64 C63 121.4(3) . . ?
C64 C65 C66 121.9(3) . . ?
C67 C66 C65 118.0(3) . . ?
C66 C67 C57 134.6(3) . . ?
C66 C67 C68 119.9(3) . . ?
C68 C67 C57 105.4(2) . . ?
C63 C68 C59 123.0(3) . . ?
C63 C68 C67 122.5(3) . . ?
C67 C68 C59 114.5(2) . . ?
C70 C69 C74 121.9(3) . . ?
C70 C69 N5 118.3(2) . . ?
C74 C69 N5 119.8(2) . . ?
C69 C70 C71 119.8(3) . . ?
C70 C71 C75 120.4(3) . . ?
C72 C71 C70 118.0(3) . . ?
C72 C71 C75 121.5(3) . . ?
C71 C72 C73 122.8(3) . . ?
C72 C73 C74 118.6(3) . . ?
C72 C73 C76 121.4(3) . . ?
C74 C73 C76 120.1(3) . . ?
C69 C74 C73 118.9(3) . . ?
C78 C77 N6 120.6(2) . . ?
C82 C77 C78 121.0(2) . . ?
C82 C77 N6 118.3(2) . . ?
C79 C78 C77 119.5(3) . . ?
C78 C79 C80 118.8(3) . . ?
C78 C79 C83 121.0(3) . . ?
C80 C79 C83 120.2(3) . . ?
C81 C80 C79 121.8(3) . . ?
C80 C81 C84 121.8(3) . . ?
C82 C81 C80 118.6(3) . . ?
C82 C81 C84 119.6(3) . . ?
C77 C82 C81 120.3(3) . . ?
C1 N1 C13 120.3(2) . . ?
C1 N1 Ga1 112.72(17) . . ?
C13 N1 Ga1 127.01(18) . . ?
C2 N2 C21 120.3(2) . . ?
C2 N2 Ga1 112.94(18) . . ?
C21 N2 Ga1 126.73(16) . . ?
C29 N3 C41 122.5(2) . . ?
C29 N3 Ga1 112.41(17) . . ?
C41 N3 Ga1 124.76(17) . . ?
C30 N4 C49 123.2(2) . . ?
C30 N4 Ga1 112.26(17) . . ?
C49 N4 Ga1 124.26(16) . . ?
C57 N5 C69 119.6(2) . . ?
C57 N5 Ga1 111.92(18) . . ?
C69 N5 Ga1 128.46(16) . . ?
C58 N6 C77 122.2(2) . . ?
C58 N6 Ga1 111.70(17) . . ?
C77 N6 Ga1 126.11(16) . . ?
N1 Ga1 N4 172.02(8) . . ?
N2 Ga1 N1 79.89(8) . . ?
N2 Ga1 N4 93.28(8) . . ?
N3 Ga1 N1 95.15(8) . . ?
N3 Ga1 N2 88.31(8) . . ?
N3 Ga1 N4 80.43(8) . . ?
N3 Ga1 N6 173.58(8) . . ?
N5 Ga1 N1 95.14(9) . . ?
N5 Ga1 N2 174.29(9) . . ?
N5 Ga1 N3 94.97(8) . . ?
N5 Ga1 N4 91.87(9) . . ?
N5 Ga1 N6 81.28(8) . . ?
N6 Ga1 N1 90.39(8) . . ?
N6 Ga1 N2 95.87(8) . . ?
N6 Ga1 N4 94.43(8) . . ?
F7 P2 F9 178.82(18) . . ?
F7 P2 F10 89.84(18) . . ?
F7 P2 F11 89.87(13) . . ?
F7 P2 F12 91.20(14) . . ?
F8 P2 F7 90.2(2) . . ?
F8 P2 F9 90.97(17) . . ?
F8 P2 F10 179.59(16) . . ?
F8 P2 F11 90.22(13) . . ?
F8 P2 F12 90.10(15) . . ?
F9 P2 F10 89.02(15) . . ?
F9 P2 F11 89.82(12) . . ?
F9 P2 F12 89.10(13) . . ?
F10 P2 F11 90.20(12) . . ?
F10 P2 F12 89.49(14) . . ?
F11 P2 F12 178.88(13) . . ?
F14 P3 F13 90.31(17) . . ?
F14 P3 F15 92.34(19) . . ?
F14 P3 F17 85.0(3) . . ?
F15 P3 F13 175.4(2) . . ?
F16 P3 F13 89.47(16) . . ?
F16 P3 F14 169.7(3) . . ?
F16 P3 F15 88.59(19) . . ?
F16 P3 F17 84.7(4) . . ?
F17 P3 F13 88.6(3) . . ?
F17 P3 F15 95.4(4) . . ?
F18 P3 F13 89.7(2) . . ?
F18 P3 F14 91.3(3) . . ?
F18 P3 F15 86.5(3) . . ?
F18 P3 F16 99.0(4) . . ?
F18 P3 F17 175.9(4) . . ?
F1 P1 F2 90.57(12) . . ?
F1 P1 F3 178.43(12) . . ?
F1 P1 F4 89.74(12) . . ?
F1 P1 F6 89.90(13) . . ?
F2 P1 F3 90.60(12) . . ?
F2 P1 F4 178.53(15) . . ?
F2 P1 F6 90.67(15) . . ?
F3 P1 F4 89.06(11) . . ?
F5 P1 F1 90.87(15) . . ?
F5 P1 F2 92.26(16) . . ?
F5 P1 F3 90.13(14) . . ?
F5 P1 F4 89.17(14) . . ?
F5 P1 F6 176.96(16) . . ?
F6 P1 F3 89.04(13) . . ?
F6 P1 F4 87.89(12) . . ?
N2S C3S C4S 179.2(6) . . ?
N1S C1S C2S 177.6(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -178.4(3) . . . . ?
C1 C2 C3 C12 2.2(3) . . . . ?
C1 C2 N2 C21 -178.1(2) . . . . ?
C1 C2 N2 Ga1 2.8(3) . . . . ?
C1 C11 C12 C3 -0.9(3) . . . . ?
C1 C11 C12 C7 180.0(2) . . . . ?
C2 C1 C11 C10 -175.6(3) . . . . ?
C2 C1 C11 C12 2.2(3) . . . . ?
C2 C1 N1 C13 179.8(2) . . . . ?
C2 C1 N1 Ga1 0.1(3) . . . . ?
C2 C3 C4 C5 -179.4(3) . . . . ?
C2 C3 C12 C7 178.3(2) . . . . ?
C2 C3 C12 C11 -0.8(3) . . . . ?
C3 C2 N2 C21 0.0(4) . . . . ?
C3 C2 N2 Ga1 -179.0(3) . . . . ?
C3 C4 C5 C6 0.9(5) . . . . ?
C4 C3 C12 C7 -1.2(4) . . . . ?
C4 C3 C12 C11 179.7(2) . . . . ?
C4 C5 C6 C7 -0.6(5) . . . . ?
C5 C6 C7 C8 178.8(3) . . . . ?
C5 C6 C7 C12 -0.6(4) . . . . ?
C6 C7 C8 C9 -178.9(3) . . . . ?
C6 C7 C12 C3 1.5(4) . . . . ?
C6 C7 C12 C11 -179.4(3) . . . . ?
C7 C8 C9 C10 -1.4(5) . . . . ?
C8 C7 C12 C3 -178.0(3) . . . . ?
C8 C7 C12 C11 1.1(4) . . . . ?
C8 C9 C10 C11 0.7(5) . . . . ?
C9 C10 C11 C1 178.5(3) . . . . ?
C9 C10 C11 C12 0.9(4) . . . . ?
C10 C11 C12 C3 177.3(2) . . . . ?
C10 C11 C12 C7 -1.8(4) . . . . ?
C11 C1 C2 C3 -2.8(3) . . . . ?
C11 C1 C2 N2 175.8(2) . . . . ?
C11 C1 N1 C13 2.6(5) . . . . ?
C11 C1 N1 Ga1 -177.1(3) . . . . ?
C12 C3 C4 C5 0.0(4) . . . . ?
C12 C7 C8 C9 0.5(4) . . . . ?
C13 C14 C15 C16 -2.0(4) . . . . ?
C13 C14 C15 C19 176.0(3) . . . . ?
C14 C13 C18 C17 0.5(5) . . . . ?
C14 C13 N1 C1 -110.1(3) . . . . ?
C14 C13 N1 Ga1 69.5(3) . . . . ?
C14 C15 C16 C17 0.3(5) . . . . ?
C15 C16 C17 C18 1.8(5) . . . . ?
C15 C16 C17 C20 -178.2(3) . . . . ?
C16 C17 C18 C13 -2.2(5) . . . . ?
C18 C13 C14 C15 1.6(4) . . . . ?
C18 C13 N1 C1 70.8(3) . . . . ?
C18 C13 N1 Ga1 -109.6(3) . . . . ?
C19 C15 C16 C17 -177.6(3) . . . . ?
C20 C17 C18 C13 177.9(3) . . . . ?
C21 C22 C23 C24 -1.7(4) . . . . ?
C21 C22 C23 C27 177.5(3) . . . . ?
C22 C21 C26 C25 2.0(4) . . . . ?
C22 C21 N2 C2 79.6(3) . . . . ?
C22 C21 N2 Ga1 -101.5(3) . . . . ?
C22 C23 C24 C25 2.6(4) . . . . ?
C23 C24 C25 C26 -1.2(4) . . . . ?
C23 C24 C25 C28 178.7(3) . . . . ?
C24 C25 C26 C21 -1.1(4) . . . . ?
C26 C21 C22 C23 -0.6(4) . . . . ?
C26 C21 N2 C2 -102.5(3) . . . . ?
C26 C21 N2 Ga1 76.4(3) . . . . ?
C27 C23 C24 C25 -176.6(3) . . . . ?
C28 C25 C26 C21 179.0(3) . . . . ?
C29 C30 C31 C32 177.8(3) . . . . ?
C29 C30 C31 C40 0.6(3) . . . . ?
C29 C30 N4 C49 178.5(2) . . . . ?
C29 C30 N4 Ga1 -6.9(3) . . . . ?
C29 C39 C40 C31 2.4(3) . . . . ?
C29 C39 C40 C35 -175.9(2) . . . . ?
C30 C29 C39 C38 -179.1(3) . . . . ?
C30 C29 C39 C40 -1.9(3) . . . . ?
C30 C29 N3 C41 177.9(2) . . . . ?
C30 C29 N3 Ga1 4.5(3) . . . . ?
C30 C31 C32 C33 -176.8(3) . . . . ?
C30 C31 C40 C35 176.4(2) . . . . ?
C30 C31 C40 C39 -1.9(3) . . . . ?
C31 C30 N4 C49 -4.4(5) . . . . ?
C31 C30 N4 Ga1 170.3(3) . . . . ?
C31 C32 C33 C34 0.7(5) . . . . ?
C32 C31 C40 C35 -1.4(4) . . . . ?
C32 C31 C40 C39 -179.7(2) . . . . ?
C32 C33 C34 C35 -0.4(5) . . . . ?
C33 C34 C35 C36 178.7(3) . . . . ?
C33 C34 C35 C40 -0.7(4) . . . . ?
C34 C35 C36 C37 178.7(3) . . . . ?
C34 C35 C40 C31 1.6(4) . . . . ?
C34 C35 C40 C39 179.8(3) . . . . ?
C35 C36 C37 C38 1.4(5) . . . . ?
C36 C35 C40 C31 -177.9(3) . . . . ?
C36 C35 C40 C39 0.2(4) . . . . ?
C36 C37 C38 C39 0.8(5) . . . . ?
C37 C38 C39 C29 174.6(3) . . . . ?
C37 C38 C39 C40 -2.3(4) . . . . ?
C38 C39 C40 C31 -179.9(3) . . . . ?
C38 C39 C40 C35 1.8(4) . . . . ?
C39 C29 C30 C31 0.8(3) . . . . ?
C39 C29 C30 N4 178.7(2) . . . . ?
C39 C29 N3 C41 1.9(5) . . . . ?
C39 C29 N3 Ga1 -171.5(3) . . . . ?
C40 C31 C32 C33 0.1(4) . . . . ?
C40 C35 C36 C37 -1.8(4) . . . . ?
C41 C42 C43 C44 -0.9(4) . . . . ?
C41 C42 C43 C47 179.2(3) . . . . ?
C42 C41 C46 C45 -1.7(4) . . . . ?
C42 C41 N3 C29 -96.7(3) . . . . ?
C42 C41 N3 Ga1 75.9(3) . . . . ?
C42 C43 C44 C45 -2.0(4) . . . . ?
C43 C44 C45 C46 3.1(4) . . . . ?
C43 C44 C45 C48 -177.9(3) . . . . ?
C44 C45 C46 C41 -1.2(4) . . . . ?
C46 C41 C42 C43 2.8(4) . . . . ?
C46 C41 N3 C29 87.7(3) . . . . ?
C46 C41 N3 Ga1 -99.8(3) . . . . ?
C47 C43 C44 C45 177.9(3) . . . . ?
C48 C45 C46 C41 179.8(3) . . . . ?
C49 C50 C51 C52 -0.7(4) . . . . ?
C49 C50 C51 C55 178.8(3) . . . . ?
C50 C49 C54 C53 3.2(4) . . . . ?
C50 C49 N4 C30 71.8(3) . . . . ?
C50 C49 N4 Ga1 -102.3(3) . . . . ?
C50 C51 C52 C53 2.9(4) . . . . ?
C51 C52 C53 C54 -2.0(4) . . . . ?
C51 C52 C53 C56 177.7(3) . . . . ?
C52 C53 C54 C49 -1.0(4) . . . . ?
C54 C49 C50 C51 -2.3(4) . . . . ?
C54 C49 N4 C30 -112.3(3) . . . . ?
C54 C49 N4 Ga1 73.7(3) . . . . ?
C55 C51 C52 C53 -176.6(3) . . . . ?
C56 C53 C54 C49 179.3(3) . . . . ?
C57 C58 C59 C60 -177.1(3) . . . . ?
C57 C58 C59 C68 2.4(3) . . . . ?
C57 C58 N6 C77 179.6(2) . . . . ?
C57 C58 N6 Ga1 -2.5(3) . . . . ?
C57 C67 C68 C59 -0.7(3) . . . . ?
C57 C67 C68 C63 -179.7(3) . . . . ?
C58 C57 C67 C66 -174.7(3) . . . . ?
C58 C57 C67 C68 2.2(3) . . . . ?
C58 C57 N5 C69 -174.2(2) . . . . ?
C58 C57 N5 Ga1 4.7(3) . . . . ?
C58 C59 C60 C61 -180.0(3) . . . . ?
C58 C59 C68 C63 177.8(3) . . . . ?
C58 C59 C68 C67 -1.1(3) . . . . ?
C59 C58 N6 C77 1.3(5) . . . . ?
C59 C58 N6 Ga1 179.3(3) . . . . ?
C59 C60 C61 C62 0.9(4) . . . . ?
C60 C59 C68 C63 -2.5(4) . . . . ?
C60 C59 C68 C67 178.5(3) . . . . ?
C60 C61 C62 C63 -0.5(5) . . . . ?
C61 C62 C63 C64 177.6(3) . . . . ?
C61 C62 C63 C68 -1.3(4) . . . . ?
C62 C63 C64 C65 -179.7(3) . . . . ?
C62 C63 C68 C59 2.9(4) . . . . ?
C62 C63 C68 C67 -178.3(3) . . . . ?
C63 C64 C65 C66 -1.5(5) . . . . ?
C64 C63 C68 C59 -176.2(3) . . . . ?
C64 C63 C68 C67 2.6(4) . . . . ?
C64 C65 C66 C67 2.0(5) . . . . ?
C65 C66 C67 C57 176.4(3) . . . . ?
C65 C66 C67 C68 -0.1(4) . . . . ?
C66 C67 C68 C59 176.7(3) . . . . ?
C66 C67 C68 C63 -2.2(4) . . . . ?
C67 C57 C58 C59 -2.9(3) . . . . ?
C67 C57 C58 N6 178.4(2) . . . . ?
C67 C57 N5 C69 5.9(5) . . . . ?
C67 C57 N5 Ga1 -175.2(3) . . . . ?
C68 C59 C60 C61 0.6(4) . . . . ?
C68 C63 C64 C65 -0.8(5) . . . . ?
C69 C70 C71 C72 -0.8(4) . . . . ?
C69 C70 C71 C75 178.0(3) . . . . ?
C70 C69 C74 C73 0.3(4) . . . . ?
C70 C69 N5 C57 72.0(3) . . . . ?
C70 C69 N5 Ga1 -106.6(3) . . . . ?
C70 C71 C72 C73 0.2(5) . . . . ?
C71 C72 C73 C74 0.7(5) . . . . ?
C71 C72 C73 C76 -179.1(3) . . . . ?
C72 C73 C74 C69 -0.9(4) . . . . ?
C74 C69 C70 C71 0.6(4) . . . . ?
C74 C69 N5 C57 -108.7(3) . . . . ?
C74 C69 N5 Ga1 72.7(3) . . . . ?
C75 C71 C72 C73 -178.6(3) . . . . ?
C76 C73 C74 C69 178.9(3) . . . . ?
C77 C78 C79 C80 -1.3(4) . . . . ?
C77 C78 C79 C83 178.1(3) . . . . ?
C78 C77 C82 C81 2.3(4) . . . . ?
C78 C77 N6 C58 64.5(3) . . . . ?
C78 C77 N6 Ga1 -113.2(2) . . . . ?
C78 C79 C80 C81 1.7(4) . . . . ?
C79 C80 C81 C82 -0.1(4) . . . . ?
C79 C80 C81 C84 -179.4(3) . . . . ?
C80 C81 C82 C77 -1.9(4) . . . . ?
C82 C77 C78 C79 -0.7(4) . . . . ?
C82 C77 N6 C58 -118.1(3) . . . . ?
C82 C77 N6 Ga1 64.3(3) . . . . ?
C83 C79 C80 C81 -177.6(3) . . . . ?
C84 C81 C82 C77 177.4(3) . . . . ?
N1 C1 C2 C3 179.3(2) . . . . ?
N1 C1 C2 N2 -2.1(3) . . . . ?
N1 C1 C11 C10 1.8(6) . . . . ?
N1 C1 C11 C12 179.6(3) . . . . ?
N1 C13 C14 C15 -177.5(3) . . . . ?
N1 C13 C18 C17 179.6(3) . . . . ?
N2 C2 C3 C4 3.3(6) . . . . ?
N2 C2 C3 C12 -176.1(3) . . . . ?
N2 C21 C22 C23 177.3(2) . . . . ?
N2 C21 C26 C25 -175.8(2) . . . . ?
N3 C29 C30 C31 -176.2(2) . . . . ?
N3 C29 C30 N4 1.7(4) . . . . ?
N3 C29 C39 C38 -2.8(6) . . . . ?
N3 C29 C39 C40 174.4(3) . . . . ?
N3 C41 C42 C43 -172.7(2) . . . . ?
N3 C41 C46 C45 173.8(2) . . . . ?
N4 C30 C31 C32 0.5(6) . . . . ?
N4 C30 C31 C40 -176.7(3) . . . . ?
N4 C49 C50 C51 173.4(2) . . . . ?
N4 C49 C54 C53 -172.7(2) . . . . ?
N5 C57 C58 C59 177.2(2) . . . . ?
N5 C57 C58 N6 -1.5(4) . . . . ?
N5 C57 C67 C66 5.2(6) . . . . ?
N5 C57 C67 C68 -177.9(3) . . . . ?
N5 C69 C70 C71 179.9(2) . . . . ?
N5 C69 C74 C73 -179.0(3) . . . . ?
N6 C58 C59 C60 1.2(6) . . . . ?
N6 C58 C59 C68 -179.3(3) . . . . ?
N6 C77 C78 C79 176.7(2) . . . . ?
N6 C77 C82 C81 -175.1(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7 27 -9 0.1141 -7.0000 27.0000 -8.9999 0.1086 0.4898 -0.8580
-21 10 9 0.0799 -21.0000 9.9999 8.9999 -0.7723 0.4554 -0.4207
-19 8 18 0.0911 -19.0000 7.9999 17.9999 -0.8000 0.5892 -0.1564
6 -16 26 0.1058 6.0000 -16.0000 26.0000 -0.1825 0.1336 0.9709
-8 23 -18 0.0907 -8.0000 23.0000 -17.9999 0.1094 0.2065 -0.9837
7 -23 -19 0.0990 7.0000 -23.0000 -19.0000 0.1902 -0.9678 0.2007
15 21 7 0.0934 15.0000 21.0000 7.0002 0.7342 0.6474 0.0185
14 12 -24 0.0843 14.0000 12.0000 -23.9998 0.8815 -0.2128 -0.4619
20 -12 9 0.0896 20.0000 -12.0000 9.0001 0.5483 -0.1329 0.8124
-14 -12 24 0.0938 -14.0000 -12.0000 23.9998 -0.8815 0.2128 0.4619
-4 -27 -14 0.1048 -4.0000 -27.0000 -14.0001 -0.3171 -0.9518 0.1698
-14 -11 -23 0.1096 -14.0000 -11.0000 -23.0001 -0.4418 -0.7308 -0.5279
11 -1 29 0.1082 11.0000 -1.0000 29.0001 0.1428 0.5609 0.8319

_exptl_crystal_recrystallization_method 
'Slow diffusion of diethyl ether into a saturated MeCN solution of the complex'
_chemical_properties_physical    Moisture-sensitive
