# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_as136210

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
1,1,1-Tris(pyrid-2-yl)ethane 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H15 N3'
_chemical_formula_sum            'C17 H15 N3'
_chemical_formula_weight         261.32

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   9.2431(2)
_cell_length_b                   9.0085(2)
_cell_length_c                   15.7722(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.397(2)
_cell_angle_gamma                90.00
_cell_volume                     1307.47(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3128
_cell_measurement_theta_min      4.80
_cell_measurement_theta_max      73.58

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             552
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5146
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.81
_diffrn_reflns_theta_max         73.87
_reflns_number_total             2555
_reflns_number_gt                2281
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied. All 
 non-H atoms are refined anisotropically. H atoms were located in the Fourier 
 map and allowed to refine, with Uiso values of 1.2xUeq of the 
 corresponding C atoms for aromatic H atoms, or 1.5xUeq{C} for the methyl 
 group.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0399P)²+0.4310P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2555
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0899
_refine_ls_wR_factor_gt          0.0864
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
C1 C 0.99277(13) 0.28420(15) 0.62734(8) 0.0183(3) Uani 1 1 d . . .
H1A H 1.0110(17) 0.3264(18) 0.6862(10) 0.028 Uiso 1 1 d . . .
H1B H 1.0471(17) 0.3454(19) 0.5890(10) 0.028 Uiso 1 1 d . . .
H1C H 1.0328(17) 0.1832(19) 0.6266(10) 0.028 Uiso 1 1 d . . .
C2 C 0.82810(12) 0.28696(13) 0.59874(7) 0.0144(2) Uani 1 1 d . . .
N1 N 0.60771(10) 0.27009(11) 0.67257(6) 0.0156(2) Uani 1 1 d . . .
C3 C 0.74146(12) 0.21573(13) 0.66671(7) 0.0138(2) Uani 1 1 d . . .
C4 C 0.79842(13) 0.10019(14) 0.71821(8) 0.0174(3) Uani 1 1 d . . .
H4 H 0.8970(17) 0.0650(17) 0.7157(9) 0.021 Uiso 1 1 d . . .
C5 C 0.71347(13) 0.03828(14) 0.77718(8) 0.0189(3) Uani 1 1 d . . .
H5 H 0.7550(16) -0.0416(18) 0.8138(10) 0.023 Uiso 1 1 d . . .
C6 C 0.57504(13) 0.09254(14) 0.78342(8) 0.0176(3) Uani 1 1 d . . .
H6 H 0.5126(16) 0.0510(17) 0.8245(9) 0.021 Uiso 1 1 d . . .
C7 C 0.52829(13) 0.20858(14) 0.73021(8) 0.0170(3) Uani 1 1 d . . .
H7 H 0.4330(16) 0.2520(18) 0.7343(9) 0.020 Uiso 1 1 d . . .
N2 N 0.67687(11) 0.11958(12) 0.50432(6) 0.0175(2) Uani 1 1 d . . .
C8 C 0.79814(12) 0.20172(13) 0.51455(7) 0.0147(2) Uani 1 1 d . . .
C9 C 0.89302(13) 0.21257(15) 0.45107(8) 0.0197(3) Uani 1 1 d . . .
H9 H 0.9773(17) 0.2751(18) 0.4609(9) 0.024 Uiso 1 1 d . . .
C10 C 0.86152(14) 0.13608(15) 0.37557(8) 0.0208(3) Uani 1 1 d . . .
H10 H 0.9276(17) 0.1419(18) 0.3307(10) 0.025 Uiso 1 1 d . . .
C11 C 0.73653(13) 0.05115(14) 0.36435(8) 0.0185(3) Uani 1 1 d . . .
H11 H 0.7108(16) -0.0031(18) 0.3111(10) 0.022 Uiso 1 1 d . . .
C12 C 0.64774(13) 0.04638(14) 0.43038(8) 0.0195(3) Uani 1 1 d . . .
H12 H 0.5564(17) -0.0130(18) 0.4249(9) 0.023 Uiso 1 1 d . . .
N3 N 0.82701(11) 0.53827(12) 0.65439(6) 0.0164(2) Uani 1 1 d . . .
C13 C 0.78128(12) 0.45038(13) 0.58844(7) 0.0144(2) Uani 1 1 d . . .
C14 C 0.69641(13) 0.50350(14) 0.51725(7) 0.0173(3) Uani 1 1 d . . .
H14 H 0.6646(16) 0.4339(17) 0.4714(10) 0.021 Uiso 1 1 d . . .
C15 C 0.65686(13) 0.65251(15) 0.51357(8) 0.0202(3) Uani 1 1 d . . .
H15 H 0.5938(17) 0.6892(18) 0.4644(10) 0.024 Uiso 1 1 d . . .
C16 C 0.70449(13) 0.74442(14) 0.58106(8) 0.0199(3) Uani 1 1 d . . .
H16 H 0.6806(16) 0.8499(19) 0.5816(10) 0.024 Uiso 1 1 d . . .
C17 C 0.78812(13) 0.68184(14) 0.64946(8) 0.0179(3) Uani 1 1 d . . .
H17 H 0.8223(16) 0.7447(18) 0.6978(10) 0.021 Uiso 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 1.5464(15) . ?
C1 H1A 1.003(16) . ?
C1 H1B 0.989(17) . ?
C1 H1C 0.983(17) . ?
C2 C8 1.5364(16) . ?
C2 C3 1.5374(15) . ?
C2 C13 1.5388(16) . ?
N1 C7 1.3409(15) . ?
N1 C3 1.3410(15) . ?
C3 C4 1.3928(17) . ?
C4 C5 1.3893(17) . ?
C4 H4 0.969(15) . ?
C5 C6 1.3818(17) . ?
C5 H5 0.979(16) . ?
C6 C7 1.3840(18) . ?
C6 H6 0.982(15) . ?
C7 H7 0.972(15) . ?
N2 C8 1.3401(15) . ?
N2 C12 1.3447(16) . ?
C8 C9 1.3951(17) . ?
C9 C10 1.3829(18) . ?
C9 H9 0.962(16) . ?
C10 C11 1.3831(18) . ?
C10 H10 0.978(16) . ?
C11 C12 1.3860(17) . ?
C11 H11 0.981(16) . ?
C12 H12 0.996(16) . ?
N3 C17 1.3427(17) . ?
N3 C13 1.3434(15) . ?
C13 C14 1.3926(17) . ?
C14 C15 1.3911(18) . ?
C14 H14 0.982(16) . ?
C15 C16 1.3872(19) . ?
C15 H15 0.982(16) . ?
C16 C17 1.3863(18) . ?
C16 H16 0.976(17) . ?
C17 H17 0.978(16) . ?

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
C2 C1 H1A 109.8(9) . . ?
C2 C1 H1B 110.8(9) . . ?
H1A C1 H1B 107.7(13) . . ?
C2 C1 H1C 111.9(9) . . ?
H1A C1 H1C 109.4(13) . . ?
H1B C1 H1C 107.2(13) . . ?
C8 C2 C3 109.31(9) . . ?
C8 C2 C13 111.15(9) . . ?
C3 C2 C13 108.25(9) . . ?
C8 C2 C1 109.66(9) . . ?
C3 C2 C1 110.66(9) . . ?
C13 C2 C1 107.78(10) . . ?
C7 N1 C3 117.57(10) . . ?
N1 C3 C4 122.21(11) . . ?
N1 C3 C2 116.09(10) . . ?
C4 C3 C2 121.70(10) . . ?
C5 C4 C3 118.95(11) . . ?
C5 C4 H4 119.3(9) . . ?
C3 C4 H4 121.7(9) . . ?
C6 C5 C4 119.42(11) . . ?
C6 C5 H5 122.2(9) . . ?
C4 C5 H5 118.4(9) . . ?
C5 C6 C7 117.54(11) . . ?
C5 C6 H6 121.2(9) . . ?
C7 C6 H6 121.3(9) . . ?
N1 C7 C6 124.31(11) . . ?
N1 C7 H7 115.9(9) . . ?
C6 C7 H7 119.8(9) . . ?
C8 N2 C12 118.17(10) . . ?
N2 C8 C9 121.83(11) . . ?
N2 C8 C2 117.43(10) . . ?
C9 C8 C2 120.72(10) . . ?
C10 C9 C8 119.17(12) . . ?
C10 C9 H9 122.1(9) . . ?
C8 C9 H9 118.7(9) . . ?
C9 C10 C11 119.44(11) . . ?
C9 C10 H10 120.1(9) . . ?
C11 C10 H10 120.5(9) . . ?
C10 C11 C12 117.88(11) . . ?
C10 C11 H11 121.1(9) . . ?
C12 C11 H11 121.0(9) . . ?
N2 C12 C11 123.51(11) . . ?
N2 C12 H12 116.0(9) . . ?
C11 C12 H12 120.5(9) . . ?
C17 N3 C13 117.37(10) . . ?
N3 C13 C14 122.28(11) . . ?
N3 C13 C2 114.66(10) . . ?
C14 C13 C2 123.05(11) . . ?
C15 C14 C13 119.42(12) . . ?
C15 C14 H14 121.7(9) . . ?
C13 C14 H14 118.8(9) . . ?
C16 C15 C14 118.73(12) . . ?
C16 C15 H15 121.8(9) . . ?
C14 C15 H15 119.5(9) . . ?
C17 C16 C15 117.90(12) . . ?
C17 C16 H16 120.0(9) . . ?
C15 C16 H16 122.1(9) . . ?
N3 C17 C16 124.29(12) . . ?
N3 C17 H17 116.6(9) . . ?
C16 C17 H17 119.2(9) . . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        73.87
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.040
_database_code_depnum_ccdc_archive 'CCDC 1023797'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_as142217

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis[1,1,1-tris(pyrid-2-yl)ethane]iron(II) diperchlorate 
tetrakis-acetonitrile solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H30 Fe N10, 2[Cl O4], 4[C2 H3 N]'
_chemical_formula_sum            'C42 H42 Cl2 Fe N10 O8'
_chemical_formula_weight         941.61

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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   12.0918(10)
_cell_length_b                   12.7748(8)
_cell_length_c                   14.8314(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.518(9)
_cell_angle_gamma                90.00
_cell_volume                     2116.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3789
_cell_measurement_theta_min      1.86
_cell_measurement_theta_max      29.34

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11384
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         29.69
_reflns_number_total             5065
_reflns_number_gt                3894
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains half a formula unit, with Fe1 lying on the 
 inversion centre 0, 1/2, 1/2. The unique perchlorate ion is 
 crystallographically ordered, but one of the two unique acetonitrile sites 
 was modelled over two disorder sites with a 0.75:0.25 ratio, which share 
 a common wholly occupied nitrile C atom. The fixed restraints C---C = 
 1.43(2), C---N = 1.16(2) and 1,3-C...N = 2.59(2) Å were applied to that 
 residue.

 All fully occupied non-H atoms were refined anisotropically, while H 
 atoms were placed in calculated positions and refined using a riding 
 model. The highest residual Fourier peak of +1.1 e.Å⁻³ is associated 
 with the ordered solvent site, and may be evidence for a small degree of
 disorder in that residue as well.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0598P)²+2.8686P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5065
_refine_ls_number_parameters     301
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1532
_refine_ls_wR_factor_gt          0.1364
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.5000 0.5000 0.01420(16) Uani 1 2 d S . .
C1 C 0.2830(3) 0.3714(3) 0.7835(2) 0.0258(7) Uani 1 1 d . . .
H1A H 0.3118 0.4278 0.8318 0.039 Uiso 1 1 calc R . .
H1B H 0.3501 0.3430 0.7697 0.039 Uiso 1 1 calc R . .
H1C H 0.2476 0.3158 0.8094 0.039 Uiso 1 1 calc R . .
C2 C 0.1878(2) 0.4149(2) 0.68888(19) 0.0187(6) Uani 1 1 d . . .
N1 N -0.0125(2) 0.49342(18) 0.62851(16) 0.0174(5) Uani 1 1 d . . .
C3 C 0.0794(3) 0.4561(2) 0.70724(19) 0.0203(6) Uani 1 1 d . . .
C4 C 0.0750(3) 0.4569(3) 0.7997(2) 0.0282(7) Uani 1 1 d . . .
H4 H 0.1403 0.4303 0.8541 0.034 Uiso 1 1 calc R . .
C5 C -0.0238(3) 0.4961(3) 0.8121(2) 0.0360(8) Uani 1 1 d . . .
H5 H -0.0268 0.4984 0.8751 0.043 Uiso 1 1 calc R . .
C6 C -0.1196(3) 0.5326(3) 0.7311(2) 0.0315(7) Uani 1 1 d . . .
H6 H -0.195(3) 0.566(3) 0.732(3) 0.038 Uiso 1 1 d . . .
C7 C -0.1106(3) 0.5295(2) 0.6411(2) 0.0224(6) Uani 1 1 d . . .
H7 H -0.1762 0.5538 0.5857 0.027 Uiso 1 1 calc R . .
N2 N 0.0647(2) 0.35641(17) 0.52226(15) 0.0157(5) Uani 1 1 d . . .
C8 C 0.1465(3) 0.3286(2) 0.6108(2) 0.0188(6) Uani 1 1 d . . .
C9 C 0.1911(3) 0.2271(2) 0.6280(2) 0.0278(7) Uani 1 1 d . . .
H9 H 0.245(3) 0.204(3) 0.688(3) 0.033 Uiso 1 1 d . . .
C10 C 0.1532(3) 0.1541(2) 0.5540(2) 0.0306(7) Uani 1 1 d . . .
H10 H 0.180(3) 0.085(3) 0.567(3) 0.037 Uiso 1 1 d . . .
C11 C 0.0716(3) 0.1826(2) 0.4631(2) 0.0248(6) Uani 1 1 d . . .
H11 H 0.0454 0.1339 0.4107 0.030 Uiso 1 1 calc R . .
C12 C 0.0294(2) 0.2837(2) 0.4508(2) 0.0188(6) Uani 1 1 d . . .
H12 H -0.0278 0.3035 0.3886 0.023 Uiso 1 1 calc R . .
N3 N 0.1654(2) 0.55207(18) 0.56682(16) 0.0161(5) Uani 1 1 d . . .
C13 C 0.2406(3) 0.5054(2) 0.64992(19) 0.0170(6) Uani 1 1 d . . .
C14 C 0.3583(3) 0.5394(2) 0.6962(2) 0.0228(6) Uani 1 1 d . . .
H14 H 0.4100 0.5061 0.7544 0.027 Uiso 1 1 calc R . .
C15 C 0.4001(3) 0.6218(3) 0.6574(2) 0.0254(7) Uani 1 1 d . . .
H15 H 0.4806 0.6449 0.6881 0.031 Uiso 1 1 calc R . .
C16 C 0.3231(3) 0.6698(2) 0.5735(2) 0.0222(6) Uani 1 1 d . . .
H16 H 0.348(3) 0.729(3) 0.547(2) 0.027 Uiso 1 1 d . . .
C17 C 0.2070(2) 0.6332(2) 0.5306(2) 0.0178(6) Uani 1 1 d . . .
H17 H 0.1542 0.6666 0.4730 0.021 Uiso 1 1 calc R . .
Cl1 Cl 0.19849(6) 0.89941(6) 0.40465(5) 0.02182(18) Uani 1 1 d . . .
O1 O 0.1502(2) 0.98752(18) 0.34119(17) 0.0346(6) Uani 1 1 d . . .
O2 O 0.1597(3) 0.9004(2) 0.48410(18) 0.0429(7) Uani 1 1 d . . .
O3 O 0.3270(2) 0.9045(2) 0.4446(2) 0.0533(8) Uani 1 1 d . . .
O4 O 0.1604(3) 0.8042(2) 0.35075(18) 0.0511(8) Uani 1 1 d . . .
C19 C 0.6260(4) 0.7158(5) 0.5501(4) 0.0712(15) Uani 1 1 d D . .
C18A C 0.6172(7) 0.8310(5) 0.5303(5) 0.0707(19) Uiso 0.75 1 d PD A 1
H18A H 0.6269 0.8447 0.4687 0.106 Uiso 0.75 1 calc PR A 1
H18B H 0.6803 0.8674 0.5836 0.106 Uiso 0.75 1 calc PR A 1
H18C H 0.5388 0.8564 0.5257 0.106 Uiso 0.75 1 calc PR A 1
N4A N 0.6265(7) 0.6274(5) 0.5595(6) 0.0809(19) Uiso 0.75 1 d PD A 1
C18B C 0.659(2) 0.7985(17) 0.6150(18) 0.098(8) Uiso 0.25 1 d PD A 2
H18D H 0.5866 0.8309 0.6180 0.148 Uiso 0.25 1 calc PR A 2
H18E H 0.7027 0.8504 0.5932 0.148 Uiso 0.25 1 calc PR A 2
H18F H 0.7096 0.7727 0.6799 0.148 Uiso 0.25 1 calc PR A 2
N4B N 0.6218(17) 0.6286(12) 0.5084(14) 0.068(5) Uiso 0.25 1 d PD A 2
C20 C 0.1250(5) 1.1284(4) 0.1545(4) 0.0681(14) Uani 1 1 d . . .
H20A H 0.1638 1.0738 0.2026 0.102 Uiso 1 1 calc R . .
H20B H 0.1863 1.1724 0.1453 0.102 Uiso 1 1 calc R . .
H20C H 0.0755 1.0959 0.0922 0.102 Uiso 1 1 calc R . .
C21 C 0.0519(4) 1.1910(4) 0.1883(3) 0.0536(11) Uani 1 1 d . . .
N5 N -0.0105(4) 1.2405(3) 0.2131(3) 0.0591(10) 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
Fe1 N1 1.971(2) . ?
Fe1 N2 1.972(2) . ?
Fe1 N3 1.976(2) . ?
C1 C2 1.538(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.531(4) . ?
C2 C13 1.535(4) . ?
C2 C8 1.538(4) . ?
N1 C7 1.350(4) . ?
N1 C3 1.354(4) . ?
C3 C4 1.393(4) . ?
C4 C5 1.371(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.380(4) . ?
C6 H6 1.01(4) . ?
C7 H7 0.9500 . ?
N2 C12 1.350(4) . ?
N2 C8 1.354(3) . ?
C8 C9 1.390(4) . ?
C9 C10 1.378(5) . ?
C9 H9 0.93(4) . ?
C10 C11 1.380(4) . ?
C10 H10 0.93(4) . ?
C11 C12 1.375(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N3 C17 1.350(4) . ?
N3 C13 1.358(3) . ?
C13 C14 1.393(4) . ?
C14 C15 1.384(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.380(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(4) . ?
C16 H16 0.95(3) . ?
C17 H17 0.9500 . ?
Cl1 O2 1.426(2) . ?
Cl1 O4 1.431(3) . ?
Cl1 O3 1.437(3) . ?
Cl1 O1 1.440(2) . ?
C19 N4A 1.139(8) . ?
C19 N4B 1.266(13) . ?
C19 C18B 1.380(14) . ?
C19 C18A 1.496(8) . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
C18B H18D 0.9800 . ?
C18B H18E 0.9800 . ?
C18B H18F 0.9800 . ?
C20 C21 1.419(7) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 N5 1.147(6) . ?

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 Fe1 N1 180.00 3_566 . ?
N1 Fe1 N2 91.66(9) . 3_566 ?
N1 Fe1 N2 88.34(9) . . ?
N2 Fe1 N2 180.00 3_566 . ?
N1 Fe1 N3 91.88(9) . 3_566 ?
N2 Fe1 N3 91.80(9) . 3_566 ?
N1 Fe1 N3 88.12(9) . . ?
N2 Fe1 N3 88.20(9) . . ?
N3 Fe1 N3 180.00 3_566 . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C13 108.4(2) . . ?
C3 C2 C1 110.7(2) . . ?
C13 C2 C1 110.0(2) . . ?
C3 C2 C8 109.1(2) . . ?
C13 C2 C8 108.6(2) . . ?
C1 C2 C8 110.0(2) . . ?
C7 N1 C3 118.4(2) . . ?
C7 N1 Fe1 121.10(19) . . ?
C3 N1 Fe1 120.5(2) . . ?
N1 C3 C4 121.2(3) . . ?
N1 C3 C2 116.4(2) . . ?
C4 C3 C2 122.4(3) . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 119.1(3) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C7 C6 C5 118.5(3) . . ?
C7 C6 H6 115(2) . . ?
C5 C6 H6 126(2) . . ?
N1 C7 C6 122.8(3) . . ?
N1 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
C12 N2 C8 118.4(2) . . ?
C12 N2 Fe1 121.49(18) . . ?
C8 N2 Fe1 120.16(18) . . ?
N2 C8 C9 120.8(3) . . ?
N2 C8 C2 116.6(2) . . ?
C9 C8 C2 122.6(2) . . ?
C10 C9 C8 119.8(3) . . ?
C10 C9 H9 117(2) . . ?
C8 C9 H9 124(2) . . ?
C9 C10 C11 119.7(3) . . ?
C9 C10 H10 119(2) . . ?
C11 C10 H10 121(2) . . ?
C12 C11 C10 117.9(3) . . ?
C12 C11 H11 121.1 . . ?
C10 C11 H11 121.1 . . ?
N2 C12 C11 123.5(3) . . ?
N2 C12 H12 118.3 . . ?
C11 C12 H12 118.3 . . ?
C17 N3 C13 118.4(2) . . ?
C17 N3 Fe1 121.27(18) . . ?
C13 N3 Fe1 120.31(19) . . ?
N3 C13 C14 120.9(3) . . ?
N3 C13 C2 116.2(2) . . ?
C14 C13 C2 122.9(2) . . ?
C15 C14 C13 120.0(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 C14 119.0(3) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C17 118.7(3) . . ?
C15 C16 H16 121(2) . . ?
C17 C16 H16 121(2) . . ?
N3 C17 C16 123.0(3) . . ?
N3 C17 H17 118.5 . . ?
C16 C17 H17 118.5 . . ?
O2 Cl1 O4 109.37(17) . . ?
O2 Cl1 O3 107.75(17) . . ?
O4 Cl1 O3 109.59(19) . . ?
O2 Cl1 O1 110.71(16) . . ?
O4 Cl1 O1 109.63(15) . . ?
O3 Cl1 O1 109.76(15) . . ?
N4B C19 C18B 163.9(16) . . ?
N4A C19 C18A 175.5(7) . . ?
C19 C18A H18A 109.5 . . ?
C19 C18A H18B 109.5 . . ?
C19 C18A H18C 109.5 . . ?
C19 C18B H18D 109.5 . . ?
C19 C18B H18E 109.5 . . ?
H18D C18B H18E 109.5 . . ?
C19 C18B H18F 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N5 C21 C20 177.7(6) . . ?

_diffrn_measured_fraction_theta_max 0.843
_diffrn_reflns_theta_full        29.69
_diffrn_measured_fraction_theta_full 0.843
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.091
_database_code_depnum_ccdc_archive 'CCDC 1023798'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_exp_830

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis[1,1,1-tris(pyrid-2-yl)ethane]cobalt(II) diperchlorate 
tetrakis-acetonitrile solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H30 Co N10, 2[Cl O4], 4[C2 H3 N]'
_chemical_formula_sum            'C42 H42 Cl2 Co N10 O8'
_chemical_formula_weight         944.69

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   12.3122(5)
_cell_length_b                   12.7314(4)
_cell_length_c                   14.6894(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.295(5)
_cell_angle_gamma                90.00
_cell_volume                     2130.45(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3808
_cell_measurement_theta_min      3.54
_cell_measurement_theta_max      27.27

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             978
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            10280
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         25.03
_reflns_number_total             3757
_reflns_number_gt                3032
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains half a formula unit, with Co1 lying on the 
 inversion centre 0, 1/2, 1/2. Bo disorder is present in the refinement, 
 and no restraints were applied. All non-H atoms were refined anisotropically, 
 while H atoms were placed in calculated positions and refined using a riding 
 model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0455P)²+1.9588P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3757
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1150
_refine_ls_wR_factor_gt          0.1044
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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 0.0000 0.5000 0.5000 0.01381(16) Uani 1 2 d S . .
C1 C 0.2895(3) 0.6282(2) 0.7841(2) 0.0219(7) Uani 1 1 d . . .
H1A H 0.3146 0.5735 0.8348 0.033 Uiso 1 1 calc R . .
H1B H 0.2558 0.6873 0.8073 0.033 Uiso 1 1 calc R . .
H1C H 0.3573 0.6526 0.7704 0.033 Uiso 1 1 calc R . .
C2 C 0.1969(2) 0.5832(2) 0.6899(2) 0.0175(6) Uani 1 1 d . . .
N1 N 0.0690(2) 0.64230(17) 0.52220(17) 0.0169(5) Uani 1 1 d . . .
C3 C 0.1550(2) 0.6685(2) 0.6090(2) 0.0170(6) Uani 1 1 d . . .
N4 N 0.9999(3) 0.2374(3) 0.7857(3) 0.0510(9) Uani 1 1 d . . .
C4 C 0.2043(3) 0.7684(2) 0.6235(2) 0.0254(7) Uani 1 1 d . . .
H4 H 0.2647 0.7860 0.6846 0.030 Uiso 1 1 calc R . .
N5 N 0.6439(3) 0.3819(3) 0.5342(3) 0.0685(12) Uani 1 1 d . . .
C5 C 0.1654(3) 0.8420(2) 0.5489(2) 0.0282(7) Uani 1 1 d . . .
H5 H 0.1987 0.9104 0.5582 0.034 Uiso 1 1 calc R . .
C6 C 0.0782(3) 0.8150(2) 0.4612(2) 0.0227(7) Uani 1 1 d . . .
H6 H 0.0497 0.8644 0.4089 0.027 Uiso 1 1 calc R . .
C7 C 0.0327(3) 0.7150(2) 0.4505(2) 0.0196(6) Uani 1 1 d . . .
H7 H -0.0273 0.6964 0.3895 0.024 Uiso 1 1 calc R . .
N2 N -0.0048(2) 0.50981(17) 0.63248(18) 0.0170(5) Uani 1 1 d . . .
C8 C 0.0902(3) 0.5432(2) 0.7105(2) 0.0186(6) Uani 1 1 d . . .
C9 C 0.0905(3) 0.5398(2) 0.8053(2) 0.0243(7) Uani 1 1 d . . .
H9 H 0.1572 0.5637 0.8594 0.029 Uiso 1 1 calc R . .
C10 C -0.0059(3) 0.5018(2) 0.8207(2) 0.0273(7) Uani 1 1 d . . .
H10 H -0.0053 0.4968 0.8854 0.033 Uiso 1 1 calc R . .
C11 C -0.1038(3) 0.4709(2) 0.7403(2) 0.0278(7) Uani 1 1 d . . .
H11 H -0.1723 0.4465 0.7487 0.033 Uiso 1 1 calc R . .
C12 C -0.0997(3) 0.4763(2) 0.6481(2) 0.0209(7) Uani 1 1 d . . .
H12 H -0.1670 0.4554 0.5930 0.025 Uiso 1 1 calc R . .
N3 N 0.1766(2) 0.44170(17) 0.57126(17) 0.0167(5) Uani 1 1 d . . .
C13 C 0.2498(2) 0.4905(2) 0.6525(2) 0.0162(6) Uani 1 1 d . . .
C14 C 0.3659(3) 0.4583(2) 0.6990(2) 0.0208(7) Uani 1 1 d . . .
H14 H 0.4169 0.4938 0.7561 0.025 Uiso 1 1 calc R . .
C15 C 0.4065(3) 0.3741(2) 0.6614(2) 0.0247(7) Uani 1 1 d . . .
H15 H 0.4855 0.3514 0.6923 0.030 Uiso 1 1 calc R . .
C16 C 0.3310(3) 0.3235(2) 0.5786(2) 0.0223(7) Uani 1 1 d . . .
H16 H 0.3568 0.2651 0.5518 0.027 Uiso 1 1 calc R . .
C17 C 0.2167(2) 0.3597(2) 0.5353(2) 0.0174(6) Uani 1 1 d . . .
H17 H 0.1646 0.3254 0.4779 0.021 Uiso 1 1 calc R . .
Cl1 Cl 0.79315(6) 0.90216(5) 0.59735(5) 0.02107(19) Uani 1 1 d . . .
O1 O 0.8420(2) 0.99159(16) 0.65956(17) 0.0318(6) Uani 1 1 d . . .
O2 O 0.8219(2) 0.80832(17) 0.65539(17) 0.0399(6) Uani 1 1 d . . .
O3 O 0.66726(19) 0.91274(19) 0.55248(18) 0.0390(6) Uani 1 1 d . . .
O4 O 0.8393(2) 0.89649(17) 0.52146(17) 0.0325(6) Uani 1 1 d . . .
C18 C 0.8796(4) 0.1201(3) 0.8555(3) 0.0472(10) Uani 1 1 d . . .
H18A H 0.8502 0.0590 0.8126 0.071 Uiso 1 1 calc R . .
H18B H 0.8133 0.1598 0.8593 0.071 Uiso 1 1 calc R . .
H18C H 0.9303 0.0965 0.9215 0.071 Uiso 1 1 calc R . .
C19 C 0.9450(3) 0.1854(3) 0.8166(3) 0.0397(9) Uani 1 1 d . . .
C20 C 0.6313(5) 0.1921(4) 0.5889(5) 0.094(2) Uani 1 1 d . . .
H20A H 0.5647 0.1576 0.5379 0.142 Uiso 1 1 calc R . .
H20B H 0.6192 0.1923 0.6511 0.142 Uiso 1 1 calc R . .
H20C H 0.7037 0.1540 0.5975 0.142 Uiso 1 1 calc R . .
C21 C 0.6407(3) 0.2986(4) 0.5597(3) 0.0487(10) 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
Co1 N2 1.973(2) . ?
Co1 N1 1.975(2) . ?
Co1 N3 2.155(2) . ?
C1 C2 1.532(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C8 1.542(4) . ?
C2 C13 1.546(4) . ?
C2 C3 1.547(4) . ?
N1 C7 1.345(4) . ?
N1 C3 1.355(4) . ?
C3 C4 1.389(4) . ?
N4 C19 1.154(5) . ?
C4 C5 1.382(4) . ?
C4 H4 0.9500 . ?
N5 C21 1.131(5) . ?
C5 C6 1.371(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.375(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
N2 C12 1.343(4) . ?
N2 C8 1.359(4) . ?
C8 C9 1.392(4) . ?
C9 C10 1.378(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N3 C13 1.344(4) . ?
N3 C17 1.346(4) . ?
C13 C14 1.392(4) . ?
C14 C15 1.383(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(4) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
Cl1 O2 1.432(2) . ?
Cl1 O4 1.433(2) . ?
Cl1 O1 1.441(2) . ?
Cl1 O3 1.442(2) . ?
C18 C19 1.419(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C20 C21 1.439(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 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
N2 Co1 N2 180.00 . 3_566 ?
N2 Co1 N1 87.20(9) . . ?
N2 Co1 N1 92.80(9) . 3_566 ?
N1 Co1 N1 180.00 . 3_566 ?
N2 Co1 N3 93.16(9) . 3_566 ?
N1 Co1 N3 93.20(9) . 3_566 ?
N2 Co1 N3 86.84(9) . . ?
N1 Co1 N3 86.80(9) . . ?
N3 Co1 N3 180.00 3_566 . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 C8 110.1(2) . . ?
C1 C2 C13 109.7(2) . . ?
C8 C2 C13 108.8(2) . . ?
C1 C2 C3 110.4(2) . . ?
C8 C2 C3 108.8(2) . . ?
C13 C2 C3 109.0(2) . . ?
C7 N1 C3 118.4(2) . . ?
C7 N1 Co1 120.54(19) . . ?
C3 N1 Co1 121.02(19) . . ?
N1 C3 C4 120.6(3) . . ?
N1 C3 C2 117.6(2) . . ?
C4 C3 C2 121.7(3) . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 119.2(3) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C7 118.6(3) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
N1 C7 C6 123.2(3) . . ?
N1 C7 H7 118.4 . . ?
C6 C7 H7 118.4 . . ?
C12 N2 C8 118.8(2) . . ?
C12 N2 Co1 120.1(2) . . ?
C8 N2 Co1 120.90(19) . . ?
N2 C8 C9 120.6(3) . . ?
N2 C8 C2 117.5(2) . . ?
C9 C8 C2 121.9(3) . . ?
C10 C9 C8 120.0(3) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C11 119.0(3) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C12 C11 C10 118.6(3) . . ?
C12 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
N2 C12 C11 122.9(3) . . ?
N2 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C13 N3 C17 119.0(2) . . ?
C13 N3 Co1 119.00(18) . . ?
C17 N3 Co1 121.95(19) . . ?
N3 C13 C14 121.1(3) . . ?
N3 C13 C2 115.9(2) . . ?
C14 C13 C2 122.9(3) . . ?
C15 C14 C13 119.5(3) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C16 C15 C14 119.4(3) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 118.5(3) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
N3 C17 C16 122.6(3) . . ?
N3 C17 H17 118.7 . . ?
C16 C17 H17 118.7 . . ?
O2 Cl1 O4 109.87(14) . . ?
O2 Cl1 O1 109.41(14) . . ?
O4 Cl1 O1 109.87(14) . . ?
O2 Cl1 O3 109.27(15) . . ?
O4 Cl1 O3 108.91(14) . . ?
O1 Cl1 O3 109.50(14) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 C18 178.8(4) . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N5 C21 C20 177.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.071
_database_code_depnum_ccdc_archive 'CCDC 1023799'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_as145259

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis[1,1,1-tris(pyrid-2-yl)ethane]cobalt(III) triperchlorate 
tetrakis-acetonitrile solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H30 Co N10, 2[Cl O4], 4[C2 H3 N]'
_chemical_formula_sum            'C42 H42 Cl3 Co N10 O12'
_chemical_formula_weight         1044.14

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   10.9979(2)
_cell_length_b                   10.8330(2)
_cell_length_c                   19.3354(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.3450(10)
_cell_angle_gamma                90.00
_cell_volume                     2301.70(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4954
_cell_measurement_theta_min      4.58
_cell_measurement_theta_max      73.26

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1076
_exptl_absorpt_coefficient_mu    5.153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8737
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.55
_diffrn_reflns_theta_max         73.38
_reflns_number_total             4491
_reflns_number_gt                4145
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains half a formula unit, with Co1 lying on the 
 inversion centre 0, 1/2, 1/2 and the half-anion centred on Cl2 spanning 
 the inversion centre 0, 1, 1/2. No disorder is present in the refinement, 
 but the following refined restraint had to be applied to the half-anion 
 to prevent Cl2 migrating to the special position: Cl---O = 1.44(2) Å. 
 All non-H atoms were refined anisotropically, while H atoms were placed in 
 calculated positions and refined using a riding model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0381P)²+1.2704P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4491
_refine_ls_number_parameters     332
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0791
_refine_ls_wR_factor_gt          0.0770
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.033
_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
Co1 Co 0.0000 0.5000 0.5000 0.00789(9) Uani 1 2 d S . .
C1 C 0.34800(14) 0.71294(16) 0.55793(9) 0.0166(3) Uani 1 1 d . . .
H1A H 0.3768 0.6898 0.6048 0.025 Uiso 1 1 calc R . .
H1B H 0.3311 0.8018 0.5564 0.025 Uiso 1 1 calc R . .
H1C H 0.4107 0.6930 0.5251 0.025 Uiso 1 1 calc R . .
C2 C 0.23135(14) 0.64144(15) 0.53845(8) 0.0120(3) Uani 1 1 d . . .
N1 N 0.02392(11) 0.61221(12) 0.57837(6) 0.0105(3) Uani 1 1 d . . .
C3 C 0.13209(14) 0.66948(14) 0.58948(8) 0.0114(3) Uani 1 1 d . . .
C4 C 0.15064(15) 0.74804(15) 0.64566(9) 0.0163(3) Uani 1 1 d . . .
H4 H 0.2268 0.7882 0.6530 0.020 Uiso 1 1 calc R . .
C5 C 0.05857(16) 0.76793(16) 0.69088(9) 0.0189(3) Uani 1 1 d . . .
H5 H 0.0709 0.8215 0.7294 0.023 Uiso 1 1 calc R . .
C6 C -0.05217(15) 0.70853(16) 0.67916(9) 0.0167(3) Uani 1 1 d . . .
H6 H -0.1169 0.7205 0.7095 0.020 Uiso 1 1 calc R . .
C7 C -0.06608(14) 0.63174(15) 0.62246(8) 0.0134(3) Uani 1 1 d . . .
H7 H -0.1418 0.5911 0.6142 0.016 Uiso 1 1 calc R . .
N2 N 0.15905(11) 0.42826(12) 0.52289(7) 0.0107(3) Uani 1 1 d . . .
C8 C 0.25449(15) 0.50172(14) 0.54042(8) 0.0115(3) Uani 1 1 d . . .
C9 C 0.36638(14) 0.45146(16) 0.56038(8) 0.0150(3) Uani 1 1 d . . .
H9 H 0.4330 0.5039 0.5728 0.018 Uiso 1 1 calc R . .
C10 C 0.38080(15) 0.32431(17) 0.56217(8) 0.0168(3) Uani 1 1 d . . .
H10 H 0.4564 0.2888 0.5771 0.020 Uiso 1 1 calc R . .
C11 C 0.28378(15) 0.25012(15) 0.54197(9) 0.0160(3) Uani 1 1 d . . .
H11 H 0.2924 0.1629 0.5413 0.019 Uiso 1 1 calc R . .
C12 C 0.17430(14) 0.30442(15) 0.52282(8) 0.0135(3) Uani 1 1 d . . .
H12 H 0.1074 0.2533 0.5091 0.016 Uiso 1 1 calc R . .
N3 N 0.07962(11) 0.61995(12) 0.44221(7) 0.0107(3) Uani 1 1 d . . .
C13 C 0.18337(14) 0.67567(14) 0.46529(8) 0.0116(3) Uani 1 1 d . . .
C14 C 0.24278(15) 0.75870(15) 0.42353(9) 0.0161(3) Uani 1 1 d . . .
H14 H 0.3156 0.7978 0.4401 0.019 Uiso 1 1 calc R . .
C15 C 0.19538(16) 0.78420(16) 0.35768(9) 0.0193(3) Uani 1 1 d . . .
H15 H 0.2358 0.8402 0.3286 0.023 Uiso 1 1 calc R . .
C16 C 0.08864(16) 0.72737(16) 0.33471(9) 0.0189(3) Uani 1 1 d . . .
H16 H 0.0544 0.7438 0.2897 0.023 Uiso 1 1 calc R . .
C17 C 0.03288(14) 0.64651(15) 0.37824(8) 0.0140(3) Uani 1 1 d . . .
H17 H -0.0410 0.6081 0.3628 0.017 Uiso 1 1 calc R . .
Cl1 Cl 0.37834(3) 0.48565(4) 0.319743(19) 0.01470(10) Uani 1 1 d . . .
O1 O 0.41711(13) 0.61118(13) 0.31230(7) 0.0281(3) Uani 1 1 d . . .
O2 O 0.47437(13) 0.40421(14) 0.30016(7) 0.0323(3) Uani 1 1 d . . .
O3 O 0.27023(12) 0.46341(15) 0.27683(7) 0.0276(3) Uani 1 1 d . . .
O4 O 0.35203(11) 0.46313(13) 0.39136(6) 0.0227(3) Uani 1 1 d . . .
Cl2 Cl 0.0000 1.0000 0.5000 0.02127(14) Uani 1 2 d SD . .
O5 O -0.0121(3) 0.9220(3) 0.43893(14) 0.0269(6) Uani 0.50 1 d PD . .
O6 O 0.1365(3) 0.9990(3) 0.51863(19) 0.0363(8) Uani 0.50 1 d PD . .
O7 O -0.0529(3) 0.9323(3) 0.55675(15) 0.0377(7) Uani 0.50 1 d PD . .
O8 O -0.0401(2) 1.1146(2) 0.49104(16) 0.0289(6) Uani 0.50 1 d PD . .
C18 C 0.2900(2) 0.5956(2) 0.80356(12) 0.0388(5) Uani 1 1 d . . .
H18A H 0.2242 0.6311 0.8299 0.058 Uiso 1 1 calc R . .
H18B H 0.3292 0.6611 0.7775 0.058 Uiso 1 1 calc R . .
H18C H 0.3501 0.5569 0.8355 0.058 Uiso 1 1 calc R . .
C19 C 0.24046(19) 0.50393(17) 0.75610(11) 0.0282(5) Uani 1 1 d . . .
N4 N 0.2038(2) 0.43127(19) 0.71863(12) 0.0497(6) Uani 1 1 d . . .
C20 C 0.6686(2) 0.8821(2) 0.63382(12) 0.0374(5) Uani 1 1 d . . .
H20A H 0.7379 0.9015 0.6054 0.056 Uiso 1 1 calc R . .
H20B H 0.6427 0.7967 0.6251 0.056 Uiso 1 1 calc R . .
H20C H 0.6928 0.8918 0.6829 0.056 Uiso 1 1 calc R . .
C21 C 0.5687(2) 0.9652(2) 0.61617(13) 0.0374(5) Uani 1 1 d . . .
N5 N 0.4914(2) 1.0308(2) 0.60226(18) 0.0683(8) 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
Co1 N3 1.9452(13) . ?
Co1 N2 1.9484(13) . ?
Co1 N1 1.9519(13) . ?
C1 C2 1.532(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.532(2) . ?
C2 C13 1.535(2) . ?
C2 C8 1.535(2) . ?
N1 C7 1.349(2) . ?
N1 C3 1.351(2) . ?
C3 C4 1.388(2) . ?
C4 C5 1.382(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.380(2) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
N2 C8 1.349(2) . ?
N2 C12 1.352(2) . ?
C8 C9 1.386(2) . ?
C9 C10 1.387(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(2) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N3 C13 1.350(2) . ?
N3 C17 1.351(2) . ?
C13 C14 1.390(2) . ?
C14 C15 1.384(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(2) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
Cl1 O1 1.4341(14) . ?
Cl1 O2 1.4386(14) . ?
Cl1 O3 1.4421(12) . ?
Cl1 O4 1.4470(12) . ?
Cl2 O8 1.327(3) . ?
Cl2 O5 1.454(3) . ?
Cl2 O7 1.460(3) . ?
Cl2 O6 1.529(3) . ?
C18 C19 1.444(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N4 1.133(3) . ?
C20 C21 1.451(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 N5 1.131(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Co1 N3 180.00 . 3_566 ?
N3 Co1 N2 88.62(5) . . ?
N3 Co1 N2 91.38(5) 3_566 . ?
N2 Co1 N2 180.00 . 3_566 ?
N3 Co1 N1 88.87(5) . . ?
N2 Co1 N1 88.90(5) . . ?
N3 Co1 N1 91.13(5) . 3_566 ?
N2 Co1 N1 91.10(5) . 3_566 ?
N1 Co1 N1 180.0 . 3_566 ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 110.68(13) . . ?
C3 C2 C13 108.57(12) . . ?
C1 C2 C13 110.93(13) . . ?
C3 C2 C8 107.54(13) . . ?
C1 C2 C8 110.86(13) . . ?
C13 C2 C8 108.15(13) . . ?
C7 N1 C3 119.44(13) . . ?
C7 N1 Co1 120.60(10) . . ?
C3 N1 Co1 119.95(10) . . ?
N1 C3 C4 120.40(14) . . ?
N1 C3 C2 116.92(13) . . ?
C4 C3 C2 122.67(14) . . ?
C5 C4 C3 120.18(15) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 119.03(16) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C7 C6 C5 118.51(15) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
N1 C7 C6 122.43(15) . . ?
N1 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
C8 N2 C12 119.35(13) . . ?
C8 N2 Co1 120.25(11) . . ?
C12 N2 Co1 120.38(11) . . ?
N2 C8 C9 120.73(14) . . ?
N2 C8 C2 116.67(14) . . ?
C9 C8 C2 122.59(14) . . ?
C8 C9 C10 119.76(15) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 119.04(15) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C12 C11 C10 119.01(15) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
N2 C12 C11 122.05(15) . . ?
N2 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C13 N3 C17 119.47(14) . . ?
C13 N3 Co1 120.19(10) . . ?
C17 N3 Co1 120.32(11) . . ?
N3 C13 C14 120.55(14) . . ?
N3 C13 C2 116.78(13) . . ?
C14 C13 C2 122.67(14) . . ?
C15 C14 C13 119.70(15) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C14 119.31(16) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C17 C16 C15 118.73(16) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
N3 C17 C16 122.22(15) . . ?
N3 C17 H17 118.9 . . ?
C16 C17 H17 118.9 . . ?
O1 Cl1 O2 109.31(9) . . ?
O1 Cl1 O3 110.01(9) . . ?
O2 Cl1 O3 110.06(8) . . ?
O1 Cl1 O4 109.14(8) . . ?
O2 Cl1 O4 109.04(9) . . ?
O3 Cl1 O4 109.27(8) . . ?
O8 Cl2 O5 114.78(17) . . ?
O8 Cl2 O7 115.30(18) . . ?
O5 Cl2 O7 106.99(16) . . ?
O8 Cl2 O6 110.83(16) . . ?
O5 Cl2 O6 104.09(17) . . ?
O7 Cl2 O6 103.71(19) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 C18 178.7(3) . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N5 C21 C20 179.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        73.38
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.053
_database_code_depnum_ccdc_archive 'CCDC 1023800'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_as19320x

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis[1,1,1-tri(pyrid-2-yl)ethane]cobalt(III) triperchlorate hydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H30 Co N6, 3[Cl O4], H2 O'
_chemical_formula_sum            'C34 H32 Cl3 Co N6 O13'
_chemical_formula_weight         897.94

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'
Cl Cl 0.1484 0.1585 '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'
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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   17.1489(4)
_cell_length_b                   13.8420(3)
_cell_length_c                   15.2436(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.216(2)
_cell_angle_gamma                90.00
_cell_volume                     3603.47(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11887
_cell_measurement_theta_min      3.48
_cell_measurement_theta_max      29.15

_exptl_crystal_description       lath
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1840
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35673
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         29.82
_reflns_number_total             9142
_reflns_number_gt                7465
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains two half-complex trications, with Co1 and Co2 
 lying on the crystallographic inversion centres 1, 1, 1 and 0.5, 1, 0.5; 
 three perchlorate anions, one of which is disordered; and one water molecule.
 The disordered anion was modelled without restraints, over two equally 
 occupied sites. All wholly occupied non-H atoms, plus the two disordered Cl 
 atoms, were refined anisotropically and C-bound H atoms were placed in 
 calculated positions and refined using a riding model. The water H atoms 
 were located in the Fourier map and allowed to refine, with Uiso fixed 
 at 1.5x that for the O atom O13.

 The highest residual Fourier peak and hole of +2.2 and -1.5 e.Å^-3 are both 
 associated with the disordered anion.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0603P)²+9.1550P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9142
_refine_ls_number_parameters     531
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1461
_refine_ls_wR_factor_gt          0.1347
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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
Co1 Co 1.0000 1.0000 1.0000 0.00996(12) Uani 1 2 d S . .
C1 C 0.77575(17) 0.8300(2) 0.9265(2) 0.0199(6) Uani 1 1 d . . .
H1A H 0.7752 0.7721 0.9634 0.030 Uiso 1 1 calc R . .
H1B H 0.7734 0.8110 0.8644 0.030 Uiso 1 1 calc R . .
H1C H 0.7304 0.8704 0.9360 0.030 Uiso 1 1 calc R . .
C2 C 0.85103(16) 0.8870(2) 0.95089(18) 0.0147(5) Uani 1 1 d . . .
N1 N 0.99368(13) 0.86673(17) 0.95789(14) 0.0130(4) Uani 1 1 d . . .
C3 C 0.92336(16) 0.8258(2) 0.93608(18) 0.0148(5) Uani 1 1 d . . .
C4 C 0.91826(19) 0.7319(2) 0.9037(2) 0.0245(7) Uani 1 1 d . . .
H4 H 0.8685 0.7040 0.8873 0.029 Uiso 1 1 calc R . .
C5 C 0.9857(2) 0.6791(2) 0.8955(3) 0.0304(8) Uani 1 1 d . . .
H5 H 0.9826 0.6149 0.8735 0.036 Uiso 1 1 calc R . .
C6 C 1.05737(19) 0.7208(2) 0.9196(2) 0.0233(6) Uani 1 1 d . . .
H6 H 1.1044 0.6853 0.9158 0.028 Uiso 1 1 calc R . .
C7 C 1.05967(17) 0.8150(2) 0.94948(18) 0.0167(6) Uani 1 1 d . . .
H7 H 1.1091 0.8444 0.9646 0.020 Uiso 1 1 calc R . .
N2 N 0.91995(13) 0.97093(17) 1.07780(14) 0.0129(4) Uani 1 1 d . . .
C8 C 0.85723(15) 0.91734(19) 1.04807(17) 0.0129(5) Uani 1 1 d . . .
C9 C 0.80110(16) 0.8925(2) 1.10461(19) 0.0173(6) Uani 1 1 d . . .
H9 H 0.7577 0.8535 1.0839 0.021 Uiso 1 1 calc R . .
C10 C 0.80863(17) 0.9245(2) 1.1909(2) 0.0209(6) Uani 1 1 d . . .
H10 H 0.7705 0.9079 1.2297 0.025 Uiso 1 1 calc R . .
C11 C 0.87221(17) 0.9810(2) 1.21992(19) 0.0187(6) Uani 1 1 d . . .
H11 H 0.8778 1.0050 1.2785 0.022 Uiso 1 1 calc R . .
C12 C 0.92733(17) 1.0019(2) 1.16243(18) 0.0145(5) Uani 1 1 d . . .
H12 H 0.9719 1.0391 1.1827 0.017 Uiso 1 1 calc R . .
N3 N 0.91792(13) 1.03472(17) 0.90922(14) 0.0129(4) Uani 1 1 d . . .
C13 C 0.85384(16) 0.9788(2) 0.89465(18) 0.0141(5) Uani 1 1 d . . .
C14 C 0.79392(17) 1.0039(2) 0.83111(19) 0.0189(6) Uani 1 1 d . . .
H14 H 0.7488 0.9642 0.8211 0.023 Uiso 1 1 calc R . .
C15 C 0.80072(18) 1.0878(2) 0.7824(2) 0.0234(6) Uani 1 1 d . . .
H15 H 0.7603 1.1058 0.7387 0.028 Uiso 1 1 calc R . .
C16 C 0.86657(17) 1.1451(2) 0.79793(19) 0.0200(6) Uani 1 1 d . . .
H16 H 0.8719 1.2030 0.7655 0.024 Uiso 1 1 calc R . .
C17 C 0.92429(16) 1.1165(2) 0.86153(18) 0.0157(5) Uani 1 1 d . . .
H17 H 0.9699 1.1553 0.8722 0.019 Uiso 1 1 calc R . .
Co2 Co 0.5000 1.0000 0.5000 0.01120(12) Uani 1 2 d S . .
C18 C 0.34921(17) 0.8205(2) 0.66920(18) 0.0166(6) Uani 1 1 d . . .
H18A H 0.3220 0.8629 0.7079 0.025 Uiso 1 1 calc R . .
H18B H 0.3829 0.7756 0.7050 0.025 Uiso 1 1 calc R . .
H18C H 0.3106 0.7839 0.6312 0.025 Uiso 1 1 calc R . .
C19 C 0.39934(16) 0.88157(19) 0.61216(17) 0.0127(5) Uani 1 1 d . . .
N4 N 0.49193(14) 0.86168(17) 0.49938(14) 0.0127(4) Uani 1 1 d . . .
C20 C 0.44452(16) 0.8167(2) 0.55223(17) 0.0129(5) Uani 1 1 d . . .
C21 C 0.43695(16) 0.7172(2) 0.55002(17) 0.0143(5) Uani 1 1 d . . .
H21 H 0.4027 0.6860 0.5865 0.017 Uiso 1 1 calc R . .
C22 C 0.47937(17) 0.6636(2) 0.49459(17) 0.0146(5) Uani 1 1 d . . .
H22 H 0.4745 0.5952 0.4929 0.018 Uiso 1 1 calc R . .
C23 C 0.52901(17) 0.7100(2) 0.44142(18) 0.0157(5) Uani 1 1 d . . .
H23 H 0.5592 0.6742 0.4035 0.019 Uiso 1 1 calc R . .
C24 C 0.53348(17) 0.8091(2) 0.44482(17) 0.0145(5) Uani 1 1 d . . .
H24 H 0.5667 0.8416 0.4079 0.017 Uiso 1 1 calc R . .
N5 N 0.50862(14) 0.99709(16) 0.62725(14) 0.0125(4) Uani 1 1 d . . .
C25 C 0.45916(16) 0.94221(19) 0.66992(17) 0.0130(5) Uani 1 1 d . . .
C26 C 0.46391(17) 0.9414(2) 0.76133(17) 0.0151(5) Uani 1 1 d . . .
H26 H 0.4278 0.9043 0.7911 0.018 Uiso 1 1 calc R . .
C27 C 0.52161(18) 0.9949(2) 0.80894(18) 0.0166(6) Uani 1 1 d . . .
H27 H 0.5256 0.9945 0.8715 0.020 Uiso 1 1 calc R . .
C28 C 0.57340(17) 1.0489(2) 0.76430(18) 0.0165(5) Uani 1 1 d . . .
H28 H 0.6143 1.0845 0.7956 0.020 Uiso 1 1 calc R . .
C29 C 0.56444(17) 1.0499(2) 0.67384(18) 0.0156(5) Uani 1 1 d . . .
H29 H 0.5985 1.0889 0.6430 0.019 Uiso 1 1 calc R . .
N6 N 0.38637(14) 1.00866(16) 0.49984(15) 0.0133(5) Uani 1 1 d . . .
C30 C 0.34838(17) 0.9510(2) 0.55299(17) 0.0148(5) Uani 1 1 d . . .
C31 C 0.26744(18) 0.9548(2) 0.5521(2) 0.0208(6) Uani 1 1 d . . .
H31 H 0.2411 0.9143 0.5901 0.025 Uiso 1 1 calc R . .
C32 C 0.22499(19) 1.0180(2) 0.4954(2) 0.0256(7) Uani 1 1 d . . .
H32 H 0.1695 1.0205 0.4939 0.031 Uiso 1 1 calc R . .
C33 C 0.26435(19) 1.0774(2) 0.4413(2) 0.0238(6) Uani 1 1 d . . .
H33 H 0.2365 1.1213 0.4021 0.029 Uiso 1 1 calc R . .
C34 C 0.34490(18) 1.0714(2) 0.44545(18) 0.0183(6) Uani 1 1 d . . .
H34 H 0.3723 1.1127 0.4090 0.022 Uiso 1 1 calc R . .
Cl1 Cl 0.61850(4) 0.73016(5) 0.72928(4) 0.01480(14) Uani 1 1 d . . .
O1 O 0.64730(14) 0.82678(17) 0.74674(15) 0.0263(5) Uani 1 1 d . . .
O2 O 0.53530(12) 0.72835(17) 0.73523(14) 0.0218(5) Uani 1 1 d . . .
O3 O 0.65635(14) 0.66385(17) 0.79261(15) 0.0271(5) Uani 1 1 d . . .
O4 O 0.63492(13) 0.70292(17) 0.64097(14) 0.0247(5) Uani 1 1 d . . .
Cl2 Cl 0.72760(4) 0.29677(5) 0.60368(4) 0.01534(15) Uani 1 1 d . . .
O5 O 0.67494(13) 0.37484(17) 0.61940(14) 0.0244(5) Uani 1 1 d . . .
O6 O 0.68802(15) 0.20612(17) 0.61442(18) 0.0335(6) Uani 1 1 d . . .
O7 O 0.79543(13) 0.30286(17) 0.66607(14) 0.0239(5) Uani 1 1 d . . .
O8 O 0.75002(13) 0.30438(19) 0.51543(14) 0.0278(5) Uani 1 1 d . . .
Cl3A Cl 0.95903(12) 0.86739(18) 0.65243(15) 0.0177(4) Uani 0.50 1 d P A 1
O9A O 1.0328(3) 0.8371(4) 0.6841(4) 0.0373(12) Uiso 0.50 1 d P A 1
O10A O 0.9150(3) 0.7822(5) 0.6142(4) 0.0339(14) Uiso 0.50 1 d P A 1
O11A O 0.9155(3) 0.8950(4) 0.7309(4) 0.0414(13) Uiso 0.50 1 d P A 1
O12A O 0.9585(4) 0.9422(5) 0.5971(4) 0.0527(16) Uiso 0.50 1 d P A 1
Cl3B Cl 0.9321(2) 0.8519(2) 0.6732(2) 0.0542(9) Uani 0.50 1 d P B 2
O9B O 0.8568(5) 0.8118(7) 0.7207(6) 0.081(2) Uiso 0.50 1 d P B 2
O10B O 0.9229(4) 0.9471(5) 0.6823(5) 0.0584(17) Uiso 0.50 1 d P B 2
O11B O 1.0005(4) 0.8149(5) 0.7229(5) 0.0566(17) Uiso 0.50 1 d P B 2
O12B O 0.9152(4) 0.8099(5) 0.5921(5) 0.0452(17) Uiso 0.50 1 d P B 2
O13 O 0.62414(14) 0.53522(18) 0.51703(17) 0.0275(5) Uani 1 1 d . . .
H13A H 0.649(3) 0.486(3) 0.545(3) 0.041 Uiso 1 1 d . . .
H13B H 0.629(3) 0.581(3) 0.558(3) 0.041 Uiso 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
Co1 N2 1.936(2) . ?
Co1 N3 1.942(2) . ?
Co1 N1 1.953(2) . ?
C1 C2 1.529(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C8 1.534(4) . ?
C2 C3 1.536(4) . ?
C2 C13 1.536(4) . ?
N1 C3 1.347(4) . ?
N1 C7 1.355(4) . ?
C3 C4 1.390(4) . ?
C4 C5 1.383(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.377(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.381(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
N2 C8 1.351(4) . ?
N2 C12 1.354(3) . ?
C8 C9 1.392(4) . ?
C9 C10 1.383(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N3 C13 1.346(4) . ?
N3 C17 1.356(4) . ?
C13 C14 1.391(4) . ?
C14 C15 1.389(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.379(4) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
Co2 N4 1.920(2) . ?
Co2 N5 1.932(2) . ?
Co2 N6 1.952(2) . ?
C18 C19 1.532(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C30 1.535(4) . ?
C19 C25 1.539(4) . ?
C19 C20 1.540(4) . ?
N4 C20 1.348(3) . ?
N4 C24 1.356(3) . ?
C20 C21 1.382(4) . ?
C21 C22 1.381(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
N5 C25 1.349(3) . ?
N5 C29 1.353(4) . ?
C25 C26 1.388(4) . ?
C26 C27 1.387(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.386(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.374(4) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
N6 C30 1.347(3) . ?
N6 C34 1.357(4) . ?
C30 C31 1.388(4) . ?
C31 C32 1.388(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.383(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.379(4) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
Cl1 O2 1.438(2) . ?
Cl1 O1 1.442(2) . ?
Cl1 O3 1.443(2) . ?
Cl1 O4 1.450(2) . ?
Cl2 O8 1.436(2) . ?
Cl2 O7 1.436(2) . ?
Cl2 O5 1.442(2) . ?
Cl2 O6 1.443(2) . ?
Cl3A O12A 1.335(7) . ?
Cl3A O9A 1.379(6) . ?
Cl3A O10A 1.490(7) . ?
Cl3A O11A 1.516(6) . ?
Cl3B O10B 1.336(8) . ?
Cl3B O12B 1.373(7) . ?
Cl3B O11B 1.432(8) . ?
Cl3B O9B 1.635(10) . ?
O13 H13A 0.89(5) . ?
O13 H13B 0.88(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
N2 Co1 N2 180.00 3_777 . ?
N2 Co1 N3 91.17(9) . 3_777 ?
N2 Co1 N3 88.83(9) . . ?
N3 Co1 N3 180.00 3_777 . ?
N2 Co1 N1 89.07(10) . . ?
N3 Co1 N1 89.12(10) . . ?
N2 Co1 N1 90.93(10) . 3_777 ?
N3 Co1 N1 90.88(10) . 3_777 ?
N1 Co1 N1 180.00 . 3_777 ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 C8 111.0(2) . . ?
C1 C2 C3 110.8(2) . . ?
C8 C2 C3 107.9(2) . . ?
C1 C2 C13 111.1(2) . . ?
C8 C2 C13 108.0(2) . . ?
C3 C2 C13 107.9(2) . . ?
C3 N1 C7 119.4(2) . . ?
C3 N1 Co1 120.03(19) . . ?
C7 N1 Co1 120.57(19) . . ?
N1 C3 C4 120.5(3) . . ?
N1 C3 C2 116.7(2) . . ?
C4 C3 C2 122.8(3) . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 119.2(3) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C7 118.8(3) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
N1 C7 C6 122.1(3) . . ?
N1 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C8 N2 C12 119.7(2) . . ?
C8 N2 Co1 119.74(18) . . ?
C12 N2 Co1 120.52(19) . . ?
N2 C8 C9 120.2(2) . . ?
N2 C8 C2 117.2(2) . . ?
C9 C8 C2 122.6(2) . . ?
C10 C9 C8 120.0(3) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C9 119.3(3) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C12 C11 C10 118.8(3) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
N2 C12 C11 122.0(3) . . ?
N2 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C13 N3 C17 119.8(2) . . ?
C13 N3 Co1 120.21(19) . . ?
C17 N3 Co1 120.02(19) . . ?
N3 C13 C14 120.8(3) . . ?
N3 C13 C2 116.8(2) . . ?
C14 C13 C2 122.5(3) . . ?
C15 C14 C13 119.3(3) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C16 C15 C14 119.7(3) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C17 C16 C15 118.6(3) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
N3 C17 C16 122.0(3) . . ?
N3 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
N4 Co2 N4 180.00 3_676 . ?
N4 Co2 N5 89.03(9) . . ?
N4 Co2 N5 90.97(9) . 3_676 ?
N5 Co2 N5 180.00 . 3_676 ?
N4 Co2 N6 89.41(10) . . ?
N5 Co2 N6 89.30(10) . . ?
N4 Co2 N6 90.59(10) . 3_676 ?
N5 Co2 N6 90.70(10) . 3_676 ?
N6 Co2 N6 180.00 . 3_676 ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C18 C19 C30 111.1(2) . . ?
C18 C19 C25 110.8(2) . . ?
C30 C19 C25 108.0(2) . . ?
C18 C19 C20 110.7(2) . . ?
C30 C19 C20 107.9(2) . . ?
C25 C19 C20 108.2(2) . . ?
C20 N4 C24 119.8(2) . . ?
C20 N4 Co2 120.35(18) . . ?
C24 N4 Co2 119.82(18) . . ?
N4 C20 C21 120.4(2) . . ?
N4 C20 C19 116.6(2) . . ?
C21 C20 C19 123.0(2) . . ?
C22 C21 C20 119.8(3) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 119.6(3) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 118.4(3) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
N4 C24 C23 121.9(2) . . ?
N4 C24 H24 119.0 . . ?
C23 C24 H24 119.0 . . ?
C25 N5 C29 119.8(2) . . ?
C25 N5 Co2 120.11(19) . . ?
C29 N5 Co2 120.10(18) . . ?
N5 C25 C26 120.4(3) . . ?
N5 C25 C19 116.5(2) . . ?
C26 C25 C19 123.0(2) . . ?
C27 C26 C25 119.6(3) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C26 119.3(3) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C29 C28 C27 118.7(3) . . ?
C29 C28 H28 120.6 . . ?
C27 C28 H28 120.6 . . ?
N5 C29 C28 122.0(3) . . ?
N5 C29 H29 119.0 . . ?
C28 C29 H29 119.0 . . ?
C30 N6 C34 119.5(3) . . ?
C30 N6 Co2 120.01(19) . . ?
C34 N6 Co2 120.52(19) . . ?
N6 C30 C31 120.6(3) . . ?
N6 C30 C19 116.3(2) . . ?
C31 C30 C19 123.0(2) . . ?
C30 C31 C32 119.9(3) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C33 C32 C31 119.3(3) . . ?
C33 C32 H32 120.4 . . ?
C31 C32 H32 120.4 . . ?
C34 C33 C32 118.6(3) . . ?
C34 C33 H33 120.7 . . ?
C32 C33 H33 120.7 . . ?
N6 C34 C33 122.2(3) . . ?
N6 C34 H34 118.9 . . ?
C33 C34 H34 118.9 . . ?
O2 Cl1 O1 109.24(14) . . ?
O2 Cl1 O3 109.59(13) . . ?
O1 Cl1 O3 109.92(15) . . ?
O2 Cl1 O4 109.37(13) . . ?
O1 Cl1 O4 108.69(14) . . ?
O3 Cl1 O4 110.01(14) . . ?
O8 Cl2 O7 110.26(13) . . ?
O8 Cl2 O5 109.01(14) . . ?
O7 Cl2 O5 109.12(14) . . ?
O8 Cl2 O6 109.80(16) . . ?
O7 Cl2 O6 109.68(14) . . ?
O5 Cl2 O6 108.94(15) . . ?
O12A Cl3A O9A 114.3(4) . . ?
O12A Cl3A O10A 113.1(4) . . ?
O9A Cl3A O10A 108.2(4) . . ?
O12A Cl3A O11A 109.2(4) . . ?
O9A Cl3A O11A 107.6(4) . . ?
O10A Cl3A O11A 103.9(3) . . ?
O10B Cl3B O12B 119.6(5) . . ?
O10B Cl3B O11B 113.4(5) . . ?
O12B Cl3B O11B 114.9(5) . . ?
O10B Cl3B O9B 100.5(5) . . ?
O12B Cl3B O9B 98.3(5) . . ?
O11B Cl3B O9B 106.6(5) . . ?
H13A O13 H13B 102(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O13 H13B O4 0.88(5) 2.11(5) 2.988(3) 172(4) .
O13 H13A O5 0.89(5) 1.94(5) 2.806(3) 164(4) .

_diffrn_measured_fraction_theta_max 0.884
_diffrn_reflns_theta_full        29.82
_diffrn_measured_fraction_theta_full 0.884
_refine_diff_density_max         2.245
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.105
_database_code_depnum_ccdc_archive 'CCDC 1023801'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_as162247

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
[1,1,1-Tris(pyrid-2-yl)ethane]dichloropalladium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H15 Cl2 N3 Pd'
_chemical_formula_sum            'C17 H15 Cl2 N3 Pd'
_chemical_formula_weight         438.62

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'
Cl Cl 0.3639 0.7018 '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'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   9.0049(2)
_cell_length_b                   18.4245(3)
_cell_length_c                   10.6172(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.445(2)
_cell_angle_gamma                90.00
_cell_volume                     1628.07(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4832
_cell_measurement_theta_min      4.79
_cell_measurement_theta_max      73.52

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    12.220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5834
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.80
_diffrn_reflns_theta_max         66.58
_reflns_number_total             2871
_reflns_number_gt                2774
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied. All 
 non-H atoms are refined anisotropically, while H atoms were placed in 
 calculated positions and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0399P)²+0.0366P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2871
_refine_ls_number_parameters     209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0642
_refine_ls_wR_factor_gt          0.0636
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.648831(19) 0.596938(9) 0.223107(15) 0.00659(9) Uani 1 1 d . . .
Cl1 Cl 0.92171(7) 0.57781(3) 0.31600(6) 0.01384(14) Uani 1 1 d . . .
Cl2 Cl 0.65937(7) 0.61745(3) 0.01332(5) 0.01115(13) Uani 1 1 d . . .
C1 C 0.3280(3) 0.73195(14) 0.3891(2) 0.0130(5) Uani 1 1 d . . .
H1A H 0.2633 0.7658 0.3182 0.019 Uiso 1 1 calc R . .
H1B H 0.3974 0.7593 0.4691 0.019 Uiso 1 1 calc R . .
H1C H 0.2570 0.7002 0.4149 0.019 Uiso 1 1 calc R . .
C2 C 0.4327(3) 0.68557(13) 0.3343(2) 0.0099(5) Uani 1 1 d . . .
N1 N 0.6320(3) 0.58586(11) 0.4079(2) 0.0095(4) Uani 1 1 d . . .
C3 C 0.5356(3) 0.63128(13) 0.4420(2) 0.0095(5) Uani 1 1 d . . .
C4 C 0.5322(3) 0.62765(14) 0.5716(2) 0.0137(5) Uani 1 1 d . . .
H4 H 0.4661 0.6602 0.5965 0.016 Uiso 1 1 calc R . .
C5 C 0.6250(3) 0.57668(16) 0.6649(3) 0.0168(5) Uani 1 1 d . . .
H5 H 0.6217 0.5736 0.7531 0.020 Uiso 1 1 calc R . .
C6 C 0.7220(3) 0.53056(14) 0.6279(2) 0.0149(5) Uani 1 1 d . . .
H6 H 0.7872 0.4954 0.6900 0.018 Uiso 1 1 calc R . .
C7 C 0.7220(3) 0.53689(14) 0.4978(2) 0.0119(5) Uani 1 1 d . . .
H7 H 0.7883 0.5053 0.4715 0.014 Uiso 1 1 calc R . .
N2 N 0.4058(3) 0.60392(11) 0.1442(2) 0.0093(4) Uani 1 1 d . . .
C8 C 0.3276(3) 0.64313(13) 0.2074(2) 0.0098(5) Uani 1 1 d . . .
C9 C 0.1617(3) 0.64222(13) 0.1575(2) 0.0113(5) Uani 1 1 d . . .
H9 H 0.1067 0.6699 0.2016 0.014 Uiso 1 1 calc R . .
C10 C 0.0746(3) 0.60111(13) 0.0434(3) 0.0132(5) Uani 1 1 d . . .
H10 H -0.0394 0.6003 0.0095 0.016 Uiso 1 1 calc R . .
C11 C 0.1562(3) 0.56147(14) -0.0201(2) 0.0131(5) Uani 1 1 d . . .
H11 H 0.0998 0.5328 -0.0982 0.016 Uiso 1 1 calc R . .
C12 C 0.3222(3) 0.56464(13) 0.0331(2) 0.0103(5) Uani 1 1 d . . .
H12 H 0.3794 0.5380 -0.0106 0.012 Uiso 1 1 calc R . .
N3 N 0.6938(3) 0.74282(11) 0.3847(2) 0.0127(4) Uani 1 1 d . . .
C13 C 0.5415(3) 0.73902(13) 0.2973(2) 0.0101(5) Uani 1 1 d . . .
C14 C 0.4778(3) 0.78206(14) 0.1816(2) 0.0135(5) Uani 1 1 d . . .
H14 H 0.3680 0.7780 0.1227 0.016 Uiso 1 1 calc R . .
C15 C 0.5787(3) 0.83122(15) 0.1542(3) 0.0180(5) Uani 1 1 d . . .
H15 H 0.5394 0.8616 0.0761 0.022 Uiso 1 1 calc R . .
C16 C 0.7379(3) 0.83486(14) 0.2434(3) 0.0166(5) Uani 1 1 d . . .
H16 H 0.8099 0.8677 0.2272 0.020 Uiso 1 1 calc R . .
C17 C 0.7901(3) 0.79018(14) 0.3559(3) 0.0144(5) Uani 1 1 d . . .
H17 H 0.8996 0.7930 0.4162 0.017 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N2 2.027(2) . ?
Pd1 N1 2.035(2) . ?
Pd1 Cl2 2.2965(5) . ?
Pd1 Cl1 2.2988(6) . ?
C1 C2 1.541(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C8 1.532(3) . ?
C2 C3 1.536(3) . ?
C2 C13 1.541(3) . ?
N1 C7 1.338(3) . ?
N1 C3 1.351(3) . ?
C3 C4 1.389(3) . ?
C4 C5 1.389(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
N2 C12 1.342(3) . ?
N2 C8 1.352(3) . ?
C8 C9 1.382(3) . ?
C9 C10 1.390(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N3 C13 1.332(3) . ?
N3 C17 1.345(3) . ?
C13 C14 1.389(3) . ?
C14 C15 1.390(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(4) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pd1 N1 86.50(8) . . ?
N2 Pd1 Cl2 91.52(6) . . ?
N1 Pd1 Cl2 175.90(6) . . ?
N2 Pd1 Cl1 174.70(6) . . ?
N1 Pd1 Cl1 91.82(6) . . ?
Cl2 Pd1 Cl1 90.46(2) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C8 C2 C3 108.47(19) . . ?
C8 C2 C13 109.96(18) . . ?
C3 C2 C13 110.16(19) . . ?
C8 C2 C1 110.7(2) . . ?
C3 C2 C1 111.20(19) . . ?
C13 C2 C1 106.34(19) . . ?
C7 N1 C3 120.2(2) . . ?
C7 N1 Pd1 120.52(17) . . ?
C3 N1 Pd1 119.23(16) . . ?
N1 C3 C4 119.7(2) . . ?
N1 C3 C2 118.1(2) . . ?
C4 C3 C2 122.3(2) . . ?
C3 C4 C5 120.3(2) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C6 C5 C4 119.2(2) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C7 118.2(2) . . ?
C5 C6 H6 120.9 . . ?
C7 C6 H6 120.9 . . ?
N1 C7 C6 122.5(2) . . ?
N1 C7 H7 118.7 . . ?
C6 C7 H7 118.7 . . ?
C12 N2 C8 120.0(2) . . ?
C12 N2 Pd1 118.91(17) . . ?
C8 N2 Pd1 120.87(17) . . ?
N2 C8 C9 119.7(2) . . ?
N2 C8 C2 116.5(2) . . ?
C9 C8 C2 123.9(2) . . ?
C8 C9 C10 120.5(2) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 119.1(2) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10 C11 C12 118.2(2) . . ?
C10 C11 H11 120.9 . . ?
C12 C11 H11 120.9 . . ?
N2 C12 C11 122.5(2) . . ?
N2 C12 H12 118.7 . . ?
C11 C12 H12 118.7 . . ?
C13 N3 C17 117.3(2) . . ?
N3 C13 C14 123.6(2) . . ?
N3 C13 C2 116.2(2) . . ?
C14 C13 C2 120.1(2) . . ?
C13 C14 C15 118.4(2) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C16 C15 C14 118.5(2) . . ?
C16 C15 H15 120.8 . . ?
C14 C15 H15 120.8 . . ?
C17 C16 C15 119.1(2) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
N3 C17 C16 123.2(2) . . ?
N3 C17 H17 118.4 . . ?
C16 C17 H17 118.4 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        66.58
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.111
_database_code_depnum_ccdc_archive 'CCDC 1023802'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_as164247

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis[1,1,1-tris(pyrid-2-yl)ethane]silver(I) nitrate 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H30 Ag N6, N O3'
_chemical_formula_sum            'C34 H30 Ag N7 O3'
_chemical_formula_weight         692.52

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'
Ag Ag 0.1306 4.2820 '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'

_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                   9.1661(2)
_cell_length_b                   10.4860(3)
_cell_length_c                   16.6632(5)
_cell_angle_alpha                99.769(2)
_cell_angle_beta                 104.448(2)
_cell_angle_gamma                100.675(2)
_cell_volume                     1484.36(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8096
_cell_measurement_theta_min      4.43
_cell_measurement_theta_max      73.73

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             708
_exptl_absorpt_coefficient_mu    5.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            10611
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.41
_diffrn_reflns_theta_max         66.60
_reflns_number_total             5059
_reflns_number_gt                4792
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied. All 
 non-H atoms are refined anisotropically. H atoms were located in the Fourier 
 map and allowed to refine, with Uiso values of 1.2xUeq of the 
 corresponding C atoms for armoatic H atoms, or 1.5xUeq{C} for the methyl 
 group.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0315P)²+0.0816P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5059
_refine_ls_number_parameters     408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0599
_refine_ls_wR_factor_gt          0.0583
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.003
_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
Ag1 Ag 0.256567(16) 0.771068(13) 0.761177(8) 0.01640(6) Uani 1 1 d . . .
C1 C -0.0521(2) 1.0220(2) 0.60390(13) 0.0170(4) Uani 1 1 d . . .
H1A H -0.0964 0.9689 0.5454 0.025 Uiso 1 1 calc R . .
H1B H 0.0236 1.1020 0.6049 0.025 Uiso 1 1 calc R . .
H1C H -0.1351 1.0480 0.6254 0.025 Uiso 1 1 calc R . .
C2 C 0.0288(2) 0.93877(19) 0.66047(12) 0.0126(4) Uani 1 1 d . . .
N1 N 0.1857(2) 0.96193(16) 0.80716(10) 0.0158(3) Uani 1 1 d . . .
C3 C 0.0955(2) 1.01725(19) 0.75360(12) 0.0127(4) Uani 1 1 d . . .
C4 C 0.0650(2) 1.1400(2) 0.78223(13) 0.0166(4) Uani 1 1 d . . .
H4 H 0.0022 1.1792 0.7438 0.020 Uiso 1 1 calc R . .
C5 C 0.1277(2) 1.2039(2) 0.86766(14) 0.0196(4) Uani 1 1 d . . .
H5 H 0.1072 1.2869 0.8883 0.024 Uiso 1 1 calc R . .
C6 C 0.2198(3) 1.1464(2) 0.92226(13) 0.0213(4) Uani 1 1 d . . .
H6 H 0.2637 1.1886 0.9809 0.026 Uiso 1 1 calc R . .
C7 C 0.2466(2) 1.0252(2) 0.88926(13) 0.0181(4) Uani 1 1 d . . .
H7 H 0.3108 0.9853 0.9264 0.022 Uiso 1 1 calc R . .
N2 N -0.02401(19) 0.70964(17) 0.67993(10) 0.0145(3) Uani 1 1 d . . .
C8 C -0.0862(2) 0.80867(19) 0.65676(11) 0.0133(4) Uani 1 1 d . . .
C9 C -0.2467(2) 0.7932(2) 0.63108(12) 0.0178(4) Uani 1 1 d . . .
H9 H -0.2893 0.8651 0.6166 0.021 Uiso 1 1 calc R . .
C10 C -0.3436(2) 0.6723(2) 0.62679(13) 0.0219(4) Uani 1 1 d . . .
H10 H -0.4530 0.6603 0.6089 0.026 Uiso 1 1 calc R . .
C11 C -0.2791(3) 0.5690(2) 0.64881(13) 0.0215(4) Uani 1 1 d . . .
H11 H -0.3427 0.4844 0.6453 0.026 Uiso 1 1 calc R . .
C12 C -0.1187(3) 0.5933(2) 0.67615(13) 0.0183(4) Uani 1 1 d . . .
H12 H -0.0735 0.5239 0.6931 0.022 Uiso 1 1 calc R . .
N3 N 0.1118(2) 0.80727(17) 0.55282(10) 0.0148(3) Uani 1 1 d . . .
C13 C 0.1586(2) 0.90681(19) 0.62298(12) 0.0126(4) Uani 1 1 d . . .
C14 C 0.3097(2) 0.98650(19) 0.65225(12) 0.0146(4) Uani 1 1 d . . .
H14 H 0.3401 1.0559 0.7021 0.017 Uiso 1 1 calc R . .
C15 C 0.4150(2) 0.9631(2) 0.60768(13) 0.0173(4) Uani 1 1 d . . .
H15 H 0.5183 1.0163 0.6266 0.021 Uiso 1 1 calc R . .
C16 C 0.3670(2) 0.8610(2) 0.53518(13) 0.0174(4) Uani 1 1 d . . .
H16 H 0.4359 0.8431 0.5029 0.021 Uiso 1 1 calc R . .
C17 C 0.2146(2) 0.7854(2) 0.51098(12) 0.0158(4) Uani 1 1 d . . .
H17 H 0.1821 0.7143 0.4619 0.019 Uiso 1 1 calc R . .
C18 C 0.5305(2) 0.4702(2) 0.88545(12) 0.0166(4) Uani 1 1 d . . .
H18A H 0.5895 0.5185 0.9437 0.025 Uiso 1 1 calc R . .
H18B H 0.6002 0.4349 0.8565 0.025 Uiso 1 1 calc R . .
H18C H 0.4489 0.3965 0.8871 0.025 Uiso 1 1 calc R . .
C19 C 0.4561(2) 0.56597(19) 0.83687(12) 0.0124(4) Uani 1 1 d . . .
N4 N 0.5267(2) 0.79359(17) 0.81841(10) 0.0158(3) Uani 1 1 d . . .
C20 C 0.5793(2) 0.6877(2) 0.83721(11) 0.0136(4) Uani 1 1 d . . .
C21 C 0.7365(2) 0.6890(2) 0.85616(12) 0.0186(4) Uani 1 1 d . . .
H21 H 0.7709 0.6113 0.8658 0.022 Uiso 1 1 calc R . .
C22 C 0.8421(3) 0.8052(2) 0.86077(13) 0.0246(5) Uani 1 1 d . . .
H22 H 0.9499 0.8084 0.8743 0.030 Uiso 1 1 calc R . .
C23 C 0.7889(3) 0.9159(2) 0.84554(13) 0.0250(5) Uani 1 1 d . . .
H23 H 0.8593 0.9978 0.8506 0.030 Uiso 1 1 calc R . .
C24 C 0.6300(3) 0.9052(2) 0.82258(13) 0.0206(4) Uani 1 1 d . . .
H24 H 0.5929 0.9801 0.8092 0.025 Uiso 1 1 calc R . .
N5 N 0.2742(2) 0.55961(16) 0.69984(10) 0.0151(3) Uani 1 1 d . . .
C25 C 0.3692(2) 0.49566(19) 0.74360(12) 0.0121(4) Uani 1 1 d . . .
C26 C 0.3914(2) 0.3755(2) 0.70482(13) 0.0165(4) Uani 1 1 d . . .
H26 H 0.4572 0.3301 0.7366 0.020 Uiso 1 1 calc R . .
C27 C 0.3154(3) 0.3226(2) 0.61858(14) 0.0205(4) Uani 1 1 d . . .
H27 H 0.3302 0.2411 0.5908 0.025 Uiso 1 1 calc R . .
C28 C 0.2191(2) 0.3888(2) 0.57378(13) 0.0202(4) Uani 1 1 d . . .
H28 H 0.1668 0.3545 0.5149 0.024 Uiso 1 1 calc R . .
C29 C 0.2007(2) 0.5069(2) 0.61703(13) 0.0175(4) Uani 1 1 d . . .
H29 H 0.1332 0.5526 0.5868 0.021 Uiso 1 1 calc R . .
N6 N 0.4221(2) 0.71050(16) 0.95785(10) 0.0150(3) Uani 1 1 d . . .
C30 C 0.3485(2) 0.61342(19) 0.88717(12) 0.0124(4) Uani 1 1 d . . .
C31 C 0.1926(2) 0.55042(19) 0.86850(12) 0.0147(4) Uani 1 1 d . . .
H31 H 0.1428 0.4834 0.8178 0.018 Uiso 1 1 calc R . .
C32 C 0.1107(2) 0.5867(2) 0.92488(13) 0.0179(4) Uani 1 1 d . . .
H32 H 0.0045 0.5439 0.9137 0.021 Uiso 1 1 calc R . .
C33 C 0.1862(3) 0.6864(2) 0.99786(13) 0.0187(4) Uani 1 1 d . . .
H33 H 0.1334 0.7133 1.0377 0.022 Uiso 1 1 calc R . .
C34 C 0.3408(3) 0.7452(2) 1.01050(12) 0.0176(4) Uani 1 1 d . . .
H34 H 0.3921 0.8145 1.0598 0.021 Uiso 1 1 calc R . .
N7 N 0.73903(19) 0.26625(16) 0.75025(10) 0.0149(3) Uani 1 1 d . . .
O1 O 0.64831(19) 0.19793(15) 0.78049(10) 0.0247(3) Uani 1 1 d . . .
O2 O 0.7258(2) 0.23809(18) 0.67298(10) 0.0319(4) Uani 1 1 d . . .
O3 O 0.84277(19) 0.36333(17) 0.79813(10) 0.0298(4) 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
Ag1 N1 2.2857(17) . ?
Ag1 N5 2.3309(17) . ?
Ag1 N4 2.3716(18) . ?
Ag1 N2 2.4930(17) . ?
C1 C2 1.539(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C13 1.538(3) . ?
C2 C3 1.538(3) . ?
C2 C8 1.543(3) . ?
N1 C7 1.341(3) . ?
N1 C3 1.342(3) . ?
C3 C4 1.398(3) . ?
C4 C5 1.390(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.377(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.387(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
N2 C8 1.341(3) . ?
N2 C12 1.342(3) . ?
C8 C9 1.396(3) . ?
C9 C10 1.386(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.387(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N3 C17 1.334(3) . ?
N3 C13 1.345(3) . ?
C13 C14 1.397(3) . ?
C14 C15 1.388(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.394(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.543(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.538(3) . ?
C19 C25 1.539(3) . ?
C19 C30 1.541(3) . ?
N4 C24 1.342(3) . ?
N4 C20 1.343(3) . ?
C20 C21 1.393(3) . ?
C21 C22 1.386(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
N5 C29 1.343(3) . ?
N5 C25 1.343(3) . ?
C25 C26 1.389(3) . ?
C26 C27 1.395(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.375(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.385(3) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
N6 C34 1.333(3) . ?
N6 C30 1.349(3) . ?
C30 C31 1.390(3) . ?
C31 C32 1.388(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.390(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.384(3) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
N7 O2 1.241(2) . ?
N7 O3 1.251(2) . ?
N7 O1 1.253(2) . ?

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 Ag1 N5 168.12(6) . . ?
N1 Ag1 N4 111.29(6) . . ?
N5 Ag1 N4 80.58(6) . . ?
N1 Ag1 N2 79.52(6) . . ?
N5 Ag1 N2 88.65(6) . . ?
N4 Ag1 N2 168.63(6) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C13 C2 C3 111.10(16) . . ?
C13 C2 C1 105.21(15) . . ?
C3 C2 C1 111.07(16) . . ?
C13 C2 C8 110.13(15) . . ?
C3 C2 C8 108.73(15) . . ?
C1 C2 C8 110.59(16) . . ?
C7 N1 C3 119.42(18) . . ?
C7 N1 Ag1 118.25(14) . . ?
C3 N1 Ag1 122.13(13) . . ?
N1 C3 C4 120.90(18) . . ?
N1 C3 C2 116.60(17) . . ?
C4 C3 C2 122.50(18) . . ?
C5 C4 C3 119.1(2) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C6 C5 C4 119.7(2) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 118.10(18) . . ?
C5 C6 H6 121.0 . . ?
C7 C6 H6 121.0 . . ?
N1 C7 C6 122.8(2) . . ?
N1 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
C8 N2 C12 118.98(18) . . ?
C8 N2 Ag1 116.71(12) . . ?
C12 N2 Ag1 122.50(14) . . ?
N2 C8 C9 121.00(18) . . ?
N2 C8 C2 116.46(17) . . ?
C9 C8 C2 122.54(18) . . ?
C10 C9 C8 119.6(2) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C11 C10 C9 119.3(2) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 117.69(19) . . ?
C10 C11 H11 121.2 . . ?
C12 C11 H11 121.2 . . ?
N2 C12 C11 123.4(2) . . ?
N2 C12 H12 118.3 . . ?
C11 C12 H12 118.3 . . ?
C17 N3 C13 118.11(17) . . ?
N3 C13 C14 121.92(18) . . ?
N3 C13 C2 115.07(17) . . ?
C14 C13 C2 122.45(17) . . ?
C15 C14 C13 119.29(18) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C16 C15 C14 118.94(19) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C17 118.03(18) . . ?
C15 C16 H16 121.0 . . ?
C17 C16 H16 121.0 . . ?
N3 C17 C16 123.70(18) . . ?
N3 C17 H17 118.1 . . ?
C16 C17 H17 118.1 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C25 107.98(15) . . ?
C20 C19 C30 108.75(15) . . ?
C25 C19 C30 112.95(16) . . ?
C20 C19 C18 111.27(16) . . ?
C25 C19 C18 111.08(16) . . ?
C30 C19 C18 104.82(15) . . ?
C24 N4 C20 118.56(18) . . ?
C24 N4 Ag1 121.22(14) . . ?
C20 N4 Ag1 119.69(13) . . ?
N4 C20 C21 121.68(19) . . ?
N4 C20 C19 116.08(17) . . ?
C21 C20 C19 122.25(18) . . ?
C22 C21 C20 119.1(2) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C23 C22 C21 119.2(2) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 118.5(2) . . ?
C22 C23 H23 120.8 . . ?
C24 C23 H23 120.8 . . ?
N4 C24 C23 122.8(2) . . ?
N4 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?
C29 N5 C25 119.31(18) . . ?
C29 N5 Ag1 119.38(14) . . ?
C25 N5 Ag1 120.96(12) . . ?
N5 C25 C26 121.13(18) . . ?
N5 C25 C19 116.28(17) . . ?
C26 C25 C19 122.54(18) . . ?
C25 C26 C27 118.9(2) . . ?
C25 C26 H26 120.5 . . ?
C27 C26 H26 120.5 . . ?
C28 C27 C26 119.82(19) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C27 C28 C29 118.00(19) . . ?
C27 C28 H28 121.0 . . ?
C29 C28 H28 121.0 . . ?
N5 C29 C28 122.8(2) . . ?
N5 C29 H29 118.6 . . ?
C28 C29 H29 118.6 . . ?
C34 N6 C30 117.92(17) . . ?
N6 C30 C31 121.97(17) . . ?
N6 C30 C19 114.30(17) . . ?
C31 C30 C19 123.19(17) . . ?
C32 C31 C30 119.14(18) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
C31 C32 C33 119.09(19) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
C34 C33 C32 117.78(18) . . ?
C34 C33 H33 121.1 . . ?
C32 C33 H33 121.1 . . ?
N6 C34 C33 124.08(19) . . ?
N6 C34 H34 118.0 . . ?
C33 C34 H34 118.0 . . ?
O2 N7 O3 120.02(17) . . ?
O2 N7 O1 120.17(17) . . ?
O3 N7 O1 119.81(17) . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        66.60
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.065
_database_code_depnum_ccdc_archive 'CCDC 1023803'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_as173

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 Iodo-[1,1,1-tris(pyrid-2-yl)ethane]copper(I) hemi-acetonitrile 
 solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H15 Cu I N3, 0.5 [C2 H3 N]'
_chemical_formula_sum            'C18 H16.50 Cu I N3.50'
_chemical_formula_weight         472.29

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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   15.7416(2)
_cell_length_b                   12.5216(2)
_cell_length_c                   17.9084(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.3790(10)
_cell_angle_gamma                90.00
_cell_volume                     3523.79(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5238
_cell_measurement_theta_min      4.49
_cell_measurement_theta_max      73.24

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848
_exptl_absorpt_coefficient_mu    15.530
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6112
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.52
_diffrn_reflns_theta_max         66.59
_reflns_number_total             3101
_reflns_number_gt                3067
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains a whole complex molecule, and half a molecule
 of acetonitrile spanning the C₂ axis 0, y, 1/4. No disorder was detected 
 during the refinement, and no restraints were applied. All non-H atoms were
 refined anisotropically, and H atoms were placed in calculated positions 
 and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+39.8512P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3101
_refine_ls_number_parameters     228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0784
_refine_ls_wR_factor_gt          0.0783
_refine_ls_goodness_of_fit_ref   1.353
_refine_ls_restrained_S_all      1.353
_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
Cu1 Cu 0.15444(4) 0.01795(6) 0.36221(4) 0.01355(17) Uani 1 1 d . . .
I1 I 0.071596(18) 0.16974(2) 0.409139(15) 0.01252(10) Uani 1 1 d . . .
C1 C 0.3410(3) -0.2330(4) 0.2847(3) 0.0157(10) Uani 1 1 d . . .
H1A H 0.3742 -0.2624 0.3279 0.023 Uiso 1 1 calc R . .
H1B H 0.3795 -0.1999 0.2504 0.023 Uiso 1 1 calc R . .
H1C H 0.3091 -0.2906 0.2588 0.023 Uiso 1 1 calc R . .
C2 C 0.2787(3) -0.1486(4) 0.3113(3) 0.0110(9) Uani 1 1 d . . .
N1 N 0.2855(3) 0.0251(3) 0.3765(2) 0.0145(8) Uani 1 1 d . . .
C3 C 0.3301(3) -0.0570(4) 0.3503(2) 0.0123(10) Uani 1 1 d . . .
C4 C 0.4188(3) -0.0595(4) 0.3604(3) 0.0187(11) Uani 1 1 d . . .
H4 H 0.4503 -0.1168 0.3410 0.022 Uiso 1 1 calc R . .
C5 C 0.4600(4) 0.0231(5) 0.3991(3) 0.0294(13) Uani 1 1 d . . .
H5 H 0.5203 0.0223 0.4068 0.035 Uiso 1 1 calc R . .
C6 C 0.4136(4) 0.1069(5) 0.4268(3) 0.0282(13) Uani 1 1 d . . .
H6 H 0.4408 0.1640 0.4536 0.034 Uiso 1 1 calc R . .
C7 C 0.3265(3) 0.1041(4) 0.4138(3) 0.0184(11) Uani 1 1 d . . .
H7 H 0.2939 0.1612 0.4322 0.022 Uiso 1 1 calc R . .
N2 N 0.1611(3) -0.0367(3) 0.2548(2) 0.0121(8) Uani 1 1 d . . .
C8 C 0.2235(3) -0.1071(4) 0.2423(3) 0.0100(9) Uani 1 1 d . . .
C9 C 0.2377(3) -0.1410(4) 0.1700(3) 0.0190(11) Uani 1 1 d . . .
H9 H 0.2832 -0.1885 0.1613 0.023 Uiso 1 1 calc R . .
C10 C 0.1845(4) -0.1047(4) 0.1107(3) 0.0219(11) Uani 1 1 d . . .
H10 H 0.1934 -0.1268 0.0611 0.026 Uiso 1 1 calc R . .
C11 C 0.1189(3) -0.0366(4) 0.1246(3) 0.0183(11) Uani 1 1 d . . .
H11 H 0.0807 -0.0126 0.0851 0.022 Uiso 1 1 calc R . .
C12 C 0.1097(3) -0.0037(4) 0.1969(3) 0.0141(10) Uani 1 1 d . . .
H12 H 0.0650 0.0444 0.2064 0.017 Uiso 1 1 calc R . .
N3 N 0.1617(3) -0.1380(3) 0.3981(2) 0.0136(8) Uani 1 1 d . . .
C13 C 0.2208(3) -0.2001(4) 0.3685(3) 0.0130(10) Uani 1 1 d . . .
C14 C 0.2308(4) -0.3059(4) 0.3918(3) 0.0248(12) Uani 1 1 d . . .
H14 H 0.2724 -0.3500 0.3709 0.030 Uiso 1 1 calc R . .
C15 C 0.1799(4) -0.3461(5) 0.4456(4) 0.0311(14) Uani 1 1 d . . .
H15 H 0.1867 -0.4179 0.4621 0.037 Uiso 1 1 calc R . .
C16 C 0.1196(3) -0.2821(5) 0.4749(3) 0.0261(13) Uani 1 1 d . . .
H16 H 0.0840 -0.3086 0.5118 0.031 Uiso 1 1 calc R . .
C17 C 0.1119(3) -0.1783(4) 0.4495(3) 0.0184(11) Uani 1 1 d . . .
H17 H 0.0698 -0.1337 0.4692 0.022 Uiso 1 1 calc R . .
C18 C -0.010(3) -0.2516(14) 0.242(3) 0.052(10) Uani 0.50 1 d P . .
H18A H -0.0272 -0.2201 0.2890 0.079 Uiso 0.50 1 calc PR . .
H18B H -0.0584 -0.2896 0.2176 0.079 Uiso 0.50 1 calc PR . .
H18C H 0.0087 -0.1950 0.2091 0.079 Uiso 0.50 1 calc PR . .
C19 C 0.0594(9) -0.3260(12) 0.2581(6) 0.032(3) Uani 0.50 1 d P . .
N4 N 0.1117(9) -0.3867(11) 0.2694(6) 0.050(3) Uani 0.50 1 d 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
Cu1 N2 2.051(4) . ?
Cu1 N3 2.056(4) . ?
Cu1 N1 2.067(4) . ?
Cu1 I1 2.4796(7) . ?
C1 C2 1.537(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.546(6) . ?
C2 C13 1.551(7) . ?
C2 C8 1.557(6) . ?
N1 C7 1.338(7) . ?
N1 C3 1.344(6) . ?
C3 C4 1.399(7) . ?
C4 C5 1.385(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.378(8) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
N2 C12 1.341(6) . ?
N2 C8 1.348(6) . ?
C8 C9 1.394(7) . ?
C9 C10 1.389(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.373(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.375(7) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N3 C17 1.343(7) . ?
N3 C13 1.346(6) . ?
C13 C14 1.395(7) . ?
C14 C15 1.384(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.371(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(8) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.45(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N4 1.129(18) . ?

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
N2 Cu1 N3 88.35(16) . . ?
N2 Cu1 N1 91.40(16) . . ?
N3 Cu1 N1 88.07(16) . . ?
N2 Cu1 I1 129.11(11) . . ?
N3 Cu1 I1 129.97(12) . . ?
N1 Cu1 I1 117.78(12) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 C3 108.9(4) . . ?
C1 C2 C13 109.2(4) . . ?
C3 C2 C13 108.8(4) . . ?
C1 C2 C8 108.6(4) . . ?
C3 C2 C8 111.3(4) . . ?
C13 C2 C8 109.9(4) . . ?
C7 N1 C3 119.6(4) . . ?
C7 N1 Cu1 122.8(3) . . ?
C3 N1 Cu1 117.5(3) . . ?
N1 C3 C4 120.6(4) . . ?
N1 C3 C2 117.1(4) . . ?
C4 C3 C2 122.3(4) . . ?
C5 C4 C3 118.9(5) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 120.2(5) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C5 117.5(5) . . ?
C7 C6 H6 121.3 . . ?
C5 C6 H6 121.3 . . ?
N1 C7 C6 123.3(5) . . ?
N1 C7 H7 118.4 . . ?
C6 C7 H7 118.4 . . ?
C12 N2 C8 119.1(4) . . ?
C12 N2 Cu1 124.1(3) . . ?
C8 N2 Cu1 116.8(3) . . ?
N2 C8 C9 120.7(4) . . ?
N2 C8 C2 117.7(4) . . ?
C9 C8 C2 121.6(4) . . ?
C10 C9 C8 119.2(5) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C11 C10 C9 119.4(5) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 118.6(5) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
N2 C12 C11 122.9(5) . . ?
N2 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
C17 N3 C13 119.9(4) . . ?
C17 N3 Cu1 123.2(3) . . ?
C13 N3 Cu1 116.9(3) . . ?
N3 C13 C14 120.0(5) . . ?
N3 C13 C2 117.8(4) . . ?
C14 C13 C2 122.1(5) . . ?
C15 C14 C13 119.6(5) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C16 C15 C14 119.8(5) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 118.2(5) . . ?
C15 C16 H16 120.9 . . ?
C17 C16 H16 120.9 . . ?
N3 C17 C16 122.5(5) . . ?
N3 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 C18 178(2) . . ?


_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        66.59
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.111
_database_code_depnum_ccdc_archive 'CCDC 1023804'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_as172g

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 Bis[iodo/hydroxo(carbonato)-bis-{1,1,1-tris(pyrid-2-yl)ethane}-
 dicopper(II)] triiodocuprate(I) tetrakis-dimethylformamide solvate 
 hydrate (2/0.4)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2[C35 H30.56 Cu2 I0.44 N16 O3.56], [Cu I3], 0.4[H2 O], 4[C3 H7 N O]'
_chemical_formula_sum            'C82 H89.92 Cu5 I3.88 N16 O11.52'
_chemical_formula_weight         2294.01

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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   38.0784(10)
_cell_length_b                   12.2951(3)
_cell_length_c                   20.3333(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.027(2)
_cell_angle_gamma                90.00
_cell_volume                     8554.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3794
_cell_measurement_theta_min      4.3460
_cell_measurement_theta_max      73.0110

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4547
_exptl_absorpt_coefficient_mu    12.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            13120
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.82
_diffrn_reflns_theta_max         66.63
_reflns_number_total             7472
_reflns_number_gt                5689
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains half a formula unit, with the [CuI₃]²⁻ ion
 lying on the C₂ axis 1, y, 3/4. One coordination site of Cu1 is occupied
 by a disordered mixture of iodide (I1) and an oxygen ligand (O1), either 
 hydroxide or water (hydroxide was assumed during the refinement). The 
 relative occupancies of these two fragments were refined to 0.44 and 0.56 
 respectively, but the Fourier hole of -2.8 e.Å⁻³ near I1 implies that 
 its occupancy may have been slightly over-estimated. 

 In addition to two ordered dmf molecules, a weak Fourier peak that is not 
 associated with any other fragment was included in the model as 0.2 equiv
 of water. This peak is within hydrogen bonding distance of two different 
 carbonato ligands (O4...O7 = 2.82 and O4...O3ⁱ = 2.81 Å; symmetry 
 code (i) = 1.5-x, -0.5+y, 0.5-z).

 No restraints were applied to the model during the final least squares 
 cycles. All wholly occupied non-H atoms were refined anisotropically, 
 while H atoms were placed in calculated positions and refined using a 
 riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0440P)²+46.3041P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7472
_refine_ls_number_parameters     543
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.1127
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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
Cu1 Cu 0.70440(2) 0.44394(7) 0.37447(5) 0.01720(19) Uani 1 1 d . . .
I1 I 0.76021(4) 0.49417(10) 0.49449(8) 0.0332(3) Uiso 0.44 1 d P A 1
O1 O 0.7519(3) 0.4808(7) 0.4691(5) 0.019(2) Uiso 0.56 1 d P A 2
C1 C 0.56949(18) 0.3959(6) 0.2829(4) 0.0244(14) Uani 1 1 d . . .
H1A H 0.5641 0.3177 0.2788 0.037 Uiso 1 1 calc R . .
H1B H 0.5561 0.4298 0.2345 0.037 Uiso 1 1 calc R . .
H1C H 0.5601 0.4286 0.3162 0.037 Uiso 1 1 calc R . .
C2 C 0.61371(18) 0.4145(5) 0.3131(3) 0.0175(12) Uani 1 1 d . A .
N1 N 0.66758(15) 0.3618(4) 0.2821(3) 0.0190(11) Uani 1 1 d . A .
C3 C 0.62884(19) 0.3622(5) 0.2609(3) 0.0204(13) Uani 1 1 d . . .
C4 C 0.6037(2) 0.3131(5) 0.1956(4) 0.0235(13) Uani 1 1 d . A .
H4 H 0.5762 0.3160 0.1795 0.028 Uiso 1 1 calc R . .
C5 C 0.6193(2) 0.2595(5) 0.1539(4) 0.0294(15) Uani 1 1 d . . .
H5 H 0.6025 0.2247 0.1094 0.035 Uiso 1 1 calc R A .
C6 C 0.6593(2) 0.2570(6) 0.1773(4) 0.0308(16) Uani 1 1 d . A .
H6 H 0.6704 0.2197 0.1501 0.037 Uiso 1 1 calc R . .
C7 C 0.6825(2) 0.3104(5) 0.2414(4) 0.0260(15) Uani 1 1 d . . .
H7 H 0.7100 0.3110 0.2575 0.031 Uiso 1 1 calc R A .
N2 N 0.67519(15) 0.3613(4) 0.4211(3) 0.0179(11) Uani 1 1 d . A .
C8 C 0.63566(18) 0.3591(5) 0.3884(3) 0.0170(12) Uani 1 1 d . . .
C9 C 0.61564(19) 0.3029(5) 0.4211(4) 0.0217(13) Uani 1 1 d . A .
H9 H 0.5879 0.3025 0.3986 0.026 Uiso 1 1 calc R . .
C10 C 0.6361(2) 0.2478(5) 0.4862(4) 0.0271(15) Uani 1 1 d . . .
H10 H 0.6224 0.2108 0.5090 0.032 Uiso 1 1 calc R A .
C11 C 0.6762(2) 0.2470(6) 0.5176(4) 0.0294(15) Uani 1 1 d . A .
H11 H 0.6908 0.2071 0.5611 0.035 Uiso 1 1 calc R . .
C12 C 0.6946(2) 0.3062(5) 0.4837(4) 0.0244(14) Uani 1 1 d . . .
H12 H 0.7224 0.3079 0.5059 0.029 Uiso 1 1 calc R A .
N3 N 0.65978(14) 0.5669(4) 0.3458(3) 0.0146(10) Uani 1 1 d . A .
C13 C 0.62234(17) 0.5385(5) 0.3205(3) 0.0145(12) Uani 1 1 d . . .
C14 C 0.59317(19) 0.6171(6) 0.3015(3) 0.0232(14) Uani 1 1 d . A .
H14 H 0.5665 0.5964 0.2838 0.028 Uiso 1 1 calc R . .
C15 C 0.6036(2) 0.7262(5) 0.3089(4) 0.0239(14) Uani 1 1 d . . .
H15 H 0.5841 0.7807 0.2970 0.029 Uiso 1 1 calc R A .
C16 C 0.64269(19) 0.7558(5) 0.3338(3) 0.0209(13) Uani 1 1 d . A .
H16 H 0.6504 0.8300 0.3382 0.025 Uiso 1 1 calc R . .
C17 C 0.66964(18) 0.6725(5) 0.3517(3) 0.0187(13) Uani 1 1 d . . .
H17 H 0.6965 0.6909 0.3691 0.022 Uiso 1 1 calc R A .
Cu2 Cu 0.81422(2) 0.43891(7) 0.30395(5) 0.01530(19) Uani 1 1 d . . .
C18 C 0.94903(18) 0.4033(5) 0.3943(4) 0.0228(14) Uani 1 1 d . . .
H18A H 0.9538 0.3650 0.3567 0.034 Uiso 1 1 calc R . .
H18B H 0.9599 0.3609 0.4397 0.034 Uiso 1 1 calc R . .
H18C H 0.9616 0.4748 0.4032 0.034 Uiso 1 1 calc R . .
C19 C 0.90483(18) 0.4178(5) 0.3680(3) 0.0181(13) Uani 1 1 d . . .
N4 N 0.84510(15) 0.3022(4) 0.3238(3) 0.0176(10) Uani 1 1 d . . .
C20 C 0.88434(18) 0.3049(5) 0.3540(3) 0.0161(12) Uani 1 1 d . . .
C21 C 0.9056(2) 0.2086(5) 0.3713(4) 0.0218(14) Uani 1 1 d . . .
H21 H 0.9334 0.2100 0.3944 0.026 Uiso 1 1 calc R . .
C22 C 0.8855(2) 0.1097(5) 0.3541(4) 0.0275(15) Uani 1 1 d . . .
H22 H 0.8996 0.0431 0.3638 0.033 Uiso 1 1 calc R . .
C23 C 0.8456(2) 0.1088(5) 0.3233(4) 0.0252(14) Uani 1 1 d . . .
H23 H 0.8316 0.0420 0.3126 0.030 Uiso 1 1 calc R . .
C24 C 0.82600(18) 0.2073(5) 0.3079(3) 0.0177(12) Uani 1 1 d . . .
H24 H 0.7982 0.2074 0.2854 0.021 Uiso 1 1 calc R . .
N5 N 0.84841(14) 0.5011(4) 0.2625(3) 0.0159(10) Uani 1 1 d . . .
C25 C 0.88741(17) 0.4824(5) 0.2950(3) 0.0145(11) Uani 1 1 d . . .
C26 C 0.91033(18) 0.5174(5) 0.2615(4) 0.0203(13) Uani 1 1 d . . .
H26 H 0.9377 0.5049 0.2843 0.024 Uiso 1 1 calc R . .
C27 C 0.8930(2) 0.5707(5) 0.1946(4) 0.0225(14) Uani 1 1 d . . .
H27 H 0.9085 0.5937 0.1711 0.027 Uiso 1 1 calc R . .
C28 C 0.85349(19) 0.5901(5) 0.1625(4) 0.0219(13) Uani 1 1 d . . .
H28 H 0.8411 0.6272 0.1171 0.026 Uiso 1 1 calc R . .
C29 C 0.83214(18) 0.5535(5) 0.1990(3) 0.0169(12) Uani 1 1 d . . .
H29 H 0.8048 0.5665 0.1775 0.020 Uiso 1 1 calc R . .
N6 N 0.85979(14) 0.4908(4) 0.4139(3) 0.0161(10) Uani 1 1 d . . .
C30 C 0.89731(17) 0.4798(5) 0.4270(3) 0.0156(12) Uani 1 1 d . . .
C31 C 0.92731(19) 0.5187(6) 0.4907(3) 0.0253(14) Uani 1 1 d . . .
H31 H 0.9537 0.5123 0.4986 0.030 Uiso 1 1 calc R . .
C32 C 0.9181(2) 0.5671(6) 0.5427(4) 0.0319(16) Uani 1 1 d . . .
H32 H 0.9383 0.5935 0.5872 0.038 Uiso 1 1 calc R . .
C33 C 0.8797(2) 0.5766(6) 0.5296(4) 0.0287(15) Uani 1 1 d . . .
H33 H 0.8729 0.6101 0.5645 0.034 Uiso 1 1 calc R . .
C34 C 0.8512(2) 0.5366(5) 0.4647(3) 0.0226(14) Uani 1 1 d . . .
H34 H 0.8246 0.5418 0.4558 0.027 Uiso 1 1 calc R . .
C35 C 0.75728(16) 0.4932(5) 0.3137(3) 0.0166(12) Uani 1 1 d . . .
O2 O 0.72723(12) 0.5233(4) 0.3198(2) 0.0228(10) Uani 1 1 d . A .
O3 O 0.77551(12) 0.5570(3) 0.2887(2) 0.0186(9) Uani 1 1 d . A .
O4 O 0.77241(12) 0.3965(3) 0.3330(2) 0.0188(9) Uani 1 1 d . A .
Cu3 Cu 1.0000 0.41171(11) 0.7500 0.0252(3) Uani 1 2 d S . .
I2 I 0.991367(12) 0.31432(3) 0.63333(2) 0.02602(12) Uani 1 1 d . . .
I3 I 1.0000 0.62204(5) 0.7500 0.01993(13) Uani 1 2 d S . .
O5 O 0.77272(13) 0.3632(4) 0.1801(3) 0.0295(11) Uani 1 1 d . . .
C36 C 0.7407(2) 0.4082(6) 0.1446(4) 0.0325(17) Uani 1 1 d . . .
H36 H 0.7369 0.4789 0.1592 0.039 Uiso 1 1 calc R . .
N7 N 0.71134(15) 0.3628(5) 0.0872(3) 0.0231(11) Uani 1 1 d . . .
C37 C 0.7175(2) 0.2598(6) 0.0605(4) 0.0399(18) Uani 1 1 d . . .
H37A H 0.7325 0.2708 0.0322 0.060 Uiso 1 1 calc R . .
H37B H 0.6922 0.2268 0.0291 0.060 Uiso 1 1 calc R . .
H37C H 0.7321 0.2115 0.1020 0.060 Uiso 1 1 calc R . .
C38 C 0.6759(2) 0.4224(7) 0.0421(4) 0.0363(17) Uani 1 1 d . . .
H38A H 0.6767 0.4942 0.0637 0.055 Uiso 1 1 calc R . .
H38B H 0.6532 0.3820 0.0395 0.055 Uiso 1 1 calc R . .
H38C H 0.6740 0.4311 -0.0072 0.055 Uiso 1 1 calc R . .
O6 O 1.03258(19) 0.9888(7) 0.6052(5) 0.083(3) Uani 1 1 d . . .
C39 C 0.9976(3) 1.0107(8) 0.5781(5) 0.055(2) Uani 1 1 d . . .
H39 H 0.9903 1.0843 0.5650 0.066 Uiso 1 1 calc R . .
N8 N 0.9690(2) 0.9392(6) 0.5656(4) 0.0437(16) Uani 1 1 d . . .
C40 C 0.9773(4) 0.8270(11) 0.5814(11) 0.126(7) Uani 1 1 d . . .
H40A H 0.9793 0.7914 0.5402 0.190 Uiso 1 1 calc R . .
H40B H 0.9561 0.7933 0.5894 0.190 Uiso 1 1 calc R . .
H40C H 1.0020 0.8190 0.6256 0.190 Uiso 1 1 calc R . .
C41 C 0.9287(2) 0.9710(9) 0.5268(5) 0.053(2) Uani 1 1 d . . .
H41A H 0.9272 1.0488 0.5155 0.079 Uiso 1 1 calc R . .
H41B H 0.9152 0.9564 0.5573 0.079 Uiso 1 1 calc R . .
H41C H 0.9163 0.9294 0.4812 0.079 Uiso 1 1 calc R . .
O7 O 0.7499(9) 0.180(3) 0.3403(17) 0.053(8) Uiso 0.20 1 d 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
Cu1 O2 1.947(4) . ?
Cu1 N2 2.024(5) . ?
Cu1 O1 2.031(10) . ?
Cu1 N1 2.050(5) . ?
Cu1 N3 2.155(5) . ?
Cu1 I1 2.5102(17) . ?
C1 C2 1.535(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C8 1.545(9) . ?
C2 C3 1.552(8) . ?
C2 C13 1.553(8) . ?
N1 C3 1.343(8) . ?
N1 C7 1.348(8) . ?
C3 C4 1.389(9) . ?
C4 C5 1.396(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.379(10) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
N2 C12 1.341(8) . ?
N2 C8 1.353(8) . ?
C8 C9 1.395(8) . ?
C9 C10 1.383(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.372(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(9) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N3 C13 1.332(8) . ?
N3 C17 1.343(8) . ?
C13 C14 1.393(9) . ?
C14 C15 1.388(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.393(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.380(9) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
Cu2 N4 1.988(5) . ?
Cu2 N5 1.988(5) . ?
Cu2 O3 1.994(4) . ?
Cu2 O4 1.996(4) . ?
Cu2 N6 2.239(5) . ?
C18 C19 1.536(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C30 1.549(8) . ?
C19 C25 1.553(8) . ?
C19 C20 1.556(8) . ?
N4 C24 1.338(8) . ?
N4 C20 1.343(8) . ?
C20 C21 1.390(8) . ?
C21 C22 1.397(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.366(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.385(9) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
N5 C29 1.328(8) . ?
N5 C25 1.354(8) . ?
C25 C26 1.390(8) . ?
C26 C27 1.388(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.373(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.393(8) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
N6 C34 1.336(8) . ?
N6 C30 1.341(8) . ?
C30 C31 1.383(9) . ?
C31 C32 1.387(10) . ?
C31 H31 0.9500 . ?
C32 C33 1.371(11) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(10) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 O2 1.259(7) . ?
C35 O3 1.290(7) . ?
C35 O4 1.305(7) . ?
Cu3 I2 2.5466(8) . ?
Cu3 I3 2.5861(15) . ?
O5 C36 1.242(9) . ?
C36 H36 0.9500 . ?
C36 N7 1.333(9) . ?
N7 C37 1.438(9) . ?
N7 C38 1.452(9) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O6 C39 1.227(11) . ?
C39 H39 0.9500 . ?
C39 N8 1.334(12) . ?
N8 C40 1.419(14) . ?
N8 C41 1.438(10) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 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
O2 Cu1 N2 173.8(2) . . ?
O2 Cu1 O1 89.6(3) . . ?
N2 Cu1 O1 96.5(3) . . ?
O2 Cu1 N1 91.17(19) . . ?
N2 Cu1 N1 83.5(2) . . ?
O1 Cu1 N1 160.8(3) . . ?
O2 Cu1 N3 89.48(18) . . ?
N2 Cu1 N3 87.06(19) . . ?
O1 Cu1 N3 111.7(3) . . ?
N1 Cu1 N3 87.5(2) . . ?
O2 Cu1 I1 91.85(14) . . ?
N2 Cu1 I1 94.17(15) . . ?
N1 Cu1 I1 163.50(15) . . ?
N3 Cu1 I1 108.73(14) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 C8 110.6(5) . . ?
C1 C2 C3 109.7(5) . . ?
C8 C2 C3 107.1(5) . . ?
C1 C2 C13 109.4(5) . . ?
C8 C2 C13 109.7(5) . . ?
C3 C2 C13 110.3(5) . . ?
C3 N1 C7 120.3(6) . . ?
C3 N1 Cu1 120.3(4) . . ?
C7 N1 Cu1 119.3(4) . . ?
N1 C3 C4 120.3(6) . . ?
N1 C3 C2 117.9(6) . . ?
C4 C3 C2 121.8(6) . . ?
C3 C4 C5 119.1(6) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C6 C5 C4 120.0(7) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C7 C6 C5 118.0(6) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
N1 C7 C6 122.3(7) . . ?
N1 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C12 N2 C8 119.2(5) . . ?
C12 N2 Cu1 120.7(4) . . ?
C8 N2 Cu1 120.1(4) . . ?
N2 C8 C9 119.9(6) . . ?
N2 C8 C2 118.7(5) . . ?
C9 C8 C2 121.3(6) . . ?
C10 C9 C8 120.2(6) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 119.5(6) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 118.0(6) . . ?
C10 C11 H11 121.0 . . ?
C12 C11 H11 121.0 . . ?
N2 C12 C11 123.1(6) . . ?
N2 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
C13 N3 C17 119.8(5) . . ?
C13 N3 Cu1 120.3(4) . . ?
C17 N3 Cu1 119.9(4) . . ?
N3 C13 C14 120.9(5) . . ?
N3 C13 C2 116.1(5) . . ?
C14 C13 C2 123.1(6) . . ?
C15 C14 C13 119.0(6) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C16 120.1(6) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 117.0(6) . . ?
C17 C16 H16 121.5 . . ?
C15 C16 H16 121.5 . . ?
N3 C17 C16 123.2(6) . . ?
N3 C17 H17 118.4 . . ?
C16 C17 H17 118.4 . . ?
N4 Cu2 N5 88.4(2) . . ?
N4 Cu2 O3 167.98(18) . . ?
N5 Cu2 O3 103.35(18) . . ?
N4 Cu2 O4 101.36(18) . . ?
N5 Cu2 O4 169.12(19) . . ?
O3 Cu2 O4 66.72(16) . . ?
N4 Cu2 N6 84.7(2) . . ?
N5 Cu2 N6 87.08(19) . . ?
O3 Cu2 N6 98.27(18) . . ?
O4 Cu2 N6 98.50(17) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C18 C19 C30 109.5(5) . . ?
C18 C19 C25 109.6(5) . . ?
C30 C19 C25 110.0(5) . . ?
C18 C19 C20 110.2(5) . . ?
C30 C19 C20 109.4(4) . . ?
C25 C19 C20 108.1(5) . . ?
C24 N4 C20 120.6(5) . . ?
C24 N4 Cu2 118.6(4) . . ?
C20 N4 Cu2 120.8(4) . . ?
N4 C20 C21 120.2(6) . . ?
N4 C20 C19 118.2(5) . . ?
C21 C20 C19 121.6(5) . . ?
C20 C21 C22 118.9(6) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
C23 C22 C21 119.9(6) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 118.5(6) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
N4 C24 C23 121.8(6) . . ?
N4 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C29 N5 C25 120.0(5) . . ?
C29 N5 Cu2 119.1(4) . . ?
C25 N5 Cu2 120.6(4) . . ?
N5 C25 C26 119.9(5) . . ?
N5 C25 C19 118.1(5) . . ?
C26 C25 C19 122.0(5) . . ?
C27 C26 C25 119.7(6) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C26 119.9(6) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C27 C28 C29 117.7(6) . . ?
C27 C28 H28 121.2 . . ?
C29 C28 H28 121.2 . . ?
N5 C29 C28 122.8(6) . . ?
N5 C29 H29 118.6 . . ?
C28 C29 H29 118.6 . . ?
C34 N6 C30 119.4(5) . . ?
C34 N6 Cu2 123.1(4) . . ?
C30 N6 Cu2 117.4(4) . . ?
N6 C30 C31 121.4(5) . . ?
N6 C30 C19 116.1(5) . . ?
C31 C30 C19 122.5(5) . . ?
C30 C31 C32 118.8(6) . . ?
C30 C31 H31 120.6 . . ?
C32 C31 H31 120.6 . . ?
C33 C32 C31 119.5(7) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C32 C33 C34 118.7(6) . . ?
C32 C33 H33 120.7 . . ?
C34 C33 H33 120.7 . . ?
N6 C34 C33 122.2(6) . . ?
N6 C34 H34 118.9 . . ?
C33 C34 H34 118.9 . . ?
O2 C35 O3 122.0(6) . . ?
O2 C35 O4 122.6(5) . . ?
O3 C35 O4 115.4(5) . . ?
C35 O2 Cu1 124.2(4) . . ?
C35 O3 Cu2 89.1(3) . . ?
C35 O4 Cu2 88.7(3) . . ?
I2 Cu3 I2 123.90(6) 2_756 . ?
I2 Cu3 I3 118.05(3) 2_756 . ?
I2 Cu3 I3 118.05(3) . . ?
O5 C36 N7 123.7(7) . . ?
O5 C36 H36 118.2 . . ?
N7 C36 H36 118.2 . . ?
C36 N7 C37 119.1(6) . . ?
C36 N7 C38 122.1(6) . . ?
C37 N7 C38 117.8(6) . . ?
N7 C37 H37A 109.5 . . ?
N7 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N7 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N7 C38 H38A 109.5 . . ?
N7 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N7 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O6 C39 N8 125.0(10) . . ?
O6 C39 H39 117.5 . . ?
N8 C39 H39 117.5 . . ?
C39 N8 C40 121.2(9) . . ?
C39 N8 C41 120.7(8) . . ?
C40 N8 C41 117.7(9) . . ?
N8 C40 H40A 109.5 . . ?
N8 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N8 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N8 C41 H41A 109.5 . . ?
N8 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N8 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        66.63
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.892
_refine_diff_density_min         -2.841
_refine_diff_density_rms         0.138
_database_code_depnum_ccdc_archive 'CCDC 1023805'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_as172260

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Carbonato-[1,1,1-tris(pyrid-2-yl)ethane]copper(II) hydrate 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H15 Cu N3 O3, 4.25[H2 O]'
_chemical_formula_sum            'C18 H23.50 Cu N3 O7.25'
_chemical_formula_weight         461.44

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'

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

_cell_length_a                   10.6195(3)
_cell_length_b                   25.6995(7)
_cell_length_c                   14.7591(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.014(3)
_cell_angle_gamma                90.00
_cell_volume                     3924.53(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9714
_cell_measurement_theta_min      3.44
_cell_measurement_theta_max      27.03

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1916
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            26458
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.73
_reflns_number_total             13638
_reflns_number_gt                12148
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains four formula units; that is, four unique 
 complex molecules and seventeen water molecules. No disorder is present 
 in the model, and no restraints were applied. All non-H atoms are refined 
 anisotropically, and C-bound H atoms were placed in calculated positions 
 and refined using a riding model. The water H atoms were all located in
 the Fourier map and allowed to refine, subject to the fixed restraints 
 O---H = 0.90(2) and H...H = 1.47(2) Å, and with Uiso equal to
 1.5xUeq for the corresponding O atom. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0265P)²+2.2643P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(8)
_refine_ls_number_reflns         13638
_refine_ls_number_parameters     1160
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.0859
_refine_ls_wR_factor_gt          0.0794
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.046
_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
Cu1 Cu 0.38680(5) 0.346660(19) 0.68307(3) 0.01320(11) Uani 1 1 d . . .
C1 C -0.0472(4) 0.36009(17) 0.6805(3) 0.0185(10) Uani 1 1 d . . .
H1A H -0.0667 0.3434 0.7354 0.028 Uiso 1 1 calc R . .
H1B H -0.0997 0.3442 0.6241 0.028 Uiso 1 1 calc R . .
H1C H -0.0669 0.3973 0.6813 0.028 Uiso 1 1 calc R . .
C2 C 0.0957(4) 0.35288(16) 0.6816(3) 0.0133(9) Uani 1 1 d . . .
N1 N 0.3096(3) 0.37435(13) 0.7835(2) 0.0131(8) Uani 1 1 d . . .
C3 C 0.1802(4) 0.37469(16) 0.7735(3) 0.0139(9) Uani 1 1 d . . .
C4 C 0.1272(4) 0.39087(16) 0.8459(3) 0.0141(9) Uani 1 1 d . . .
H4 H 0.0360 0.3915 0.8386 0.017 Uiso 1 1 calc R . .
C5 C 0.2072(4) 0.40619(17) 0.9290(3) 0.0173(9) Uani 1 1 d . . .
H5 H 0.1708 0.4176 0.9788 0.021 Uiso 1 1 calc R . .
C6 C 0.3382(4) 0.40492(16) 0.9397(3) 0.0152(9) Uani 1 1 d . . .
H6 H 0.3945 0.4148 0.9966 0.018 Uiso 1 1 calc R . .
C7 C 0.3861(4) 0.38872(16) 0.8645(3) 0.0146(9) Uani 1 1 d . . .
H7 H 0.4771 0.3878 0.8707 0.018 Uiso 1 1 calc R . .
N2 N 0.2519(3) 0.38204(13) 0.5893(2) 0.0141(8) Uani 1 1 d . . .
C8 C 0.1275(4) 0.37979(16) 0.5944(3) 0.0142(9) Uani 1 1 d . . .
C9 C 0.0312(4) 0.40019(17) 0.5231(3) 0.0183(10) Uani 1 1 d . . .
H9 H -0.0568 0.3983 0.5269 0.022 Uiso 1 1 calc R . .
C10 C 0.0640(5) 0.42308(17) 0.4470(3) 0.0229(11) Uani 1 1 d . . .
H10 H -0.0013 0.4364 0.3975 0.027 Uiso 1 1 calc R . .
C11 C 0.1929(4) 0.42649(17) 0.4435(3) 0.0198(10) Uani 1 1 d . . .
H11 H 0.2181 0.4431 0.3928 0.024 Uiso 1 1 calc R . .
C12 C 0.2835(4) 0.40522(17) 0.5153(3) 0.0172(10) Uani 1 1 d . . .
H12 H 0.3720 0.4069 0.5129 0.021 Uiso 1 1 calc R . .
N3 N 0.2509(3) 0.28197(14) 0.6798(2) 0.0140(8) Uani 1 1 d . . .
C13 C 0.1292(4) 0.29390(17) 0.6795(3) 0.0142(9) Uani 1 1 d . . .
C14 C 0.0368(4) 0.25531(17) 0.6818(3) 0.0156(9) Uani 1 1 d . . .
H14 H -0.0507 0.2643 0.6795 0.019 Uiso 1 1 calc R . .
C15 C 0.0757(4) 0.20375(18) 0.6876(3) 0.0186(10) Uani 1 1 d . . .
H15 H 0.0153 0.1770 0.6912 0.022 Uiso 1 1 calc R . .
C16 C 0.2028(5) 0.19116(18) 0.6883(3) 0.0206(10) Uani 1 1 d . . .
H16 H 0.2308 0.1560 0.6918 0.025 Uiso 1 1 calc R . .
C17 C 0.2878(5) 0.23148(17) 0.6836(3) 0.0185(10) Uani 1 1 d . . .
H17 H 0.3749 0.2234 0.6831 0.022 Uiso 1 1 calc R . .
C18 C 0.5896(4) 0.31160(17) 0.6767(3) 0.0148(9) Uani 1 1 d . . .
O1 O 0.5521(3) 0.31935(11) 0.75565(19) 0.0180(7) Uani 1 1 d . . .
O2 O 0.5048(3) 0.32817(12) 0.60476(19) 0.0171(7) Uani 1 1 d . . .
O3 O 0.6943(3) 0.29000(12) 0.6728(2) 0.0191(7) Uani 1 1 d . . .
Cu2 Cu 0.43558(5) 0.53141(2) 0.86105(4) 0.01664(12) Uani 1 1 d . A 2
C19 C 0.3716(4) 0.56269(18) 0.5449(3) 0.0183(10) Uani 1 1 d . A 2
H19A H 0.4525 0.5752 0.5313 0.027 Uiso 1 1 calc R A 2
H19B H 0.3036 0.5887 0.5247 0.027 Uiso 1 1 calc R A 2
H19C H 0.3464 0.5300 0.5117 0.027 Uiso 1 1 calc R A 2
C20 C 0.3909(4) 0.55355(17) 0.6501(3) 0.0141(9) Uani 1 1 d . A 2
N4 N 0.5310(3) 0.50113(14) 0.7736(2) 0.0149(8) Uani 1 1 d . A 2
C21 C 0.4988(4) 0.51323(16) 0.6821(3) 0.0154(9) Uani 1 1 d . A 2
C22 C 0.5605(4) 0.48876(18) 0.6216(3) 0.0209(10) Uani 1 1 d . A 2
H22 H 0.5390 0.4977 0.5575 0.025 Uiso 1 1 calc R A 2
C23 C 0.6545(4) 0.45075(19) 0.6530(3) 0.0227(11) Uani 1 1 d . A 2
H23 H 0.6948 0.4330 0.6107 0.027 Uiso 1 1 calc R A 2
C24 C 0.6872(4) 0.43974(17) 0.7466(3) 0.0206(10) Uani 1 1 d . A 2
H24 H 0.7522 0.4147 0.7702 0.025 Uiso 1 1 calc R A 2
C25 C 0.6250(4) 0.46528(17) 0.8053(3) 0.0176(10) Uani 1 1 d . A 2
H25 H 0.6480 0.4578 0.8700 0.021 Uiso 1 1 calc R A 2
N5 N 0.2663(3) 0.52430(14) 0.7632(2) 0.0138(8) Uani 1 1 d . A 2
C26 C 0.2638(4) 0.53385(16) 0.6723(3) 0.0135(9) Uani 1 1 d . A 2
C27 C 0.1501(4) 0.52854(17) 0.6053(3) 0.0161(9) Uani 1 1 d . A 2
H27 H 0.1497 0.5341 0.5416 0.019 Uiso 1 1 calc R A 2
C28 C 0.0372(4) 0.51504(16) 0.6314(3) 0.0177(10) Uani 1 1 d . A 2
H28 H -0.0411 0.5114 0.5857 0.021 Uiso 1 1 calc R A 2
C29 C 0.0390(4) 0.50692(17) 0.7242(3) 0.0199(10) Uani 1 1 d . A 2
H29 H -0.0376 0.4986 0.7441 0.024 Uiso 1 1 calc R A 2
C30 C 0.1574(4) 0.51144(16) 0.7872(3) 0.0156(9) Uani 1 1 d . A 2
H30 H 0.1605 0.5050 0.8510 0.019 Uiso 1 1 calc R A 2
N6 N 0.4474(3) 0.60501(14) 0.7958(2) 0.0158(8) Uani 1 1 d . A 2
C31 C 0.4241(4) 0.60672(17) 0.7024(3) 0.0160(9) Uani 1 1 d . A 2
C32 C 0.4210(4) 0.65341(17) 0.6560(3) 0.0185(10) Uani 1 1 d . A 2
H32 H 0.4049 0.6540 0.5901 0.022 Uiso 1 1 calc R A 2
C33 C 0.4414(4) 0.69953(18) 0.7063(3) 0.0217(10) Uani 1 1 d . A 2
H33 H 0.4407 0.7319 0.6750 0.026 Uiso 1 1 calc R A 2
C34 C 0.4627(4) 0.69802(18) 0.8018(3) 0.0213(10) Uani 1 1 d . A 2
H34 H 0.4749 0.7290 0.8378 0.026 Uiso 1 1 calc R A 2
C35 C 0.4659(4) 0.64944(17) 0.8437(3) 0.0177(10) Uani 1 1 d . A 2
H35 H 0.4819 0.6478 0.9096 0.021 Uiso 1 1 calc R A 2
C36 C 0.4600(4) 0.52083(17) 1.0238(3) 0.0184(10) Uani 1 1 d . A 2
O4 O 0.5467(3) 0.50548(13) 0.9793(2) 0.0207(7) Uani 1 1 d . A 2
O5 O 0.3632(3) 0.54532(12) 0.9693(2) 0.0224(7) Uani 1 1 d . A 2
O6 O 0.4667(3) 0.51182(11) 1.1075(2) 0.0200(7) Uani 1 1 d . A 2
Cu3 Cu 1.04578(5) 0.707000(19) 1.57233(3) 0.01457(12) Uani 1 1 d . B 3
C37 C 1.0566(4) 0.83392(18) 1.7946(3) 0.0187(10) Uani 1 1 d . B 3
H37A H 1.1438 0.8366 1.8343 0.028 Uiso 1 1 calc R B 3
H37B H 0.9947 0.8263 1.8331 0.028 Uiso 1 1 calc R B 3
H37C H 1.0336 0.8669 1.7617 0.028 Uiso 1 1 calc R B 3
C38 C 1.0531(4) 0.78998(16) 1.7236(3) 0.0148(9) Uani 1 1 d . B 3
N7 N 1.1482(3) 0.77201(14) 1.5892(2) 0.0149(8) Uani 1 1 d . B 3
C39 C 1.1473(4) 0.80386(16) 1.6618(3) 0.0138(9) Uani 1 1 d . B 3
C40 C 1.2291(4) 0.84653(18) 1.6783(3) 0.0177(9) Uani 1 1 d . B 3
H40 H 1.2296 0.8686 1.7299 0.021 Uiso 1 1 calc R B 3
C41 C 1.3101(4) 0.85671(18) 1.6188(3) 0.0193(10) Uani 1 1 d . B 3
H41 H 1.3659 0.8860 1.6294 0.023 Uiso 1 1 calc R B 3
C42 C 1.3099(4) 0.82412(18) 1.5439(3) 0.0184(10) Uani 1 1 d . B 3
H42 H 1.3650 0.8304 1.5025 0.022 Uiso 1 1 calc R B 3
C43 C 1.2269(4) 0.78253(17) 1.5320(3) 0.0164(9) Uani 1 1 d . B 3
H43 H 1.2249 0.7600 1.4806 0.020 Uiso 1 1 calc R B 3
C44 C 0.9143(4) 0.78322(16) 1.6644(3) 0.0145(9) Uani 1 1 d . B 3
N8 N 0.8942(3) 0.74619(15) 1.5992(2) 0.0150(8) Uani 1 1 d . B 3
C45 C 0.8111(4) 0.81251(17) 1.6801(3) 0.0186(10) Uani 1 1 d . B 3
H45 H 0.8247 0.8393 1.7257 0.022 Uiso 1 1 calc R B 3
C46 C 0.6870(5) 0.8018(2) 1.6274(3) 0.0256(11) Uani 1 1 d . B 3
H46 H 0.6158 0.8217 1.6371 0.031 Uiso 1 1 calc R B 3
C47 C 0.6667(4) 0.76302(18) 1.5622(3) 0.0225(11) Uani 1 1 d . B 3
H47 H 0.5825 0.7550 1.5269 0.027 Uiso 1 1 calc R B 3
C48 C 0.7747(4) 0.73600(19) 1.5498(3) 0.0207(10) Uani 1 1 d . B 3
H48 H 0.7634 0.7092 1.5044 0.025 Uiso 1 1 calc R B 3
N9 N 1.0975(3) 0.69588(13) 1.7223(2) 0.0131(8) Uani 1 1 d . B 3
C49 C 1.0939(4) 0.73821(16) 1.7762(3) 0.0128(9) Uani 1 1 d . B 3
C50 C 1.1224(4) 0.73428(18) 1.8726(3) 0.0153(9) Uani 1 1 d . B 3
H50 H 1.1219 0.7643 1.9100 0.018 Uiso 1 1 calc R B 3
C51 C 1.1514(4) 0.68579(18) 1.9135(3) 0.0206(11) Uani 1 1 d . B 3
H51 H 1.1705 0.6825 1.9793 0.025 Uiso 1 1 calc R B 3
C52 C 1.1527(4) 0.64267(18) 1.8592(3) 0.0200(10) Uani 1 1 d . B 3
H52 H 1.1719 0.6092 1.8861 0.024 Uiso 1 1 calc R B 3
C53 C 1.1248(4) 0.64963(18) 1.7627(3) 0.0180(10) Uani 1 1 d . B 3
H53 H 1.1253 0.6200 1.7243 0.022 Uiso 1 1 calc R B 3
C54 C 1.0504(4) 0.63337(17) 1.4770(3) 0.0170(10) Uani 1 1 d . B 3
O7 O 1.1438(3) 0.66777(11) 1.4946(2) 0.0182(7) Uani 1 1 d . B 3
O8 O 0.9598(3) 0.64216(11) 1.5217(2) 0.0190(7) Uani 1 1 d . B 3
O9 O 1.0481(3) 0.59587(12) 1.4218(2) 0.0217(7) Uani 1 1 d . B 3
Cu4 Cu 0.20441(5) 0.248361(19) 1.01244(4) 0.01366(12) Uani 1 1 d . C 4
C55 C 0.1645(4) 0.07517(16) 0.9266(3) 0.0175(10) Uani 1 1 d . C 4
H55A H 0.0887 0.0597 0.9436 0.026 Uiso 1 1 calc R C 4
H55B H 0.2421 0.0557 0.9565 0.026 Uiso 1 1 calc R C 4
H55C H 0.1539 0.0738 0.8590 0.026 Uiso 1 1 calc R C 4
C56 C 0.1784(4) 0.13214(16) 0.9592(3) 0.0110(9) Uani 1 1 d . C 4
N10 N 0.0547(3) 0.21450(14) 0.9286(2) 0.0136(8) Uani 1 1 d . C 4
C57 C 0.0560(4) 0.16270(16) 0.9137(3) 0.0118(9) Uani 1 1 d . C 4
C58 C -0.0532(4) 0.13843(17) 0.8593(3) 0.0160(9) Uani 1 1 d . C 4
H58 H -0.0534 0.1019 0.8499 0.019 Uiso 1 1 calc R C 4
C59 C -0.1610(4) 0.16763(18) 0.8190(3) 0.0181(10) Uani 1 1 d . C 4
H59 H -0.2346 0.1515 0.7808 0.022 Uiso 1 1 calc R C 4
C60 C -0.1595(4) 0.22067(18) 0.8352(3) 0.0199(10) Uani 1 1 d . C 4
H60 H -0.2325 0.2414 0.8086 0.024 Uiso 1 1 calc R C 4
C61 C -0.0506(4) 0.24319(18) 0.8906(3) 0.0160(9) Uani 1 1 d . C 4
H61 H -0.0498 0.2796 0.9021 0.019 Uiso 1 1 calc R C 4
N11 N 0.3223(3) 0.20731(14) 0.9525(2) 0.0138(7) Uani 1 1 d . C 4
C62 C 0.2983(4) 0.15642(16) 0.9326(3) 0.0128(9) Uani 1 1 d . C 4
C63 C 0.3818(4) 0.12767(18) 0.8917(3) 0.0167(9) Uani 1 1 d . C 4
H63 H 0.3643 0.0921 0.8760 0.020 Uiso 1 1 calc R C 4
C64 C 0.4908(4) 0.15158(18) 0.8740(3) 0.0197(10) Uani 1 1 d . C 4
H64 H 0.5489 0.1323 0.8466 0.024 Uiso 1 1 calc R C 4
C65 C 0.5151(4) 0.20273(19) 0.8959(3) 0.0215(10) Uani 1 1 d . C 4
H65 H 0.5901 0.2193 0.8847 0.026 Uiso 1 1 calc R C 4
C66 C 0.4280(4) 0.22975(18) 0.9346(3) 0.0179(10) Uani 1 1 d . C 4
H66 H 0.4435 0.2655 0.9491 0.021 Uiso 1 1 calc R C 4
N12 N 0.2045(3) 0.18210(13) 1.1047(2) 0.0128(8) Uani 1 1 d . C 4
C67 C 0.1956(4) 0.13482(16) 1.0667(3) 0.0126(9) Uani 1 1 d . C 4
C68 C 0.2038(4) 0.09017(17) 1.1215(3) 0.0159(9) Uani 1 1 d . C 4
H68 H 0.1992 0.0565 1.0941 0.019 Uiso 1 1 calc R C 4
C69 C 0.2189(4) 0.09604(18) 1.2175(3) 0.0171(10) Uani 1 1 d . C 4
H69 H 0.2237 0.0663 1.2564 0.020 Uiso 1 1 calc R C 4
C70 C 0.2267(4) 0.14519(18) 1.2554(3) 0.0172(10) Uani 1 1 d . C 4
H70 H 0.2370 0.1500 1.3204 0.021 Uiso 1 1 calc R C 4
C71 C 0.2193(4) 0.18696(17) 1.1966(3) 0.0164(10) Uani 1 1 d . C 4
H71 H 0.2249 0.2210 1.2225 0.020 Uiso 1 1 calc R C 4
C72 C 0.2346(4) 0.32849(17) 1.0944(3) 0.0153(9) Uani 1 1 d . C 4
O10 O 0.1217(3) 0.31076(11) 1.0519(2) 0.0179(7) Uani 1 1 d . C 4
O11 O 0.3296(3) 0.29767(11) 1.0854(2) 0.0168(7) Uani 1 1 d . C 4
O12 O 0.2509(3) 0.37034(11) 1.1387(2) 0.0179(7) Uani 1 1 d . C 4
O13 O 0.3459(3) 0.68982(14) 1.4053(3) 0.0318(9) Uani 1 1 d D D 5
H13A H 0.276(3) 0.6785(18) 1.422(4) 0.048 Uiso 1 1 d D E 5
H13B H 0.329(5) 0.7196(13) 1.373(3) 0.048 Uiso 1 1 d D F 5
O14 O 0.7464(3) 0.48836(15) 1.4591(3) 0.0354(9) Uani 1 1 d D G 5
H14A H 0.667(3) 0.4748(18) 1.439(4) 0.053 Uiso 1 1 d D H 5
H14B H 0.739(5) 0.5206(11) 1.482(4) 0.053 Uiso 1 1 d D I 5
O15 O 0.5582(3) 0.63283(14) 1.3907(3) 0.0349(9) Uani 1 1 d D J 5
H15A H 0.488(3) 0.6510(17) 1.399(4) 0.052 Uiso 1 1 d D K 5
H15B H 0.526(4) 0.6048(14) 1.355(3) 0.052 Uiso 1 1 d D L 5
O16 O 0.4826(4) 0.46577(14) 1.3786(2) 0.0343(9) Uani 1 1 d D M 5
H16A H 0.470(5) 0.4435(14) 1.329(3) 0.051 Uiso 1 1 d D N 5
H16B H 0.453(5) 0.4974(10) 1.358(3) 0.051 Uiso 1 1 d D O 5
O17 O 0.7371(3) 0.58777(14) 1.5337(3) 0.0299(8) Uani 1 1 d D P 5
H17A H 0.810(3) 0.6051(17) 1.538(4) 0.045 Uiso 1 1 d D Q 5
H17B H 0.671(3) 0.6052(18) 1.499(3) 0.045 Uiso 1 1 d D R 5
O18 O 0.8299(4) 0.54808(15) 1.3184(2) 0.0368(9) Uani 1 1 d D S 5
H18A H 0.895(4) 0.5660(19) 1.357(3) 0.055 Uiso 1 1 d D T 5
H18B H 0.792(5) 0.5277(19) 1.356(3) 0.055 Uiso 1 1 d D U 5
O19 O 0.1347(3) 0.52856(14) 1.0345(2) 0.0287(8) Uani 1 1 d D V 5
H19D H 0.141(4) 0.5122(19) 1.088(2) 0.043 Uiso 1 1 d D W 5
H19E H 0.209(3) 0.529(2) 1.018(3) 0.043 Uiso 1 1 d D X 5
O20 O 0.1322(4) 0.46190(14) 1.1870(3) 0.0366(9) Uani 1 1 d D Y 5
H20A H 0.149(5) 0.4344(16) 1.154(4) 0.055 Uiso 1 1 d D Z 5
H20B H 0.049(3) 0.460(2) 1.190(4) 0.055 Uiso 1 1 d D A 5
O21 O 0.4241(4) 0.55841(16) 1.2671(3) 0.0461(11) Uani 1 1 d D B 5
H21A H 0.430(5) 0.546(2) 1.211(2) 0.069 Uiso 1 1 d D C 5
H21B H 0.339(3) 0.552(2) 1.271(4) 0.069 Uiso 1 1 d D D 5
O22 O 0.4869(3) 0.41699(14) 1.2092(3) 0.0321(8) Uani 1 1 d D E 5
H22A H 0.480(5) 0.4444(14) 1.172(3) 0.048 Uiso 1 1 d D F 5
H22B H 0.412(3) 0.4000(17) 1.202(4) 0.048 Uiso 1 1 d D G 5
O23 O 0.5824(3) 0.32893(12) 1.0798(2) 0.0240(8) Uani 1 1 d D H 5
H23A H 0.500(2) 0.3222(16) 1.081(4) 0.036 Uiso 1 1 d D I 5
H23B H 0.601(4) 0.3619(10) 1.094(4) 0.036 Uiso 1 1 d D J 5
O24 O 0.7136(3) 0.42877(14) 1.0754(2) 0.0323(8) Uani 1 1 d D K 5
H24A H 0.782(3) 0.425(2) 1.048(3) 0.049 Uiso 1 1 d D L 5
H24B H 0.657(4) 0.4499(19) 1.036(3) 0.049 Uiso 1 1 d D M 5
O25 O 0.8977(4) 0.46336(13) 1.2286(2) 0.0309(8) Uani 1 1 d D N 5
H25A H 0.870(5) 0.4918(14) 1.253(3) 0.046 Uiso 1 1 d D O 5
H25B H 0.842(4) 0.4563(19) 1.173(2) 0.046 Uiso 1 1 d D P 5
O26 O 0.7025(3) 0.31381(14) 0.9327(2) 0.0246(8) Uani 1 1 d D Q 5
H26A H 0.655(4) 0.317(2) 0.975(2) 0.037 Uiso 1 1 d D R 5
H26B H 0.656(4) 0.315(2) 0.8755(14) 0.037 Uiso 1 1 d D S 5
O27 O 0.9048(3) 0.37852(13) 0.9805(2) 0.0266(8) Uani 1 1 d D T 5
H27A H 0.834(3) 0.3607(16) 0.952(3) 0.040 Uiso 1 1 d D U 5
H27B H 0.971(3) 0.3571(15) 0.999(3) 0.040 Uiso 1 1 d D V 5
O28 O 0.9289(3) 0.47827(13) 0.9116(2) 0.0255(8) Uani 1 1 d D W 5
H28A H 0.916(4) 0.4476(12) 0.939(3) 0.038 Uiso 1 1 d D X 5
H28B H 1.002(3) 0.4927(16) 0.946(3) 0.038 Uiso 1 1 d D Y 5
O29 O 0.1878(4) 0.55231(16) 1.3032(3) 0.0521(11) Uani 1 1 d D Z 5
H29A H 0.137(5) 0.565(2) 1.340(4) 0.078 Uiso 1 1 d D A 5
H29B H 0.160(6) 0.5200(13) 1.284(4) 0.078 Uiso 1 1 d D B 5


_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
Cu1 O2 1.945(3) . ?
Cu1 O1 1.968(3) . ?
Cu1 N2 1.975(3) . ?
Cu1 N1 1.981(3) . ?
Cu1 N3 2.195(4) . ?
C1 C2 1.525(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.553(6) . ?
C2 C13 1.559(6) . ?
C2 C8 1.563(6) . ?
N1 C7 1.337(5) . ?
N1 C3 1.349(5) . ?
C3 C4 1.378(5) . ?
C4 C5 1.383(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.365(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.385(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
N2 C8 1.341(5) . ?
N2 C12 1.351(5) . ?
C8 C9 1.394(6) . ?
C9 C10 1.381(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.374(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N3 C13 1.327(5) . ?
N3 C17 1.353(6) . ?
C13 C14 1.401(6) . ?
C14 C15 1.385(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(6) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 O3 1.255(5) . ?
C18 O2 1.299(5) . ?
C18 O1 1.329(5) . ?
Cu2 O5 1.956(3) . ?
Cu2 N4 1.971(3) . ?
Cu2 O4 1.988(3) . ?
Cu2 N5 2.045(3) . ?
Cu2 N6 2.139(4) . ?
C19 C20 1.537(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.538(6) . ?
C20 C26 1.545(6) . ?
C20 C31 1.570(6) . ?
N4 C21 1.353(5) . ?
N4 C25 1.361(5) . ?
C21 C22 1.373(6) . ?
C22 C23 1.399(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.375(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.370(6) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
N5 C30 1.325(5) . ?
N5 C26 1.358(5) . ?
C26 C27 1.384(5) . ?
C27 C28 1.384(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.381(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.391(6) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
N6 C35 1.334(6) . ?
N6 C31 1.345(5) . ?
C31 C32 1.378(6) . ?
C32 C33 1.389(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.378(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.390(6) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 O6 1.243(5) . ?
C36 O4 1.307(5) . ?
C36 O5 1.314(5) . ?
Cu3 O8 1.965(3) . ?
Cu3 N7 1.978(4) . ?
Cu3 O7 1.988(3) . ?
Cu3 N8 2.012(3) . ?
Cu3 N9 2.176(3) . ?
C37 C38 1.535(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.539(6) . ?
C38 C44 1.545(6) . ?
C38 C49 1.552(6) . ?
N7 C43 1.343(5) . ?
N7 C39 1.350(5) . ?
C39 C40 1.386(6) . ?
C40 C41 1.385(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.387(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.372(6) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 N8 1.336(5) . ?
C44 C45 1.391(6) . ?
N8 C48 1.339(5) . ?
C45 C46 1.398(7) . ?
C45 H45 0.9500 . ?
C46 C47 1.368(7) . ?
C46 H46 0.9500 . ?
C47 C48 1.388(6) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
N9 C53 1.332(5) . ?
N9 C49 1.353(5) . ?
C49 C50 1.390(6) . ?
C50 C51 1.389(6) . ?
C50 H50 0.9500 . ?
C51 C52 1.369(6) . ?
C51 H51 0.9500 . ?
C52 C53 1.399(6) . ?
C52 H52 0.9500 . ?
C53 H53 0.9500 . ?
C54 O9 1.259(5) . ?
C54 O8 1.303(5) . ?
C54 O7 1.310(5) . ?
Cu4 O11 1.972(3) . ?
Cu4 O10 1.978(3) . ?
Cu4 N10 1.982(3) . ?
Cu4 N11 1.990(3) . ?
Cu4 N12 2.180(3) . ?
C55 C56 1.538(6) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 C57 1.538(5) . ?
C56 C62 1.545(5) . ?
C56 C67 1.557(6) . ?
N10 C57 1.350(5) . ?
N10 C61 1.351(5) . ?
C57 C58 1.400(6) . ?
C58 C59 1.386(6) . ?
C58 H58 0.9500 . ?
C59 C60 1.383(6) . ?
C59 H59 0.9500 . ?
C60 C61 1.384(6) . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?
N11 C66 1.340(5) . ?
N11 C62 1.352(5) . ?
C62 C63 1.392(6) . ?
C63 C64 1.387(6) . ?
C63 H63 0.9500 . ?
C64 C65 1.364(6) . ?
C64 H64 0.9500 . ?
C65 C66 1.380(6) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
N12 C67 1.333(5) . ?
N12 C71 1.336(5) . ?
C67 C68 1.395(6) . ?
C68 C69 1.398(6) . ?
C68 H68 0.9500 . ?
C69 C70 1.376(6) . ?
C69 H69 0.9500 . ?
C70 C71 1.371(6) . ?
C70 H70 0.9500 . ?
C71 H71 0.9500 . ?
C72 O12 1.250(5) . ?
C72 O10 1.304(5) . ?
C72 O11 1.312(5) . ?
O13 H13A 0.888(19) . ?
O13 H13B 0.899(19) . ?
O14 H14A 0.903(19) . ?
O14 H14B 0.903(19) . ?
O15 H15A 0.908(19) . ?
O15 H15B 0.912(19) . ?
O16 H16A 0.912(19) . ?
O16 H16B 0.901(19) . ?
O17 H17A 0.886(19) . ?
O17 H17B 0.891(19) . ?
O18 H18A 0.91(2) . ?
O18 H18B 0.916(19) . ?
O19 H19D 0.880(19) . ?
O19 H19E 0.883(19) . ?
O20 H20A 0.899(19) . ?
O20 H20B 0.897(19) . ?
O21 H21A 0.909(19) . ?
O21 H21B 0.94(2) . ?
O22 H22A 0.882(19) . ?
O22 H22B 0.894(19) . ?
O23 H23A 0.891(19) . ?
O23 H23B 0.884(19) . ?
O24 H24A 0.913(19) . ?
O24 H24B 0.915(19) . ?
O25 H25A 0.893(19) . ?
O25 H25B 0.916(19) . ?
O26 H26A 0.881(18) . ?
O26 H26B 0.876(19) . ?
O27 H27A 0.899(19) . ?
O27 H27B 0.888(19) . ?
O28 H28A 0.909(19) . ?
O28 H28B 0.905(19) . ?
O29 H29A 0.907(19) . ?
O29 H29B 0.91(2) . ?

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
O2 Cu1 O1 67.76(12) . . ?
O2 Cu1 N2 99.15(13) . . ?
O1 Cu1 N2 164.31(13) . . ?
O2 Cu1 N1 164.36(13) . . ?
O1 Cu1 N1 100.93(13) . . ?
N2 Cu1 N1 90.09(14) . . ?
O2 Cu1 N3 108.07(13) . . ?
O1 Cu1 N3 104.07(13) . . ?
N2 Cu1 N3 87.92(14) . . ?
N1 Cu1 N3 84.70(13) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 C3 110.0(3) . . ?
C1 C2 C13 110.4(3) . . ?
C3 C2 C13 106.2(3) . . ?
C1 C2 C8 109.7(3) . . ?
C3 C2 C8 111.7(3) . . ?
C13 C2 C8 108.7(3) . . ?
C7 N1 C3 119.6(3) . . ?
C7 N1 Cu1 119.9(3) . . ?
C3 N1 Cu1 120.3(3) . . ?
N1 C3 C4 120.1(4) . . ?
N1 C3 C2 117.8(3) . . ?
C4 C3 C2 122.0(4) . . ?
C3 C4 C5 119.8(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 120.1(4) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 117.6(4) . . ?
C5 C6 H6 121.2 . . ?
C7 C6 H6 121.2 . . ?
N1 C7 C6 122.7(4) . . ?
N1 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
C8 N2 C12 119.4(4) . . ?
C8 N2 Cu1 120.6(3) . . ?
C12 N2 Cu1 119.7(3) . . ?
N2 C8 C9 120.4(4) . . ?
N2 C8 C2 117.6(4) . . ?
C9 C8 C2 122.0(4) . . ?
C10 C9 C8 119.9(4) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 119.3(4) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C12 C11 C10 118.2(4) . . ?
C12 C11 H11 120.9 . . ?
C10 C11 H11 120.9 . . ?
N2 C12 C11 122.8(4) . . ?
N2 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C13 N3 C17 119.6(4) . . ?
C13 N3 Cu1 117.4(3) . . ?
C17 N3 Cu1 122.9(3) . . ?
N3 C13 C14 121.6(4) . . ?
N3 C13 C2 116.8(4) . . ?
C14 C13 C2 121.6(4) . . ?
C15 C14 C13 118.5(4) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C14 C15 C16 120.0(4) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C17 C16 C15 118.0(4) . . ?
C17 C16 H16 121.0 . . ?
C15 C16 H16 121.0 . . ?
N3 C17 C16 122.2(4) . . ?
N3 C17 H17 118.9 . . ?
C16 C17 H17 118.9 . . ?
O3 C18 O2 124.5(4) . . ?
O3 C18 O1 123.3(4) . . ?
O2 C18 O1 112.2(4) . . ?
C18 O1 Cu1 89.0(2) . . ?
C18 O2 Cu1 90.9(2) . . ?
O5 Cu2 N4 164.03(14) . . ?
O5 Cu2 O4 67.00(12) . . ?
N4 Cu2 O4 98.68(13) . . ?
O5 Cu2 N5 98.55(13) . . ?
N4 Cu2 N5 90.13(14) . . ?
O4 Cu2 N5 147.52(13) . . ?
O5 Cu2 N6 106.26(13) . . ?
N4 Cu2 N6 87.90(14) . . ?
O4 Cu2 N6 127.44(13) . . ?
N5 Cu2 N6 83.82(14) . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C19 C20 C21 109.5(3) . . ?
C19 C20 C26 109.9(3) . . ?
C21 C20 C26 109.9(3) . . ?
C19 C20 C31 109.2(3) . . ?
C21 C20 C31 111.5(3) . . ?
C26 C20 C31 106.9(3) . . ?
C21 N4 C25 120.0(4) . . ?
C21 N4 Cu2 120.7(3) . . ?
C25 N4 Cu2 119.2(3) . . ?
N4 C21 C22 119.6(4) . . ?
N4 C21 C20 117.7(4) . . ?
C22 C21 C20 122.7(4) . . ?
C21 C22 C23 120.9(4) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C24 C23 C22 118.5(4) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C25 C24 C23 119.2(4) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
N4 C25 C24 121.8(4) . . ?
N4 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
C30 N5 C26 119.0(4) . . ?
C30 N5 Cu2 120.9(3) . . ?
C26 N5 Cu2 120.0(3) . . ?
N5 C26 C27 120.5(4) . . ?
N5 C26 C20 116.5(3) . . ?
C27 C26 C20 122.9(4) . . ?
C28 C27 C26 119.8(4) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C29 C28 C27 119.7(4) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 117.3(4) . . ?
C28 C29 H29 121.3 . . ?
C30 C29 H29 121.3 . . ?
N5 C30 C29 123.6(4) . . ?
N5 C30 H30 118.2 . . ?
C29 C30 H30 118.2 . . ?
C35 N6 C31 119.1(4) . . ?
C35 N6 Cu2 122.3(3) . . ?
C31 N6 Cu2 118.3(3) . . ?
N6 C31 C32 121.1(4) . . ?
N6 C31 C20 116.4(4) . . ?
C32 C31 C20 122.3(4) . . ?
C31 C32 C33 119.6(4) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
C34 C33 C32 119.5(4) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 117.5(4) . . ?
C33 C34 H34 121.2 . . ?
C35 C34 H34 121.2 . . ?
N6 C35 C34 123.2(4) . . ?
N6 C35 H35 118.4 . . ?
C34 C35 H35 118.4 . . ?
O6 C36 O4 123.7(4) . . ?
O6 C36 O5 124.0(4) . . ?
O4 C36 O5 112.3(4) . . ?
C36 O4 Cu2 89.7(3) . . ?
C36 O5 Cu2 90.9(2) . . ?
O8 Cu3 N7 163.56(13) . . ?
O8 Cu3 O7 67.00(12) . . ?
N7 Cu3 O7 99.01(13) . . ?
O8 Cu3 N8 100.12(14) . . ?
N7 Cu3 N8 89.66(14) . . ?
O7 Cu3 N8 155.95(13) . . ?
O8 Cu3 N9 105.35(12) . . ?
N7 Cu3 N9 88.68(13) . . ?
O7 Cu3 N9 118.37(13) . . ?
N8 Cu3 N9 83.99(13) . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C37 C38 C39 108.4(3) . . ?
C37 C38 C44 110.0(3) . . ?
C39 C38 C44 110.8(3) . . ?
C37 C38 C49 109.1(3) . . ?
C39 C38 C49 110.5(3) . . ?
C44 C38 C49 108.0(3) . . ?
C43 N7 C39 119.6(4) . . ?
C43 N7 Cu3 119.5(3) . . ?
C39 N7 Cu3 120.7(3) . . ?
N7 C39 C40 120.2(4) . . ?
N7 C39 C38 116.8(4) . . ?
C40 C39 C38 123.0(4) . . ?
C41 C40 C39 119.5(4) . . ?
C41 C40 H40 120.2 . . ?
C39 C40 H40 120.2 . . ?
C40 C41 C42 120.1(4) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C41 117.3(4) . . ?
C43 C42 H42 121.4 . . ?
C41 C42 H42 121.4 . . ?
N7 C43 C42 123.3(4) . . ?
N7 C43 H43 118.3 . . ?
C42 C43 H43 118.3 . . ?
N8 C44 C45 120.1(4) . . ?
N8 C44 C38 117.7(4) . . ?
C45 C44 C38 122.2(4) . . ?
C44 N8 C48 120.6(4) . . ?
C44 N8 Cu3 119.6(3) . . ?
C48 N8 Cu3 119.8(3) . . ?
C44 C45 C46 118.6(4) . . ?
C44 C45 H45 120.7 . . ?
C46 C45 H45 120.7 . . ?
C47 C46 C45 121.0(4) . . ?
C47 C46 H46 119.5 . . ?
C45 C46 H46 119.5 . . ?
C46 C47 C48 116.9(4) . . ?
C46 C47 H47 121.6 . . ?
C48 C47 H47 121.6 . . ?
N8 C48 C47 122.7(4) . . ?
N8 C48 H48 118.6 . . ?
C47 C48 H48 118.6 . . ?
C53 N9 C49 119.1(4) . . ?
C53 N9 Cu3 123.5(3) . . ?
C49 N9 Cu3 117.3(3) . . ?
N9 C49 C50 121.0(4) . . ?
N9 C49 C38 115.9(3) . . ?
C50 C49 C38 123.1(4) . . ?
C51 C50 C49 119.1(4) . . ?
C51 C50 H50 120.5 . . ?
C49 C50 H50 120.5 . . ?
C52 C51 C50 120.1(4) . . ?
C52 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C51 C52 C53 117.7(4) . . ?
C51 C52 H52 121.2 . . ?
C53 C52 H52 121.2 . . ?
N9 C53 C52 123.0(4) . . ?
N9 C53 H53 118.5 . . ?
C52 C53 H53 118.5 . . ?
O9 C54 O8 123.5(4) . . ?
O9 C54 O7 123.3(4) . . ?
O8 C54 O7 113.3(4) . . ?
C54 O7 Cu3 89.2(2) . . ?
C54 O8 Cu3 90.4(3) . . ?
O11 Cu4 O10 66.89(12) . . ?
O11 Cu4 N10 166.00(13) . . ?
O10 Cu4 N10 101.11(13) . . ?
O11 Cu4 N11 99.75(13) . . ?
O10 Cu4 N11 157.84(13) . . ?
N10 Cu4 N11 89.22(14) . . ?
O11 Cu4 N12 104.79(13) . . ?
O10 Cu4 N12 112.76(12) . . ?
N10 Cu4 N12 86.24(14) . . ?
N11 Cu4 N12 87.23(13) . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C56 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C55 C56 C57 109.7(3) . . ?
C55 C56 C62 109.4(3) . . ?
C57 C56 C62 110.3(3) . . ?
C55 C56 C67 110.0(3) . . ?
C57 C56 C67 108.4(3) . . ?
C62 C56 C67 109.1(3) . . ?
C57 N10 C61 120.5(4) . . ?
C57 N10 Cu4 119.9(3) . . ?
C61 N10 Cu4 119.5(3) . . ?
N10 C57 C58 119.7(4) . . ?
N10 C57 C56 118.1(3) . . ?
C58 C57 C56 122.2(4) . . ?
C59 C58 C57 120.2(4) . . ?
C59 C58 H58 119.9 . . ?
C57 C58 H58 119.9 . . ?
C60 C59 C58 118.9(4) . . ?
C60 C59 H59 120.5 . . ?
C58 C59 H59 120.5 . . ?
C59 C60 C61 119.3(4) . . ?
C59 C60 H60 120.3 . . ?
C61 C60 H60 120.3 . . ?
N10 C61 C60 121.4(4) . . ?
N10 C61 H61 119.3 . . ?
C60 C61 H61 119.3 . . ?
C66 N11 C62 119.9(4) . . ?
C66 N11 Cu4 119.9(3) . . ?
C62 N11 Cu4 120.2(3) . . ?
N11 C62 C63 120.0(4) . . ?
N11 C62 C56 117.5(3) . . ?
C63 C62 C56 122.5(4) . . ?
C64 C63 C62 119.1(4) . . ?
C64 C63 H63 120.4 . . ?
C62 C63 H63 120.4 . . ?
C65 C64 C63 120.3(4) . . ?
C65 C64 H64 119.9 . . ?
C63 C64 H64 119.9 . . ?
C64 C65 C66 118.3(4) . . ?
C64 C65 H65 120.8 . . ?
C66 C65 H65 120.8 . . ?
N11 C66 C65 122.3(4) . . ?
N11 C66 H66 118.8 . . ?
C65 C66 H66 118.8 . . ?
C67 N12 C71 119.6(4) . . ?
C67 N12 Cu4 117.3(3) . . ?
C71 N12 Cu4 123.0(3) . . ?
N12 C67 C68 121.1(4) . . ?
N12 C67 C56 116.8(4) . . ?
C68 C67 C56 122.1(4) . . ?
C67 C68 C69 118.5(4) . . ?
C67 C68 H68 120.8 . . ?
C69 C68 H68 120.8 . . ?
C70 C69 C68 119.6(4) . . ?
C70 C69 H69 120.2 . . ?
C68 C69 H69 120.2 . . ?
C71 C70 C69 118.2(4) . . ?
C71 C70 H70 120.9 . . ?
C69 C70 H70 120.9 . . ?
N12 C71 C70 123.1(4) . . ?
N12 C71 H71 118.5 . . ?
C70 C71 H71 118.5 . . ?
O12 C72 O10 123.8(4) . . ?
O12 C72 O11 123.6(4) . . ?
O10 C72 O11 112.6(4) . . ?
C72 O10 Cu4 90.2(2) . . ?
C72 O11 Cu4 90.2(2) . . ?
H13A O13 H13B 111(3) . . ?
H14A O14 H14B 109(3) . . ?
H15A O15 H15B 105(3) . . ?
H16A O16 H16B 108(3) . . ?
H17A O17 H17B 111(3) . . ?
H18A O18 H18B 106(3) . . ?
H19D O19 H19E 111(3) . . ?
H20A O20 H20B 108(3) . . ?
H21A O21 H21B 105(3) . . ?
H22A O22 H22B 111(3) . . ?
H23A O23 H23B 110(3) . . ?
H24A O24 H24B 106(3) . . ?
H25A O25 H25B 108(3) . . ?
H26A O26 H26B 113(3) . . ?
H27A O27 H27B 111(3) . . ?
H28A O28 H28B 107(3) . . ?
H29A O29 H29B 108(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O13 H13B O3 0.899(19) 1.93(2) 2.814(5) 168(5) 2_657
O13 H13A O7 0.888(19) 1.96(3) 2.818(4) 161(5) 1_455
O14 H14A O16 0.903(19) 1.97(3) 2.846(5) 163(5) .
O14 H14B O17 0.903(19) 1.892(19) 2.793(5) 176(5) .
O15 H15A O13 0.908(19) 1.83(2) 2.737(5) 175(6) .
O15 H15B O21 0.912(19) 1.91(2) 2.801(5) 165(5) .
O16 H16B O21 0.901(19) 2.04(3) 2.882(6) 155(5) .
O16 H16A O22 0.912(19) 1.94(3) 2.806(5) 157(5) .
O17 H17A O8 0.886(19) 1.91(2) 2.787(4) 169(5) .
O17 H17B O15 0.891(19) 1.91(3) 2.757(5) 159(5) .
O18 H18A O9 0.91(2) 1.86(2) 2.759(5) 168(5) .
O18 H18B O14 0.916(19) 1.98(2) 2.878(5) 167(4) .
O19 H19E O5 0.883(19) 1.97(2) 2.837(4) 167(5) .
O19 H19D O20 0.880(19) 1.97(2) 2.833(5) 166(5) .
O20 H20A O12 0.899(19) 2.01(3) 2.835(5) 152(5) .
O20 H20B O25 0.897(19) 1.82(2) 2.696(5) 165(5) 1_455
O21 H21A O6 0.909(19) 1.87(2) 2.768(5) 169(6) .
O21 H21B O29 0.94(2) 1.77(2) 2.685(6) 164(5) .
O22 H22A O6 0.882(19) 1.97(2) 2.845(5) 171(5) .
O22 H22B O12 0.894(19) 1.91(3) 2.762(5) 158(5) .
O23 H23A O11 0.891(19) 1.936(19) 2.821(4) 172(4) .
O23 H23B O24 0.884(19) 2.15(3) 2.928(5) 147(4) .
O24 H24B O4 0.915(19) 1.92(2) 2.813(5) 166(5) .
O24 H24A O27 0.913(19) 2.17(3) 3.006(5) 152(5) .
O25 H25A O18 0.893(19) 1.842(19) 2.729(5) 172(4) .
O25 H25B O24 0.916(19) 1.88(2) 2.780(5) 166(5) .
O26 H26B O1 0.876(19) 1.87(2) 2.742(4) 177(5) .
O26 H26A O23 0.881(18) 1.912(19) 2.782(4) 169(4) .
O27 H27B O10 0.888(19) 2.01(2) 2.891(4) 175(5) 1_655
O27 H27A O26 0.899(19) 1.82(3) 2.682(5) 161(5) .
O28 H28B O19 0.905(19) 1.93(2) 2.820(5) 169(5) 1_655
O28 H28A O27 0.909(19) 1.89(2) 2.791(5) 170(5) .
O29 H29A O9 0.907(19) 1.87(2) 2.772(5) 173(5) 1_455
O29 H29B O20 0.91(2) 2.05(3) 2.869(5) 150(5) .

_diffrn_measured_fraction_theta_max 0.903
_diffrn_reflns_theta_full        27.73
_diffrn_measured_fraction_theta_full 0.903
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 1023806'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_exp_1161

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis[1,1,1-tris(pyrid-2-yl)ethane]copper(II) diiodide 
octa-hydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H30 Cu N6, 2I, 8[H2 O]'
_chemical_formula_sum            'C34 H46 Cu I2 N6 O8'
_chemical_formula_weight         984.11

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'

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

_cell_length_a                   12.9173(8)
_cell_length_b                   13.3786(11)
_cell_length_c                   11.6292(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.060(6)
_cell_angle_gamma                90.00
_cell_volume                     1957.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1793
_cell_measurement_theta_min      3.3180
_cell_measurement_theta_max      25.6740

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             982
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4691
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_sigmaI/netI    0.1029
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.73
_reflns_number_total             2048
_reflns_number_gt                1666
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains one-quarter of a formula unit, with Cu1 lying 
 on the 2/m site 1/2, 1/2, 1; atoms N1 and C1-C7 lying on the mirror plane 
 x, 1/2, z; one half-iodide ion and a half-water molecule lying on the same 
 mirror plane; half a water molecule on the C₂ axis 1/2, y, 1/2; and a 
 whole water molecule on a general crystallographic site.

 All non-H atoms were refined anisotropically, and C-bound H atoms were 
 placed in calculated positions and refined using a riding model. The water 
 H atoms were located in the Fourier map and allowed to refine, with 
 Uiso contrained to 1.5xUeq for the equivalent O atom. The H atoms for 
 the two half-water sites are disordered about those special positions, 
 leading to significant disorder in the hydrogen bonding network. The model 
 also implies H atom disorder on O1, possibly involving an additional  
 hydrogen bond between O1 and O1ⁱ ,(O1...O1ⁱ = 2.769(6) Å; 
 symmetry code (i) 3/2-x, 3/2-y, 1-z). This extra partial H atom site was 
 not located in the Fourier map, however.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0332P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2048
_refine_ls_number_parameters     151
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1198
_refine_ls_wR_factor_gt          0.1039
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.5000 1.0000 0.0113(3) Uani 1 4 d S . .
C1 C 0.8656(5) 0.5000 1.0080(6) 0.0115(16) Uani 1 2 d S . .
H1A H 0.8994 0.4486 1.0642 0.017 Uiso 0.50 1 calc PR . .
H1B H 0.8950 0.5656 1.0351 0.017 Uiso 0.50 1 calc PR . .
H1C H 0.8794 0.4858 0.9301 0.017 Uiso 0.50 1 calc PR . .
C2 C 0.7442(5) 0.5000 0.9996(6) 0.0139(17) Uani 1 2 d S . .
C3 C 0.7248(6) 0.5000 1.1263(6) 0.0132(16) Uani 1 2 d S . .
N1 N 0.6236(4) 0.5000 1.1385(5) 0.0136(14) Uani 1 2 d S . .
C7 C 0.6056(6) 0.5000 1.2485(6) 0.021(2) Uani 1 2 d S . .
H7 H 0.5341 0.5000 1.2570 0.025 Uiso 1 2 calc SR . .
C6 C 0.6859(6) 0.5000 1.3482(7) 0.023(2) Uani 1 2 d S . .
H6 H 0.6705 0.5000 1.4243 0.027 Uiso 1 2 calc SR . .
C5 C 0.7890(6) 0.5000 1.3358(6) 0.0183(18) Uani 1 2 d S . .
H5 H 0.8462 0.5000 1.4034 0.022 Uiso 1 2 calc SR . .
C4 C 0.8086(6) 0.5000 1.2245(6) 0.0195(19) Uani 1 2 d S . .
H4 H 0.8797 0.5000 1.2149 0.023 Uiso 1 2 calc SR . .
C8 C 0.6935(4) 0.4070(5) 0.9307(4) 0.0158(13) Uani 1 1 d . . .
N2 N 0.5898(3) 0.3899(4) 0.9266(4) 0.0268(13) Uani 1 1 d . . .
C12 C 0.5423(5) 0.3115(5) 0.8651(5) 0.0288(16) Uani 1 1 d . . .
H12 H 0.4697 0.2996 0.8646 0.035 Uiso 1 1 calc R . .
C11 C 0.5917(4) 0.2473(6) 0.8026(5) 0.0272(15) Uani 1 1 d . . .
H11 H 0.5543 0.1936 0.7583 0.033 Uiso 1 1 calc R . .
C10 C 0.6979(4) 0.2639(5) 0.8068(5) 0.0224(14) Uani 1 1 d . . .
H10 H 0.7357 0.2207 0.7659 0.027 Uiso 1 1 calc R . .
C9 C 0.7492(4) 0.3441(5) 0.8713(4) 0.0193(13) Uani 1 1 d . . .
H9 H 0.8223 0.3560 0.8748 0.023 Uiso 1 1 calc R . .
I1 I 0.89388(3) 0.5000 0.67349(4) 0.0183(2) Uani 1 2 d S . .
O1 O 0.8440(4) 0.7520(4) 0.5854(5) 0.0555(15) Uani 1 1 d D . .
H1D H 0.857(6) 0.688(2) 0.605(8) 0.083 Uiso 1 1 d D . .
H1E H 0.892(5) 0.778(5) 0.551(7) 0.083 Uiso 1 1 d D . .
O2 O 0.5000 0.3526(5) 0.5000 0.0290(14) Uani 1 2 d SD . .
H2A H 0.446(7) 0.384(9) 0.450(7) 0.044 Uiso 0.50 1 d PD . .
H2B H 0.541(8) 0.321(9) 0.458(8) 0.044 Uiso 0.50 1 d PD . .
O3 O 0.6081(4) 0.5000 0.6477(5) 0.0249(14) Uani 1 2 d SD . .
H3A H 0.678(2) 0.5000 0.647(7) 0.037 Uiso 1 2 d SD . .
H3B H 0.580(4) 0.441(4) 0.620(10) 0.037 Uiso 0.50 1 d PD . .


_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
Cu1 N1 1.995(5) . ?
Cu1 N2 2.166(5) . ?
C1 C2 1.550(9) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C8 1.543(7) . ?
C2 C3 1.550(9) . ?
C3 N1 1.346(9) . ?
C3 C4 1.385(10) . ?
N1 C7 1.351(8) . ?
C7 C6 1.370(10) . ?
C7 H7 0.9500 . ?
C6 C5 1.372(10) . ?
C6 H6 0.9500 . ?
C5 C4 1.374(10) . ?
C5 H5 0.9500 . ?
C4 H4 0.9500 . ?
C8 N2 1.349(6) . ?
C8 C9 1.388(8) . ?
N2 C12 1.338(8) . ?
C12 C11 1.372(9) . ?
C12 H12 0.9500 . ?
C11 C10 1.379(7) . ?
C11 H11 0.9500 . ?
C10 C9 1.389(8) . ?
C10 H10 0.9500 . ?
C9 H9 0.9500 . ?
O1 H1D 0.89(2) . ?
O1 H1E 0.88(2) . ?
O2 H2A 0.90(2) . ?
O2 H2B 0.90(2) . ?
O3 H3A 0.91(2) . ?
O3 H3B 0.90(2) . ?

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 Cu1 N1 180.00 5_667 . ?
N1 Cu1 N2 85.17(16) . . ?
N1 Cu1 N2 94.83(16) . 2_657 ?
N2 Cu1 N2 94.3(3) . 2_657 ?
N2 Cu1 N2 85.7(3) . 6_565 ?
N2 Cu1 N2 180.00 . 5_667 ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C8 C2 C8 107.5(5) . 6_565 ?
C8 C2 C1 109.7(4) . . ?
C8 C2 C3 110.7(4) . . ?
C1 C2 C3 108.6(5) . . ?
N1 C3 C4 120.7(6) . . ?
N1 C3 C2 118.0(6) . . ?
C4 C3 C2 121.3(6) . . ?
C3 N1 C7 118.6(6) . . ?
C3 N1 Cu1 122.3(4) . . ?
C7 N1 Cu1 119.1(5) . . ?
N1 C7 C6 122.8(7) . . ?
N1 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
C7 C6 C5 118.5(7) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
C6 C5 C4 119.3(7) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C4 C3 120.0(7) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N2 C8 C9 120.1(5) . . ?
N2 C8 C2 117.2(5) . . ?
C9 C8 C2 122.7(5) . . ?
C12 N2 C8 119.0(5) . . ?
C12 N2 Cu1 121.4(4) . . ?
C8 N2 Cu1 119.1(4) . . ?
N2 C12 C11 124.2(5) . . ?
N2 C12 H12 117.9 . . ?
C11 C12 H12 117.9 . . ?
C12 C11 C10 117.3(6) . . ?
C12 C11 H11 121.4 . . ?
C10 C11 H11 121.4 . . ?
C11 C10 C9 119.5(6) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C8 C9 C10 120.0(5) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
H1D O1 H1E 113(3) . . ?
H2A O2 H2B 109(3) . . ?
H3A O3 H3B 109(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1D I1 0.89(2) 2.65(2) 3.540(6) 178(7) .
O1 H1E O2 0.88(2) 1.92(2) 2.786(6) 169(8) 3
O2 H2B O1 0.90(2) 1.91(4) 2.786(6) 163(10) 4_646
O2 H2A O3 0.90(2) 1.96(7) 2.775(6) 150(12) 2_656
O3 H3A I1 0.91(2) 2.73(2) 3.636(5) 173(7) .
O3 H3B O2 0.90(2) 1.94(6) 2.775(6) 154(11) .

_diffrn_measured_fraction_theta_max 0.854
_diffrn_reflns_theta_full        27.73
_diffrn_measured_fraction_theta_full 0.854
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.185
_database_code_depnum_ccdc_archive 'CCDC 1023807'
