data_4a-3EtOH-150K
_publ_requested_journal          ?
_publ_contact_author_name        'Assoc. Prof. Colette Boskovic'
_publ_contact_author_address     
;School of Chemistry 
University of Melbourne 
VIC 3010 
Australia 
;
_publ_contact_author_email       c.boskovic@unimelb.edu.au
_publ_contact_author_phone       '+61 3 8344 4971'
_publ_contact_author_fax         '+61 3 9347 5180'
_publ_contact_author_id_orcid    0000-0002-1882-2139
loop_
_publ_author_name
_publ_author_address
'Boskovic, Colette'
;School of Chemistry 
University of Melbourne 
VIC 3010 
Australia 
;
'Gransbury, Gemma K.'
;School of Chemistry 
University of Melbourne 
VIC 3010 
Australia 
;
'Gable, Robert W.'
;School of Chemistry 
University of Melbourne 
VIC 3010 
Australia 
;
'Livesay, Brooke N.'
;Department of Chemistry 
Colorado State University 
Fort Collins 80523 
USA
;
'Shores, Matthew P.'
;Department of Chemistry 
Colorado State University 
Fort Collins 80523 
USA
;
'Starikova, Alyona'
;Institute of Physical and Organic Chemistry 
Southern Federal University 
344090 Rostov-on-Don
Russian Federation 
;
_audit_creation_date             2019-01-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
loop_
_audit_author_name
_audit_author_address
'Gransbury, Gemma K.'
;
School of Chemistry 
University of Melbourne 
VIC 3010 
Australia 
;
'Gable, Robert W.'
;
School of Chemistry 
University of Melbourne 
VIC 3010 
Australia 
;
_audit_contact_author_address    
;School of Chemistry 
University of Melbourne 
VIC 3010 
Australia 
;
_audit_contact_author_email      robertwg@unimelb.edu.au
_audit_contact_author_name       'Robert W. Gable'
_audit_contact_author_phone      '+61 3 8344 6471'
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_systematic        
"(mu2-3,3,3',3'-tetramethyl-1,1'-spirobi(indan)-4,4'-7,7'-tetrabromo-5,5'-6,6'-tetraolato)-bis(tris(6-methyl-2-pyridylmethyl)amine)-di-cobalt bis(hexafluorophosphate) ethanol solvate"
_chemical_name_common            ?
_chemical_formula_moiety         'C63 H64 Br4 Co2 N8 O4, 2(F6 P)'
_chemical_formula_sum            'C69 H82 Br4 Co2 F12 N8 O7 P2'
_chemical_properties_physical    paramagnetic
_chemical_formula_weight         1862.86
_exptl_crystal_recrystallization_method 'Crystallised from toluene'
_chemical_melting_point          ?
_exptl_crystal_description       prism
_exptl_crystal_colour            'dark green'
_diffrn_ambient_temperature      149.99(10)
_chemical_oxdiff_formula         'C63 H64 Br4 Co2 N8 O4 P2 F12'
_chemical_oxdiff_usercomment     'dark green prism crystals from EtOH'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   26.0240(3)
_cell_length_b                   14.43890(10)
_cell_length_c                   20.3551(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7648.59(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16188
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      76.2710
_cell_measurement_theta_min      2.7490
_shelx_estimated_absorpt_T_max   0.744
_shelx_estimated_absorpt_T_min   0.215
_exptl_absorpt_coefficient_mu    6.982
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.258
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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_absorpt_special_details   ?
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3760
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 0 -11 0.0192
13 4 -6 0.0878
13 0 -9 0.0457
10 5 -8 0.0969
9 -7 -5 0.1175
-7 -8 6 0.1324
-13 0 9 0.0481
10 0 11 0.0258
-1 9 0 0.1540
-9 7 5 0.1287

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.045
loop_
_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
-10.0001 0.0008 -11.0002 1.0139 -0.0363 -0.1190
13.0009 4.0003 -6.0003 -0.1901 0.0259 -0.9717
13.0006 0.0003 -9.0005 0.0177 0.4591 -0.9196
10.0010 5.0005 -8.0003 0.0306 -0.1030 -0.9951
8.9997 -7.0001 -5.0005 0.0044 0.9614 -0.2467
-7.0011 -8.0005 6.0001 -0.0041 0.4927 0.9292
-13.0006 -0.0003 9.0005 -0.0177 -0.4591 0.9196
10.0001 -0.0008 11.0002 -1.0139 0.0363 0.1190
-0.9992 9.0003 0.0002 -0.0422 -0.8785 -0.3896
-8.9997 7.0001 5.0005 -0.0044 -0.9614 0.2467

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46089
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.997
_diffrn_reflns_theta_min         2.756
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -61.00  21.00   0.50    3.59    --  -48.30  87.00 -36.00  164
  2  ω   -116.00 -39.00   0.50    3.59    --  -48.30 -38.00-180.00  154
  3  ω   -114.00 -71.00   0.50    3.59    --  -48.30-125.00   0.00   86
  4  ω   -129.00 -69.00   0.50   15.00    --  -86.25 -66.00  81.00  120
  5  ω     99.00 177.00   0.50   15.00    --  107.75  87.00 -36.00  156
  6  ω     97.00 178.00   0.50   15.00    --  107.75  45.00   0.00  162
  7  ω     98.00 126.00   0.50   15.00    --  107.75 -70.00 -48.00   56
  8  ω    100.00 177.00   0.50   15.00    --  107.75  30.00 -90.00  154
  9  ω     87.00 175.00   0.50   15.00    --  107.75  77.00 -90.00  176
 10  ω     93.00 178.00   0.50   15.00    --  107.75  61.00 -60.00  170
 11  ω     39.00  80.00   0.50   15.00    --  107.75 -70.00 -48.00   82
 12  ω     38.00 124.00   0.50   15.00    --  107.75 -66.00  81.00  172
 13  ω     38.00  74.00   0.50   15.00    --  107.75 -45.00 120.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0383255000
_diffrn_orient_matrix_UB_12      -0.0089436000
_diffrn_orient_matrix_UB_13      -0.0573275000
_diffrn_orient_matrix_UB_21      0.0230756000
_diffrn_orient_matrix_UB_22      -0.0950422000
_diffrn_orient_matrix_UB_23      -0.0176823000
_diffrn_orient_matrix_UB_31      -0.0388184000
_diffrn_orient_matrix_UB_32      -0.0475976000
_diffrn_orient_matrix_UB_33      0.0461028000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6500
_reflns_number_total             8071
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.709
_refine_diff_density_min         -2.842
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8071
_refine_ls_number_restraints     121
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.1097
_refine_ls_restrained_S_all      1.149
_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)+(0.1318P)²+33.8845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3012
_refine_ls_wR_factor_ref         0.3139
_refine_special_details          
;
There were peaks attributed to disordered/diffuse solvent which was 
modelled using the OLEX2 solvent mask routine. These peaks are situated in
channels which lie along the b-axis. The solvent mask routine gave a large 
cavity volume suggesting partial occupation of solvent while electron density
peaks were consistent with 6 ethanol molecules per channel per unit cell or 3
ethanol molecules per formula unit. 

The PF6- anion was disordered over three orientations with each component
restrained to ideal geometry.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F1-F2 = F1-F3 = F1-F4 = F1-F5
 2.2627 with sigma of 0.001
 F6-F2 = F6-F3 = F6-F4 = F6-F5
 2.2627 with sigma of 0.001
 F2-F3 = F3-F5 = F5-F4 = F4-F2
 2.2627 with sigma of 0.001
 F1A-F2A = F1A-F3A = F1A-F4A = F1A-F5A
 2.2627 with sigma of 0.001
 F6A-F2A = F6A-F3A = F6A-F4A = F6A-F5A
 2.2627 with sigma of 0.001
 F2A-F3A = F3A-F5A = F5A-F4A = F4A-F2A
 2.2627 with sigma of 0.001
 F1B-F2B = F1B-F3B = F1B-F4B = F1B-F5B
 2.2627 with sigma of 0.001
 F6B-F2B = F6B-F3B = F6B-F4B = F6B-F5B
 2.2627 with sigma of 0.001
 F2B-F3B = F3B-F5B = F5B-F4B = F4B-F2B
 2.2627 with sigma of 0.001
 P1-F1 = P1-F2 = P1-F3 = P1-F4 = P1-F5 = P1-F6
 1.6 with sigma of 0.001
 P1A-F1A = P1A-F2A = P1A-F3A = P1A-F4A = P1A-F5A = P1A-F6A
 1.6 with sigma of 0.001
 P1B-F1B = P1B-F2B = P1B-F3B = P1B-F4B = P1B-F5B = P1B-F6B
 1.6 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C7) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(F1) = Uanis(F1A) = Uanis(F1B)
Uanis(F2) = Uanis(F2A) = Uanis(F2B)
Uanis(F3) = Uanis(F3A) = Uanis(F3B)
Uanis(F4) = Uanis(F4A) = Uanis(F4B)
Uanis(F5) = Uanis(F5A) = Uanis(F5B)
Uanis(F6) = Uanis(F6A) = Uanis(F6B)
Uanis(P1) = Uanis(P1A) = Uanis(P1B)
4. Others
 1*[Sof(P1)+Sof(F1)+Sof(F2)+Sof(F3)+Sof(F4)+Sof(F5)+Sof(F6)]+1*[Sof(P1A)+
 Sof(F1A)+Sof(F2A)+Sof(F3A)+Sof(F4A)+Sof(F5A)+Sof(F6A)]+1*[Sof(P1B)+Sof(F1B)+
 Sof(F2B)+Sof(F3B)+Sof(F4B)+Sof(F5B)+Sof(F6B)]=1 with esd of 0.0001
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(P1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(2)
 Sof(P1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=FVAR(3)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C17(H17A,H17B), C23(H23A,H23B), C29(H29A,H29B)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C25(H25),
 C26(H26), C27(H27)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Br1 Br 0.20162(9) 0.13859(9) 0.50123(12) 0.2035(13) Uani 1 1 d . . . . .
Br2 Br 0.29816(4) 0.39179(6) 0.73969(6) 0.0887(4) Uani 1 1 d . . . . .
Co1 Co 0.36240(5) 0.32661(11) 0.51491(7) 0.0718(4) Uani 1 1 d . . . . .
O1 O 0.3364(2) 0.3555(4) 0.6013(4) 0.090(2) Uani 1 1 d . . . . .
O2 O 0.2948(4) 0.2610(6) 0.5058(6) 0.124(4) Uani 1 1 d . . . . .
N1 N 0.3788(3) 0.2830(6) 0.4239(3) 0.083(2) Uani 1 1 d . . . . .
N2 N 0.4384(2) 0.3736(6) 0.5170(3) 0.079(2) Uani 1 1 d . . . . .
N3 N 0.3340(2) 0.4425(5) 0.4637(3) 0.0675(16) Uani 1 1 d . . . . .
N4 N 0.3957(3) 0.1954(7) 0.5373(3) 0.088(2) Uani 1 1 d . . . . .
C1 C 0.2938(3) 0.3105(5) 0.6162(6) 0.082(3) Uani 1 1 d . . . . .
C2 C 0.2732(4) 0.2578(6) 0.5610(7) 0.096(4) Uani 1 1 d . . . . .
C3 C 0.2289(5) 0.2044(6) 0.5741(8) 0.107(4) Uani 1 1 d . U . . .
C4 C 0.2072(4) 0.2024(6) 0.6339(8) 0.107(4) Uani 1 1 d . U . . .
C5 C 0.2262(3) 0.2588(5) 0.6861(6) 0.092(3) Uani 1 1 d . U . . .
C6 C 0.2689(3) 0.3135(5) 0.6745(6) 0.085(3) Uani 1 1 d . . . . .
C7 C 0.1596(4) 0.1500(8) 0.6629(9) 0.129(5) Uani 1 1 d . U . . .
C8 C 0.1103(5) 0.1929(12) 0.6318(10) 0.169(7) Uani 1 1 d . U . . .
H8A H 0.1047 0.2549 0.6500 0.254 Uiso 1 1 calc GR . . . .
H8B H 0.0807 0.1535 0.6419 0.254 Uiso 1 1 calc GR . . . .
H8C H 0.1147 0.1972 0.5841 0.254 Uiso 1 1 calc GR . . . .
C9 C 0.1625(7) 0.0438(9) 0.6422(10) 0.185(9) Uani 1 1 d . U . . .
H9A H 0.1552 0.0379 0.5952 0.277 Uiso 1 1 calc GR . . . .
H9B H 0.1371 0.0084 0.6673 0.277 Uiso 1 1 calc GR . . . .
H9C H 0.1970 0.0198 0.6514 0.277 Uiso 1 1 calc GR . . . .
C10 C 0.1630(4) 0.1626(8) 0.7374(8) 0.126(5) Uani 1 1 d . U . . .
H10A H 0.1793 0.1078 0.7579 0.151 Uiso 1 1 calc R . . . .
H10B H 0.1282 0.1703 0.7564 0.151 Uiso 1 1 calc R . . . .
C11 C 0.1957(5) 0.2500 0.7500 0.101(5) Uani 1 2 d S TU P . .
C12 C 0.4657(4) 0.4087(11) 0.5674(5) 0.122(5) Uani 1 1 d . . . . .
C13 C 0.5200(5) 0.3994(13) 0.5660(6) 0.138(5) Uani 1 1 d . U . . .
H13 H 0.5403 0.4182 0.6024 0.166 Uiso 1 1 calc R . . . .
C14 C 0.5422(5) 0.3631(15) 0.5113(9) 0.153(6) Uani 1 1 d . U . . .
H14 H 0.5786 0.3608 0.5090 0.184 Uiso 1 1 calc R . . . .
C15 C 0.5145(5) 0.3298(13) 0.4600(8) 0.136(5) Uani 1 1 d . U . . .
H15 H 0.5311 0.3017 0.4235 0.163 Uiso 1 1 calc R . . . .
C16 C 0.4630(3) 0.3375(9) 0.4617(5) 0.097(3) Uani 1 1 d . . . . .
C17 C 0.4301(4) 0.3136(9) 0.4060(4) 0.096(3) Uani 1 1 d . . . . .
H17A H 0.4271 0.3685 0.3771 0.115 Uiso 1 1 calc R . . . .
H17B H 0.4470 0.2639 0.3804 0.115 Uiso 1 1 calc R . . . .
C18 C 0.3214(3) 0.5286(6) 0.4854(5) 0.074(2) Uani 1 1 d . . . . .
C19 C 0.3082(3) 0.5979(7) 0.4423(6) 0.088(3) Uani 1 1 d . . . . .
H19 H 0.2993 0.6576 0.4583 0.105 Uiso 1 1 calc R . . . .
C20 C 0.3079(5) 0.5811(9) 0.3776(8) 0.123(5) Uani 1 1 d . . . . .
H20 H 0.2994 0.6289 0.3474 0.148 Uiso 1 1 calc R . . . .
C21 C 0.3204(6) 0.4930(9) 0.3552(6) 0.123(5) Uani 1 1 d . . . . .
H21 H 0.3205 0.4799 0.3095 0.147 Uiso 1 1 calc R . . . .
C22 C 0.3323(4) 0.4256(7) 0.3993(5) 0.087(3) Uani 1 1 d . . . . .
C23 C 0.3409(5) 0.3266(8) 0.3780(5) 0.102(4) Uani 1 1 d . . . . .
H23A H 0.3081 0.2920 0.3791 0.122 Uiso 1 1 calc R . . . .
H23B H 0.3543 0.3251 0.3325 0.122 Uiso 1 1 calc R . . . .
C24 C 0.4172(3) 0.1616(11) 0.5929(4) 0.105(4) Uani 1 1 d . . . . .
C25 C 0.4420(4) 0.0777(12) 0.5931(6) 0.122(5) Uani 1 1 d . . . . .
H25 H 0.4576 0.0568 0.6325 0.147 Uiso 1 1 calc R . . . .
C26 C 0.4447(4) 0.0249(11) 0.5398(7) 0.121(5) Uani 1 1 d . . . . .
H26 H 0.4613 -0.0336 0.5414 0.146 Uiso 1 1 calc R . . . .
C27 C 0.4225(4) 0.0570(8) 0.4808(5) 0.099(4) Uani 1 1 d . . . . .
H27 H 0.4240 0.0212 0.4417 0.118 Uiso 1 1 calc R . . . .
C28 C 0.3983(3) 0.1434(7) 0.4821(4) 0.082(3) Uani 1 1 d . . . . .
C29 C 0.3727(5) 0.1814(7) 0.4236(4) 0.090(3) Uani 1 1 d . . . . .
H29A H 0.3358 0.1650 0.4242 0.108 Uiso 1 1 calc R . . . .
H29B H 0.3883 0.1550 0.3834 0.108 Uiso 1 1 calc R . . . .
C30 C 0.4401(5) 0.4526(13) 0.6257(6) 0.153(7) Uani 1 1 d . . . . .
H30A H 0.4451 0.5199 0.6242 0.230 Uiso 1 1 calc GR . . . .
H30B H 0.4552 0.4280 0.6662 0.230 Uiso 1 1 calc GR . . . .
H30C H 0.4032 0.4388 0.6249 0.230 Uiso 1 1 calc GR . . . .
C31 C 0.3213(5) 0.5502(7) 0.5563(6) 0.102(3) Uani 1 1 d . . . . .
H31A H 0.2946 0.5137 0.5783 0.152 Uiso 1 1 calc GR . . . .
H31B H 0.3144 0.6163 0.5625 0.152 Uiso 1 1 calc GR . . . .
H31C H 0.3550 0.5350 0.5751 0.152 Uiso 1 1 calc GR . . . .
C32 C 0.4143(4) 0.2165(13) 0.6556(4) 0.146(7) Uani 1 1 d . . . . .
H32A H 0.4317 0.2761 0.6496 0.219 Uiso 1 1 calc GR . . . .
H32B H 0.4310 0.1819 0.6911 0.219 Uiso 1 1 calc GR . . . .
H32C H 0.3782 0.2274 0.6669 0.219 Uiso 1 1 calc GR . . . .
P1 P 0.45627(18) 0.4450(3) 0.2331(2) 0.0880(13) Uani 0.575(3) 1 d D . . A 1
F1 F 0.4150(2) 0.3630(5) 0.2346(4) 0.101(2) Uani 0.575(3) 1 d D . . A 1
F2 F 0.4933(2) 0.3862(4) 0.2799(3) 0.095(3) Uani 0.575(3) 1 d D . . A 1
F3 F 0.4298(3) 0.4906(5) 0.2962(3) 0.113(3) Uani 0.575(3) 1 d D . . A 1
F4 F 0.4828(3) 0.3995(5) 0.1700(3) 0.093(2) Uani 0.575(3) 1 d D . . A 1
F5 F 0.4192(3) 0.5039(5) 0.1863(3) 0.123(3) Uani 0.575(3) 1 d D . . A 1
F6 F 0.4975(3) 0.5271(4) 0.2317(3) 0.125(5) Uani 0.575(3) 1 d D . . A 1
P1A P 0.4697(3) 0.4244(6) 0.2250(4) 0.0880(13) Uani 0.250(3) 1 d D . . B 2
F1A F 0.4132(4) 0.3806(10) 0.2250(8) 0.101(2) Uani 0.250(3) 1 d D . . B 2
F2A F 0.4892(6) 0.3430(8) 0.2721(6) 0.095(3) Uani 0.250(3) 1 d D . . B 2
F3A F 0.4551(6) 0.4855(9) 0.2878(5) 0.113(3) Uani 0.250(3) 1 d D . . B 2
F4A F 0.4843(6) 0.3633(9) 0.1621(5) 0.093(2) Uani 0.250(3) 1 d D . . B 2
F5A F 0.4502(5) 0.5058(8) 0.1778(6) 0.123(3) Uani 0.250(3) 1 d D . . B 2
F6A F 0.5262(4) 0.4682(9) 0.2249(7) 0.125(5) Uani 0.250(3) 1 d D . . B 2
P1B P 0.4643(4) 0.4536(7) 0.2273(5) 0.0880(13) Uani 0.174(3) 1 d D . . C 3
F1B F 0.4300(5) 0.3631(9) 0.2389(9) 0.101(2) Uani 0.174(3) 1 d D . . C 3
F2B F 0.5108(5) 0.4062(11) 0.2660(7) 0.095(3) Uani 0.174(3) 1 d D . . C 3
F3B F 0.4434(7) 0.4965(12) 0.2947(6) 0.113(3) Uani 0.174(3) 1 d D . . C 3
F4B F 0.4852(7) 0.4108(12) 0.1599(6) 0.093(2) Uani 0.174(3) 1 d D . . C 3
F5B F 0.4177(5) 0.5011(12) 0.1885(8) 0.123(3) Uani 0.174(3) 1 d D . . C 3
F6B F 0.4986(6) 0.5442(9) 0.2157(9) 0.125(5) Uani 0.174(3) 1 d D . . C 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C3 1.900(11) . ?
Br2 C6 1.902(10) . ?
Co1 O1 1.930(7) . ?
Co1 O2 2.006(9) . ?
Co1 N1 2.003(6) . ?
Co1 N2 2.092(7) . ?
Co1 N3 2.105(7) . ?
Co1 N4 2.133(9) . ?
O1 C1 1.322(10) . ?
O2 C2 1.258(16) . ?
N1 C17 1.451(14) . ?
N1 C23 1.498(11) . ?
N1 C29 1.476(13) . ?
N2 C12 1.347(12) . ?
N2 C16 1.395(12) . ?
N3 C18 1.359(10) . ?
N3 C22 1.335(12) . ?
N4 C24 1.354(12) . ?
N4 C28 1.354(12) . ?
C1 C2 1.458(14) . ?
C1 C6 1.353(15) . ?
C2 C3 1.413(18) . ?
C3 C4 1.342(19) . ?
C4 C5 1.428(17) . ?
C4 C7 1.566(17) . ?
C5 C6 1.383(11) . ?
C5 C11 1.530(13) . ?
C7 C8 1.558(16) . ?
C7 C9 1.59(2) . ?
C7 C10 1.53(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.543(12) . ?
C11 C5 1.530(13) 4_556 ?
C11 C10 1.543(12) 4_556 ?
C12 C13 1.419(17) . ?
C12 C30 1.502(18) . ?
C13 H13 0.9500 . ?
C13 C14 1.36(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.36(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.345(15) . ?
C16 C17 1.462(15) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.376(14) . ?
C18 C31 1.476(15) . ?
C19 H19 0.9500 . ?
C19 C20 1.339(18) . ?
C20 H20 0.9500 . ?
C20 C21 1.390(17) . ?
C21 H21 0.9500 . ?
C21 C22 1.359(14) . ?
C22 C23 1.511(14) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.37(2) . ?
C24 C32 1.504(18) . ?
C25 H25 0.9500 . ?
C25 C26 1.33(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.409(16) . ?
C27 H27 0.9500 . ?
C27 C28 1.398(14) . ?
C28 C29 1.469(12) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
P1 F1 1.6001(9) . ?
P1 F2 1.5998(9) . ?
P1 F3 1.6000(9) . ?
P1 F4 1.5999(9) . ?
P1 F5 1.6002(9) . ?
P1 F6 1.5998(9) . ?
P1A F1A 1.6001(9) . ?
P1A F2A 1.5999(9) . ?
P1A F3A 1.5999(9) . ?
P1A F4A 1.6000(9) . ?
P1A F5A 1.6000(9) . ?
P1A F6A 1.5999(9) . ?
P1B F1B 1.6000(9) . ?
P1B F2B 1.5999(9) . ?
P1B F3B 1.6000(9) . ?
P1B F4B 1.6000(9) . ?
P1B F5B 1.6000(9) . ?
P1B F6B 1.5999(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O2 83.1(4) . . ?
O1 Co1 N1 170.3(3) . . ?
O1 Co1 N2 104.0(3) . . ?
O1 Co1 N3 99.0(3) . . ?
O1 Co1 N4 98.0(3) . . ?
O2 Co1 N2 169.7(3) . . ?
O2 Co1 N3 91.2(3) . . ?
O2 Co1 N4 87.5(3) . . ?
N1 Co1 O2 87.3(4) . . ?
N1 Co1 N2 85.3(3) . . ?
N1 Co1 N3 82.4(3) . . ?
N1 Co1 N4 80.3(3) . . ?
N2 Co1 N3 94.9(3) . . ?
N2 Co1 N4 84.2(3) . . ?
N3 Co1 N4 162.7(3) . . ?
C1 O1 Co1 113.4(6) . . ?
C2 O2 Co1 109.0(6) . . ?
C17 N1 Co1 109.4(6) . . ?
C17 N1 C23 108.7(9) . . ?
C17 N1 C29 113.6(8) . . ?
C23 N1 Co1 107.7(5) . . ?
C29 N1 Co1 107.0(6) . . ?
C29 N1 C23 110.2(8) . . ?
C12 N2 Co1 129.4(6) . . ?
C12 N2 C16 121.0(8) . . ?
C16 N2 Co1 107.2(7) . . ?
C18 N3 Co1 130.6(6) . . ?
C22 N3 Co1 110.7(6) . . ?
C22 N3 C18 118.5(8) . . ?
C24 N4 Co1 131.8(8) . . ?
C28 N4 Co1 109.6(6) . . ?
C28 N4 C24 118.2(10) . . ?
O1 C1 C2 112.8(11) . . ?
O1 C1 C6 126.0(8) . . ?
C6 C1 C2 121.1(9) . . ?
O2 C2 C1 120.4(10) . . ?
O2 C2 C3 123.6(11) . . ?
C3 C2 C1 116.0(13) . . ?
C2 C3 Br1 115.5(12) . . ?
C4 C3 Br1 122.7(9) . . ?
C4 C3 C2 121.8(11) . . ?
C3 C4 C5 121.1(9) . . ?
C3 C4 C7 133.3(12) . . ?
C5 C4 C7 105.6(14) . . ?
C4 C5 C11 113.9(8) . . ?
C6 C5 C4 118.5(12) . . ?
C6 C5 C11 127.6(11) . . ?
C1 C6 Br2 116.1(6) . . ?
C1 C6 C5 121.0(10) . . ?
C5 C6 Br2 122.8(10) . . ?
C4 C7 C9 109.2(14) . . ?
C8 C7 C4 107.8(9) . . ?
C8 C7 C9 108.3(12) . . ?
C10 C7 C4 105.7(10) . . ?
C10 C7 C8 113.7(15) . . ?
C10 C7 C9 112.0(10) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 110.3 . . ?
C7 C10 H10B 110.3 . . ?
C7 C10 C11 107.1(8) . . ?
H10A C10 H10B 108.6 . . ?
C11 C10 H10A 110.3 . . ?
C11 C10 H10B 110.3 . . ?
C5 C11 C5 117.4(10) 4_556 . ?
C5 C11 C10 102.3(7) . . ?
C5 C11 C10 111.1(6) . 4_556 ?
C5 C11 C10 111.1(6) 4_556 . ?
C5 C11 C10 102.3(7) 4_556 4_556 ?
C10 C11 C10 113.2(12) . 4_556 ?
N2 C12 C13 118.2(12) . . ?
N2 C12 C30 121.9(10) . . ?
C13 C12 C30 119.9(11) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 C12 118.5(12) . . ?
C14 C13 H13 120.7 . . ?
C13 C14 H14 118.6 . . ?
C15 C14 C13 122.7(12) . . ?
C15 C14 H14 118.6 . . ?
C14 C15 H15 120.7 . . ?
C16 C15 C14 118.7(14) . . ?
C16 C15 H15 120.7 . . ?
N2 C16 C17 116.5(7) . . ?
C15 C16 N2 120.6(12) . . ?
C15 C16 C17 122.9(11) . . ?
N1 C17 C16 114.5(7) . . ?
N1 C17 H17A 108.6 . . ?
N1 C17 H17B 108.6 . . ?
C16 C17 H17A 108.6 . . ?
C16 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
N3 C18 C19 121.2(9) . . ?
N3 C18 C31 120.8(9) . . ?
C19 C18 C31 118.0(9) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.8(10) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 120.4 . . ?
C19 C20 C21 119.1(11) . . ?
C21 C20 H20 120.4 . . ?
C20 C21 H21 120.3 . . ?
C22 C21 C20 119.5(11) . . ?
C22 C21 H21 120.3 . . ?
N3 C22 C21 121.7(9) . . ?
N3 C22 C23 116.7(8) . . ?
C21 C22 C23 121.4(10) . . ?
N1 C23 C22 108.5(8) . . ?
N1 C23 H23A 110.0 . . ?
N1 C23 H23B 110.0 . . ?
C22 C23 H23A 110.0 . . ?
C22 C23 H23B 110.0 . . ?
H23A C23 H23B 108.4 . . ?
N4 C24 C25 121.0(11) . . ?
N4 C24 C32 119.9(13) . . ?
C25 C24 C32 119.1(11) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 C24 122.0(10) . . ?
C26 C25 H25 119.0 . . ?
C25 C26 H26 120.5 . . ?
C25 C26 C27 119.0(12) . . ?
C27 C26 H26 120.5 . . ?
C26 C27 H27 121.2 . . ?
C28 C27 C26 117.5(12) . . ?
C28 C27 H27 121.2 . . ?
N4 C28 C27 122.2(9) . . ?
N4 C28 C29 116.2(8) . . ?
C27 C28 C29 121.5(9) . . ?
N1 C29 H29A 110.0 . . ?
N1 C29 H29B 110.0 . . ?
C28 C29 N1 108.7(8) . . ?
C28 C29 H29A 110.0 . . ?
C28 C29 H29B 110.0 . . ?
H29A C29 H29B 108.3 . . ?
C12 C30 H30A 109.5 . . ?
C12 C30 H30B 109.5 . . ?
C12 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C18 C31 H31A 109.5 . . ?
C18 C31 H31B 109.5 . . ?
C18 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C24 C32 H32A 109.5 . . ?
C24 C32 H32B 109.5 . . ?
C24 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
F2 P1 F1 90.00(6) . . ?
F2 P1 F3 90.01(6) . . ?
F2 P1 F4 90.02(6) . . ?
F2 P1 F5 179.98(10) . . ?
F3 P1 F1 89.99(6) . . ?
F3 P1 F5 89.98(6) . . ?
F4 P1 F1 90.00(6) . . ?
F4 P1 F3 179.96(10) . . ?
F4 P1 F5 89.98(6) . . ?
F5 P1 F1 89.99(6) . . ?
F6 P1 F1 179.98(10) . . ?
F6 P1 F2 90.02(6) . . ?
F6 P1 F3 90.00(6) . . ?
F6 P1 F4 90.01(6) . . ?
F6 P1 F5 90.00(6) . . ?
F2A P1A F1A 90.00(6) . . ?
F2A P1A F3A 90.01(6) . . ?
F2A P1A F5A 179.99(10) . . ?
F3A P1A F1A 90.00(6) . . ?
F4A P1A F1A 90.00(6) . . ?
F4A P1A F2A 90.01(6) . . ?
F4A P1A F3A 179.99(10) . . ?
F4A P1A F5A 89.99(6) . . ?
F5A P1A F1A 89.99(6) . . ?
F5A P1A F3A 90.00(6) . . ?
F6A P1A F1A 180.00(10) . . ?
F6A P1A F2A 90.00(6) . . ?
F6A P1A F3A 90.00(6) . . ?
F6A P1A F4A 90.00(6) . . ?
F6A P1A F5A 90.00(6) . . ?
F1B P1B F4B 90.00(6) . . ?
F1B P1B F5B 90.00(6) . . ?
F2B P1B F1B 90.00(6) . . ?
F2B P1B F3B 90.00(6) . . ?
F2B P1B F4B 90.00(6) . . ?
F2B P1B F5B 180.0(9) . . ?
F2B P1B F6B 90.00(6) . . ?
F3B P1B F1B 90.00(6) . . ?
F3B P1B F4B 179.99(10) . . ?
F3B P1B F5B 90.00(6) . . ?
F3B P1B F6B 90.00(6) . . ?
F4B P1B F5B 89.99(6) . . ?
F6B P1B F1B 179.99(10) . . ?
F6B P1B F4B 90.00(6) . . ?
F6B P1B F5B 90.00(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
Br1 C3 C4 C5 -174.7(6) . . . . ?
Br1 C3 C4 C7 2.6(16) . . . . ?
Co1 O1 C1 C2 -6.6(9) . . . . ?
Co1 O1 C1 C6 176.1(7) . . . . ?
Co1 O2 C2 C1 9.6(10) . . . . ?
Co1 O2 C2 C3 -170.0(7) . . . . ?
Co1 N1 C17 C16 20.3(11) . . . . ?
Co1 N1 C23 C22 40.1(11) . . . . ?
Co1 N1 C29 C28 -46.1(9) . . . . ?
Co1 N2 C12 C13 153.7(10) . . . . ?
Co1 N2 C12 C30 -23(2) . . . . ?
Co1 N2 C16 C15 -158.4(12) . . . . ?
Co1 N2 C16 C17 24.7(12) . . . . ?
Co1 N3 C18 C19 173.3(6) . . . . ?
Co1 N3 C18 C31 -6.9(11) . . . . ?
Co1 N3 C22 C21 -173.0(11) . . . . ?
Co1 N3 C22 C23 10.7(11) . . . . ?
Co1 N4 C24 C25 -171.9(7) . . . . ?
Co1 N4 C24 C32 8.0(13) . . . . ?
Co1 N4 C28 C27 174.4(8) . . . . ?
Co1 N4 C28 C29 -7.6(11) . . . . ?
O1 C1 C2 O2 -2.5(12) . . . . ?
O1 C1 C2 C3 177.1(7) . . . . ?
O1 C1 C6 Br2 1.3(12) . . . . ?
O1 C1 C6 C5 -175.9(8) . . . . ?
O2 C2 C3 Br1 -1.9(12) . . . . ?
O2 C2 C3 C4 179.6(10) . . . . ?
N2 C12 C13 C14 6(2) . . . . ?
N2 C16 C17 N1 -31.6(15) . . . . ?
N3 C18 C19 C20 -0.5(15) . . . . ?
N3 C22 C23 N1 -34.2(14) . . . . ?
N4 C24 C25 C26 -1.9(16) . . . . ?
N4 C28 C29 N1 35.7(12) . . . . ?
C1 C2 C3 Br1 178.5(6) . . . . ?
C1 C2 C3 C4 -0.1(13) . . . . ?
C2 C1 C6 Br2 -175.9(6) . . . . ?
C2 C1 C6 C5 7.0(13) . . . . ?
C2 C3 C4 C5 3.8(15) . . . . ?
C2 C3 C4 C7 -178.9(9) . . . . ?
C3 C4 C5 C6 -2.3(13) . . . . ?
C3 C4 C5 C11 178.1(8) . . . . ?
C3 C4 C7 C8 -69.9(18) . . . . ?
C3 C4 C7 C9 47.6(15) . . . . ?
C3 C4 C7 C10 168.2(11) . . . . ?
C4 C5 C6 Br2 180.0(6) . . . . ?
C4 C5 C6 C1 -3.1(12) . . . . ?
C4 C5 C11 C5 135.5(7) . . . 4_556 ?
C4 C5 C11 C10 -107.3(9) . . . 4_556 ?
C4 C5 C11 C10 13.7(9) . . . . ?
C4 C7 C10 C11 23.0(12) . . . . ?
C5 C4 C7 C8 107.7(13) . . . . ?
C5 C4 C7 C9 -134.9(10) . . . . ?
C5 C4 C7 C10 -14.3(11) . . . . ?
C6 C1 C2 O2 175.0(9) . . . . ?
C6 C1 C2 C3 -5.4(12) . . . . ?
C6 C5 C11 C5 -44.0(7) . . . 4_556 ?
C6 C5 C11 C10 -165.8(8) . . . . ?
C6 C5 C11 C10 73.1(12) . . . 4_556 ?
C7 C4 C5 C6 179.7(7) . . . . ?
C7 C4 C5 C11 0.1(9) . . . . ?
C7 C10 C11 C5 -22.0(11) . . . . ?
C7 C10 C11 C5 -148.1(9) . . . 4_556 ?
C7 C10 C11 C10 97.5(9) . . . 4_556 ?
C8 C7 C10 C11 -95.1(11) . . . . ?
C9 C7 C10 C11 141.7(11) . . . . ?
C11 C5 C6 Br2 -0.5(11) . . . . ?
C11 C5 C6 C1 176.4(8) . . . . ?
C12 N2 C16 C15 5.6(19) . . . . ?
C12 N2 C16 C17 -171.4(11) . . . . ?
C12 C13 C14 C15 -4(3) . . . . ?
C13 C14 C15 C16 4(3) . . . . ?
C14 C15 C16 N2 -4(2) . . . . ?
C14 C15 C16 C17 172.9(15) . . . . ?
C15 C16 C17 N1 151.5(13) . . . . ?
C16 N2 C12 C13 -6.3(19) . . . . ?
C16 N2 C12 C30 176.6(13) . . . . ?
C17 N1 C23 C22 -78.4(11) . . . . ?
C17 N1 C29 C28 74.8(9) . . . . ?
C18 N3 C22 C21 2.7(16) . . . . ?
C18 N3 C22 C23 -173.6(9) . . . . ?
C18 C19 C20 C21 1(2) . . . . ?
C19 C20 C21 C22 0(2) . . . . ?
C20 C21 C22 N3 -2(2) . . . . ?
C20 C21 C22 C23 173.9(13) . . . . ?
C21 C22 C23 N1 149.5(12) . . . . ?
C22 N3 C18 C19 -1.3(12) . . . . ?
C22 N3 C18 C31 178.4(9) . . . . ?
C23 N1 C17 C16 137.7(9) . . . . ?
C23 N1 C29 C28 -162.9(8) . . . . ?
C24 N4 C28 C27 -0.2(14) . . . . ?
C24 N4 C28 C29 177.8(9) . . . . ?
C24 C25 C26 C27 1.5(16) . . . . ?
C25 C26 C27 C28 -0.5(15) . . . . ?
C26 C27 C28 N4 -0.1(15) . . . . ?
C26 C27 C28 C29 -178.1(10) . . . . ?
C27 C28 C29 N1 -146.3(9) . . . . ?
C28 N4 C24 C25 1.2(14) . . . . ?
C28 N4 C24 C32 -178.8(9) . . . . ?
C29 N1 C17 C16 -99.2(10) . . . . ?
C29 N1 C23 C22 156.5(9) . . . . ?
C30 C12 C13 C14 -177.2(16) . . . . ?
C31 C18 C19 C20 179.8(11) . . . . ?
C32 C24 C25 C26 178.1(10) . . . . ?

_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 0.250 -0.738 0.250 696.0 153.8 '6 (C2 H6 O)'
2 -0.250 -0.398 0.750 696.0 151.8 '6 (C2 H6 O)'

_olex2_exptl_crystal_mounting_method 
'Mounted on MiTeGen mount in cryoprotectant oil'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.661
_oxdiff_exptl_absorpt_empirical_full_min 0.629
_vrf_DIFMN02_4a-3EtOH-150K    
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*0.75
RESPONSE: The valence tautomeric transition results in changes in conformation
of the ligand and changes in atom positions. The large electron density peaks
and minima were close to Br atoms suggesting the Br atom is now distributed
over two positions. Attemps to refine the ligand over two positions were not
successful. 
;
_vrf_DIFMN03_4a-3EtOH-150K    
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*0.75
RESPONSE: The valence tautomeric transition results in changes in conformation
of the ligand and changes in atom positions. The large electron density peaks
and minima were close to Br atoms suggesting the Br atom is now distributed
over two positions. Attemps to refine the ligand over two positions were not
successful. 
;
_vrf_DIFMX02_4a-3EtOH-150K    
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: The valence tautomeric transition results in changes in conformation
of the ligand and changes in atom positions. The large electron density peaks
and minima were close to Br atoms suggesting the Br atom is now distributed
over two positions. Attempts to refine the ligand over two positions were not
successful. 
;
_vrf_PLAT082_4a-3EtOH-150K    
;
PROBLEM: High R1 Value ..................................       0.11 Report
RESPONSE: Although the quality of the crystal appeared to be fine, the 
structure shows significant disorder, with all atoms having large
anisotropic displacement parameters, which is consistent with the 
compound undergoing a valence tautomeric transition on lowering the 
temperature from 300K.
;
_vrf_PLAT084_4a-3EtOH-150K    
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.31 Report
RESPONSE: Although the quality of the crystal appeared to be fine, the 
structure shows significant disorder, with all atoms having large
anisotropic displacement parameters, which is consistent with the 
compound undergoing a valence tautomeric transition on lowering the 
temperature from 300K.
;
_vrf_PLAT097_4a-3EtOH-150K    
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       2.71 eA-3  
RESPONSE: The valence tautomeric transition results in changes in conformation
of the ligand and changes in atom positions. The large electron density peaks
and minima were close to Br atoms suggesting the Br atom is now distributed
over two positions. Attempts to refine the ligand over two positions were not
successful.
;
_vrf_PLAT098_4a-3EtOH-150K    
;
PROBLEM: Large Reported Min.  (Negative) Residual Density      -2.84 eA-3  
RESPONSE: The valence tautomeric transition results in changes in conformation
of the ligand and changes in atom positions. The large electron density peaks
and minima were close to Br atoms suggesting the Br atom is now distributed
over two positions. Attempts to refine the ligand over two positions were not
successful.
;
_vrf_PLAT213_4a-3EtOH-150K    
;
PROBLEM: Atom Br1             has ADP max/min Ratio .....        3.4 prolat
RESPONSE: The valence tautomeric transition results in changes in conformation
of the ligand and changes in atom positions. The large electron density peaks
and minima were close to Br atoms suggesting the Br atom is now distributed
over two positions. Attempts to refine the ligand over two positions were not
successful, and as a result the Br atom has large anisotropic thermal 
displacement parameters.
;
_vrf_PLAT234_4a-3EtOH-150K    
;
PROBLEM: Large Hirshfeld Difference C19      --C20      .       0.16 Ang.  
RESPONSE: These atoms are correctly assigned, C19 and C20 are part of a
pyridine ring that displays disorder. Br1, C1, C2 and C3 belong to a 
disordered dioxolene ring involved in the valence tautomeric transition.
;
_vrf_PLAT241_4a-3EtOH-150K    
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O2 Check 
RESPONSE: O2 is bonded to the metal which has lower displacement parameters.
C14, C20-C21 are part of pyridine rings that show disorder. 
Carbon atoms further from the coordinating N atom in the pyridine rings 
display greater thermal displacement parameters. C23 is a methylene carbon
adjacent to a coordinating N and an aromatic ring.
;
_vrf_PLAT242_4a-3EtOH-150K    
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Co1 Check 
RESPONSE: Co1 is the metal center, N2 is a coordinating N atom that is more
tightly bound and C12 is adjacent to a coordinating N atom in a disordered 
pyridine ring. C2 belongs to a disordered ligand.
;
_vrf_PLAT250_4a-3EtOH-150K    
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.4 Note  
RESPONSE: Crystal displays anisotropic disorder associated with a valence
tautomeric transition.
;
_vrf_PLAT260_4a-3EtOH-150K    
;
PROBLEM: Large Average Ueq of Residue Including       Br1      0.111 Check 
RESPONSE: The PF6 anion is disordered over three orientations. The structure
shows significant disorder, with all atoms having large anisotropic
displacement parameters, which is consistent with the compound undergoing
a valence tautomeric transition on lowering the temperature from 300K.
;
_vrf_PLAT341_4a-3EtOH-150K    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.01667 Ang.  
RESPONSE: Due to the presence of Bromine atoms and significant disorder.
;
_vrf_PLAT906_4a-3EtOH-150K    
;
PROBLEM: Large K Value in the Analysis of Variance ......      3.073 Check 
RESPONSE: This arises from the low intensity reflections which are the most
affected by any inaccuracies in the processing of the data - any over or under
estimation of the peak and background intensities will have a relativity large
effect on the lower intensity data than the high intensity data.
;
_vrf_PLAT911_4a-3EtOH-150K    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          5 Report
RESPONSE: In detector rejection region or otherwise not measured.
;
_vrf_PLAT975_4a-3EtOH-150K    
;
PROBLEM: Check Calcd Resid. Dens.  0.56A   From O2              0.41 eA-3  
RESPONSE: The valence tautomeric transition results in changes in conformation
of the ligand containing O2 and changes in atom positions. Attempts to refine
the ligand over two positions were not successful.
;
_vrf_PLAT978_4a-3EtOH-150K    
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: Noted.
;

