# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Jason Love'
_publ_contact_author_email       JASON.LOVE@ED.AC.UK

_publ_section_title              
;
Tautomerisation and hydrogen-bonding
interactions in four-coordinate metal halide and azide
complexes of N-donor-extended dipyrromethanes

;
loop_
_publ_author_name
'Jason Love'
'Alexander J. Blake'
'Stuart D. Reid'
'Claire Wilson'

# Attachment 'combined.CIF'

data_FE2MTB
_database_code_depnum_ccdc_archive 'CCDC 731449'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H32 Br2 Fe N4'
_chemical_formula_sum            'C21 H32 Br2 Fe N4'
_chemical_formula_weight         556.16

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_Int_Tables_number      2

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

_cell_length_a                   8.9170(8)
_cell_length_b                   9.4120(9)
_cell_length_c                   14.4922(14)
_cell_angle_alpha                99.138(2)
_cell_angle_beta                 96.256(2)
_cell_angle_gamma                92.283(2)
_cell_volume                     1191.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3844
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       tablet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             564
_exptl_absorpt_coefficient_mu    3.999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0610
_exptl_absorpt_correction_T_max  0.122
_exptl_absorpt_process_details   '(SHELXTL version 6.12; Bruker, 2001)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7254
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.42
_diffrn_reflns_theta_max         27.5
_reflns_number_total             5172
_reflns_number_gt                4257
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'enCIFer (CCDC, 2003); PLATON (Spek, 2003)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     'Patterson heavy-atom'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5169
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0619
_refine_ls_goodness_of_fit_ref   0.94
_refine_ls_restrained_S_all      0.94
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.38988(4) 0.39438(3) 0.23478(2) 0.02283(8) Uani 1 1 d . . .
Br1 Br 0.41133(3) 0.16435(2) 0.288386(17) 0.03008(7) Uani 1 1 d . . .
Br2 Br 0.21003(3) 0.37190(3) 0.093702(17) 0.03712(8) Uani 1 1 d . . .
N1 N 0.0782(2) 0.32974(19) 0.33625(13) 0.0250(4) Uani 1 1 d . . .
H1 H 0.1715 0.3028 0.3356 0.030 Uiso 1 1 calc R . .
N2 N 0.3258(2) 0.54945(19) 0.33766(12) 0.0220(4) Uani 1 1 d . . .
N3 N 0.5866(2) 0.50703(19) 0.22612(12) 0.0232(4) Uani 1 1 d . . .
N4 N 0.7346(2) 0.3249(2) 0.01606(13) 0.0303(4) Uani 1 1 d . . .
H4 H 0.8101 0.3854 0.0113 0.036 Uiso 1 1 calc R . .
C1 C -0.1835(3) 0.2732(3) 0.36434(19) 0.0377(6) Uani 1 1 d . . .
H1B H -0.1616 0.3181 0.4305 0.057 Uiso 1 1 calc R . .
H1C H -0.2616 0.1950 0.3584 0.057 Uiso 1 1 calc R . .
H1D H -0.2194 0.3454 0.3266 0.057 Uiso 1 1 calc R . .
C2 C -0.0711(3) 0.1422(3) 0.22648(18) 0.0444(7) Uani 1 1 d . . .
H2A H 0.0223 0.1046 0.2051 0.067 Uiso 1 1 calc R . .
H2B H -0.1070 0.2139 0.1883 0.067 Uiso 1 1 calc R . .
H2C H -0.1482 0.0630 0.2198 0.067 Uiso 1 1 calc R . .
C3 C 0.0224(3) 0.1059(3) 0.39030(19) 0.0359(6) Uani 1 1 d . . .
H3A H 0.0413 0.1536 0.4560 0.054 Uiso 1 1 calc R . .
H3B H 0.1172 0.0718 0.3690 0.054 Uiso 1 1 calc R . .
H3C H -0.0509 0.0238 0.3851 0.054 Uiso 1 1 calc R . .
C4 C -0.0405(3) 0.2126(2) 0.32934(16) 0.0283(5) Uani 1 1 d . . .
C5 C 0.0614(2) 0.4686(2) 0.34317(15) 0.0243(5) Uani 1 1 d . . .
H5 H -0.0384 0.4993 0.3460 0.029 Uiso 1 1 calc R . .
C6 C 0.1757(2) 0.5759(2) 0.34686(15) 0.0242(5) Uani 1 1 d . . .
C7 C 0.1611(3) 0.7244(2) 0.37394(16) 0.0297(5) Uani 1 1 d . . .
H7 H 0.0701 0.7708 0.3837 0.036 Uiso 1 1 calc R . .
C8 C 0.3041(3) 0.7894(2) 0.38359(16) 0.0285(5) Uani 1 1 d . . .
H8 H 0.3310 0.8894 0.4019 0.034 Uiso 1 1 calc R . .
C9 C 0.4031(2) 0.6794(2) 0.36109(14) 0.0225(5) Uani 1 1 d . . .
C10 C 0.5749(2) 0.6935(2) 0.36994(15) 0.0227(5) Uani 1 1 d . . .
C11 C 0.6362(3) 0.6089(2) 0.44796(15) 0.0289(5) Uani 1 1 d . . .
H11A H 0.6034 0.5067 0.4295 0.043 Uiso 1 1 calc R . .
H11B H 0.5972 0.6473 0.5070 0.043 Uiso 1 1 calc R . .
H11C H 0.7469 0.6191 0.4567 0.043 Uiso 1 1 calc R . .
C12 C 0.6287(3) 0.8529(2) 0.40131(17) 0.0315(5) Uani 1 1 d . . .
H12A H 0.5914 0.9088 0.3529 0.047 Uiso 1 1 calc R . .
H12B H 0.7394 0.8616 0.4105 0.047 Uiso 1 1 calc R . .
H12C H 0.5896 0.8899 0.4606 0.047 Uiso 1 1 calc R . .
C13 C 0.6389(2) 0.6334(2) 0.28032(14) 0.0225(5) Uani 1 1 d . . .
C14 C 0.7666(3) 0.6893(2) 0.24439(16) 0.0291(5) Uani 1 1 d . . .
H14 H 0.8240 0.7766 0.2699 0.035 Uiso 1 1 calc R . .
C15 C 0.7920(3) 0.5950(3) 0.16651(16) 0.0305(5) Uani 1 1 d . . .
H15 H 0.8700 0.6043 0.1278 0.037 Uiso 1 1 calc R . .
C16 C 0.6809(3) 0.4819(2) 0.15468(15) 0.0245(5) Uani 1 1 d . . .
C17 C 0.6572(3) 0.3579(2) 0.08665(15) 0.0254(5) Uani 1 1 d . . .
H17 H 0.5771 0.2914 0.0925 0.030 Uiso 1 1 calc R . .
C18 C 0.7066(3) 0.1935(2) -0.05768(16) 0.0294(5) Uani 1 1 d . . .
C19 C 0.5487(3) 0.1965(3) -0.10796(19) 0.0432(7) Uani 1 1 d . . .
H19A H 0.5413 0.2835 -0.1370 0.065 Uiso 1 1 calc R . .
H19B H 0.4748 0.1968 -0.0626 0.065 Uiso 1 1 calc R . .
H19C H 0.5279 0.1110 -0.1568 0.065 Uiso 1 1 calc R . .
C20 C 0.8263(3) 0.2020(3) -0.12429(19) 0.0463(7) Uani 1 1 d . . .
H20A H 0.8146 0.2886 -0.1535 0.069 Uiso 1 1 calc R . .
H20B H 0.8142 0.1163 -0.1733 0.069 Uiso 1 1 calc R . .
H20C H 0.9270 0.2066 -0.0889 0.069 Uiso 1 1 calc R . .
C21 C 0.7242(3) 0.0598(3) -0.01167(18) 0.0420(7) Uani 1 1 d . . .
H21A H 0.6465 0.0546 0.0308 0.063 Uiso 1 1 calc R . .
H21B H 0.8245 0.0649 0.0242 0.063 Uiso 1 1 calc R . .
H21C H 0.7129 -0.0262 -0.0604 0.063 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe 0.02506(17) 0.01970(16) 0.02336(16) 0.00158(12) 0.00498(13) -0.00107(12)
Br1 0.02772(13) 0.02240(12) 0.04032(14) 0.00578(10) 0.00377(10) 0.00183(9)
Br2 0.04560(16) 0.03627(15) 0.02736(13) 0.00663(10) -0.00409(11) -0.00633(11)
N1 0.0181(9) 0.0270(10) 0.0303(10) 0.0056(8) 0.0025(8) 0.0012(7)
N2 0.0223(9) 0.0210(9) 0.0223(9) 0.0025(7) 0.0024(7) 0.0011(7)
N3 0.0251(10) 0.0225(10) 0.0222(9) 0.0029(7) 0.0052(8) -0.0002(7)
N4 0.0344(11) 0.0279(11) 0.0280(10) -0.0001(8) 0.0106(9) -0.0043(8)
C1 0.0213(12) 0.0409(15) 0.0534(17) 0.0159(13) 0.0042(11) -0.0002(11)
C2 0.0495(17) 0.0377(15) 0.0402(15) -0.0012(12) -0.0058(13) -0.0064(13)
C3 0.0282(13) 0.0318(14) 0.0501(16) 0.0173(12) 0.0019(11) -0.0016(10)
C4 0.0231(12) 0.0267(12) 0.0348(13) 0.0081(10) -0.0009(10) -0.0033(9)
C5 0.0213(11) 0.0279(12) 0.0240(11) 0.0045(9) 0.0031(9) 0.0037(9)
C6 0.0249(12) 0.0256(12) 0.0216(11) 0.0027(9) 0.0023(9) 0.0031(9)
C7 0.0276(13) 0.0278(13) 0.0338(13) 0.0017(10) 0.0066(10) 0.0074(10)
C8 0.0326(13) 0.0208(12) 0.0304(12) -0.0019(9) 0.0050(10) 0.0021(9)
C9 0.0272(12) 0.0224(11) 0.0177(10) 0.0026(8) 0.0024(9) 0.0009(9)
C10 0.0232(11) 0.0213(11) 0.0225(11) 0.0010(9) 0.0013(9) 0.0009(9)
C11 0.0291(13) 0.0334(13) 0.0233(11) 0.0032(10) 0.0014(9) 0.0000(10)
C12 0.0283(13) 0.0278(13) 0.0352(13) -0.0018(10) 0.0008(10) -0.0025(10)
C13 0.0242(12) 0.0224(11) 0.0208(11) 0.0053(9) -0.0002(9) 0.0018(9)
C14 0.0277(13) 0.0285(13) 0.0290(12) 0.0016(10) 0.0013(10) -0.0063(10)
C15 0.0258(12) 0.0361(14) 0.0299(12) 0.0044(10) 0.0072(10) -0.0019(10)
C16 0.0254(12) 0.0256(12) 0.0229(11) 0.0041(9) 0.0041(9) 0.0015(9)
C17 0.0277(12) 0.0249(12) 0.0243(11) 0.0060(9) 0.0043(9) 0.0005(9)
C18 0.0381(14) 0.0249(12) 0.0244(12) 0.0005(9) 0.0053(10) 0.0014(10)
C19 0.0510(17) 0.0383(15) 0.0357(15) -0.0024(12) -0.0046(12) 0.0086(13)
C20 0.0578(19) 0.0401(16) 0.0400(15) -0.0065(12) 0.0221(14) 0.0000(13)
C21 0.0606(19) 0.0314(14) 0.0324(14) 0.0030(11) 0.0008(13) 0.0047(12)

_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
Fe Br1 2.4213(4) . ?
Fe Br2 2.4327(4) . ?
Fe N2 2.0591(18) . ?
Fe N3 2.0392(17) . ?
N1 C5 1.310(3) . ?
N1 C4 1.481(3) . ?
N1 H1 0.8800 . ?
N2 C9 1.355(3) . ?
N2 C6 1.388(3) . ?
N3 C13 1.352(3) . ?
N3 C16 1.401(3) . ?
N4 C17 1.300(3) . ?
N4 C18 1.494(3) . ?
N4 H4 0.8800 . ?
C1 C4 1.521(3) . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C2 C4 1.523(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.524(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 C6 1.397(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.406(3) . ?
C7 C8 1.375(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.410(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.521(3) . ?
C10 C13 1.512(3) . ?
C10 C12 1.539(3) . ?
C10 C11 1.548(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.419(3) . ?
C14 C15 1.366(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.402(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.396(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.517(4) . ?
C18 C21 1.521(3) . ?
C18 C20 1.523(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe N2 93.20(7) . . ?
N3 Fe Br1 116.90(5) . . ?
N2 Fe Br1 111.43(5) . . ?
N3 Fe Br2 113.64(5) . . ?
N2 Fe Br2 109.78(5) . . ?
Br1 Fe Br2 110.596(14) . . ?
C5 N1 C4 128.02(19) . . ?
C5 N1 H1 116.0 . . ?
C4 N1 H1 116.0 . . ?
C9 N2 C6 105.89(18) . . ?
C9 N2 Fe 120.73(14) . . ?
C6 N2 Fe 122.75(14) . . ?
C13 N3 C16 106.31(17) . . ?
C13 N3 Fe 126.13(14) . . ?
C16 N3 Fe 126.87(14) . . ?
C17 N4 C18 125.7(2) . . ?
C17 N4 H4 117.1 . . ?
C18 N4 H4 117.1 . . ?
C4 C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C1 H1D 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 C1 110.26(19) . . ?
N1 C4 C2 107.58(19) . . ?
C1 C4 C2 110.7(2) . . ?
N1 C4 C3 106.82(18) . . ?
C1 C4 C3 110.5(2) . . ?
C2 C4 C3 110.9(2) . . ?
N1 C5 C6 126.5(2) . . ?
N1 C5 H5 116.8 . . ?
C6 C5 H5 116.8 . . ?
N2 C6 C5 124.3(2) . . ?
N2 C6 C7 109.91(19) . . ?
C5 C6 C7 125.2(2) . . ?
C8 C7 C6 106.7(2) . . ?
C8 C7 H7 126.7 . . ?
C6 C7 H7 126.7 . . ?
C7 C8 C9 106.92(19) . . ?
C7 C8 H8 126.5 . . ?
C9 C8 H8 126.5 . . ?
N2 C9 C8 110.59(19) . . ?
N2 C9 C10 121.76(19) . . ?
C8 C9 C10 127.37(19) . . ?
C13 C10 C9 113.35(17) . . ?
C13 C10 C12 110.07(17) . . ?
C9 C10 C12 109.35(18) . . ?
C13 C10 C11 108.19(17) . . ?
C9 C10 C11 107.78(17) . . ?
C12 C10 C11 107.93(18) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 109.69(19) . . ?
N3 C13 C10 122.88(18) . . ?
C14 C13 C10 127.21(19) . . ?
C15 C14 C13 107.63(19) . . ?
C15 C14 H14 126.2 . . ?
C13 C14 H14 126.2 . . ?
C14 C15 C16 106.9(2) . . ?
C14 C15 H15 126.6 . . ?
C16 C15 H15 126.6 . . ?
C17 C16 N3 120.54(19) . . ?
C17 C16 C15 130.0(2) . . ?
N3 C16 C15 109.47(19) . . ?
N4 C17 C16 126.0(2) . . ?
N4 C17 H17 117.0 . . ?
C16 C17 H17 117.0 . . ?
N4 C18 C19 108.1(2) . . ?
N4 C18 C21 109.38(19) . . ?
C19 C18 C21 111.5(2) . . ?
N4 C18 C20 106.37(19) . . ?
C19 C18 C20 111.4(2) . . ?
C21 C18 C20 109.9(2) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.943
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.943

_refine_diff_density_max         0.58
_refine_diff_density_min         -0.26
_refine_diff_density_rms         0.07

data_cotmaz
_database_code_depnum_ccdc_archive 'CCDC 731450'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H32 Cl0.25 Co N9.25'
_chemical_formula_weight         481.85

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.980(2)
_cell_length_b                   9.841(2)
_cell_length_c                   14.576(3)
_cell_angle_alpha                104.675(3)
_cell_angle_beta                 95.490(3)
_cell_angle_gamma                98.661(3)
_cell_volume                     1219.7(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2712
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      27.15

_exptl_crystal_description       tablet
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             508
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'sadabs v2.05'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            10550
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4309
_reflns_number_gt                3653
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'

_refine_special_details          
;

Widespread disorder. Azide/Cl 0.75/0.25 modelled, N8 isotropic.
tBu C1 modelled over 2 sites 70:30. CNtBu arm 85:15. Positioning
of C17' not ideal with respect to C15 etc, probably minor disorder
of this ring too but this was not modelled.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+1.9261P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4282
_refine_ls_number_parameters     279
_refine_ls_number_restraints     133
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1325
_refine_ls_wR_factor_gt          0.1272
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.07848(6) 0.11145(5) 0.26322(3) 0.03448(18) Uani 1 1 d . . .
N1 N 0.4132(3) 0.1893(3) 0.2030(2) 0.0395(8) Uani 1 1 d . B .
H1A H 0.3228 0.2127 0.2070 0.047 Uiso 1 1 calc R . .
N2 N 0.1421(3) -0.0372(3) 0.1627(2) 0.0305(6) Uani 1 1 d . B .
N3 N -0.1092(3) -0.0139(3) 0.2741(2) 0.0350(7) Uani 1 1 d . A .
N4 N -0.2149(4) 0.1582(4) 0.5037(3) 0.0391(9) Uani 0.85 1 d P A 1
H4A H -0.3023 0.1040 0.5039 0.047 Uiso 0.85 1 calc PR A 1
N4' N -0.0989(19) 0.1698(17) 0.4822(12) 0.017(3) Uiso 0.15 1 d P A 2
H4'A H -0.0144 0.1768 0.4564 0.020 Uiso 0.15 1 calc PR A 2
C1 C 0.5060(9) 0.4324(7) 0.3056(5) 0.068(2) Uiso 0.70 1 d PD B 1
H1B H 0.4154 0.4634 0.2809 0.103 Uiso 0.70 1 calc PR B 1
H1C H 0.5918 0.5128 0.3237 0.103 Uiso 0.70 1 calc PR B 1
H1D H 0.4863 0.3990 0.3619 0.103 Uiso 0.70 1 calc PR B 1
C2 C 0.5717(9) 0.3582(9) 0.1404(5) 0.075(2) Uiso 0.70 1 d PD B 1
H2A H 0.5979 0.2801 0.0916 0.112 Uiso 0.70 1 calc PR B 1
H2B H 0.6557 0.4401 0.1573 0.112 Uiso 0.70 1 calc PR B 1
H2C H 0.4794 0.3861 0.1152 0.112 Uiso 0.70 1 calc PR B 1
C3 C 0.6871(6) 0.2693(7) 0.2716(5) 0.0540(16) Uiso 0.70 1 d PD B 1
H3A H 0.7169 0.1910 0.2249 0.081 Uiso 0.70 1 calc PR B 1
H3B H 0.6657 0.2388 0.3287 0.081 Uiso 0.70 1 calc PR B 1
H3C H 0.7700 0.3522 0.2895 0.081 Uiso 0.70 1 calc PR B 1
C1' C 0.5508(19) 0.3816(17) 0.3310(6) 0.067(5) Uiso 0.30 1 d PD B 2
H1'A H 0.6002 0.3280 0.3694 0.101 Uiso 0.30 1 calc PR B 2
H1'B H 0.4472 0.3852 0.3460 0.101 Uiso 0.30 1 calc PR B 2
H1'C H 0.6090 0.4789 0.3457 0.101 Uiso 0.30 1 calc PR B 2
C2' C 0.5083(16) 0.4028(13) 0.1622(8) 0.048(3) Uiso 0.30 1 d PD B 2
H2'A H 0.5236 0.3565 0.0968 0.072 Uiso 0.30 1 calc PR B 2
H2'B H 0.5757 0.4961 0.1851 0.072 Uiso 0.30 1 calc PR B 2
H2'C H 0.4023 0.4155 0.1628 0.072 Uiso 0.30 1 calc PR B 2
C3' C 0.6869(14) 0.2527(17) 0.1995(11) 0.066(4) Uiso 0.30 1 d PD B 2
H3'A H 0.6598 0.1735 0.1410 0.100 Uiso 0.30 1 calc PR B 2
H3'B H 0.7325 0.2188 0.2514 0.100 Uiso 0.30 1 calc PR B 2
H3'C H 0.7600 0.3291 0.1881 0.100 Uiso 0.30 1 calc PR B 2
C4 C 0.5448(4) 0.3096(4) 0.2275(3) 0.0444(10) Uani 1 1 d D . .
C5 C 0.4163(4) 0.0532(4) 0.1763(3) 0.0389(9) Uani 1 1 d . . .
H5A H 0.5135 0.0267 0.1732 0.047 Uiso 1 1 calc R B .
C6 C 0.2905(4) -0.0572(4) 0.1519(3) 0.0358(8) Uani 1 1 d . B .
C7 C 0.2871(5) -0.1997(4) 0.1019(3) 0.0443(10) Uani 1 1 d . . .
H7A H 0.3726 -0.2426 0.0863 0.053 Uiso 1 1 calc R B .
C8 C 0.1375(5) -0.2655(4) 0.0799(3) 0.0423(9) Uani 1 1 d . B .
H8A H 0.0996 -0.3622 0.0452 0.051 Uiso 1 1 calc R . .
C9 C 0.0507(4) -0.1626(4) 0.1186(2) 0.0315(8) Uani 1 1 d . . .
C10 C -0.1221(4) -0.1780(4) 0.1092(2) 0.0324(8) Uani 1 1 d . B .
C11 C -0.1955(5) -0.3330(4) 0.0582(3) 0.0442(10) Uani 1 1 d . . .
H11A H -0.1654 -0.3955 0.0966 0.066 Uiso 1 1 calc R B .
H11B H -0.1616 -0.3609 -0.0047 0.066 Uiso 1 1 calc R . .
H11C H -0.3065 -0.3419 0.0501 0.066 Uiso 1 1 calc R . .
C12 C -0.1715(4) -0.0829(4) 0.0470(3) 0.0395(9) Uani 1 1 d . . .
H12A H -0.1252 0.0170 0.0782 0.059 Uiso 1 1 calc R B .
H12B H -0.2826 -0.0927 0.0392 0.059 Uiso 1 1 calc R . .
H12C H -0.1383 -0.1125 -0.0160 0.059 Uiso 1 1 calc R . .
C13 C -0.1794(4) -0.1319(4) 0.2050(2) 0.0317(8) Uani 1 1 d . . .
C14 C -0.3122(4) -0.1933(5) 0.2341(3) 0.0440(10) Uani 1 1 d . B .
H14A H -0.3816 -0.2772 0.1989 0.053 Uiso 1 1 calc R . .
C15 C -0.3225(5) -0.1085(5) 0.3237(3) 0.0493(11) Uani 1 1 d . . .
H15A H -0.4010 -0.1228 0.3614 0.059 Uiso 1 1 calc R B 2
C16 C -0.1966(4) 0.0018(5) 0.3485(3) 0.0415(9) Uani 1 1 d . A .
C17 C -0.1433(6) 0.1209(5) 0.4320(3) 0.0358(10) Uiso 0.85 1 d P A 1
H17A H -0.0464 0.1768 0.4341 0.043 Uiso 0.85 1 calc PR A 1
C17' C -0.214(2) 0.059(2) 0.4341(14) 0.020(4) Uiso 0.15 1 d P A 2
H17B H -0.2991 0.0285 0.4624 0.024 Uiso 0.15 1 calc PR A 2
C18 C -0.1611(5) 0.2865(5) 0.5869(3) 0.0364(10) Uiso 0.85 1 d PD A 1
C19 C -0.2001(8) 0.4141(7) 0.5565(5) 0.058(2) Uiso 0.85 1 d PD A 1
H19A H -0.3102 0.3996 0.5372 0.086 Uiso 0.85 1 calc PR A 1
H19B H -0.1471 0.4252 0.5024 0.086 Uiso 0.85 1 calc PR A 1
H19C H -0.1683 0.5002 0.6101 0.086 Uiso 0.85 1 calc PR A 1
C20 C -0.2456(6) 0.2603(6) 0.6667(4) 0.0564(14) Uiso 0.85 1 d PD A 1
H20A H -0.3553 0.2457 0.6461 0.085 Uiso 0.85 1 calc PR A 1
H20B H -0.2162 0.3431 0.7230 0.085 Uiso 0.85 1 calc PR A 1
H20C H -0.2204 0.1751 0.6832 0.085 Uiso 0.85 1 calc PR A 1
C21 C 0.0099(6) 0.3061(7) 0.6167(4) 0.0538(14) Uiso 0.85 1 d PD A 1
H21A H 0.0334 0.2226 0.6364 0.081 Uiso 0.85 1 calc PR A 1
H21B H 0.0432 0.3920 0.6704 0.081 Uiso 0.85 1 calc PR A 1
H21C H 0.0632 0.3162 0.5625 0.081 Uiso 0.85 1 calc PR A 1
C18' C -0.1014(19) 0.2774(17) 0.5720(12) 0.020(4) Uiso 0.15 1 d PD A 2
C19' C -0.187(2) 0.215(2) 0.6410(15) 0.033(5) Uiso 0.15 1 d PD A 2
H19D H -0.2942 0.1832 0.6140 0.049 Uiso 0.15 1 calc PR A 2
H19E H -0.1775 0.2885 0.7020 0.049 Uiso 0.15 1 calc PR A 2
H19F H -0.1434 0.1340 0.6517 0.049 Uiso 0.15 1 calc PR A 2
C20' C 0.0657(19) 0.328(3) 0.6109(19) 0.044(7) Uiso 0.15 1 d PD A 2
H20D H 0.1095 0.2482 0.6238 0.066 Uiso 0.15 1 calc PR A 2
H20E H 0.0771 0.4047 0.6704 0.066 Uiso 0.15 1 calc PR A 2
H20F H 0.1188 0.3639 0.5637 0.066 Uiso 0.15 1 calc PR A 2
C21' C -0.166(3) 0.402(3) 0.551(2) 0.039(9) Uiso 0.15 1 d PD A 2
H21D H -0.2745 0.3700 0.5249 0.059 Uiso 0.15 1 calc PR A 2
H21E H -0.1115 0.4364 0.5039 0.059 Uiso 0.15 1 calc PR A 2
H21F H -0.1553 0.4789 0.6100 0.059 Uiso 0.15 1 calc PR A 2
N6 N 0.3228(4) 0.1445(4) 0.4183(2) 0.0432(8) Uani 1 1 d D . .
N5 N 0.2079(4) 0.1698(4) 0.3888(2) 0.0558(10) Uani 1 1 d D C .
N7 N 0.4362(5) 0.1226(5) 0.4510(3) 0.0672(12) Uani 1 1 d . C .
Cl1 Cl 0.0809(7) 0.3089(8) 0.2012(4) 0.0518(15) Uani 0.25 1 d P C 1
N8 N 0.1007(9) 0.2887(9) 0.2299(6) 0.069(3) Uiso 0.75 1 d PD C 2
N9 N 0.0408(6) 0.3520(6) 0.1873(4) 0.0362(16) Uiso 0.75 1 d PD C 2
N10 N -0.0143(7) 0.4326(6) 0.1584(4) 0.0675(15) Uiso 0.75 1 d P C 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0315(3) 0.0378(3) 0.0304(3) 0.0034(2) 0.0035(2) 0.0054(2)
N1 0.0257(16) 0.047(2) 0.051(2) 0.0207(16) 0.0087(14) 0.0066(14)
N2 0.0297(15) 0.0378(17) 0.0262(15) 0.0113(13) 0.0067(12) 0.0069(13)
N3 0.0347(17) 0.0440(18) 0.0246(15) 0.0050(13) 0.0067(13) 0.0080(14)
N4 0.032(2) 0.049(2) 0.033(2) 0.0068(17) 0.0100(16) 0.0001(17)
C4 0.029(2) 0.050(2) 0.059(3) 0.026(2) 0.0079(18) 0.0020(17)
C5 0.0300(19) 0.055(3) 0.038(2) 0.0199(19) 0.0100(16) 0.0116(18)
C6 0.0299(19) 0.049(2) 0.0330(19) 0.0153(17) 0.0093(15) 0.0096(17)
C7 0.042(2) 0.048(2) 0.046(2) 0.0113(19) 0.0164(19) 0.0156(19)
C8 0.044(2) 0.039(2) 0.040(2) 0.0022(17) 0.0121(18) 0.0069(18)
C9 0.037(2) 0.036(2) 0.0213(17) 0.0074(15) 0.0073(14) 0.0035(16)
C10 0.0334(19) 0.036(2) 0.0252(17) 0.0067(15) 0.0045(14) 0.0022(15)
C11 0.043(2) 0.044(2) 0.038(2) 0.0028(18) 0.0087(18) -0.0008(18)
C12 0.036(2) 0.052(2) 0.0290(19) 0.0149(17) 0.0002(16) -0.0001(18)
C13 0.0314(19) 0.038(2) 0.0258(17) 0.0087(15) 0.0029(14) 0.0076(15)
C14 0.030(2) 0.062(3) 0.036(2) 0.0130(19) 0.0024(16) 0.0002(18)
C15 0.034(2) 0.081(3) 0.040(2) 0.023(2) 0.0156(18) 0.017(2)
C16 0.034(2) 0.061(3) 0.031(2) 0.0116(19) 0.0057(16) 0.0144(19)
N6 0.038(2) 0.057(2) 0.0304(17) 0.0080(16) 0.0063(15) 0.0023(16)
N5 0.043(2) 0.075(3) 0.038(2) -0.0057(18) 0.0000(16) 0.0139(19)
N7 0.043(2) 0.109(4) 0.053(2) 0.027(2) 0.0054(19) 0.017(2)
Cl1 0.040(3) 0.082(4) 0.029(3) 0.023(3) -0.001(2) -0.010(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
Co1 N8 1.914(8) . ?
Co1 N5 1.973(4) . ?
Co1 N3 1.977(3) . ?
Co1 N2 1.985(3) . ?
Co1 Cl1 2.339(9) . ?
N1 C5 1.301(5) . ?
N1 C4 1.487(5) . ?
N1 H1A 0.8800 . ?
N2 C9 1.342(5) . ?
N2 C6 1.393(4) . ?
N3 C13 1.351(5) . ?
N3 C16 1.390(5) . ?
N4 C17 1.283(6) . ?
N4 C18 1.492(6) . ?
N4 H4A 0.8800 . ?
N4' C17' 1.37(3) . ?
N4' C18' 1.46(2) . ?
N4' H4'A 0.8800 . ?
C1 C4 1.544(6) . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C2 C4 1.493(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.526(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C1' C4 1.487(7) . ?
C1' H1'A 0.9800 . ?
C1' H1'B 0.9800 . ?
C1' H1'C 0.9800 . ?
C2' C4 1.525(7) . ?
C2' H2'A 0.9800 . ?
C2' H2'B 0.9800 . ?
C2' H2'C 0.9800 . ?
C3' C4 1.518(7) . ?
C3' H3'A 0.9800 . ?
C3' H3'B 0.9800 . ?
C3' H3'C 0.9800 . ?
C5 C6 1.394(5) . ?
C5 H5A 0.9500 . ?
C6 C7 1.401(6) . ?
C7 C8 1.370(6) . ?
C7 H7A 0.9500 . ?
C8 C9 1.409(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.526(5) . ?
C10 C13 1.519(5) . ?
C10 C11 1.531(5) . ?
C10 C12 1.541(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.406(5) . ?
C14 C15 1.379(6) . ?
C14 H14A 0.9500 . ?
C15 C16 1.393(6) . ?
C15 H15A 0.9500 . ?
C16 C17 1.442(6) . ?
C17 H17A 0.9500 . ?
C17' H17B 0.9500 . ?
C18 C20 1.502(5) . ?
C18 C19 1.510(5) . ?
C18 C21 1.525(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C18' C19' 1.513(8) . ?
C18' C20' 1.514(8) . ?
C18' C21' 1.517(8) . ?
C19' H19D 0.9800 . ?
C19' H19E 0.9800 . ?
C19' H19F 0.9800 . ?
C20' H20D 0.9800 . ?
C20' H20E 0.9800 . ?
C20' H20F 0.9800 . ?
C21' H21D 0.9800 . ?
C21' H21E 0.9800 . ?
C21' H21F 0.9800 . ?
N6 N7 1.156(5) . ?
N6 N5 1.165(5) . ?
N8 N9 1.138(8) . ?
N9 N10 1.139(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
N8 Co1 N5 100.7(3) . . ?
N8 Co1 N3 129.1(3) . . ?
N5 Co1 N3 107.74(14) . . ?
N8 Co1 N2 110.2(3) . . ?
N5 Co1 N2 115.71(14) . . ?
N3 Co1 N2 94.39(12) . . ?
N8 Co1 Cl1 8.7(3) . . ?
N5 Co1 Cl1 109.33(18) . . ?
N3 Co1 Cl1 123.99(17) . . ?
N2 Co1 Cl1 105.33(16) . . ?
C5 N1 C4 127.5(3) . . ?
C5 N1 H1A 116.3 . . ?
C4 N1 H1A 116.3 . . ?
C9 N2 C6 106.7(3) . . ?
C9 N2 Co1 122.4(2) . . ?
C6 N2 Co1 126.7(2) . . ?
C13 N3 C16 107.0(3) . . ?
C13 N3 Co1 124.2(2) . . ?
C16 N3 Co1 128.7(3) . . ?
C17 N4 C18 124.9(4) . . ?
C17 N4 H4A 117.6 . . ?
C18 N4 H4A 117.6 . . ?
C17' N4' C18' 127.0(16) . . ?
C17' N4' H4'A 116.5 . . ?
C18' N4' H4'A 116.5 . . ?
C4 C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C1 H1D 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 C1' H1'A 109.5 . . ?
C4 C1' H1'B 109.5 . . ?
H1'A C1' H1'B 109.5 . . ?
C4 C1' H1'C 109.5 . . ?
H1'A C1' H1'C 109.5 . . ?
H1'B C1' H1'C 109.5 . . ?
C4 C2' H2'A 109.5 . . ?
C4 C2' H2'B 109.5 . . ?
H2'A C2' H2'B 109.5 . . ?
C4 C2' H2'C 109.5 . . ?
H2'A C2' H2'C 109.5 . . ?
H2'B C2' H2'C 109.5 . . ?
C4 C3' H3'A 109.5 . . ?
C4 C3' H3'B 109.5 . . ?
H3'A C3' H3'B 109.5 . . ?
C4 C3' H3'C 109.5 . . ?
H3'A C3' H3'C 109.5 . . ?
H3'B C3' H3'C 109.5 . . ?
N1 C4 C1' 106.2(7) . . ?
N1 C4 C2 109.6(4) . . ?
N1 C4 C3' 109.3(7) . . ?
C1' C4 C3' 115.4(8) . . ?
N1 C4 C2' 104.7(6) . . ?
C1' C4 C2' 113.5(7) . . ?
C3' C4 C2' 107.2(7) . . ?
N1 C4 C3 111.7(4) . . ?
C2 C4 C3 111.6(4) . . ?
N1 C4 C1 107.9(4) . . ?
C2 C4 C1 110.0(5) . . ?
C3' C4 C1 136.9(7) . . ?
C2' C4 C1 83.2(6) . . ?
C3 C4 C1 105.9(4) . . ?
N1 C5 C6 126.2(4) . . ?
N1 C5 H5A 116.9 . . ?
C6 C5 H5A 116.9 . . ?
N2 C6 C5 123.9(3) . . ?
N2 C6 C7 108.8(3) . . ?
C5 C6 C7 126.7(3) . . ?
C8 C7 C6 107.2(3) . . ?
C8 C7 H7A 126.4 . . ?
C6 C7 H7A 126.4 . . ?
C7 C8 C9 106.9(3) . . ?
C7 C8 H8A 126.5 . . ?
C9 C8 H8A 126.5 . . ?
N2 C9 C8 110.2(3) . . ?
N2 C9 C10 121.5(3) . . ?
C8 C9 C10 128.2(3) . . ?
C13 C10 C9 112.9(3) . . ?
C13 C10 C11 109.8(3) . . ?
C9 C10 C11 109.6(3) . . ?
C13 C10 C12 108.0(3) . . ?
C9 C10 C12 108.2(3) . . ?
C11 C10 C12 108.1(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 109.8(3) . . ?
N3 C13 C10 122.2(3) . . ?
C14 C13 C10 127.9(3) . . ?
C15 C14 C13 106.9(4) . . ?
C15 C14 H14A 126.6 . . ?
C13 C14 H14A 126.6 . . ?
C14 C15 C16 107.4(3) . . ?
C14 C15 C17' 144.9(7) . . ?
C14 C15 H15A 126.3 . . ?
C16 C15 H15A 126.3 . . ?
C17' C16 N3 150.8(11) . . ?
C17' C16 C15 99.7(11) . . ?
N3 C16 C15 108.9(3) . . ?
N3 C16 C17 117.5(4) . . ?
C15 C16 C17 133.7(4) . . ?
N4 C17 C16 125.9(5) . . ?
N4 C17 H17A 117.1 . . ?
C16 C17 H17A 117.1 . . ?
C16 C17' N4' 114.2(18) . . ?
N4' C17' C15 156.4(17) . . ?
C16 C17' H17B 122.9 . . ?
N4' C17' H17B 122.9 . . ?
C15 C17' H17B 80.5 . . ?
N4 C18 C20 106.2(4) . . ?
N4 C18 C19 107.3(4) . . ?
C20 C18 C19 111.6(4) . . ?
N4 C18 C21 110.8(4) . . ?
C20 C18 C21 110.3(4) . . ?
C19 C18 C21 110.4(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4' C18' C19' 112.2(15) . . ?
N4' C18' C20' 102.9(16) . . ?
C19' C18' C20' 111.2(10) . . ?
N4' C18' C21' 109.8(17) . . ?
C19' C18' C21' 111.7(11) . . ?
C20' C18' C21' 108.7(10) . . ?
C18' C19' H19D 109.5 . . ?
C18' C19' H19E 109.5 . . ?
H19D C19' H19E 109.5 . . ?
C18' C19' H19F 109.5 . . ?
H19D C19' H19F 109.5 . . ?
H19E C19' H19F 109.5 . . ?
C18' C20' H20D 109.5 . . ?
C18' C20' H20E 109.5 . . ?
H20D C20' H20E 109.5 . . ?
C18' C20' H20F 109.5 . . ?
H20D C20' H20F 109.5 . . ?
H20E C20' H20F 109.5 . . ?
C18' C21' H21D 109.5 . . ?
C18' C21' H21E 109.5 . . ?
H21D C21' H21E 109.5 . . ?
C18' C21' H21F 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
N7 N6 N5 177.3(4) . . ?
N6 N5 Co1 134.8(3) . . ?
N9 N8 Co1 143.1(7) . . ?
N8 N9 N10 168.8(8) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.067