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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dh_152b_0ma
_database_code_depnum_ccdc_archive 'CCDC 1038274'
_audit_update_record             
;
2015-10-27 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_date             2013-07-10T11:03:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 Complex 1
;
_chemical_name_common            dh_152b
_chemical_formula_moiety         'C18 H28 Co N8 O2, Cl O4, C2 H6 O S'
_chemical_formula_sum            'C20 H34 Cl Co N8 O7 S'
_chemical_formula_weight         624.99
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P n'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_Int_Tables_number      7
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y, z+1/2'



_cell_length_a                   6.8158(16)
_cell_length_b                   12.780(3)
_cell_length_c                   15.038(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.125(14)
_cell_angle_gamma                90
_cell_volume                     1309.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    105
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             652
_exptl_special_details           
;
 30 seconds, 1 degree, 40 mm
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.8529
_exptl_absorpt_correction_T_max  0.9452

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.1065
_diffrn_reflns_av_unetI/netI     0.092
_diffrn_reflns_number            32970
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             4775
_reflns_number_gt                3653
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0174P)²+0.4180P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4775
_refine_ls_number_parameters     351
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.0691
_refine_ls_wR_factor_gt          0.0611
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(15)
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.084

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.1818(7) 0.1337(4) 0.4265(3) 0.0149(11) Uani 1 1 d . . .
C2 C 0.3724(6) 0.1836(3) 0.4155(3) 0.0145(10) Uani 1 1 d . . .
C3 C 0.5836(6) 0.2521(4) 0.2993(3) 0.0182(11) Uani 1 1 d . . .
H3A H 0.7041 0.2364 0.3356 0.022 Uiso 1 1 calc R . .
H3B H 0.5585 0.3283 0.3027 0.022 Uiso 1 1 calc R . .
C4 C 0.6117(6) 0.2207(4) 0.2037(3) 0.0199(11) Uani 1 1 d . . .
H4A H 0.6477 0.2827 0.1684 0.024 Uiso 1 1 calc R . .
H4B H 0.7194 0.1689 0.2008 0.024 Uiso 1 1 calc R . .
C5 C 0.3841(6) 0.1495(3) 0.0848(3) 0.0156(11) Uani 1 1 d . . .
C6 C 0.1932(7) 0.0987(4) 0.0708(3) 0.0164(11) Uani 1 1 d . . .
C7 C 0.0974(6) 0.1156(3) 0.5157(3) 0.0194(11) Uani 1 1 d . . .
H7A H -0.0436 0.1017 0.5082 0.029 Uiso 1 1 calc R . .
H7B H 0.1183 0.1779 0.5528 0.029 Uiso 1 1 calc R . .
H7C H 0.1623 0.0554 0.5443 0.029 Uiso 1 1 calc R . .
C8 C 0.4958(6) 0.2174(4) 0.4940(3) 0.0219(12) Uani 1 1 d . . .
H8A H 0.6277 0.235 0.4749 0.033 Uiso 1 1 calc R . .
H8B H 0.5043 0.1604 0.5376 0.033 Uiso 1 1 calc R . .
H8C H 0.4366 0.279 0.521 0.033 Uiso 1 1 calc R . .
C9 C 0.5142(6) 0.1703(4) 0.0092(3) 0.0241(12) Uani 1 1 d . . .
H9A H 0.4736 0.2354 -0.0206 0.036 Uiso 1 1 calc R . .
H9B H 0.5041 0.1123 -0.0334 0.036 Uiso 1 1 calc R . .
H9C H 0.6504 0.1768 0.0317 0.036 Uiso 1 1 calc R . .
C10 C 0.1065(6) 0.0699(4) -0.0189(3) 0.0223(12) Uani 1 1 d . . .
H10A H -0.0197 0.0347 -0.0119 0.033 Uiso 1 1 calc R . .
H10B H 0.1963 0.0229 -0.049 0.033 Uiso 1 1 calc R . .
H10C H 0.0863 0.1334 -0.0546 0.033 Uiso 1 1 calc R . .
C11 C 0.0517(6) 0.3218(3) 0.1528(3) 0.0159(11) Uani 1 1 d . . .
H11 H 0.0579 0.2907 0.0956 0.019 Uiso 1 1 calc R . .
C12 C -0.0181(6) 0.4183(4) 0.1687(3) 0.0170(11) Uani 1 1 d . . .
H12 H -0.0707 0.4663 0.1259 0.02 Uiso 1 1 calc R . .
C13 C 0.0812(6) 0.3460(4) 0.2944(3) 0.0178(11) Uani 1 1 d . . .
H13 H 0.1108 0.3364 0.3561 0.021 Uiso 1 1 calc R . .
C14 C -0.0501(6) 0.5280(3) 0.3056(3) 0.0211(11) Uani 1 1 d . . .
H14A H -0.0758 0.5109 0.3676 0.032 Uiso 1 1 calc R . .
H14B H -0.168 0.559 0.2771 0.032 Uiso 1 1 calc R . .
H14C H 0.0586 0.5781 0.3038 0.032 Uiso 1 1 calc R . .
C15 C 0.2467(6) -0.0868(4) 0.2846(3) 0.0172(11) Uani 1 1 d . . .
H15 H 0.1111 -0.0882 0.2971 0.021 Uiso 1 1 calc R . .
C16 C 0.3695(6) -0.1715(3) 0.2851(3) 0.0163(11) Uani 1 1 d . . .
H16 H 0.3368 -0.2418 0.2986 0.02 Uiso 1 1 calc R . .
C17 C 0.5349(6) -0.0310(3) 0.2506(3) 0.0131(10) Uani 1 1 d . . .
H17 H 0.6396 0.0139 0.2356 0.016 Uiso 1 1 calc R . .
C18 C 0.7300(7) -0.1940(3) 0.2555(3) 0.0196(10) Uani 1 1 d . . .
H18A H 0.8297 -0.1512 0.2275 0.029 Uiso 1 1 calc R . .
H18B H 0.7037 -0.2566 0.2193 0.029 Uiso 1 1 calc R . .
H18C H 0.7778 -0.2149 0.3151 0.029 Uiso 1 1 calc R . .
C19 C -0.5222(7) 0.4551(3) 0.0822(3) 0.0215(11) Uani 1 1 d . . .
H19A H -0.418 0.4133 0.0564 0.032 Uiso 1 1 calc R . .
H19B H -0.65 0.4325 0.0571 0.032 Uiso 1 1 calc R . .
H19C H -0.5187 0.4454 0.1469 0.032 Uiso 1 1 calc R . .
C20 C -0.6837(6) 0.6388(4) 0.1190(3) 0.0235(11) Uani 1 1 d . . .
H20A H -0.6656 0.6182 0.1815 0.035 Uiso 1 1 calc R . .
H20B H -0.8079 0.6102 0.0947 0.035 Uiso 1 1 calc R . .
H20C H -0.6865 0.7153 0.1147 0.035 Uiso 1 1 calc R . .
N1 N 0.0865(5) 0.1103(3) 0.3514(2) 0.0151(9) Uani 1 1 d . . .
N2 N 0.4177(5) 0.1948(3) 0.3342(2) 0.0140(9) Uani 1 1 d . . .
N3 N 0.4264(5) 0.1744(3) 0.1662(2) 0.0132(9) Uani 1 1 d . . .
N4 N 0.0983(5) 0.0852(3) 0.1445(2) 0.0112(8) Uani 1 1 d . . .
N5 N 0.1132(5) 0.2746(3) 0.2316(2) 0.0118(8) Uani 1 1 d . . .
N6 N 0.0018(5) 0.4333(3) 0.2585(2) 0.0147(9) Uani 1 1 d . . .
N7 N 0.3510(5) -0.0002(3) 0.2630(2) 0.0139(9) Uani 1 1 d . . .
N8 N 0.5503(5) -0.1339(3) 0.2622(2) 0.0163(8) Uani 1 1 d . . .
O1 O -0.0866(4) 0.0686(2) 0.34946(18) 0.0171(7) Uani 1 1 d . . .
O2 O -0.0731(4) 0.0417(2) 0.14302(18) 0.0181(7) Uani 1 1 d . . .
O3 O 0.1438(4) 0.3497(3) -0.0709(2) 0.0295(8) Uani 1 1 d . . .
O4 O 0.0480(5) 0.5224(3) -0.0433(2) 0.0445(10) Uani 1 1 d . . .
O5 O -0.1873(5) 0.3866(3) -0.0489(2) 0.0530(12) Uani 1 1 d . . .
O6 O -0.0447(4) 0.4439(3) -0.17915(18) 0.0307(9) Uani 1 1 d . . .
O7 O -0.2979(4) 0.6214(2) 0.10598(19) 0.0244(8) Uani 1 1 d . . .
Cl1 Cl -0.01070(16) 0.42596(10) -0.08541(7) 0.0233(3) Uani 1 1 d . . .
Co1 Co 0.23875(7) 0.13894(5) 0.24832(4) 0.01279(15) Uani 1 1 d . . .
S1 S -0.48566(16) 0.58924(9) 0.05727(7) 0.0219(3) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.316(5) . ?
C1 C2 1.462(6) . ?
C1 C7 1.496(6) . ?
C2 N2 1.280(5) . ?
C2 C8 1.487(6) . ?
C3 N2 1.461(5) . ?
C3 C4 1.513(6) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 N3 1.486(5) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 N3 1.287(5) . ?
C5 C6 1.462(6) . ?
C5 C9 1.492(6) . ?
C6 N4 1.315(5) . ?
C6 C10 1.499(5) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C12 1.346(6) . ?
C11 N5 1.381(5) . ?
C11 H11 0.95 . ?
C12 N6 1.366(5) . ?
C12 H12 0.95 . ?
C13 N5 1.337(5) . ?
C13 N6 1.344(5) . ?
C13 H13 0.95 . ?
C14 N6 1.453(5) . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 N7 1.361(5) . ?
C15 C16 1.368(6) . ?
C15 H15 0.95 . ?
C16 N8 1.379(5) . ?
C16 H16 0.95 . ?
C17 N8 1.329(5) . ?
C17 N7 1.334(5) . ?
C17 H17 0.95 . ?
C18 N8 1.453(5) . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C19 S1 1.774(4) . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C20 S1 1.783(4) . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
N1 O1 1.294(4) . ?
N1 Co1 1.932(3) . ?
N2 Co1 1.884(3) . ?
N3 Co1 1.866(3) . ?
N4 O2 1.293(4) . ?
N4 Co1 1.927(3) . ?
N5 Co1 1.945(3) . ?
N7 Co1 1.945(4) . ?
O3 Cl1 1.445(3) . ?
O4 Cl1 1.435(3) . ?
O5 Cl1 1.432(3) . ?
O6 Cl1 1.438(3) . ?
O7 S1 1.508(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
N1 C1 C2 114.5(4) . . ?
N1 C1 C7 122.7(4) . . ?
C2 C1 C7 122.7(4) . . ?
N2 C2 C1 113.8(4) . . ?
N2 C2 C8 125.2(4) . . ?
C1 C2 C8 121.1(4) . . ?
N2 C3 C4 109.6(3) . . ?
N2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
N2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
N3 C4 C3 109.3(3) . . ?
N3 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
N3 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
N3 C5 C6 114.5(4) . . ?
N3 C5 C9 124.2(4) . . ?
C6 C5 C9 121.3(4) . . ?
N4 C6 C5 113.5(4) . . ?
N4 C6 C10 122.5(4) . . ?
C5 C6 C10 123.9(4) . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10A 109.5 . . ?
C6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N5 110.3(4) . . ?
C12 C11 H11 124.9 . . ?
N5 C11 H11 124.9 . . ?
C11 C12 N6 106.3(4) . . ?
C11 C12 H12 126.8 . . ?
N6 C12 H12 126.8 . . ?
N5 C13 N6 110.9(4) . . ?
N5 C13 H13 124.5 . . ?
N6 C13 H13 124.5 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 C16 108.7(4) . . ?
N7 C15 H15 125.7 . . ?
C16 C15 H15 125.7 . . ?
C15 C16 N8 106.0(4) . . ?
C15 C16 H16 127 . . ?
N8 C16 H16 127 . . ?
N8 C17 N7 110.1(4) . . ?
N8 C17 H17 124.9 . . ?
N7 C17 H17 124.9 . . ?
N8 C18 H18A 109.5 . . ?
N8 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N8 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
S1 C19 H19A 109.5 . . ?
S1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
S1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
S1 C20 H20A 109.5 . . ?
S1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
S1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1 N1 C1 122.2(4) . . ?
O1 N1 Co1 125.2(3) . . ?
C1 N1 Co1 112.5(3) . . ?
C2 N2 C3 128.0(4) . . ?
C2 N2 Co1 116.1(3) . . ?
C3 N2 Co1 115.7(3) . . ?
C5 N3 C4 128.0(4) . . ?
C5 N3 Co1 115.7(3) . . ?
C4 N3 Co1 116.1(3) . . ?
O2 N4 C6 120.9(4) . . ?
O2 N4 Co1 126.1(3) . . ?
C6 N4 Co1 113.0(3) . . ?
C13 N5 C11 104.7(4) . . ?
C13 N5 Co1 126.8(3) . . ?
C11 N5 Co1 128.2(3) . . ?
C13 N6 C12 107.7(4) . . ?
C13 N6 C14 126.7(4) . . ?
C12 N6 C14 125.6(4) . . ?
C17 N7 C15 107.1(4) . . ?
C17 N7 Co1 128.5(3) . . ?
C15 N7 Co1 124.3(3) . . ?
C17 N8 C16 108.1(3) . . ?
C17 N8 C18 125.2(4) . . ?
C16 N8 C18 126.6(4) . . ?
O5 Cl1 O4 110.9(2) . . ?
O5 Cl1 O6 108.9(2) . . ?
O4 Cl1 O6 109.1(2) . . ?
O5 Cl1 O3 108.9(2) . . ?
O4 Cl1 O3 108.8(2) . . ?
O6 Cl1 O3 110.19(19) . . ?
N3 Co1 N2 85.38(15) . . ?
N3 Co1 N4 83.27(15) . . ?
N2 Co1 N4 168.52(15) . . ?
N3 Co1 N1 168.07(16) . . ?
N2 Co1 N1 82.80(15) . . ?
N4 Co1 N1 108.48(16) . . ?
N3 Co1 N7 91.19(15) . . ?
N2 Co1 N7 91.52(15) . . ?
N4 Co1 N7 86.99(14) . . ?
N1 Co1 N7 87.49(15) . . ?
N3 Co1 N5 90.40(14) . . ?
N2 Co1 N5 91.23(15) . . ?
N4 Co1 N5 90.58(14) . . ?
N1 Co1 N5 91.49(14) . . ?
N7 Co1 N5 176.92(15) . . ?
O7 S1 C19 106.5(2) . . ?
O7 S1 C20 107.18(19) . . ?
C19 S1 C20 96.8(2) . . ?




# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dh_160_0ma
_database_code_depnum_ccdc_archive 'CCDC 1038275'
_audit_update_record             
;
2015-10-27 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_date             2013-07-23T12:51:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
Complex 2
;
_chemical_name_common            dh_160
_chemical_formula_moiety         'C18 H28 Br2 Co N8 O2 Zn, Cl O4'
_chemical_formula_sum            'C18 H28 Br2 Cl Co N8 O6 Zn'
_chemical_formula_weight         772.05
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P c'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_Int_Tables_number      7
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'



_cell_length_a                   17.567(3)
_cell_length_b                   10.0243(16)
_cell_length_c                   15.749(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.334(9)
_cell_angle_gamma                90
_cell_volume                     2709.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    326
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_special_details           
;
 30 sec. 0.5 deg., 40 mm
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.7927
_exptl_absorpt_correction_T_max  0.9457

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_number            123719
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             13533
_reflns_number_gt                11634
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0193P)²+4.0205P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         13533
_refine_ls_number_parameters     741
_refine_ls_number_restraints     83
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0666
_refine_ls_wR_factor_gt          0.0621
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.102(5)
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.087

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.8129(2) 0.8547(3) 0.9771(2) 0.0196(7) Uani 1 1 d . . .
C2 C 0.7785(2) 0.7610(3) 1.0298(2) 0.0202(7) Uani 1 1 d . . .
C3 C 0.7039(2) 0.7531(3) 1.1446(2) 0.0219(8) Uani 1 1 d . . .
H3A H 0.743 0.7051 1.1886 0.026 Uiso 1 1 calc R . .
H3B H 0.6654 0.6874 1.1144 0.026 Uiso 1 1 calc R . .
C4 C 0.6628(3) 0.8586(4) 1.1892(3) 0.0271(9) Uani 1 1 d . . .
H4A H 0.6063 0.8585 1.1633 0.032 Uiso 1 1 calc R . .
H4B H 0.67 0.8378 1.2518 0.032 Uiso 1 1 calc R . .
C5 C 0.6848(2) 1.0993(3) 1.2164(2) 0.0174(7) Uani 1 1 d . . .
C6 C 0.7187(2) 1.2164(3) 1.1830(2) 0.0169(7) Uani 1 1 d . . .
C7 C 0.7141(2) 1.3557(3) 1.2139(2) 0.0194(7) Uani 1 1 d . . .
H7A H 0.6837 1.41 1.1668 0.029 Uiso 1 1 calc R . .
H7B H 0.7667 1.3926 1.2316 0.029 Uiso 1 1 calc R . .
H7C H 0.6887 1.3564 1.2636 0.029 Uiso 1 1 calc R . .
C8 C 0.6430(2) 1.1083(4) 1.2889(2) 0.0218(8) Uani 1 1 d . . .
H8A H 0.6445 1.0214 1.3177 0.033 Uiso 1 1 d R . .
H8B H 0.5887 1.1342 1.2659 0.033 Uiso 1 1 d R . .
H8C H 0.6683 1.1753 1.3309 0.033 Uiso 1 1 d R . .
C9 C 0.7881(2) 0.6144(3) 1.0223(3) 0.0238(8) Uani 1 1 d . . .
H9A H 0.7556 0.5829 0.9675 0.036 Uiso 1 1 calc R . .
H9B H 0.7722 0.5698 1.0711 0.036 Uiso 1 1 calc R . .
H9C H 0.8429 0.594 1.0235 0.036 Uiso 1 1 calc R . .
C10 C 0.8525(3) 0.8150(4) 0.9058(2) 0.0281(9) Uani 1 1 d . . .
H10A H 0.9076 0.8409 0.9213 0.042 Uiso 1 1 calc R . .
H10B H 0.8274 0.8599 0.8518 0.042 Uiso 1 1 calc R . .
H10C H 0.8486 0.7181 0.8974 0.042 Uiso 1 1 calc R . .
N5 N 0.6559(15) 1.0356(18) 1.008(3) 0.0187(15) Uani 0.7111(15) 1 d PDU A 1
N6 N 0.5382(4) 1.0110(6) 0.9298(4) 0.0224(16) Uani 0.7111(15) 1 d PD A 1
C11 C 0.6318(5) 1.1553(11) 0.9660(7) 0.024(2) Uani 0.7111(15) 1 d PD A 1
H11 H 0.6619 1.2348 0.9696 0.029 Uiso 0.7111(15) 1 calc PR A 1
C12 C 0.5573(7) 1.1390(9) 0.9184(8) 0.030(2) Uani 0.7111(15) 1 d PD A 1
H12 H 0.5256 1.2046 0.8844 0.035 Uiso 0.7111(15) 1 calc PR A 1
C13 C 0.5978(7) 0.9517(8) 0.9830(7) 0.022(2) Uani 0.7111(15) 1 d PD A 1
H13 H 0.5982 0.8611 1.0006 0.027 Uiso 0.7111(15) 1 calc PR A 1
C14 C 0.4643(4) 0.9525(6) 0.8947(4) 0.0354(13) Uani 0.7111(15) 1 d PD A 1
H14A H 0.4687 0.8551 0.8982 0.053 Uiso 0.7111(15) 1 calc PR A 1
H14B H 0.4469 0.9795 0.8338 0.053 Uiso 0.7111(15) 1 calc PR A 1
H14C H 0.4263 0.9828 0.928 0.053 Uiso 0.7111(15) 1 calc PR A 1
N5B N 0.652(4) 1.021(5) 1.006(7) 0.0187(15) Uani 0.2889(15) 1 d PD A 2
N6B N 0.5521(14) 1.110(2) 0.9173(16) 0.0224(16) Uani 0.2889(15) 1 d PD A 2
C11B C 0.595(2) 0.924(3) 0.981(2) 0.024(2) Uani 0.2889(15) 1 d PD A 2
H11B H 0.5971 0.8348 1.0019 0.029 Uiso 0.2889(15) 1 calc PR A 2
C12B C 0.5344(17) 0.979(3) 0.9195(17) 0.030(2) Uani 0.2889(15) 1 d PD A 2
H12B H 0.4903 0.9342 0.8863 0.035 Uiso 0.2889(15) 1 calc PR A 2
C13B C 0.6203(13) 1.132(3) 0.9700(18) 0.022(2) Uani 0.2889(15) 1 d PD A 2
H13B H 0.6437 1.2179 0.9807 0.027 Uiso 0.2889(15) 1 calc PR A 2
C14B C 0.5030(9) 1.2087(15) 0.8633(10) 0.0354(13) Uani 0.2889(15) 1 d PD A 2
H14D H 0.535 1.2845 0.853 0.053 Uiso 0.2889(15) 1 calc PR A 2
H14E H 0.4627 1.2396 0.8931 0.053 Uiso 0.2889(15) 1 calc PR A 2
H14F H 0.4784 1.168 0.8076 0.053 Uiso 0.2889(15) 1 calc PR A 2
N7 N 0.8469(10) 0.9821(16) 1.1736(16) 0.0166(12) Uani 0.7111(15) 1 d PD A 1
N8 N 0.9685(4) 1.0139(5) 1.2382(4) 0.0316(14) Uani 0.7111(15) 1 d PD A 1
C15 C 0.8613(4) 0.9167(8) 1.2513(4) 0.0253(15) Uani 0.7111(15) 1 d PD A 1
H15 H 0.8244 0.8661 1.2739 0.03 Uiso 0.7111(15) 1 calc PR A 1
C16 C 0.9364(4) 0.9354(10) 1.2909(5) 0.0287(17) Uani 0.7111(15) 1 d PD A 1
H16 H 0.962 0.9001 1.3455 0.034 Uiso 0.7111(15) 1 calc PR A 1
C17 C 0.9136(4) 1.0404(6) 1.1672(4) 0.0250(14) Uani 0.7111(15) 1 d PD A 1
H17 H 0.9211 1.0928 1.1194 0.03 Uiso 0.7111(15) 1 calc PR A 1
C18 C 1.0492(4) 1.0541(7) 1.2525(5) 0.0444(15) Uani 0.7111(15) 1 d PD A 1
H18A H 1.082 0.9753 1.2513 0.067 Uiso 0.7111(15) 1 calc PR A 1
H18B H 1.0644 1.0981 1.3091 0.067 Uiso 0.7111(15) 1 calc PR A 1
H18C H 1.056 1.1162 1.2066 0.067 Uiso 0.7111(15) 1 calc PR A 1
N7B N 0.857(3) 0.997(4) 1.175(4) 0.0166(12) Uani 0.2889(15) 1 d PD A 2
N8B N 0.9513(7) 0.9415(19) 1.2834(11) 0.0316(14) Uani 0.2889(15) 1 d PD A 2
C15B C 0.9159(10) 1.0864(14) 1.1802(9) 0.0253(15) Uani 0.2889(15) 1 d PD A 2
H15B H 0.9154 1.162 1.1437 0.03 Uiso 0.2889(15) 1 calc PR A 2
C16B C 0.9751(10) 1.0501(16) 1.2454(12) 0.0287(17) Uani 0.2889(15) 1 d PD A 2
H16B H 1.0243 1.0928 1.2616 0.034 Uiso 0.2889(15) 1 calc PR A 2
C17B C 0.8797(7) 0.910(2) 1.2393(11) 0.0250(14) Uani 0.2889(15) 1 d PD A 2
H17B H 0.8499 0.8363 1.252 0.03 Uiso 0.2889(15) 1 calc PR A 2
C18B C 0.9985(8) 0.8618(15) 1.3511(9) 0.0444(15) Uani 0.2889(15) 1 d PD A 2
H18D H 0.9699 0.7811 1.3603 0.067 Uiso 0.2889(15) 1 calc PR A 2
H18E H 1.0108 0.9136 1.4051 0.067 Uiso 0.2889(15) 1 calc PR A 2
H18F H 1.047 0.8367 1.3339 0.067 Uiso 0.2889(15) 1 calc PR A 2
C19 C 0.2683(2) 0.2797(3) 0.8423(2) 0.0152(7) Uani 1 1 d . . .
C20 C 0.3056(2) 0.3924(3) 0.8951(2) 0.0166(7) Uani 1 1 d . . .
C21 C 0.3242(2) 0.6356(4) 0.8922(2) 0.0237(8) Uani 1 1 d . . .
H21A H 0.3814 0.6364 0.8981 0.028 Uiso 1 1 calc R . .
H21B H 0.3128 0.6506 0.9504 0.028 Uiso 1 1 calc R . .
C22 C 0.2871(2) 0.7457(4) 0.8302(2) 0.0234(8) Uani 1 1 d . . .
H22A H 0.2463 0.7915 0.8539 0.028 Uiso 1 1 calc R . .
H22B H 0.3271 0.8124 0.8239 0.028 Uiso 1 1 calc R . .
C23 C 0.2229(2) 0.7512(3) 0.6748(2) 0.0221(8) Uani 1 1 d . . .
C24 C 0.1877(2) 0.6641(3) 0.6020(2) 0.0176(7) Uani 1 1 d . . .
C25 C 0.1574(2) 0.7134(4) 0.5122(2) 0.0260(8) Uani 1 1 d . . .
H25A H 0.1004 0.7084 0.4986 0.039 Uiso 1 1 d R . .
H25B H 0.1782 0.6582 0.4711 0.039 Uiso 1 1 d R . .
H25C H 0.1737 0.8062 0.5078 0.039 Uiso 1 1 d R . .
C26 C 0.2221(3) 0.8984(4) 0.6660(3) 0.0363(11) Uani 1 1 d . . .
H26A H 0.2591 0.9253 0.6306 0.054 Uiso 1 1 calc R . .
H26B H 0.2371 0.9392 0.7237 0.054 Uiso 1 1 calc R . .
H26C H 0.1696 0.928 0.6379 0.054 Uiso 1 1 calc R . .
C27 C 0.3546(2) 0.3744(4) 0.9854(2) 0.0270(9) Uani 1 1 d . . .
H27A H 0.3383 0.4386 1.0248 0.041 Uiso 1 1 d R . .
H27B H 0.4096 0.3892 0.9843 0.041 Uiso 1 1 d R . .
H27C H 0.3479 0.2835 1.0055 0.041 Uiso 1 1 d R . .
C28 C 0.2740(2) 0.1374(3) 0.8678(2) 0.0228(8) Uani 1 1 d . . .
H28A H 0.3013 0.0881 0.8295 0.034 Uiso 1 1 calc R . .
H28B H 0.2215 0.1005 0.8626 0.034 Uiso 1 1 calc R . .
H28C H 0.3029 0.1293 0.9281 0.034 Uiso 1 1 calc R . .
N13B N 0.1370(15) 0.524(11) 0.777(3) 0.015(2) Uani 0.2889(15) 1 d PD A 2
N14B N 0.0141(10) 0.502(2) 0.7797(15) 0.0318(19) Uani 0.2889(15) 1 d PD A 2
C29B C 0.1226(15) 0.582(2) 0.8510(16) 0.0164(16) Uani 0.2889(15) 1 d PD A 2
H29B H 0.1612 0.6209 0.8957 0.02 Uiso 0.2889(15) 1 calc PR A 2
C30B C 0.0464(16) 0.576(4) 0.8516(18) 0.023(2) Uani 0.2889(15) 1 d PD A 2
H30B H 0.0205 0.615 0.8927 0.027 Uiso 0.2889(15) 1 calc PR A 2
C31B C 0.0682(12) 0.481(2) 0.7337(14) 0.0275(17) Uani 0.2889(15) 1 d PD A 2
H31B H 0.059 0.4397 0.678 0.033 Uiso 0.2889(15) 1 calc PR A 2
C32B C -0.0697(11) 0.468(2) 0.7497(16) 0.054(2) Uani 0.2889(15) 1 d PD A 2
H32A H -0.0982 0.5462 0.7225 0.08 Uiso 0.2889(15) 1 calc PR A 2
H32B H -0.091 0.4398 0.7995 0.08 Uiso 0.2889(15) 1 calc PR A 2
H32C H -0.0751 0.395 0.7073 0.08 Uiso 0.2889(15) 1 calc PR A 2
N13 N 0.1382(6) 0.535(4) 0.7792(14) 0.015(2) Uani 0.7111(15) 1 d PDU A 1
N14 N 0.0135(4) 0.5428(7) 0.7736(5) 0.0318(19) Uani 0.7111(15) 1 d PDU A 1
C29 C 0.1267(5) 0.5539(7) 0.8624(5) 0.0164(16) Uani 0.7111(15) 1 d PDU A 1
H29 H 0.1666 0.5636 0.9133 0.02 Uiso 0.7111(15) 1 calc PR A 1
C30 C 0.0496(6) 0.5564(14) 0.8596(7) 0.023(2) Uani 0.7111(15) 1 d PDU A 1
H30 H 0.025 0.5656 0.9074 0.027 Uiso 0.7111(15) 1 calc PR A 1
C31 C 0.0678(5) 0.5285(6) 0.7269(5) 0.0275(17) Uani 0.7111(15) 1 d PDU A 1
H31 H 0.058 0.5158 0.6657 0.033 Uiso 0.7111(15) 1 calc PR A 1
C32 C -0.0721(4) 0.5368(10) 0.7382(6) 0.054(2) Uani 0.7111(15) 1 d PDU A 1
H32D H -0.091 0.6251 0.7166 0.08 Uiso 0.7111(15) 1 calc PR A 1
H32E H -0.0985 0.5093 0.7843 0.08 Uiso 0.7111(15) 1 calc PR A 1
H32F H -0.0833 0.4722 0.6905 0.08 Uiso 0.7111(15) 1 calc PR A 1
C33 C 0.3479(2) 0.3496(4) 0.6646(2) 0.0219(8) Uani 1 1 d . . .
H33 H 0.3141 0.2754 0.6497 0.026 Uiso 1 1 calc R . .
C34 C 0.4211(2) 0.3586(4) 0.6520(2) 0.0232(8) Uani 1 1 d . . .
H34 H 0.4483 0.2926 0.627 0.028 Uiso 1 1 calc R . .
C35 C 0.3931(2) 0.5434(4) 0.7123(2) 0.0189(7) Uani 1 1 d . . .
H35 H 0.3977 0.6302 0.737 0.023 Uiso 1 1 calc R . .
C36 C 0.5278(2) 0.5318(5) 0.6865(3) 0.0317(10) Uani 1 1 d . . .
H36A H 0.5273 0.6295 0.6887 0.048 Uiso 1 1 calc R . .
H36B H 0.5462 0.5027 0.635 0.048 Uiso 1 1 calc R . .
H36C H 0.5627 0.4972 0.7389 0.048 Uiso 1 1 calc R . .
N1 N 0.80498(19) 0.9800(3) 0.99764(18) 0.0195(6) Uani 1 1 d . A .
N2 N 0.74239(19) 0.8186(3) 1.08174(19) 0.0196(6) Uani 1 1 d . A .
N3 N 0.69601(17) 0.9908(3) 1.17804(18) 0.0180(6) Uani 1 1 d . A .
N4 N 0.75315(18) 1.1882(3) 1.11919(18) 0.0171(6) Uani 1 1 d . A .
N9 N 0.22928(17) 0.3174(3) 0.76554(17) 0.0140(6) Uani 1 1 d . A .
N10 N 0.29227(17) 0.5057(3) 0.85769(17) 0.0162(6) Uani 1 1 d . A .
N11 N 0.25264(17) 0.6874(3) 0.74486(18) 0.0175(6) Uani 1 1 d . A .
N12 N 0.18632(16) 0.5390(3) 0.62435(18) 0.0150(6) Uani 1 1 d . A .
N15 N 0.33027(17) 0.4669(3) 0.70305(18) 0.0159(6) Uani 1 1 d . A .
N16 N 0.44895(17) 0.4811(3) 0.68210(19) 0.0209(6) Uani 1 1 d . . .
O1 O 0.83326(18) 1.0717(2) 0.95370(17) 0.0292(7) Uani 1 1 d . A .
O2 O 0.78508(15) 1.2868(2) 1.08418(15) 0.0201(5) Uani 1 1 d . A .
O3 O 0.19413(14) 0.2246(2) 0.71155(15) 0.0162(5) Uani 1 1 d . . .
O4 O 0.15776(15) 0.4501(2) 0.56492(15) 0.0180(5) Uani 1 1 d . . .
O5 O 0.60733(19) 0.4690(3) 1.00486(18) 0.0353(7) Uani 1 1 d . . .
O6 O 0.60595(18) 0.6384(3) 0.9033(2) 0.0380(7) Uani 1 1 d . . .
O7 O 0.52215(18) 0.6482(3) 1.0006(2) 0.0408(8) Uani 1 1 d . . .
O8 O 0.5009(2) 0.4888(5) 0.8884(2) 0.0687(13) Uani 1 1 d . . .
O9 O 0.4163(3) 0.8543(4) 0.6997(3) 0.0784(14) Uani 1 1 d . . .
O10 O 0.5036(3) 0.8562(4) 0.6083(3) 0.0687(12) Uani 1 1 d . . .
O11 O 0.4766(2) 1.0496(3) 0.6759(3) 0.0599(11) Uani 1 1 d . . .
O12 O 0.3817(2) 0.9576(5) 0.5667(3) 0.0809(14) Uani 1 1 d . . .
Cl1 Cl 0.55943(6) 0.56078(10) 0.94870(6) 0.0262(2) Uani 1 1 d . . .
Cl2 Cl 0.44366(7) 0.93199(11) 0.63798(7) 0.0367(2) Uani 1 1 d . . .
Co1 Co 0.75118(3) 1.00357(4) 1.09029(3) 0.01574(10) Uani 1 1 d . . .
Co2 Co 0.23589(3) 0.50425(4) 0.74311(3) 0.01295(9) Uani 1 1 d . . .
Zn1 Zn 0.83135(3) 1.26301(4) 0.98112(3) 0.03295(12) Uani 1 1 d . . .
Zn2 Zn 0.13203(3) 0.26379(4) 0.59259(3) 0.02152(9) Uani 1 1 d . . .
Br1 Br 0.95545(6) 1.33990(10) 1.01297(8) 0.0553(3) Uani 0.7111(15) 1 d P A 1
Br2 Br 0.74702(7) 1.36603(7) 0.85563(5) 0.0424(3) Uani 0.7111(15) 1 d P A 1
Br2B Br 0.79140(17) 1.3699(2) 0.86040(13) 0.0424(3) Uani 0.2889(15) 1 d P A 2
Br1B Br 0.97129(16) 1.3375(3) 1.05716(19) 0.0553(3) Uani 0.2889(15) 1 d P A 2
Br3 Br 0.17658(4) 0.13142(4) 0.48925(3) 0.04618(14) Uani 1 1 d . . .
Br4 Br 0.00020(3) 0.23793(6) 0.59718(4) 0.05813(17) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.311(4) . ?
C1 C2 1.467(5) . ?
C1 C10 1.497(5) . ?
C2 N2 1.275(5) . ?
C2 C9 1.487(5) . ?
C3 N2 1.468(5) . ?
C3 C4 1.532(5) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 N3 1.473(5) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 N3 1.279(4) . ?
C5 C6 1.463(5) . ?
C5 C8 1.487(5) . ?
C6 N4 1.310(4) . ?
C6 C7 1.487(5) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
N5 C13 1.316(14) . ?
N5 C11 1.392(15) . ?
N5 Co1 1.913(10) . ?
N6 C13 1.333(9) . ?
N6 C12 1.348(8) . ?
N6 C14 1.424(9) . ?
C11 C12 1.373(11) . ?
C11 H11 0.95 . ?
C12 H12 0.95 . ?
C13 H13 0.95 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
N5B C13B 1.31(3) . ?
N5B C11B 1.39(3) . ?
N5B Co1 1.97(2) . ?
N6B C13B 1.323(19) . ?
N6B C12B 1.355(15) . ?
N6B C14B 1.458(17) . ?
C11B C12B 1.39(2) . ?
C11B H11B 0.95 . ?
C12B H12B 0.95 . ?
C13B H13B 0.95 . ?
C14B H14D 0.98 . ?
C14B H14E 0.98 . ?
C14B H14F 0.98 . ?
N7 C17 1.333(18) . ?
N7 C15 1.364(17) . ?
N7 Co1 1.911(4) . ?
N8 C17 1.338(8) . ?
N8 C16 1.351(7) . ?
N8 C18 1.444(9) . ?
C15 C16 1.346(9) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?
C17 H17 0.95 . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
N7B C17B 1.332(18) . ?
N7B C15B 1.364(17) . ?
N7B Co1 2.039(11) . ?
N8B C17B 1.338(8) . ?
N8B C16B 1.351(7) . ?
N8B C18B 1.445(9) . ?
C15B C16B 1.346(9) . ?
C15B H15B 0.95 . ?
C16B H16B 0.95 . ?
C17B H17B 0.95 . ?
C18B H18D 0.98 . ?
C18B H18E 0.98 . ?
C18B H18F 0.98 . ?
C19 N9 1.312(4) . ?
C19 C20 1.471(5) . ?
C19 C28 1.479(5) . ?
C20 N10 1.278(4) . ?
C20 C27 1.507(5) . ?
C21 N10 1.475(4) . ?
C21 C22 1.525(5) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C22 N11 1.472(4) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C23 N11 1.285(5) . ?
C23 C24 1.469(5) . ?
C23 C26 1.482(5) . ?
C24 N12 1.304(4) . ?
C24 C25 1.485(5) . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
C28 H28A 0.98 . ?
C28 H28B 0.98 . ?
C28 H28C 0.98 . ?
N13B C31B 1.328(18) . ?
N13B C29B 1.376(18) . ?
N13B Co2 1.93(2) . ?
N14B C31B 1.330(14) . ?
N14B C30B 1.374(16) . ?
N14B C32B 1.485(14) . ?
C29B C30B 1.342(15) . ?
C29B H29B 0.95 . ?
C30B H30B 0.95 . ?
C31B H31B 0.95 . ?
C32B H32A 0.98 . ?
C32B H32B 0.98 . ?
C32B H32C 0.98 . ?
N13 C31 1.333(13) . ?
N13 C29 1.382(13) . ?
N13 Co2 1.944(10) . ?
N14 C31 1.332(7) . ?
N14 C30 1.374(9) . ?
N14 C32 1.489(8) . ?
C29 C30 1.346(7) . ?
C29 H29 0.95 . ?
C30 H30 0.95 . ?
C31 H31 0.95 . ?
C32 H32D 0.98 . ?
C32 H32E 0.98 . ?
C32 H32F 0.98 . ?
C33 C34 1.345(5) . ?
C33 N15 1.387(4) . ?
C33 H33 0.95 . ?
C34 N16 1.368(5) . ?
C34 H34 0.95 . ?
C35 N15 1.326(4) . ?
C35 N16 1.334(5) . ?
C35 H35 0.95 . ?
C36 N16 1.463(5) . ?
C36 H36A 0.98 . ?
C36 H36B 0.98 . ?
C36 H36C 0.98 . ?
N1 O1 1.311(4) . ?
N1 Co1 1.915(3) . ?
N2 Co1 1.863(3) . ?
N3 Co1 1.854(3) . ?
N4 O2 1.315(4) . ?
N4 Co1 1.904(3) . ?
N9 O3 1.321(4) . ?
N9 Co2 1.914(3) . ?
N10 Co2 1.864(3) . ?
N11 Co2 1.859(3) . ?
N12 O4 1.312(4) . ?
N12 Co2 1.919(3) . ?
N15 Co2 1.932(3) . ?
O1 Zn1 1.967(3) . ?
O2 Zn1 1.979(2) . ?
O3 Zn2 1.995(2) . ?
O4 Zn2 1.991(2) . ?
O5 Cl1 1.421(3) . ?
O6 Cl1 1.426(3) . ?
O7 Cl1 1.447(3) . ?
O8 Cl1 1.436(3) . ?
O9 Cl2 1.407(4) . ?
O10 Cl2 1.455(4) . ?
O11 Cl2 1.391(3) . ?
O12 Cl2 1.410(4) . ?
Zn1 Br2B 2.165(2) . ?
Zn1 Br1 2.2652(12) . ?
Zn1 Br2 2.4323(11) . ?
Zn1 Br1B 2.603(3) . ?
Zn2 Br4 2.3469(8) . ?
Zn2 Br3 2.3592(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 113.3(3) . . ?
N1 C1 C10 122.1(3) . . ?
C2 C1 C10 124.6(3) . . ?
N2 C2 C1 113.2(3) . . ?
N2 C2 C9 125.4(3) . . ?
C1 C2 C9 121.4(3) . . ?
N2 C3 C4 109.3(3) . . ?
N2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
N2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
N3 C4 C3 109.2(3) . . ?
N3 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
N3 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
N3 C5 C6 113.4(3) . . ?
N3 C5 C8 124.4(3) . . ?
C6 C5 C8 122.2(3) . . ?
N4 C6 C5 113.1(3) . . ?
N4 C6 C7 121.3(3) . . ?
C5 C6 C7 125.6(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C9 H9A 109.5 . . ?
C2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 N5 C11 105.7(6) . . ?
C13 N5 Co1 127.3(13) . . ?
C11 N5 Co1 126.9(10) . . ?
C13 N6 C12 108.8(7) . . ?
C13 N6 C14 126.1(7) . . ?
C12 N6 C14 124.9(7) . . ?
C12 C11 N5 108.3(7) . . ?
C12 C11 H11 125.9 . . ?
N5 C11 H11 125.9 . . ?
N6 C12 C11 106.1(7) . . ?
N6 C12 H12 127 . . ?
C11 C12 H12 127 . . ?
N5 C13 N6 111.0(8) . . ?
N5 C13 H13 124.5 . . ?
N6 C13 H13 124.5 . . ?
C13B N5B C11B 105.3(15) . . ?
C13B N5B Co1 127(3) . . ?
C11B N5B Co1 127(3) . . ?
C13B N6B C12B 109.2(18) . . ?
C13B N6B C14B 127(2) . . ?
C12B N6B C14B 124.2(18) . . ?
C12B C11B N5B 108(2) . . ?
C12B C11B H11B 125.9 . . ?
N5B C11B H11B 125.9 . . ?
N6B C12B C11B 105.0(18) . . ?
N6B C12B H12B 127.5 . . ?
C11B C12B H12B 127.5 . . ?
N5B C13B N6B 111.6(18) . . ?
N5B C13B H13B 124.2 . . ?
N6B C13B H13B 124.2 . . ?
N6B C14B H14D 109.5 . . ?
N6B C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
N6B C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C17 N7 C15 106.3(4) . . ?
C17 N7 Co1 123.9(11) . . ?
C15 N7 Co1 129.6(13) . . ?
C17 N8 C16 107.9(6) . . ?
C17 N8 C18 125.6(7) . . ?
C16 N8 C18 126.3(7) . . ?
C16 C15 N7 108.9(7) . . ?
C16 C15 H15 125.6 . . ?
N7 C15 H15 125.6 . . ?
C15 C16 N8 107.1(6) . . ?
C15 C16 H16 126.5 . . ?
N8 C16 H16 126.5 . . ?
N7 C17 N8 109.8(8) . . ?
N7 C17 H17 125.1 . . ?
N8 C17 H17 125.1 . . ?
C17B N7B C15B 106.3(4) . . ?
C17B N7B Co1 127.3(18) . . ?
C15B N7B Co1 126.3(13) . . ?
C17B N8B C16B 107.9(7) . . ?
C17B N8B C18B 125.4(8) . . ?
C16B N8B C18B 126.2(7) . . ?
C16B C15B N7B 108.9(7) . . ?
C16B C15B H15B 125.6 . . ?
N7B C15B H15B 125.6 . . ?
C15B C16B N8B 107.1(6) . . ?
C15B C16B H16B 126.4 . . ?
N8B C16B H16B 126.4 . . ?
N7B C17B N8B 109.8(8) . . ?
N7B C17B H17B 125.1 . . ?
N8B C17B H17B 125.1 . . ?
N8B C18B H18D 109.5 . . ?
N8B C18B H18E 109.5 . . ?
H18D C18B H18E 109.5 . . ?
N8B C18B H18F 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
N9 C19 C20 112.4(3) . . ?
N9 C19 C28 121.3(3) . . ?
C20 C19 C28 126.3(3) . . ?
N10 C20 C19 114.0(3) . . ?
N10 C20 C27 123.6(3) . . ?
C19 C20 C27 122.5(3) . . ?
N10 C21 C22 109.0(3) . . ?
N10 C21 H21A 109.9 . . ?
C22 C21 H21A 109.9 . . ?
N10 C21 H21B 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
N11 C22 C21 109.5(3) . . ?
N11 C22 H22A 109.8 . . ?
C21 C22 H22A 109.8 . . ?
N11 C22 H22B 109.8 . . ?
C21 C22 H22B 109.8 . . ?
H22A C22 H22B 108.2 . . ?
N11 C23 C24 113.6(3) . . ?
N11 C23 C26 124.7(3) . . ?
C24 C23 C26 121.6(3) . . ?
N12 C24 C23 112.9(3) . . ?
N12 C24 C25 123.6(3) . . ?
C23 C24 C25 123.4(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C20 C27 H27A 109.5 . . ?
C20 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C20 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C19 C28 H28A 109.5 . . ?
C19 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C19 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C31B N13B C29B 105.2(14) . . ?
C31B N13B Co2 127(2) . . ?
C29B N13B Co2 128.1(18) . . ?
C31B N14B C30B 108.6(13) . . ?
C31B N14B C32B 124.4(17) . . ?
C30B N14B C32B 126.4(17) . . ?
C30B C29B N13B 110.6(15) . . ?
C30B C29B H29B 124.7 . . ?
N13B C29B H29B 124.7 . . ?
C29B C30B N14B 104.8(14) . . ?
C29B C30B H30B 127.6 . . ?
N14B C30B H30B 127.6 . . ?
N13B C31B N14B 110.3(14) . . ?
N13B C31B H31B 124.9 . . ?
N14B C31B H31B 124.9 . . ?
N14B C32B H32A 109.5 . . ?
N14B C32B H32B 109.5 . . ?
H32A C32B H32B 109.5 . . ?
N14B C32B H32C 109.5 . . ?
H32A C32B H32C 109.5 . . ?
H32B C32B H32C 109.5 . . ?
C31 N13 C29 106.8(6) . . ?
C31 N13 Co2 124.9(9) . . ?
C29 N13 Co2 128.0(12) . . ?
C31 N14 C30 108.7(6) . . ?
C31 N14 C32 125.1(7) . . ?
C30 N14 C32 126.1(7) . . ?
C30 C29 N13 108.7(7) . . ?
C30 C29 H29 125.7 . . ?
N13 C29 H29 125.7 . . ?
C29 C30 N14 106.3(6) . . ?
C29 C30 H30 126.8 . . ?
N14 C30 H30 126.8 . . ?
N14 C31 N13 109.5(7) . . ?
N14 C31 H31 125.3 . . ?
N13 C31 H31 125.3 . . ?
C34 C33 N15 108.5(3) . . ?
C34 C33 H33 125.8 . . ?
N15 C33 H33 125.8 . . ?
C33 C34 N16 107.0(3) . . ?
C33 C34 H34 126.5 . . ?
N16 C34 H34 126.5 . . ?
N15 C35 N16 110.4(3) . . ?
N15 C35 H35 124.8 . . ?
N16 C35 H35 124.8 . . ?
N16 C36 H36A 109.5 . . ?
N16 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N16 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O1 N1 C1 118.0(3) . . ?
O1 N1 Co1 128.3(2) . . ?
C1 N1 Co1 113.7(2) . . ?
C2 N2 C3 126.4(3) . . ?
C2 N2 Co1 116.9(3) . . ?
C3 N2 Co1 116.1(2) . . ?
C5 N3 C4 127.1(3) . . ?
C5 N3 Co1 116.8(2) . . ?
C4 N3 Co1 115.7(2) . . ?
C6 N4 O2 117.9(3) . . ?
C6 N4 Co1 113.9(2) . . ?
O2 N4 Co1 128.2(2) . . ?
C19 N9 O3 118.1(3) . . ?
C19 N9 Co2 114.3(2) . . ?
O3 N9 Co2 127.5(2) . . ?
C20 N10 C21 126.6(3) . . ?
C20 N10 Co2 116.6(2) . . ?
C21 N10 Co2 116.4(2) . . ?
C23 N11 C22 126.8(3) . . ?
C23 N11 Co2 116.4(2) . . ?
C22 N11 Co2 116.0(2) . . ?
C24 N12 O4 119.1(3) . . ?
C24 N12 Co2 114.0(2) . . ?
O4 N12 Co2 126.6(2) . . ?
C35 N15 C33 106.2(3) . . ?
C35 N15 Co2 127.1(2) . . ?
C33 N15 Co2 126.5(2) . . ?
C35 N16 C34 107.9(3) . . ?
C35 N16 C36 125.5(3) . . ?
C34 N16 C36 126.4(3) . . ?
N1 O1 Zn1 122.8(2) . . ?
N4 O2 Zn1 122.69(19) . . ?
N9 O3 Zn2 123.53(19) . . ?
N12 O4 Zn2 123.44(19) . . ?
O5 Cl1 O6 109.79(19) . . ?
O5 Cl1 O8 109.3(2) . . ?
O6 Cl1 O8 110.4(2) . . ?
O5 Cl1 O7 108.65(18) . . ?
O6 Cl1 O7 109.25(19) . . ?
O8 Cl1 O7 109.3(2) . . ?
O11 Cl2 O9 110.1(3) . . ?
O11 Cl2 O12 111.5(3) . . ?
O9 Cl2 O12 109.3(3) . . ?
O11 Cl2 O10 108.5(3) . . ?
O9 Cl2 O10 108.1(3) . . ?
O12 Cl2 O10 109.2(3) . . ?
N3 Co1 N2 86.37(13) . . ?
N3 Co1 N4 82.80(12) . . ?
N2 Co1 N4 168.94(13) . . ?
N3 Co1 N7 90.2(10) . . ?
N2 Co1 N7 89.1(5) . . ?
N4 Co1 N7 88.7(7) . . ?
N3 Co1 N5 89.8(16) . . ?
N2 Co1 N5 94.1(6) . . ?
N4 Co1 N5 88.1(7) . . ?
N7 Co1 N5 176.8(8) . . ?
N3 Co1 N1 168.82(13) . . ?
N2 Co1 N1 82.47(13) . . ?
N4 Co1 N1 108.38(12) . . ?
N7 Co1 N1 90.2(10) . . ?
N5 Co1 N1 90.4(16) . . ?
N3 Co1 N5B 89(4) . . ?
N2 Co1 N5B 89.6(14) . . ?
N4 Co1 N5B 92.4(17) . . ?
N7 Co1 N5B 179(2) . . ?
N5 Co1 N5B 4.5(19) . . ?
N1 Co1 N5B 90(4) . . ?
N3 Co1 N7B 93(2) . . ?
N2 Co1 N7B 93.7(12) . . ?
N4 Co1 N7B 84.7(16) . . ?
N7 Co1 N7B 5.3(10) . . ?
N5 Co1 N7B 171.8(9) . . ?
N1 Co1 N7B 88(3) . . ?
N5B Co1 N7B 176(2) . . ?
N11 Co2 N10 85.89(12) . . ?
N11 Co2 N9 168.37(12) . . ?
N10 Co2 N9 82.49(12) . . ?
N11 Co2 N12 82.68(12) . . ?
N10 Co2 N12 168.23(12) . . ?
N9 Co2 N12 108.95(12) . . ?
N11 Co2 N15 92.99(12) . . ?
N10 Co2 N15 90.11(12) . . ?
N9 Co2 N15 87.75(12) . . ?
N12 Co2 N15 87.67(12) . . ?
N11 Co2 N13B 92(3) . . ?
N10 Co2 N13B 93.2(15) . . ?
N9 Co2 N13B 88(3) . . ?
N12 Co2 N13B 90(2) . . ?
N15 Co2 N13B 174(2) . . ?
N11 Co2 N13 89.2(12) . . ?
N10 Co2 N13 92.0(6) . . ?
N9 Co2 N13 90.5(14) . . ?
N12 Co2 N13 90.6(8) . . ?
N15 Co2 N13 177.0(6) . . ?
N13B Co2 N13 3(4) . . ?
O1 Zn1 O2 109.08(10) . . ?
O1 Zn1 Br2B 107.89(10) . . ?
O2 Zn1 Br2B 123.22(10) . . ?
O1 Zn1 Br1 108.63(10) . . ?
O2 Zn1 Br1 108.78(8) . . ?
Br2B Zn1 Br1 98.18(8) . . ?
O1 Zn1 Br2 105.75(9) . . ?
O2 Zn1 Br2 109.25(8) . . ?
Br2B Zn1 Br2 18.05(7) . . ?
Br1 Zn1 Br2 115.20(4) . . ?
O1 Zn1 Br1B 108.77(12) . . ?
O2 Zn1 Br1B 95.80(10) . . ?
Br2B Zn1 Br1B 111.05(9) . . ?
Br1 Zn1 Br1B 14.30(5) . . ?
Br2 Zn1 Br1B 127.11(7) . . ?
O4 Zn2 O3 106.62(9) . . ?
O4 Zn2 Br4 112.45(8) . . ?
O3 Zn2 Br4 107.12(7) . . ?
O4 Zn2 Br3 104.61(7) . . ?
O3 Zn2 Br3 109.98(7) . . ?
Br4 Zn2 Br3 115.73(3) . . ?



# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dh2_135c_0ma
_database_code_depnum_ccdc_archive 'CCDC 1038276'
_audit_update_record             
;
2014-12-09 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_date             2014-02-25T14:35:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 dh2_135c
;
_chemical_name_common            dh2_135c
_chemical_formula_moiety         '16(C38 H44 Co N12 O2 Ru), C8 H12 N4, 48(F6 P)'
_chemical_formula_sum            'C616 H716 Co16 F288 N196 O32 P48 Ru16'
_chemical_formula_weight         20896.41

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_Int_Tables_number      88
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'



_cell_length_a                   40.556(5)
_cell_length_b                   40.556(5)
_cell_length_c                   12.276(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     20191(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10488
_exptl_special_details           
;
 120 seconds, 0.5 degrees, 40 mm
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.9208
_exptl_absorpt_correction_T_max  0.9753

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.3615
_diffrn_reflns_av_unetI/netI     0.2667
_diffrn_reflns_number            90430
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_reflns_number_total             9314
_reflns_number_gt                3292
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0913P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9314
_refine_ls_number_parameters     791
_refine_ls_number_restraints     546
_refine_ls_R_factor_all          0.27
_refine_ls_R_factor_gt           0.0861
_refine_ls_wR_factor_ref         0.2331
_refine_ls_wR_factor_gt          0.1621
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.105

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.8400(3) 0.3609(3) 0.0645(11) 0.059(4) Uani 1 1 d . . .
H1 H 0.8628 0.3552 0.0666 0.071 Uiso 1 1 calc R . .
C2 C 0.8205(3) 0.3444(3) -0.0088(11) 0.052(3) Uani 1 1 d . . .
H2 H 0.8295 0.3283 -0.0564 0.062 Uiso 1 1 calc R . .
C3 C 0.7875(3) 0.3519(3) -0.0112(12) 0.062(4) Uani 1 1 d . . .
H3 H 0.7728 0.3398 -0.0562 0.074 Uiso 1 1 calc R . .
C4 C 0.7762(3) 0.3776(3) 0.0540(10) 0.052(3) Uani 1 1 d . . .
H4 H 0.7539 0.3845 0.0495 0.063 Uiso 1 1 calc R . .
C5 C 0.7975(3) 0.3931(3) 0.1252(10) 0.048(3) Uani 1 1 d . . .
C6 C 0.7882(3) 0.4220(3) 0.1920(11) 0.051(3) Uani 1 1 d . . .
C7 C 0.7569(3) 0.4339(3) 0.2020(11) 0.059(4) Uani 1 1 d . . .
H7 H 0.7387 0.4231 0.1684 0.07 Uiso 1 1 calc R . .
C8 C 0.7524(4) 0.4624(4) 0.2632(12) 0.074(4) Uani 1 1 d . . .
H8 H 0.7309 0.4714 0.2704 0.089 Uiso 1 1 calc R . .
C9 C 0.7780(4) 0.4778(4) 0.3131(13) 0.076(4) Uani 1 1 d . . .
H9 H 0.7751 0.498 0.3511 0.091 Uiso 1 1 calc R . .
C10 C 0.8077(3) 0.4634(3) 0.3065(10) 0.060(4) Uani 1 1 d . . .
H10 H 0.8253 0.473 0.3463 0.072 Uiso 1 1 calc R . .
C11 C 0.8766(3) 0.4377(3) 0.4691(11) 0.056(4) Uani 1 1 d . . .
H11 H 0.8581 0.4267 0.4997 0.067 Uiso 1 1 calc R . .
C12 C 0.8967(3) 0.4550(3) 0.5358(10) 0.057(4) Uani 1 1 d . . .
H12 H 0.8918 0.457 0.6112 0.069 Uiso 1 1 calc R . .
C13 C 0.9241(3) 0.4695(3) 0.4928(13) 0.055(4) Uani 1 1 d . . .
H13 H 0.9391 0.4806 0.5395 0.066 Uiso 1 1 calc R . .
C14 C 0.9303(3) 0.4682(3) 0.3838(11) 0.049(3) Uani 1 1 d . . .
H14 H 0.9493 0.4785 0.3537 0.059 Uiso 1 1 calc R . .
C15 C 0.9083(3) 0.4515(3) 0.3186(10) 0.039(3) Uani 1 1 d . . .
C16 C 0.9096(3) 0.4521(3) 0.1979(11) 0.046(3) Uani 1 1 d . . .
C17 C 0.9337(3) 0.4685(3) 0.1360(12) 0.054(3) Uani 1 1 d . . .
H17 H 0.9515 0.4793 0.1712 0.065 Uiso 1 1 calc R . .
C18 C 0.9313(3) 0.4689(3) 0.0254(12) 0.062(4) Uani 1 1 d . . .
H18 H 0.9482 0.4787 -0.0171 0.074 Uiso 1 1 calc R . .
C19 C 0.9041(3) 0.4548(3) -0.0246(10) 0.055(4) Uani 1 1 d . . .
H19 H 0.9015 0.4561 -0.1014 0.066 Uiso 1 1 calc R . .
C20 C 0.8807(3) 0.4385(3) 0.0399(12) 0.050(3) Uani 1 1 d . . .
H20 H 0.8623 0.4284 0.0057 0.06 Uiso 1 1 calc R . .
C21 C 0.9502(3) 0.3423(3) 0.1662(11) 0.064(4) Uani 1 1 d . . .
H21A H 0.9378 0.3479 0.1003 0.097 Uiso 1 1 calc R . .
H21B H 0.9659 0.3246 0.1498 0.097 Uiso 1 1 calc R . .
H21C H 0.9622 0.3618 0.1918 0.097 Uiso 1 1 calc R . .
C22 C 0.9272(3) 0.3312(3) 0.2517(13) 0.058(4) Uani 1 1 d . . .
C23 C 0.9299(4) 0.3000(3) 0.3144(15) 0.075(5) Uani 1 1 d . . .
C24 C 0.9556(3) 0.2757(3) 0.2872(15) 0.099(6) Uani 1 1 d . . .
H24A H 0.9772 0.2844 0.3084 0.149 Uiso 1 1 calc R . .
H24B H 0.9553 0.2715 0.2086 0.149 Uiso 1 1 calc R . .
H24C H 0.9513 0.2551 0.3264 0.149 Uiso 1 1 calc R . .
C25 C 0.9008(4) 0.2693(4) 0.4582(17) 0.106(6) Uani 1 1 d . . .
H25A H 0.9217 0.2596 0.4844 0.128 Uiso 1 1 calc R . .
H25B H 0.8885 0.2521 0.4176 0.128 Uiso 1 1 calc R . .
C26 C 0.8804(4) 0.2816(3) 0.5542(14) 0.082(5) Uani 1 1 d . . .
H26A H 0.8669 0.2633 0.5842 0.098 Uiso 1 1 calc R . .
H26B H 0.8951 0.2898 0.6125 0.098 Uiso 1 1 calc R . .
C27 C 0.8212(4) 0.3106(3) 0.6750(10) 0.085(5) Uani 1 1 d . . .
H27A H 0.8347 0.2923 0.702 0.128 Uiso 1 1 calc R . .
H27B H 0.7982 0.3034 0.6691 0.128 Uiso 1 1 calc R . .
H27C H 0.8226 0.3292 0.7257 0.128 Uiso 1 1 calc R . .
C28 C 0.8335(4) 0.3212(4) 0.5645(12) 0.065(4) Uani 1 1 d . . .
C29 C 0.8198(4) 0.3504(3) 0.5090(12) 0.062(4) Uani 1 1 d . . .
C30 C 0.7881(3) 0.3658(3) 0.5316(10) 0.065(4) Uani 1 1 d . . .
H30A H 0.789 0.3892 0.5119 0.097 Uiso 1 1 calc R . .
H30B H 0.783 0.3637 0.6094 0.097 Uiso 1 1 calc R . .
H30C H 0.7709 0.3549 0.4888 0.097 Uiso 1 1 calc R . .
N9 N 0.9035(2) 0.3572(2) 0.4970(10) 0.054(3) Uani 1 1 d D A .
N10 N 0.9204(3) 0.3820(2) 0.6460(10) 0.060(3) Uani 1 1 d D . .
C31 C 0.8965(3) 0.3642(3) 0.5969(12) 0.062(4) Uani 1 1 d D . .
H31 H 0.8766 0.3577 0.6319 0.074 Uiso 1 1 calc R . .
C32 C 0.9346(3) 0.3698(3) 0.4787(12) 0.075(5) Uani 1 1 d D . .
H32 H 0.9469 0.3677 0.4132 0.09 Uiso 1 1 calc R . .
C33 C 0.9445(3) 0.3855(3) 0.5700(13) 0.075(5) Uani 1 1 d D . .
H33 H 0.9647 0.397 0.5793 0.09 Uiso 1 1 calc R . .
C34 C 0.9208(3) 0.3938(3) 0.7590(11) 0.084(5) Uani 1 1 d D . .
H34A H 0.8987 0.3917 0.7903 0.125 Uiso 1 1 calc R . .
H34B H 0.9276 0.4169 0.7605 0.125 Uiso 1 1 calc R . .
H34C H 0.9364 0.3805 0.8017 0.125 Uiso 1 1 calc R . .
N11 N 0.8471(7) 0.3093(13) 0.297(3) 0.056(5) Uani 0.71(4) 1 d PD A 1
N12 N 0.8301(6) 0.2783(11) 0.161(2) 0.050(5) Uani 0.71(4) 1 d PD A 1
C35 C 0.8559(6) 0.2915(17) 0.214(4) 0.067(8) Uani 0.71(4) 1 d PD A 1
H35 H 0.8782 0.2883 0.1923 0.081 Uiso 0.71(4) 1 calc PR A 1
C36 C 0.8131(5) 0.3110(8) 0.2890(15) 0.054(7) Uani 0.71(4) 1 d PD A 1
H36 H 0.7992 0.3244 0.3327 0.064 Uiso 0.71(4) 1 calc PR A 1
C37 C 0.8028(5) 0.2906(7) 0.2092(16) 0.050(7) Uani 0.71(4) 1 d PD A 1
H37 H 0.7806 0.2858 0.1906 0.061 Uiso 0.71(4) 1 calc PR A 1
C38 C 0.8309(8) 0.2566(8) 0.065(3) 0.067(9) Uani 0.71(4) 1 d PD A 1
H38A H 0.8519 0.2593 0.0269 0.101 Uiso 0.71(4) 1 calc PR A 1
H38B H 0.8127 0.2623 0.0158 0.101 Uiso 0.71(4) 1 calc PR A 1
H38C H 0.8285 0.2336 0.0883 0.101 Uiso 0.71(4) 1 calc PR A 1
N11B N 0.8500(17) 0.305(3) 0.277(8) 0.056(5) Uani 0.29(4) 1 d PD A 2
N12B N 0.8363(16) 0.276(3) 0.133(6) 0.050(5) Uani 0.29(4) 1 d PD A 2
C35B C 0.8607(14) 0.291(4) 0.189(9) 0.067(8) Uani 0.29(4) 1 d PD A 2
H35B H 0.8832 0.2911 0.1666 0.081 Uiso 0.29(4) 1 calc PR A 2
C36B C 0.8192(14) 0.2914(17) 0.293(4) 0.054(7) Uani 0.29(4) 1 d PD A 2
H36B H 0.8066 0.2927 0.3576 0.064 Uiso 0.29(4) 1 calc PR A 2
C37B C 0.8100(12) 0.2758(16) 0.201(4) 0.054(7) Uani 0.29(4) 1 d PD A 2
H37B H 0.7891 0.2661 0.1866 0.064 Uiso 0.29(4) 1 calc PR A 2
C38B C 0.838(2) 0.262(2) 0.024(5) 0.067(9) Uani 0.29(4) 1 d PD A 2
H38D H 0.8568 0.2712 -0.0162 0.101 Uiso 0.29(4) 1 calc PR A 2
H38E H 0.8176 0.2662 -0.0162 0.101 Uiso 0.29(4) 1 calc PR A 2
H38F H 0.8411 0.2378 0.0302 0.101 Uiso 0.29(4) 1 calc PR A 2
N1 N 0.8297(2) 0.3845(2) 0.1334(7) 0.040(2) Uani 1 1 d . . .
N2 N 0.8142(2) 0.4364(2) 0.2478(8) 0.050(3) Uani 1 1 d . . .
N3 N 0.8817(2) 0.4353(2) 0.3613(8) 0.041(2) Uani 1 1 d . . .
N4 N 0.8835(2) 0.4369(2) 0.1496(9) 0.043(2) Uani 1 1 d . . .
N5 N 0.9011(2) 0.3497(2) 0.2793(7) 0.043(3) Uani 1 1 d . A .
N6 N 0.9074(3) 0.2980(2) 0.3871(11) 0.072(4) Uani 1 1 d . A .
N7 N 0.8588(3) 0.3082(3) 0.5156(10) 0.066(3) Uani 1 1 d . A .
N8 N 0.8397(2) 0.3592(2) 0.4260(9) 0.048(3) Uani 1 1 d . A .
O1 O 0.89685(16) 0.37791(17) 0.2315(6) 0.042(2) Uani 1 1 d . . .
O2 O 0.82838(17) 0.3833(2) 0.3666(6) 0.050(2) Uani 1 1 d . . .
P1 P 0.77914(7) 0.23950(6) 0.5005(3) 0.0441(8) Uani 1 1 d D . .
F1 F 0.79919(17) 0.23786(15) 0.6078(6) 0.092(3) Uani 1 1 d D . .
F2 F 0.76019(14) 0.24317(14) 0.3840(5) 0.062(2) Uani 1 1 d D . .
F3 F 0.81358(14) 0.23991(15) 0.4360(6) 0.087(3) Uani 1 1 d D . .
F4 F 0.78046(14) 0.27902(12) 0.5053(5) 0.065(2) Uani 1 1 d D . .
F5 F 0.74540(15) 0.24008(14) 0.5615(5) 0.073(2) Uani 1 1 d D . .
F6 F 0.77694(14) 0.20016(11) 0.4899(5) 0.0567(18) Uani 1 1 d D . .
P2 P 0.81318(16) 0.42891(12) 0.7587(5) 0.107(3) Uani 0.750(7) 1 d PDU B 3
F7 F 0.8310(2) 0.39539(19) 0.7522(8) 0.101(3) Uani 0.750(7) 1 d PDU B 3
F8 F 0.7943(2) 0.46472(19) 0.7675(8) 0.111(4) Uani 0.750(7) 1 d PDU B 3
F9 F 0.8112(2) 0.4251(2) 0.8885(6) 0.083(3) Uani 0.750(7) 1 d PDU B 3
F10 F 0.84756(18) 0.44756(18) 0.7710(9) 0.072(3) Uani 0.750(7) 1 d PDU B 3
F11 F 0.8141(2) 0.4342(2) 0.6321(6) 0.125(5) Uani 0.750(7) 1 d PDU B 3
F12 F 0.77679(19) 0.4129(2) 0.7461(8) 0.114(5) Uani 0.750(7) 1 d PDU B 3
P3 P 0.9176(2) 0.2954(2) -0.1203(9) 0.0781(14) Uani 0.50(2) 1 d PDU C 4
F13 F 0.8938(3) 0.3212(4) -0.0710(17) 0.103(8) Uani 0.50(2) 1 d PDU C 4
F14 F 0.9442(4) 0.2685(4) -0.1664(14) 0.165(11) Uani 0.50(2) 1 d PDU C 4
F15 F 0.9220(6) 0.2803(4) -0.0005(10) 0.109(8) Uani 0.50(2) 1 d PDU C 4
F16 F 0.9480(3) 0.3196(5) -0.0973(12) 0.101(8) Uani 0.50(2) 1 d PDU C 4
F17 F 0.9144(5) 0.3097(3) -0.2380(10) 0.079(6) Uani 0.50(2) 1 d PDU C 4
F18 F 0.8888(4) 0.2693(4) -0.1465(16) 0.121(6) Uani 0.50(2) 1 d PDU C 4
P4 P 0.9181(2) 0.2969(2) -0.1068(9) 0.0781(14) Uani 0.50(2) 1 d PDU C 5
F19 F 0.9035(5) 0.2624(3) -0.1289(15) 0.121(6) Uani 0.50(2) 1 d PDU C 5
F20 F 0.9356(5) 0.3327(3) -0.0844(16) 0.137(10) Uani 0.50(2) 1 d PDU C 5
F21 F 0.9431(5) 0.2911(7) -0.2061(15) 0.201(13) Uani 0.50(2) 1 d PDU C 5
F22 F 0.9446(4) 0.2811(4) -0.0258(17) 0.120(9) Uani 0.50(2) 1 d PDU C 5
F23 F 0.8947(4) 0.3037(5) -0.0080(14) 0.117(8) Uani 0.50(2) 1 d PDU C 5
F24 F 0.8926(6) 0.3155(4) -0.1864(18) 0.146(10) Uani 0.50(2) 1 d PDU C 5
P5 P 0.8287(4) 0.4188(4) 0.7792(14) 0.107(3) Uani 0.250(7) 1 d PDU B 6
F25 F 0.8499(5) 0.3910(5) 0.830(2) 0.101(3) Uani 0.250(7) 1 d PDU B 6
F26 F 0.8075(7) 0.4483(6) 0.721(2) 0.111(4) Uani 0.250(7) 1 d PDU B 6
F27 F 0.8389(6) 0.4053(7) 0.6612(16) 0.101(3) Uani 0.250(7) 1 d PDU B 6
F28 F 0.8600(6) 0.4427(5) 0.778(3) 0.072(3) Uani 0.250(7) 1 d PDU B 6
F29 F 0.8183(7) 0.4328(7) 0.8929(16) 0.083(3) Uani 0.250(7) 1 d PDU B 6
F30 F 0.7958(5) 0.3965(6) 0.777(2) 0.101(3) Uani 0.250(7) 1 d PDU B 6
Co1 Co 0.87596(4) 0.33139(4) 0.39707(15) 0.0570(6) Uani 1 1 d . . .
Ru1 Ru 0.85603(2) 0.40846(2) 0.24894(8) 0.0401(3) Uani 1 1 d . . .
N13 N 0.984(2) 0.2301(14) -0.334(5) 0.15(2) Uani 0.25 1 d PD . 7
C39 C 0.981(2) 0.2548(14) -0.378(7) 0.15(2) Uani 0.25 1 d PD . 7
C40 C 0.976(2) 0.2884(13) -0.420(7) 0.15(2) Uani 0.25 1 d PD D 7
H40A H 0.9852 0.3031 -0.3637 0.218 Uiso 0.25 1 d PR D 7
H40B H 0.9529 0.2929 -0.431 0.218 Uiso 0.25 1 d PR D 7
H40C H 0.9883 0.2921 -0.4885 0.218 Uiso 0.25 1 d PR D 7



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.345(14) . ?
C1 C2 1.373(16) . ?
C1 H1 0.95 . ?
C2 C3 1.372(15) . ?
C2 H2 0.95 . ?
C3 C4 1.393(16) . ?
C3 H3 0.95 . ?
C4 C5 1.379(15) . ?
C4 H4 0.95 . ?
C5 N1 1.354(13) . ?
C5 C6 1.480(16) . ?
C6 C7 1.365(15) . ?
C6 N2 1.385(14) . ?
C7 C8 1.391(17) . ?
C7 H7 0.95 . ?
C8 C9 1.359(18) . ?
C8 H8 0.95 . ?
C9 C10 1.340(17) . ?
C9 H9 0.95 . ?
C10 N2 1.338(14) . ?
C10 H10 0.95 . ?
C11 N3 1.342(14) . ?
C11 C12 1.351(15) . ?
C11 H11 0.95 . ?
C12 C13 1.366(16) . ?
C12 H12 0.95 . ?
C13 C14 1.362(16) . ?
C13 H13 0.95 . ?
C14 C15 1.376(14) . ?
C14 H14 0.95 . ?
C15 N3 1.369(13) . ?
C15 C16 1.484(15) . ?
C16 N4 1.360(13) . ?
C16 C17 1.403(16) . ?
C17 C18 1.361(16) . ?
C17 H17 0.95 . ?
C18 C19 1.385(16) . ?
C18 H18 0.95 . ?
C19 C20 1.403(15) . ?
C19 H19 0.95 . ?
C20 N4 1.354(14) . ?
C20 H20 0.95 . ?
C21 C22 1.475(17) . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 N5 1.341(14) . ?
C22 C23 1.484(18) . ?
C23 N6 1.278(18) . ?
C23 C24 1.471(19) . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 N6 1.482(18) . ?
C25 C26 1.52(2) . ?
C25 H25A 0.99 . ?
C25 H25B 0.99 . ?
C26 N7 1.469(16) . ?
C26 H26A 0.99 . ?
C26 H26B 0.99 . ?
C27 C28 1.508(18) . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
C28 N7 1.300(16) . ?
C28 C29 1.474(19) . ?
C29 N8 1.347(15) . ?
C29 C30 1.458(17) . ?
C30 H30A 0.98 . ?
C30 H30B 0.98 . ?
C30 H30C 0.98 . ?
N9 C31 1.291(13) . ?
N9 C32 1.379(14) . ?
N9 Co1 1.961(9) . ?
N10 C31 1.351(12) . ?
N10 C33 1.358(14) . ?
N10 C34 1.468(14) . ?
C31 H31 0.95 . ?
C32 C33 1.351(15) . ?
C32 H32 0.95 . ?
C33 H33 0.95 . ?
C34 H34A 0.98 . ?
C34 H34B 0.98 . ?
C34 H34C 0.98 . ?
N11 C35 1.306(16) . ?
N11 C36 1.38(2) . ?
N11 Co1 1.92(2) . ?
N12 C35 1.344(14) . ?
N12 C37 1.351(18) . ?
N12 C38 1.469(16) . ?
C35 H35 0.95 . ?
C36 C37 1.348(16) . ?
C36 H36 0.95 . ?
C37 H37 0.95 . ?
C38 H38A 0.98 . ?
C38 H38B 0.98 . ?
C38 H38C 0.98 . ?
N11B C35B 1.305(19) . ?
N11B C36B 1.38(2) . ?
N11B Co1 2.10(5) . ?
N12B C35B 1.347(18) . ?
N12B C37B 1.36(2) . ?
N12B C38B 1.468(19) . ?
C35B H35B 0.95 . ?
C36B C37B 1.35(2) . ?
C36B H36B 0.95 . ?
C37B H37B 0.95 . ?
C38B H38D 0.98 . ?
C38B H38E 0.98 . ?
C38B H38F 0.98 . ?
N1 Ru1 2.023(9) . ?
N2 Ru1 2.040(9) . ?
N3 Ru1 2.042(9) . ?
N4 Ru1 2.015(9) . ?
N5 O1 1.297(10) . ?
N5 Co1 1.919(9) . ?
N6 Co1 1.865(12) . ?
N7 Co1 1.867(11) . ?
N8 O2 1.305(10) . ?
N8 Co1 1.887(10) . ?
O1 Ru1 2.079(7) . ?
O2 Ru1 2.094(7) . ?
P1 F1 1.550(6) . ?
P1 F5 1.561(6) . ?
P1 F6 1.603(5) . ?
P1 F3 1.605(6) . ?
P1 F4 1.605(5) . ?
P1 F2 1.630(6) . ?
P2 F7 1.541(7) . ?
P2 F11 1.570(7) . ?
P2 F10 1.593(6) . ?
P2 F9 1.602(7) . ?
P2 F12 1.620(6) . ?
P2 F8 1.646(7) . ?
P3 F13 1.544(7) . ?
P3 F17 1.563(7) . ?
P3 F16 1.601(6) . ?
P3 F15 1.603(7) . ?
P3 F18 1.608(6) . ?
P3 F14 1.638(7) . ?
P4 F19 1.542(7) . ?
P4 F23 1.564(7) . ?
P4 F22 1.600(6) . ?
P4 F21 1.603(7) . ?
P4 F24 1.609(6) . ?
P4 F20 1.640(7) . ?
P5 F25 1.546(7) . ?
P5 F29 1.564(7) . ?
P5 F28 1.598(6) . ?
P5 F27 1.604(7) . ?
P5 F30 1.613(6) . ?
P5 F26 1.637(7) . ?
N13 C39 0.67(9) 16_644 ?
N13 C40 0.90(10) 16_644 ?
N13 C39 1.142(5) . ?
N13 C39 1.64(10) 2_755 ?
N13 N13 1.80(8) 15_664 ?
N13 N13 1.80(8) 16_644 ?
N13 C39 1.85(6) 15_664 ?
C39 N13 0.67(9) 15_664 ?
C39 C39 1.11(13) 15_664 ?
C39 C39 1.11(13) 16_644 ?
C39 C40 1.472(5) . ?
C39 C40 1.51(11) 16_644 ?
C39 C39 1.57(18) 2_755 ?
C39 N13 1.64(10) 2_755 ?
C39 N13 1.85(6) 16_644 ?
C40 N13 0.90(10) 15_664 ?
C40 C39 1.51(11) 15_664 ?
C40 H40A 0.98 . ?
C40 H40B 0.98 . ?
C40 H40C 0.98 . ?

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 C1 C2 125.4(12) . . ?
N1 C1 H1 117.3 . . ?
C2 C1 H1 117.3 . . ?
C3 C2 C1 118.0(13) . . ?
C3 C2 H2 121 . . ?
C1 C2 H2 121 . . ?
C2 C3 C4 118.2(12) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C5 C4 C3 120.0(12) . . ?
C5 C4 H4 120 . . ?
C3 C4 H4 120 . . ?
N1 C5 C4 122.3(12) . . ?
N1 C5 C6 114.1(11) . . ?
C4 C5 C6 123.5(12) . . ?
C7 C6 N2 121.0(13) . . ?
C7 C6 C5 124.6(13) . . ?
N2 C6 C5 114.4(11) . . ?
C6 C7 C8 117.6(13) . . ?
C6 C7 H7 121.2 . . ?
C8 C7 H7 121.2 . . ?
C9 C8 C7 121.8(13) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C10 C9 C8 117.3(14) . . ?
C10 C9 H9 121.4 . . ?
C8 C9 H9 121.4 . . ?
N2 C10 C9 124.5(14) . . ?
N2 C10 H10 117.7 . . ?
C9 C10 H10 117.7 . . ?
N3 C11 C12 122.9(11) . . ?
N3 C11 H11 118.6 . . ?
C12 C11 H11 118.6 . . ?
C11 C12 C13 118.7(13) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C14 C13 C12 121.0(12) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 118.0(12) . . ?
C13 C14 H14 121 . . ?
C15 C14 H14 121 . . ?
N3 C15 C14 121.7(11) . . ?
N3 C15 C16 114.7(11) . . ?
C14 C15 C16 123.4(12) . . ?
N4 C16 C17 121.3(12) . . ?
N4 C16 C15 113.6(12) . . ?
C17 C16 C15 124.9(12) . . ?
C18 C17 C16 119.7(12) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C19 119.6(13) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C20 118.9(12) . . ?
C18 C19 H19 120.6 . . ?
C20 C19 H19 120.6 . . ?
N4 C20 C19 121.8(11) . . ?
N4 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C21 120.4(11) . . ?
N5 C22 C23 113.9(13) . . ?
C21 C22 C23 125.6(13) . . ?
N6 C23 C24 128.3(14) . . ?
N6 C23 C22 111.3(14) . . ?
C24 C23 C22 120.3(16) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N6 C25 C26 107.3(13) . . ?
N6 C25 H25A 110.3 . . ?
C26 C25 H25A 110.3 . . ?
N6 C25 H25B 110.3 . . ?
C26 C25 H25B 110.3 . . ?
H25A C25 H25B 108.5 . . ?
N7 C26 C25 108.4(13) . . ?
N7 C26 H26A 110 . . ?
C25 C26 H26A 110 . . ?
N7 C26 H26B 110 . . ?
C25 C26 H26B 110 . . ?
H26A C26 H26B 108.4 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N7 C28 C29 114.0(14) . . ?
N7 C28 C27 124.2(15) . . ?
C29 C28 C27 121.3(15) . . ?
N8 C29 C30 123.9(12) . . ?
N8 C29 C28 109.8(14) . . ?
C30 C29 C28 126.0(14) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C31 N9 C32 106.0(10) . . ?
C31 N9 Co1 125.8(9) . . ?
C32 N9 Co1 128.1(10) . . ?
C31 N10 C33 105.5(11) . . ?
C31 N10 C34 127.0(12) . . ?
C33 N10 C34 127.4(11) . . ?
N9 C31 N10 112.4(12) . . ?
N9 C31 H31 123.8 . . ?
N10 C31 H31 123.8 . . ?
C33 C32 N9 108.1(12) . . ?
C33 C32 H32 125.9 . . ?
N9 C32 H32 125.9 . . ?
C32 C33 N10 107.9(11) . . ?
C32 C33 H33 126.1 . . ?
N10 C33 H33 126.1 . . ?
N10 C34 H34A 109.5 . . ?
N10 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N10 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 N11 C36 104.0(15) . . ?
C35 N11 Co1 126.4(17) . . ?
C36 N11 Co1 129.3(18) . . ?
C35 N12 C37 106.1(15) . . ?
C35 N12 C38 127.4(16) . . ?
C37 N12 C38 126.3(15) . . ?
N11 C35 N12 112.8(14) . . ?
N11 C35 H35 123.6 . . ?
N12 C35 H35 123.6 . . ?
C37 C36 N11 109.4(13) . . ?
C37 C36 H36 125.3 . . ?
N11 C36 H36 125.3 . . ?
C36 C37 N12 107.0(12) . . ?
C36 C37 H37 126.5 . . ?
N12 C37 H37 126.5 . . ?
C35B N11B C36B 104(3) . . ?
C35B N11B Co1 130(4) . . ?
C36B N11B Co1 124(4) . . ?
C35B N12B C37B 106(2) . . ?
C35B N12B C38B 128(3) . . ?
C37B N12B C38B 127(2) . . ?
N11B C35B N12B 112(2) . . ?
N11B C35B H35B 124 . . ?
N12B C35B H35B 124 . . ?
C37B C36B N11B 109(2) . . ?
C37B C36B H36B 125.4 . . ?
N11B C36B H36B 125.4 . . ?
C36B C37B N12B 106.9(18) . . ?
C36B C37B H37B 126.6 . . ?
N12B C37B H37B 126.6 . . ?
N12B C38B H38D 109.5 . . ?
N12B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
N12B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C1 N1 C5 115.9(10) . . ?
C1 N1 Ru1 128.1(8) . . ?
C5 N1 Ru1 116.0(8) . . ?
C10 N2 C6 117.5(11) . . ?
C10 N2 Ru1 127.9(9) . . ?
C6 N2 Ru1 113.8(8) . . ?
C11 N3 C15 117.6(10) . . ?
C11 N3 Ru1 128.8(8) . . ?
C15 N3 Ru1 113.5(8) . . ?
C20 N4 C16 118.5(11) . . ?
C20 N4 Ru1 125.6(9) . . ?
C16 N4 Ru1 115.2(9) . . ?
O1 N5 C22 119.1(10) . . ?
O1 N5 Co1 127.7(8) . . ?
C22 N5 Co1 113.1(9) . . ?
C23 N6 C25 126.3(14) . . ?
C23 N6 Co1 119.2(10) . . ?
C25 N6 Co1 114.1(11) . . ?
C28 N7 C26 128.2(14) . . ?
C28 N7 Co1 116.9(10) . . ?
C26 N7 Co1 113.5(11) . . ?
O2 N8 C29 114.3(10) . . ?
O2 N8 Co1 128.1(8) . . ?
C29 N8 Co1 116.8(9) . . ?
N5 O1 Ru1 125.8(6) . . ?
N8 O2 Ru1 124.3(7) . . ?
F1 P1 F5 93.0(4) . . ?
F1 P1 F6 93.2(3) . . ?
F5 P1 F6 90.3(3) . . ?
F1 P1 F3 87.9(4) . . ?
F5 P1 F3 178.3(4) . . ?
F6 P1 F3 91.1(3) . . ?
F1 P1 F4 89.6(3) . . ?
F5 P1 F4 89.8(3) . . ?
F6 P1 F4 177.2(4) . . ?
F3 P1 F4 88.8(3) . . ?
F1 P1 F2 175.6(4) . . ?
F5 P1 F2 90.4(3) . . ?
F6 P1 F2 89.6(3) . . ?
F3 P1 F2 88.7(4) . . ?
F4 P1 F2 87.5(3) . . ?
F7 P2 F11 93.4(5) . . ?
F7 P2 F10 90.8(4) . . ?
F11 P2 F10 90.5(4) . . ?
F7 P2 F9 89.4(5) . . ?
F11 P2 F9 177.2(6) . . ?
F10 P2 F9 89.8(4) . . ?
F7 P2 F12 93.8(4) . . ?
F11 P2 F12 88.9(4) . . ?
F10 P2 F12 175.4(5) . . ?
F9 P2 F12 90.6(4) . . ?
F7 P2 F8 179.2(6) . . ?
F11 P2 F8 87.3(5) . . ?
F10 P2 F8 89.0(4) . . ?
F9 P2 F8 89.8(5) . . ?
F12 P2 F8 86.4(4) . . ?
F13 P3 F17 93.4(5) . . ?
F13 P3 F16 89.8(5) . . ?
F17 P3 F16 89.9(5) . . ?
F13 P3 F15 88.3(6) . . ?
F17 P3 F15 178.1(6) . . ?
F16 P3 F15 89.3(5) . . ?
F13 P3 F18 94.0(5) . . ?
F17 P3 F18 90.0(5) . . ?
F16 P3 F18 176.2(6) . . ?
F15 P3 F18 90.7(5) . . ?
F13 P3 F14 176.6(6) . . ?
F17 P3 F14 89.0(5) . . ?
F16 P3 F14 87.8(5) . . ?
F15 P3 F14 89.3(5) . . ?
F18 P3 F14 88.4(5) . . ?
F19 P4 F23 93.7(5) . . ?
F19 P4 F22 90.1(5) . . ?
F23 P4 F22 89.8(5) . . ?
F19 P4 F21 88.6(6) . . ?
F23 P4 F21 177.5(6) . . ?
F22 P4 F21 89.3(5) . . ?
F19 P4 F24 94.1(5) . . ?
F23 P4 F24 90.0(5) . . ?
F22 P4 F24 175.8(6) . . ?
F21 P4 F24 90.8(5) . . ?
F19 P4 F20 176.9(6) . . ?
F23 P4 F20 88.6(5) . . ?
F22 P4 F20 87.7(5) . . ?
F21 P4 F20 89.0(5) . . ?
F24 P4 F20 88.0(5) . . ?
F25 P5 F29 93.3(6) . . ?
F25 P5 F28 90.2(5) . . ?
F29 P5 F28 90.3(5) . . ?
F25 P5 F27 88.2(6) . . ?
F29 P5 F27 178.5(7) . . ?
F28 P5 F27 89.4(5) . . ?
F25 P5 F30 93.3(5) . . ?
F29 P5 F30 89.8(5) . . ?
F28 P5 F30 176.4(6) . . ?
F27 P5 F30 90.4(5) . . ?
F25 P5 F26 177.1(6) . . ?
F29 P5 F26 89.2(5) . . ?
F28 P5 F26 88.2(5) . . ?
F27 P5 F26 89.3(5) . . ?
F30 P5 F26 88.2(5) . . ?
N6 Co1 N7 86.6(6) . . ?
N6 Co1 N8 168.4(5) . . ?
N7 Co1 N8 82.1(6) . . ?
N6 Co1 N11 92.1(15) . . ?
N7 Co1 N11 91.9(16) . . ?
N8 Co1 N11 85.6(13) . . ?
N6 Co1 N5 82.4(5) . . ?
N7 Co1 N5 168.6(5) . . ?
N8 Co1 N5 109.0(5) . . ?
N11 Co1 N5 91.5(14) . . ?
N6 Co1 N9 92.2(4) . . ?
N7 Co1 N9 89.6(4) . . ?
N8 Co1 N9 90.5(4) . . ?
N11 Co1 N9 175.5(17) . . ?
N5 Co1 N9 87.8(4) . . ?
N6 Co1 N11B 86(3) . . ?
N7 Co1 N11B 96(3) . . ?
N8 Co1 N11B 92(3) . . ?
N11 Co1 N11B 8(3) . . ?
N5 Co1 N11B 86(3) . . ?
N9 Co1 N11B 174(3) . . ?
N4 Ru1 N1 98.2(4) . . ?
N4 Ru1 N2 98.0(4) . . ?
N1 Ru1 N2 79.7(4) . . ?
N4 Ru1 N3 79.7(4) . . ?
N1 Ru1 N3 176.5(4) . . ?
N2 Ru1 N3 97.6(4) . . ?
N4 Ru1 O1 80.7(3) . . ?
N1 Ru1 O1 93.6(3) . . ?
N2 Ru1 O1 173.0(4) . . ?
N3 Ru1 O1 88.9(3) . . ?
N4 Ru1 O2 173.0(4) . . ?
N1 Ru1 O2 88.1(3) . . ?
N2 Ru1 O2 80.2(3) . . ?
N3 Ru1 O2 93.8(3) . . ?
O1 Ru1 O2 102.0(3) . . ?
C39 N13 C40 137(10) 16_644 16_644 ?
C39 N13 C39 70(10) 16_644 . ?
C40 N13 C39 95(10) 16_644 . ?
C39 N13 C39 30(10) 16_644 2_755 ?
C40 N13 C39 159(9) 16_644 2_755 ?
C39 N13 C39 66(8) . 2_755 ?
C39 N13 N13 66(10) 16_644 15_664 ?
C40 N13 N13 95(9) 16_644 15_664 ?
C39 N13 N13 6(5) . 15_664 ?
C39 N13 N13 65(2) 2_755 15_664 ?
C39 N13 N13 11(8) 16_644 16_644 ?
C40 N13 N13 148(10) 16_644 16_644 ?
C39 N13 N13 74(4) . 16_644 ?
C39 N13 N13 22(2) 2_755 16_644 ?
N13 N13 N13 71(5) 15_664 16_644 ?
C39 N13 C39 56(10) 16_644 15_664 ?
C40 N13 C39 127(9) 16_644 15_664 ?
C39 N13 C39 34(6) . 15_664 ?
C39 N13 C39 37(4) 2_755 15_664 ?
N13 N13 C39 36.4(11) 15_664 15_664 ?
N13 N13 C39 54(3) 16_644 15_664 ?
N13 C39 C39 75(9) 15_664 15_664 ?
N13 C39 C39 133(10) 15_664 16_644 ?
C39 C39 C39 89.8(9) 15_664 16_644 ?
N13 C39 N13 163(10) 15_664 . ?
C39 C39 N13 110(8) 15_664 . ?
C39 C39 N13 35(6) 16_644 . ?
N13 C39 C40 25(10) 15_664 . ?
C39 C39 C40 70(8) 15_664 . ?
C39 C39 C40 152(6) 16_644 . ?
N13 C39 C40 172(5) . . ?
N13 C39 C40 140(10) 15_664 16_644 ?
C39 C39 C40 145(9) 15_664 16_644 ?
C39 C39 C40 66(4) 16_644 16_644 ?
N13 C39 C40 37(6) . 16_644 ?
C40 C39 C40 140(6) . 16_644 ?
N13 C39 C39 104(10) 15_664 2_755 ?
C39 C39 C39 45.1(5) 15_664 2_755 ?
C39 C39 C39 45.1(5) 16_644 2_755 ?
N13 C39 C39 73(6) . 2_755 ?
C40 C39 C39 111(8) . 2_755 ?
C40 C39 C39 109(4) 16_644 2_755 ?
N13 C39 N13 92(9) 15_664 2_755 ?
C39 C39 N13 18(6) 15_664 2_755 ?
C39 C39 N13 82(6) 16_644 2_755 ?
N13 C39 N13 96(10) . 2_755 ?
C40 C39 N13 83(6) . 2_755 ?
C40 C39 N13 128(7) 16_644 2_755 ?
C39 C39 N13 41(3) 2_755 2_755 ?
N13 C39 N13 101(10) 15_664 16_644 ?
C39 C39 N13 62(4) 15_664 16_644 ?
C39 C39 N13 35(3) 16_644 16_644 ?
N13 C39 N13 69(4) . 16_644 ?
C40 C39 N13 117(6) . 16_644 ?
C40 C39 N13 101(4) 16_644 16_644 ?
C39 C39 N13 21(2) 2_755 16_644 ?
N13 C39 N13 61(4) 2_755 16_644 ?
N13 C40 C39 18(8) 15_664 . ?
N13 C40 C39 49(6) 15_664 15_664 ?
C39 C40 C39 44(6) . 15_664 ?
N13 C40 H40A 120.3 15_664 . ?
C39 C40 H40A 105.3 . . ?
C39 C40 H40A 76.8 15_664 . ?
N13 C40 H40B 110.5 15_664 . ?
C39 C40 H40B 110.4 . . ?
C39 C40 H40B 152.7 15_664 . ?
H40A C40 H40B 109.5 . . ?
N13 C40 H40C 96.7 15_664 . ?
C39 C40 H40C 112.6 . . ?
C39 C40 H40C 92.3 15_664 . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?



# start Validation Reply Form 
_vrf_RINTA01_I                   
; 
PROBLEM: The value of Rint is greater than 0.25 
RESPONSE: When samples are extremely small, data variance becomes large.
Rint does not improve with more data, just becomes more certain in
its value. Our sample was very small indeed, yet for the sake of 
quality the best we could do.
;
_vrf_PLAT020_I                   
; 
PROBLEM: The value of Rint is greater than 0.12 ......... 0.361 
RESPONSE: See above
;
# end Validation Reply Form


# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_twin5
_database_code_depnum_ccdc_archive 'CCDC 1038277'
_audit_update_record             
;
2015-10-27 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_date             2013-11-22T14:21:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
Complex 1-H+
;
_chemical_name_common            dh2_48
_chemical_formula_moiety         'C18 H29 Co N8 O2, 2(Cl O4)'
_chemical_formula_sum            'C18 H29 Cl2 Co N8 O10'
_chemical_formula_weight         647.32

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
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                   14.714(2)
_cell_length_b                   11.4270(18)
_cell_length_c                   15.237(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.610(11)
_cell_angle_gamma                90
_cell_volume                     2559.2(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4080
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       piece
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.68
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_special_details           
;
 0.5 deg, 20 sec., 40 mm
 180 deg. rot. twin about [0 0 1] resolved with
 multi-domain integration.
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.6605
_exptl_absorpt_correction_T_max  0.9452

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.1198
_diffrn_reflns_av_unetI/netI     0.1302
_diffrn_reflns_number            8597
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         25.7
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.944
_reflns_number_total             9118
_reflns_number_gt                6483
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1868P)²+32.6873P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9118
_refine_ls_number_parameters     378
_refine_ls_number_restraints     235
_refine_ls_R_factor_all          0.1723
_refine_ls_R_factor_gt           0.1287
_refine_ls_wR_factor_ref         0.3501
_refine_ls_wR_factor_gt          0.312
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.1
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         2.27
_refine_diff_density_min         -1.41
_refine_diff_density_rms         0.233

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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 0.8626(8) 0.5248(9) 0.9835(7) 0.025(2) Uani 1 1 d U . .
H1A H 0.9032 0.5904 0.9825 0.038 Uiso 1 1 calc R . .
H1B H 0.8823 0.4722 1.0297 0.038 Uiso 1 1 calc R . .
H1C H 0.8022 0.5517 0.9937 0.038 Uiso 1 1 calc R . .
C2 C 0.8627(7) 0.4633(7) 0.8987(7) 0.019(2) Uani 1 1 d DU . .
C3 C 0.8718(8) 0.3309(8) 0.8830(7) 0.021(2) Uani 1 1 d DU . .
C4 C 0.8767(8) 0.2522(9) 0.9618(7) 0.026(3) Uani 1 1 d U . .
H4A H 0.8222 0.2607 0.9936 0.039 Uiso 1 1 calc R . .
H4B H 0.9285 0.273 0.9992 0.039 Uiso 1 1 calc R . .
H4C H 0.8825 0.1724 0.9431 0.039 Uiso 1 1 calc R . .
C5 C 0.8846(8) 0.1833(9) 0.7676(7) 0.026(2) Uani 1 1 d U . .
H5A H 0.8422 0.1285 0.792 0.031 Uiso 1 1 calc R . .
H5B H 0.9458 0.1561 0.7824 0.031 Uiso 1 1 calc R . .
C6 C 0.8691(8) 0.1876(8) 0.6665(7) 0.022(2) Uani 1 1 d U . .
H6A H 0.9126 0.137 0.6393 0.026 Uiso 1 1 calc R . .
H6B H 0.8084 0.1596 0.6502 0.026 Uiso 1 1 calc R . .
C7 C 0.9012(8) 0.2767(10) 0.4776(8) 0.026(2) Uani 1 1 d U . .
H7A H 0.9595 0.2389 0.4828 0.039 Uiso 1 1 calc R . .
H7B H 0.8992 0.3275 0.4274 0.039 Uiso 1 1 calc R . .
H7C H 0.8543 0.2187 0.4706 0.039 Uiso 1 1 calc R . .
C8 C 0.8872(7) 0.3446(8) 0.5559(7) 0.017(2) Uani 1 1 d DU . .
C9 C 0.8794(7) 0.4786(8) 0.5538(7) 0.020(2) Uani 1 1 d DU . .
C10 C 0.8801(8) 0.5514(9) 0.4698(7) 0.024(2) Uani 1 1 d U . .
H10A H 0.8188 0.5715 0.4514 0.035 Uiso 1 1 calc R . .
H10B H 0.9072 0.5069 0.4245 0.035 Uiso 1 1 calc R . .
H10C H 0.9146 0.6216 0.4808 0.035 Uiso 1 1 calc R . .
C11 C 1.0406(7) 0.5411(9) 0.7641(8) 0.020(2) Uani 1 1 d U . .
H11 H 1.0122 0.6122 0.7742 0.024 Uiso 1 1 calc R . .
C12 C 1.1310(8) 0.5217(9) 0.7726(8) 0.027(2) Uani 1 1 d U . .
H12 H 1.1753 0.5757 0.7906 0.032 Uiso 1 1 calc R . .
C13 C 1.0640(7) 0.3601(9) 0.7294(8) 0.018(2) Uani 1 1 d U . .
H13 H 1.0559 0.2828 0.7117 0.022 Uiso 1 1 calc R . .
C14 C 1.2326(7) 0.3527(9) 0.7511(7) 0.019(2) Uani 1 1 d U . .
H14A H 1.237 0.2973 0.7985 0.029 Uiso 1 1 calc R . .
H14B H 1.2799 0.4101 0.759 0.029 Uiso 1 1 calc R . .
H14C H 1.2393 0.3126 0.6964 0.029 Uiso 1 1 calc R . .
C15 C 0.6853(7) 0.4061(9) 0.6312(7) 0.021(2) Uani 1 1 d U . .
H15 H 0.708 0.4132 0.5755 0.025 Uiso 1 1 calc R . .
C16 C 0.5937(7) 0.3946(8) 0.6500(7) 0.018(2) Uani 1 1 d U . .
H16 H 0.5441 0.3914 0.6099 0.021 Uiso 1 1 calc R . .
C17 C 0.6780(6) 0.3920(8) 0.7706(7) 0.019(2) Uani 1 1 d U . .
H17 H 0.6937 0.3852 0.8302 0.022 Uiso 1 1 calc R . .
C18 C 0.5092(7) 0.3778(9) 0.7896(8) 0.022(2) Uani 1 1 d U . .
H18A H 0.4661 0.4372 0.7717 0.034 Uiso 1 1 calc R . .
H18B H 0.5255 0.3868 0.8509 0.034 Uiso 1 1 calc R . .
H18C H 0.4825 0.302 0.7796 0.034 Uiso 1 1 calc R . .
N1 N 0.8546(7) 0.5106(8) 0.8217(6) 0.026(2) Uani 1 1 d U . .
N2 N 0.8718(6) 0.2980(7) 0.8057(6) 0.0174(18) Uani 1 1 d U . .
N3 N 0.8800(6) 0.3113(7) 0.6340(6) 0.0170(18) Uani 1 1 d U . .
N4 N 0.8672(6) 0.5237(7) 0.6290(6) 0.0198(19) Uani 1 1 d U . .
N5 N 0.9963(5) 0.4380(7) 0.7378(6) 0.0151(18) Uani 1 1 d U . .
N6 N 1.1450(6) 0.4097(7) 0.7502(5) 0.0203(18) Uani 1 1 d U . .
N7 N 0.7371(5) 0.4053(6) 0.7107(5) 0.0091(15) Uani 1 1 d U . .
N8 N 0.5920(5) 0.3891(7) 0.7376(6) 0.0148(17) Uani 1 1 d U . .
O1 O 0.8462(5) 0.6265(5) 0.8109(5) 0.0219(16) Uani 1 1 d U . .
H1 H 0.8387 0.6414 0.7584 0.033 Uiso 1 1 calc R . .
O2 O 0.8557(5) 0.6406(6) 0.6436(5) 0.0256(17) Uani 1 1 d U . .
O3 O 1.0584(6) 0.1464(8) 0.5861(7) 0.041(2) Uani 1 1 d U . .
O4 O 1.1405(6) 0.0855(9) 0.4687(6) 0.047(2) Uani 1 1 d U . .
O5 O 1.1506(7) -0.0190(8) 0.5990(7) 0.051(3) Uani 1 1 d U . .
O6 O 1.2160(7) 0.1640(8) 0.5917(8) 0.047(2) Uani 1 1 d U . .
O7 O 1.1162(6) 0.0990(6) 0.7972(5) 0.0304(18) Uani 1 1 d U A 1
O8 O 1.1273(13) -0.0212(16) 0.9186(12) 0.040(4) Uani 0.5 1 d PU A 1
O9 O 1.2157(7) 0.1334(10) 0.9152(8) 0.057(3) Uani 1 1 d U A 1
O10 O 1.0537(13) 0.1596(18) 0.9277(14) 0.043(5) Uani 0.5 1 d PU A 1
O11 O 1.0894(17) 0.228(2) 0.9101(17) 0.066(6) Uani 0.5 1 d PU A 2
O12 O 1.076(2) 0.034(3) 0.939(2) 0.087(9) Uani 0.5 1 d PU A 2
Cl1 Cl 1.13974(18) 0.0936(2) 0.55937(17) 0.0229(6) Uani 1 1 d . . .
Cl2 Cl 1.12862(19) 0.1035(2) 0.88827(19) 0.0288(6) Uani 1 1 d . . .
Co1 Co 0.86698(9) 0.41762(10) 0.72347(9) 0.0139(3) Uani 1 1 d U . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.472(14) . ?
C1 H1A 0.96 . ?
C1 H1B 0.96 . ?
C1 H1C 0.96 . ?
C2 N1 1.292(13) . ?
C2 C3 1.538(10) . ?
C3 N2 1.236(13) . ?
C3 C4 1.500(14) . ?
C4 H4A 0.96 . ?
C4 H4B 0.96 . ?
C4 H4C 0.96 . ?
C5 N2 1.448(13) . ?
C5 C6 1.548(15) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C6 N3 1.509(12) . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C7 C8 1.447(14) . ?
C7 H7A 0.96 . ?
C7 H7B 0.96 . ?
C7 H7C 0.96 . ?
C8 N3 1.258(13) . ?
C8 C9 1.535(10) . ?
C9 N4 1.276(13) . ?
C9 C10 1.527(14) . ?
C10 H10A 0.96 . ?
C10 H10B 0.96 . ?
C10 H10C 0.96 . ?
C11 C12 1.349(16) . ?
C11 N5 1.396(13) . ?
C11 H11 0.93 . ?
C12 N6 1.343(13) . ?
C12 H12 0.93 . ?
C13 N6 1.344(13) . ?
C13 N5 1.346(13) . ?
C13 H13 0.93 . ?
C14 N6 1.445(13) . ?
C14 H14A 0.96 . ?
C14 H14B 0.96 . ?
C14 H14C 0.96 . ?
C15 C16 1.397(14) . ?
C15 N7 1.403(14) . ?
C15 H15 0.93 . ?
C16 N8 1.338(14) . ?
C16 H16 0.93 . ?
C17 N7 1.297(13) . ?
C17 N8 1.342(12) . ?
C17 H17 0.93 . ?
C18 N8 1.488(13) . ?
C18 H18A 0.96 . ?
C18 H18B 0.96 . ?
C18 H18C 0.96 . ?
N1 O1 1.339(11) . ?
N1 Co1 1.852(9) . ?
N2 Co1 1.854(8) . ?
N3 Co1 1.842(8) . ?
N4 O2 1.366(11) . ?
N4 Co1 1.882(8) . ?
N5 Co1 1.920(8) . ?
N7 Co1 1.917(7) . ?
O1 H1 0.82 . ?
O3 Cl1 1.417(9) . ?
O4 Cl1 1.385(9) . ?
O5 Cl1 1.427(9) . ?
O6 Cl1 1.449(10) . ?
O7 Cl2 1.393(8) . ?
O8 Cl2 1.498(18) . ?
O9 Cl2 1.370(10) . ?
O10 Cl2 1.431(19) . ?
O11 Cl2 1.58(2) . ?
O12 Cl2 1.37(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
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 . . ?
N1 C2 C1 126.4(9) . . ?
N1 C2 C3 106.0(8) . . ?
C1 C2 C3 127.6(9) . . ?
N2 C3 C4 125.3(9) . . ?
N2 C3 C2 116.8(9) . . ?
C4 C3 C2 117.8(9) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 110.8(9) . . ?
N2 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N3 C6 C5 110.1(8) . . ?
N3 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
N3 C6 H6B 109.7 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.2 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C7 129.8(9) . . ?
N3 C8 C9 108.2(9) . . ?
C7 C8 C9 122.1(9) . . ?
N4 C9 C10 122.6(9) . . ?
N4 C9 C8 113.4(9) . . ?
C10 C9 C8 123.9(9) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N5 109.6(9) . . ?
C12 C11 H11 125.2 . . ?
N5 C11 H11 125.2 . . ?
N6 C12 C11 107.1(10) . . ?
N6 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
N6 C13 N5 110.5(9) . . ?
N6 C13 H13 124.8 . . ?
N5 C13 H13 124.8 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N7 108.3(9) . . ?
C16 C15 H15 125.9 . . ?
N7 C15 H15 125.9 . . ?
N8 C16 C15 105.7(9) . . ?
N8 C16 H16 127.1 . . ?
C15 C16 H16 127.1 . . ?
N7 C17 N8 113.0(9) . . ?
N7 C17 H17 123.5 . . ?
N8 C17 H17 123.5 . . ?
N8 C18 H18A 109.5 . . ?
N8 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N8 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C2 N1 O1 122.0(9) . . ?
C2 N1 Co1 119.0(7) . . ?
O1 N1 Co1 118.7(7) . . ?
C3 N2 C5 131.5(9) . . ?
C3 N2 Co1 114.7(7) . . ?
C5 N2 Co1 113.4(7) . . ?
C8 N3 C6 127.5(9) . . ?
C8 N3 Co1 121.1(7) . . ?
C6 N3 Co1 111.0(6) . . ?
C9 N4 O2 124.4(8) . . ?
C9 N4 Co1 115.6(7) . . ?
O2 N4 Co1 120.0(6) . . ?
C13 N5 C11 104.3(8) . . ?
C13 N5 Co1 130.0(7) . . ?
C11 N5 Co1 125.6(7) . . ?
C12 N6 C13 108.5(9) . . ?
C12 N6 C14 125.1(9) . . ?
C13 N6 C14 126.4(8) . . ?
C17 N7 C15 104.7(8) . . ?
C17 N7 Co1 129.3(7) . . ?
C15 N7 Co1 125.9(7) . . ?
C16 N8 C17 108.2(8) . . ?
C16 N8 C18 126.0(8) . . ?
C17 N8 C18 125.7(9) . . ?
N1 O1 H1 109.5 . . ?
O4 Cl1 O3 111.2(6) . . ?
O4 Cl1 O5 110.9(6) . . ?
O3 Cl1 O5 110.0(6) . . ?
O4 Cl1 O6 109.6(6) . . ?
O3 Cl1 O6 108.4(6) . . ?
O5 Cl1 O6 106.6(7) . . ?
O9 Cl2 O12 121.0(14) . . ?
O9 Cl2 O7 112.7(7) . . ?
O12 Cl2 O7 119.4(13) . . ?
O9 Cl2 O10 119.3(10) . . ?
O12 Cl2 O10 63.8(16) . . ?
O7 Cl2 O10 111.5(9) . . ?
O9 Cl2 O8 99.8(9) . . ?
O12 Cl2 O8 42.2(14) . . ?
O7 Cl2 O8 105.6(8) . . ?
O10 Cl2 O8 106.0(11) . . ?
O9 Cl2 O11 93.3(11) . . ?
O12 Cl2 O11 100.6(17) . . ?
O7 Cl2 O11 102.1(10) . . ?
O10 Cl2 O11 38.0(11) . . ?
O8 Cl2 O11 141.6(12) . . ?
N3 Co1 N1 173.7(4) . . ?
N3 Co1 N2 90.7(3) . . ?
N1 Co1 N2 83.1(4) . . ?
N3 Co1 N4 81.6(3) . . ?
N1 Co1 N4 104.6(4) . . ?
N2 Co1 N4 172.2(4) . . ?
N3 Co1 N7 90.8(4) . . ?
N1 Co1 N7 89.4(4) . . ?
N2 Co1 N7 91.2(3) . . ?
N4 Co1 N7 90.4(4) . . ?
N3 Co1 N5 91.6(4) . . ?
N1 Co1 N5 88.4(4) . . ?
N2 Co1 N5 90.3(4) . . ?
N4 Co1 N5 88.4(4) . . ?
N7 Co1 N5 177.1(3) . . ?




# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dh2_73_0ma
_database_code_depnum_ccdc_archive 'CCDC 1038278'
_audit_update_record             
;
2015-10-27 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_date             2013-12-03T11:49:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
[(DO)2en(ImMe)2CoNa][PF6]2
;
_chemical_name_common            dh2_73
_chemical_formula_moiety         'C18 H28 Co N8 O2, 2(F6 P), Na'
_chemical_formula_sum            'C18 H28 Co F12 N8 Na O2 P2'
_chemical_formula_weight         760.34

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_Int_Tables_number      60
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
'x-1/2, y-1/2, -z-1/2'



_cell_length_a                   8.6942(9)
_cell_length_b                   22.063(2)
_cell_length_c                   14.9541(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2868.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    438
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_special_details           
;
  10 seconds, 0.5 degrees, 40 mm
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.7305
_exptl_absorpt_correction_T_max  0.9457

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.1143
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_number            110617
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.97
_reflns_number_total             3538
_reflns_number_gt                2829
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0795P)²+11.9636P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0022(5)
_refine_ls_number_reflns         3538
_refine_ls_number_parameters     204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0692
_refine_ls_wR_factor_ref         0.1849
_refine_ls_wR_factor_gt          0.1719
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.134

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.0764(5) 0.9498(2) 0.3621(3) 0.0258(9) Uani 1 1 d . . .
H1A H 0.0818 0.9506 0.4275 0.039 Uiso 1 1 calc R . .
H1B H -0.0148 0.927 0.3434 0.039 Uiso 1 1 calc R . .
H1C H 0.0697 0.9914 0.3393 0.039 Uiso 1 1 calc R . .
C2 C 0.2163(5) 0.92026(19) 0.3259(2) 0.0208(8) Uani 1 1 d . . .
C3 C 0.2415(5) 0.85490(19) 0.3231(2) 0.0201(8) Uani 1 1 d . . .
C4 C 0.1239(5) 0.8121(2) 0.3577(3) 0.0272(9) Uani 1 1 d . . .
H4A H 0.1392 0.7721 0.3305 0.041 Uiso 1 1 calc R . .
H4B H 0.021 0.8271 0.3427 0.041 Uiso 1 1 calc R . .
H4C H 0.1338 0.8088 0.4228 0.041 Uiso 1 1 calc R . .
C5 C 0.4347(5) 0.77727(18) 0.2843(3) 0.0229(8) Uani 1 1 d . . .
H5A H 0.3541 0.748 0.2663 0.027 Uiso 1 1 calc R . .
H5B H 0.4744 0.7652 0.3437 0.027 Uiso 1 1 calc R . .
C6 C 0.6091(5) 0.95693(19) 0.4165(3) 0.0225(8) Uani 1 1 d . . .
H6 H 0.5634 0.9949 0.4024 0.027 Uiso 1 1 calc R . .
C7 C 0.6935(5) 0.9440(2) 0.4915(3) 0.0253(9) Uani 1 1 d . . .
H7 H 0.7168 0.9711 0.539 0.03 Uiso 1 1 calc R . .
C8 C 0.6809(4) 0.86268(18) 0.4080(2) 0.0190(7) Uani 1 1 d . . .
H8 H 0.6952 0.8224 0.3873 0.023 Uiso 1 1 calc R . .
C9 C 0.8274(6) 0.8513(2) 0.5502(3) 0.0311(10) Uani 1 1 d . . .
H9A H 0.8408 0.8095 0.5294 0.047 Uiso 1 1 calc R . .
H9B H 0.7737 0.8512 0.6078 0.047 Uiso 1 1 calc R . .
H9C H 0.9284 0.8705 0.5572 0.047 Uiso 1 1 calc R . .
N1 N 0.3367(4) 0.95186(15) 0.2960(2) 0.0183(6) Uani 1 1 d . . .
N2 N 0.3702(4) 0.83858(15) 0.2885(2) 0.0199(7) Uani 1 1 d . . .
N3 N 0.6023(4) 0.90529(15) 0.3651(2) 0.0185(7) Uani 1 1 d . . .
N4 N 0.7374(4) 0.88501(17) 0.4850(2) 0.0219(7) Uani 1 1 d . . .
O1 O 0.3349(3) 1.00998(13) 0.29764(18) 0.0218(6) Uani 1 1 d . . .
F1 F 0.3615(4) 1.22666(15) 0.1636(2) 0.0465(8) Uani 1 1 d . . .
F2 F 0.4946(4) 1.14268(19) 0.1262(2) 0.0591(11) Uani 1 1 d . . .
F3 F 0.3950(4) 1.20222(15) 0.01912(18) 0.0426(8) Uani 1 1 d . . .
F4 F 0.1609(3) 1.19599(15) 0.08442(19) 0.0420(7) Uani 1 1 d . . .
F5 F 0.2631(4) 1.13501(15) 0.1911(2) 0.0452(8) Uani 1 1 d . . .
F6 F 0.2883(6) 1.11158(16) 0.0448(3) 0.0656(12) Uani 1 1 d . . .
P1 P 0.32641(13) 1.16869(5) 0.10401(7) 0.0235(3) Uani 1 1 d . . .
Co1 Co 0.5 0.90097(3) 0.25 0.0165(2) Uani 1 2 d S . .
Na1 Na 0.5 1.08153(11) 0.25 0.0265(5) Uani 1 2 d S . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.483(6) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 N1 1.335(5) . ?
C2 C3 1.459(6) . ?
C3 N2 1.285(5) . ?
C3 C4 1.485(6) . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 N2 1.466(5) . ?
C5 C5 1.529(8) 3_655 ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 C7 1.371(5) . ?
C6 N3 1.375(5) . ?
C6 H6 0.95 . ?
C7 N4 1.359(6) . ?
C7 H7 0.95 . ?
C8 N3 1.328(5) . ?
C8 N4 1.346(5) . ?
C8 H8 0.95 . ?
C9 N4 1.454(5) . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
N1 O1 1.283(4) . ?
N1 Co1 1.936(3) . ?
N2 Co1 1.870(3) . ?
N3 Co1 1.939(3) . ?
O1 Na1 2.249(3) . ?
F1 P1 1.588(3) . ?
F2 P1 1.605(3) . ?
F2 Na1 2.292(3) . ?
F3 P1 1.586(3) . ?
F4 P1 1.587(3) . ?
F5 P1 1.597(3) . ?
F5 Na1 2.532(4) . ?
F6 P1 1.576(3) . ?
P1 Na1 3.2775(18) . ?
Co1 N2 1.870(3) 3_655 ?
Co1 N1 1.936(3) 3_655 ?
Co1 N3 1.939(3) 3_655 ?
Na1 O1 2.249(3) 3_655 ?
Na1 F2 2.292(3) 3_655 ?
Na1 F5 2.532(4) 3_655 ?
Na1 P1 3.2775(18) 3_655 ?

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 109.5 . . ?
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 . . ?
N1 C2 C3 112.9(4) . . ?
N1 C2 C1 122.4(4) . . ?
C3 C2 C1 124.6(4) . . ?
N2 C3 C2 114.8(4) . . ?
N2 C3 C4 124.2(4) . . ?
C2 C3 C4 121.0(4) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C5 108.2(2) . 3_655 ?
N2 C5 H5A 110.1 . . ?
C5 C5 H5A 110.1 3_655 . ?
N2 C5 H5B 110.1 . . ?
C5 C5 H5B 110.1 3_655 . ?
H5A C5 H5B 108.4 . . ?
C7 C6 N3 107.9(4) . . ?
C7 C6 H6 126 . . ?
N3 C6 H6 126 . . ?
N4 C7 C6 107.0(4) . . ?
N4 C7 H7 126.5 . . ?
C6 C7 H7 126.5 . . ?
N3 C8 N4 110.0(4) . . ?
N3 C8 H8 125 . . ?
N4 C8 H8 125 . . ?
N4 C9 H9A 109.5 . . ?
N4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 N1 C2 120.4(3) . . ?
O1 N1 Co1 126.6(3) . . ?
C2 N1 Co1 113.0(3) . . ?
C3 N2 C5 127.5(3) . . ?
C3 N2 Co1 116.3(3) . . ?
C5 N2 Co1 115.8(3) . . ?
C8 N3 C6 107.1(3) . . ?
C8 N3 Co1 129.0(3) . . ?
C6 N3 Co1 123.8(3) . . ?
C8 N4 C7 108.0(3) . . ?
C8 N4 C9 125.6(4) . . ?
C7 N4 C9 126.4(4) . . ?
N1 O1 Na1 133.4(2) . . ?
P1 F2 Na1 113.32(18) . . ?
P1 F5 Na1 102.71(16) . . ?
F6 P1 F3 90.1(2) . . ?
F6 P1 F4 90.5(2) . . ?
F3 P1 F4 90.93(17) . . ?
F6 P1 F1 178.9(2) . . ?
F3 P1 F1 90.06(18) . . ?
F4 P1 F1 88.41(18) . . ?
F6 P1 F5 90.8(2) . . ?
F3 P1 F5 178.00(19) . . ?
F4 P1 F5 90.83(18) . . ?
F1 P1 F5 89.06(18) . . ?
F6 P1 F2 91.2(2) . . ?
F3 P1 F2 89.39(17) . . ?
F4 P1 F2 178.2(2) . . ?
F1 P1 F2 89.8(2) . . ?
F5 P1 F2 88.82(18) . . ?
F6 P1 Na1 90.12(17) . . ?
F3 P1 Na1 129.33(12) . . ?
F4 P1 Na1 139.73(12) . . ?
F1 P1 Na1 90.59(14) . . ?
F5 P1 Na1 48.90(13) . . ?
N2 Co1 N2 85.2(2) . 3_655 ?
N2 Co1 N1 168.03(15) . 3_655 ?
N2 Co1 N1 82.83(15) 3_655 3_655 ?
N2 Co1 N1 82.83(15) . . ?
N2 Co1 N1 168.03(15) 3_655 . ?
N1 Co1 N1 109.1(2) 3_655 . ?
N2 Co1 N3 91.87(14) . 3_655 ?
N2 Co1 N3 92.28(14) 3_655 3_655 ?
N1 Co1 N3 89.58(13) 3_655 3_655 ?
N1 Co1 N3 87.15(14) . 3_655 ?
N2 Co1 N3 92.28(14) . . ?
N2 Co1 N3 91.87(14) 3_655 . ?
N1 Co1 N3 87.15(14) 3_655 . ?
N1 Co1 N3 89.58(13) . . ?
N3 Co1 N3 174.4(2) 3_655 . ?
O1 Na1 O1 90.87(17) . 3_655 ?
O1 Na1 F2 130.99(13) . . ?
O1 Na1 F2 99.81(11) 3_655 . ?
O1 Na1 F2 99.81(11) . 3_655 ?
O1 Na1 F2 130.99(13) 3_655 3_655 ?
F2 Na1 F2 107.9(2) . 3_655 ?
O1 Na1 F5 137.39(11) . 3_655 ?
O1 Na1 F5 85.30(10) 3_655 3_655 ?
F2 Na1 F5 91.34(15) . 3_655 ?
F2 Na1 F5 55.09(11) 3_655 3_655 ?
O1 Na1 F5 85.30(10) . . ?
O1 Na1 F5 137.39(11) 3_655 . ?
F2 Na1 F5 55.09(11) . . ?
F2 Na1 F5 91.34(15) 3_655 . ?
F5 Na1 F5 124.44(18) 3_655 . ?
O1 Na1 P1 119.64(7) . 3_655 ?
O1 Na1 P1 109.20(8) 3_655 3_655 ?
F2 Na1 P1 101.67(14) . 3_655 ?
F2 Na1 P1 26.73(9) 3_655 3_655 ?
F5 Na1 P1 28.38(7) 3_655 3_655 ?
F5 Na1 P1 109.44(11) . 3_655 ?
O1 Na1 P1 109.20(8) . . ?
O1 Na1 P1 119.64(7) 3_655 . ?
F2 Na1 P1 26.73(9) . . ?
F2 Na1 P1 101.67(14) 3_655 . ?
F5 Na1 P1 109.44(11) 3_655 . ?
F5 Na1 P1 28.38(7) . . ?
P1 Na1 P1 108.15(8) 3_655 . ?



# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dh_177b_0m
_database_code_depnum_ccdc_archive 'CCDC 1038279'
_audit_update_record             
;
2015-10-27 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_date             2013-09-04T09:15:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 [((DO)2en(ImMe)2Co)2Zn(HOMe)][ClO4]4

;
_chemical_name_common            DH_197
_chemical_formula_moiety         'C37 H60 Co2 N16 O5 Zn, 4(Cl O4), H2 O'
_chemical_formula_sum            'C37 H62 Cl4 Co2 N16 O22 Zn'
_chemical_formula_weight         1408.06

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'



_cell_length_a                   13.3205(16)
_cell_length_b                   15.0242(18)
_cell_length_c                   17.218(2)
_cell_angle_alpha                70.715(6)
_cell_angle_beta                 76.405(7)
_cell_angle_gamma                67.308(6)
_cell_volume                     2977.7(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    321
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.57
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_special_details           
;
 10 sec, 0.5 deg., 40mm. Voids filled
 with delocalized methanol-water were
 removed with sqeeze
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.8719
_exptl_absorpt_correction_T_max  0.9457

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_number            125072
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_reflns_number_total             14926
_reflns_number_gt                11568
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0407P)²+6.3042P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         14926
_refine_ls_number_parameters     822
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0473
_refine_ls_wR_factor_ref         0.1138
_refine_ls_wR_factor_gt          0.1069
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.104
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.088

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.0782(2) 0.6202(2) 0.02650(18) 0.0247(6) Uani 1 1 d . . .
C2 C 0.0632(2) 0.7278(2) 0.00441(19) 0.0253(6) Uani 1 1 d . . .
C3 C 0.0062(3) 0.8682(2) 0.0687(2) 0.0315(7) Uani 1 1 d . . .
H3A H -0.023 0.9178 0.0178 0.038 Uiso 1 1 calc R . .
H3B H 0.0773 0.8727 0.0717 0.038 Uiso 1 1 calc R . .
C4 C -0.0741(3) 0.8904(2) 0.1448(2) 0.0295(7) Uani 1 1 d . . .
H4A H -0.0554 0.9345 0.1668 0.035 Uiso 1 1 calc R . .
H4B H -0.1497 0.9249 0.1299 0.035 Uiso 1 1 calc R . .
C5 C -0.1108(2) 0.7816(2) 0.2835(2) 0.0270(6) Uani 1 1 d . . .
C6 C -0.0921(3) 0.6764(2) 0.3282(2) 0.0293(7) Uani 1 1 d . . .
C7 C -0.1266(4) 0.6385(3) 0.4183(2) 0.0547(12) Uani 1 1 d . . .
H7A H -0.1714 0.5971 0.4254 0.082 Uiso 1 1 calc R . .
H7B H -0.1696 0.6953 0.4418 0.082 Uiso 1 1 calc R . .
H7C H -0.0615 0.5983 0.4469 0.082 Uiso 1 1 calc R . .
C8 C -0.1776(3) 0.8635(3) 0.3240(2) 0.0375(8) Uani 1 1 d . . .
H8A H -0.1779 0.9282 0.285 0.056 Uiso 1 1 calc R . .
H8B H -0.1459 0.8536 0.3734 0.056 Uiso 1 1 calc R . .
H8C H -0.253 0.8627 0.3401 0.056 Uiso 1 1 calc R . .
C9 C 0.0980(3) 0.7840(3) -0.0804(2) 0.0370(8) Uani 1 1 d . . .
H9A H 0.0452 0.8522 -0.0938 0.056 Uiso 1 1 calc R . .
H9B H 0.1009 0.7499 -0.1209 0.056 Uiso 1 1 calc R . .
H9C H 0.1708 0.7869 -0.0821 0.056 Uiso 1 1 calc R . .
C10 C 0.1156(3) 0.5604(3) -0.0351(2) 0.0329(7) Uani 1 1 d . . .
H10A H 0.125 0.49 -0.0062 0.049 Uiso 1 1 calc R . .
H10B H 0.1856 0.5659 -0.0663 0.049 Uiso 1 1 calc R . .
H10C H 0.0607 0.5858 -0.0734 0.049 Uiso 1 1 calc R . .
C11 C 0.1690(2) 0.7092(2) 0.2275(2) 0.0270(6) Uani 1 1 d . . .
H11 H 0.1201 0.7673 0.2438 0.032 Uiso 1 1 calc R . .
C12 C 0.2348(2) 0.5794(2) 0.1793(2) 0.0258(6) Uani 1 1 d . . .
H12 H 0.2404 0.529 0.155 0.031 Uiso 1 1 calc R . .
C13 C 0.3174(2) 0.5870(2) 0.2063(2) 0.0294(7) Uani 1 1 d . . .
H13 H 0.3914 0.5433 0.2048 0.035 Uiso 1 1 calc R . .
C14 C 0.3364(3) 0.7089(3) 0.2693(2) 0.0385(8) Uani 1 1 d . . .
H14A H 0.2849 0.762 0.2943 0.058 Uiso 1 1 calc R . .
H14B H 0.3857 0.7361 0.2241 0.058 Uiso 1 1 calc R . .
H14C H 0.3795 0.655 0.3114 0.058 Uiso 1 1 calc R . .
C15 C -0.2144(2) 0.7697(2) 0.10046(18) 0.0219(6) Uani 1 1 d . . .
H15 H -0.2052 0.8328 0.0736 0.026 Uiso 1 1 calc R . .
C16 C -0.1895(2) 0.6164(2) 0.1741(2) 0.0271(6) Uani 1 1 d . . .
H16 H -0.1578 0.5517 0.2091 0.033 Uiso 1 1 calc R . .
C17 C -0.2849(2) 0.6494(2) 0.1432(2) 0.0282(6) Uani 1 1 d . . .
H17 H -0.3326 0.6126 0.1519 0.034 Uiso 1 1 calc R . .
C18 C -0.3936(2) 0.8116(2) 0.0515(2) 0.0301(7) Uani 1 1 d . . .
H18A H -0.3998 0.8815 0.0418 0.045 Uiso 1 1 calc R . .
H18B H -0.461 0.8008 0.084 0.045 Uiso 1 1 calc R . .
H18C H -0.3825 0.7968 -0.0018 0.045 Uiso 1 1 calc R . .
C19 C 0.3554(2) 0.3106(2) 0.36203(19) 0.0258(6) Uani 1 1 d . . .
C20 C 0.4549(2) 0.2217(2) 0.36526(19) 0.0260(6) Uani 1 1 d . . .
C21 C 0.5374(2) 0.0666(2) 0.31879(19) 0.0249(6) Uani 1 1 d . . .
H21A H 0.525 0.0162 0.3707 0.03 Uiso 1 1 calc R . .
H21B H 0.6131 0.0668 0.313 0.03 Uiso 1 1 calc R . .
C22 C 0.5214(2) 0.0412(2) 0.24397(18) 0.0226(6) Uani 1 1 d . . .
H22A H 0.5688 0.065 0.1941 0.027 Uiso 1 1 calc R . .
H22B H 0.5416 -0.0321 0.2551 0.027 Uiso 1 1 calc R . .
C23 C 0.3510(2) 0.0706(2) 0.18920(17) 0.0195(5) Uani 1 1 d . . .
C24 C 0.2408(2) 0.1447(2) 0.17934(17) 0.0208(5) Uani 1 1 d . . .
C25 C 0.1615(3) 0.1448(2) 0.1318(2) 0.0282(6) Uani 1 1 d . . .
H25A H 0.0933 0.143 0.1683 0.042 Uiso 1 1 calc R . .
H25B H 0.1926 0.0859 0.11 0.042 Uiso 1 1 calc R . .
H25C H 0.1462 0.2056 0.0857 0.042 Uiso 1 1 calc R . .
C26 C 0.3926(2) -0.0166(2) 0.15374(19) 0.0238(6) Uani 1 1 d . . .
H26A H 0.4073 0.0063 0.0933 0.036 Uiso 1 1 calc R . .
H26B H 0.3374 -0.0496 0.1683 0.036 Uiso 1 1 calc R . .
H26C H 0.4604 -0.064 0.1763 0.036 Uiso 1 1 calc R . .
C27 C 0.5396(3) 0.1986(3) 0.4187(2) 0.0330(7) Uani 1 1 d . . .
H27A H 0.5141 0.1701 0.4764 0.049 Uiso 1 1 calc R . .
H27B H 0.5524 0.2602 0.4141 0.049 Uiso 1 1 calc R . .
H27C H 0.608 0.1503 0.4006 0.049 Uiso 1 1 calc R . .
C28 C 0.3342(3) 0.3883(3) 0.4053(2) 0.0309(7) Uani 1 1 d . . .
H28A H 0.2575 0.4322 0.4041 0.046 Uiso 1 1 calc R . .
H28B H 0.3824 0.428 0.3773 0.046 Uiso 1 1 calc R . .
H28C H 0.3489 0.3557 0.463 0.046 Uiso 1 1 calc R . .
C29 C 0.2849(2) 0.0295(2) 0.39216(18) 0.0237(6) Uani 1 1 d . . .
H29 H 0.3402 -0.017 0.3652 0.028 Uiso 1 1 calc R . .
C30 C 0.1793(2) 0.1668(3) 0.42411(19) 0.0278(6) Uani 1 1 d . . .
H30 H 0.1475 0.2356 0.4235 0.033 Uiso 1 1 calc R . .
C31 C 0.1467(2) 0.0913(3) 0.47846(19) 0.0292(7) Uani 1 1 d . . .
H31 H 0.088 0.0972 0.5223 0.035 Uiso 1 1 calc R . .
C32 C 0.2072(3) -0.0953(3) 0.4969(2) 0.0325(7) Uani 1 1 d . . .
H32A H 0.1383 -0.0966 0.4869 0.049 Uiso 1 1 calc R . .
H32B H 0.2091 -0.1125 0.5567 0.049 Uiso 1 1 calc R . .
H32C H 0.2692 -0.144 0.4729 0.049 Uiso 1 1 calc R . .
C33 C 0.4895(2) 0.2847(2) 0.14232(19) 0.0257(6) Uani 1 1 d . . .
H33 H 0.5493 0.2478 0.1739 0.031 Uiso 1 1 calc R . .
C34 C 0.3271(2) 0.3469(2) 0.10455(18) 0.0241(6) Uani 1 1 d . . .
H34 H 0.2509 0.362 0.1052 0.029 Uiso 1 1 calc R . .
C35 C 0.3943(3) 0.3841(2) 0.04042(19) 0.0274(6) Uani 1 1 d . . .
H35 H 0.3744 0.4288 -0.0117 0.033 Uiso 1 1 calc R . .
C36 C 0.5950(3) 0.3623(2) 0.0151(2) 0.0330(7) Uani 1 1 d . . .
H36A H 0.6432 0.361 0.0509 0.05 Uiso 1 1 calc R . .
H36B H 0.5744 0.4279 -0.0255 0.05 Uiso 1 1 calc R . .
H36C H 0.6336 0.31 -0.0141 0.05 Uiso 1 1 calc R . .
C37 C -0.0764(3) 0.2675(3) 0.3292(3) 0.0446(9) Uani 1 1 d . . .
H37A H -0.0815 0.263 0.2749 0.067 Uiso 1 1 calc R . .
H37B H -0.1448 0.2667 0.3657 0.067 Uiso 1 1 calc R . .
H37C H -0.0152 0.2104 0.3536 0.067 Uiso 1 1 calc R . .
N1 N 0.05501(18) 0.58291(17) 0.10654(14) 0.0197(5) Uani 1 1 d . . .
N2 N -0.0398(2) 0.61540(18) 0.28075(15) 0.0237(5) Uani 1 1 d . . .
N3 N 0.02194(19) 0.76671(18) 0.06573(16) 0.0231(5) Uani 1 1 d . . .
N4 N -0.06668(19) 0.79452(18) 0.20799(17) 0.0243(5) Uani 1 1 d . . .
N5 N 0.14061(18) 0.65688(17) 0.19282(15) 0.0205(5) Uani 1 1 d . . .
N6 N 0.2752(2) 0.66915(19) 0.23630(16) 0.0245(5) Uani 1 1 d . . .
N7 N -0.14503(19) 0.69285(18) 0.14644(15) 0.0225(5) Uani 1 1 d . . .
N8 N -0.30025(19) 0.74557(19) 0.09716(16) 0.0252(5) Uani 1 1 d . . .
N9 N 0.28549(19) 0.31250(18) 0.31906(15) 0.0221(5) Uani 1 1 d . . .
N10 N 0.21781(18) 0.21535(17) 0.21576(14) 0.0192(5) Uani 1 1 d . . .
N11 N 0.45781(19) 0.16644(19) 0.32127(15) 0.0221(5) Uani 1 1 d . . .
N12 N 0.40554(19) 0.09067(17) 0.23010(14) 0.0194(5) Uani 1 1 d . . .
N13 N 0.26699(19) 0.12666(19) 0.36966(14) 0.0213(5) Uani 1 1 d . . .
N14 N 0.2145(2) 0.0053(2) 0.45803(15) 0.0252(5) Uani 1 1 d . . .
N15 N 0.38743(19) 0.28398(17) 0.16830(15) 0.0208(5) Uani 1 1 d . . .
N16 N 0.4961(2) 0.34440(18) 0.06569(16) 0.0258(5) Uani 1 1 d . . .
O1 O 0.06625(17) 0.48696(15) 0.13561(13) 0.0245(4) Uani 1 1 d . . .
O2 O -0.01929(19) 0.51945(15) 0.31320(13) 0.0297(5) Uani 1 1 d . . .
O3 O 0.19085(16) 0.38690(16) 0.31322(14) 0.0273(5) Uani 1 1 d . . .
O4 O 0.12240(16) 0.28683(15) 0.20894(13) 0.0243(4) Uani 1 1 d . . .
O5 O -0.05824(19) 0.35818(17) 0.31969(17) 0.0407(6) Uani 1 1 d . . .
H5 H -0.1044 0.3892 0.3526 0.061 Uiso 1 1 calc R . .
O6 O 0.4450(3) -0.1853(3) 0.3475(3) 0.0652(12) Uani 0.845(6) 1 d PD A 1
O7 O 0.5838(6) -0.3409(3) 0.3789(4) 0.122(3) Uani 0.845(6) 1 d PD A 1
O8 O 0.6137(4) -0.2127(3) 0.2659(2) 0.0737(16) Uani 0.845(6) 1 d PD A 1
O9 O 0.5969(4) -0.1984(5) 0.3965(2) 0.0841(19) Uani 0.845(6) 1 d PD A 1
Cl1 Cl 0.55711(8) -0.23755(7) 0.34986(6) 0.0447(2) Uani 1 1 d D . .
O6B O 0.506(2) -0.1522(13) 0.3811(14) 0.086(8) Uani 0.155(6) 1 d PDU A 2
O7B O 0.5007(14) -0.3084(11) 0.4145(9) 0.039(5) Uani 0.155(6) 1 d PDU A 2
O8B O 0.5423(17) -0.2267(15) 0.2714(8) 0.050(5) Uani 0.155(6) 1 d PDU A 2
O9B O 0.6614(13) -0.2875(19) 0.3703(16) 0.089(9) Uani 0.155(6) 1 d PDU A 2
O10 O -0.4556(3) 0.3906(4) 0.2801(3) 0.0558(14) Uani 0.706(6) 1 d P B 1
O11 O -0.3029(4) 0.3185(3) 0.1941(3) 0.0448(10) Uani 0.706(6) 1 d P B 1
O12 O -0.2960(5) 0.4372(5) 0.2527(5) 0.0599(19) Uani 0.706(6) 1 d P B 1
O13 O -0.4089(8) 0.4903(5) 0.1489(5) 0.0293(13) Uani 0.706(6) 1 d P B 1
Cl2 Cl -0.36638(6) 0.40945(5) 0.22069(5) 0.02775(16) Uani 1 1 d D . .
O10B O -0.4438(9) 0.4357(10) 0.2898(7) 0.0558(14) Uani 0.294(6) 1 d PD B 2
O11B O -0.3505(10) 0.3086(7) 0.2237(7) 0.0448(10) Uani 0.294(6) 1 d PD B 2
O12B O -0.2696(12) 0.4197(15) 0.2240(13) 0.0599(19) Uani 0.294(6) 1 d PD B 2
O13B O -0.413(2) 0.4699(14) 0.1486(12) 0.0293(13) Uani 0.294(6) 1 d PD B 2
O14 O 0.3295(2) 0.83080(18) 0.06359(15) 0.0395(6) Uani 1 1 d . C 2
O15 O 0.28632(18) 0.88311(17) -0.07267(14) 0.0298(5) Uani 1 1 d . C 2
O16 O 0.4034(2) 0.9443(2) -0.03972(15) 0.0413(6) Uani 1 1 d . C 2
O17 O 0.2180(2) 0.99502(19) 0.01052(16) 0.0427(6) Uani 1 1 d . C 2
O18 O 0.0548(14) 0.8592(9) 0.3456(8) 0.044(2) Uani 0.577(4) 1 d P D 1
O19 O -0.0001(4) 1.0170(4) 0.2412(3) 0.0355(8) Uani 0.577(4) 1 d P D 1
O20 O 0.1817(11) 0.9497(19) 0.2878(14) 0.035(2) Uani 0.577(4) 1 d P D 1
O21 O 0.0162(5) 1.0143(5) 0.3744(4) 0.0309(11) Uani 0.577(4) 1 d P D 1
Cl4 Cl 0.06817(6) 0.95597(6) 0.31152(5) 0.02982(16) Uani 1 1 d D . .
O18B O 0.072(2) 0.8579(12) 0.3654(11) 0.044(2) Uani 0.423(4) 1 d PD D 2
O19B O 0.0524(5) 0.9541(5) 0.2325(3) 0.0355(8) Uani 0.423(4) 1 d PD D 2
O20B O 0.1742(15) 0.960(3) 0.301(2) 0.035(2) Uani 0.423(4) 1 d PD D 2
O21B O -0.0037(8) 1.0263(7) 0.3463(5) 0.0309(11) Uani 0.423(4) 1 d PD D 2
Cl3 Cl 0.31034(5) 0.91198(5) -0.00945(4) 0.02116(14) Uani 1 1 d . . .
Co1 Co -0.00420(3) 0.68073(3) 0.16843(2) 0.01862(9) Uani 1 1 d . . .
Co2 Co 0.33307(3) 0.20301(3) 0.27054(2) 0.01835(9) Uani 1 1 d . . .
Zn1 Zn 0.06763(3) 0.40787(2) 0.25583(2) 0.02205(8) Uani 1 1 d . . .
O22 O -0.2270(2) 1.11378(19) 0.29282(17) 0.0395(6) Uani 1 1 d D . .
H22P H -0.244(3) 1.1721(9) 0.269(3) 0.059 Uiso 1 1 d D . .
H22O H -0.1614(5) 1.094(3) 0.286(3) 0.059 Uiso 1 1 d D . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.316(4) . ?
C1 C2 1.476(4) . ?
C1 C10 1.490(4) . ?
C2 N3 1.283(4) . ?
C2 C9 1.493(4) . ?
C3 N3 1.473(4) . ?
C3 C4 1.527(5) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 N4 1.475(4) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 N4 1.278(4) . ?
C5 C6 1.461(4) . ?
C5 C8 1.491(4) . ?
C6 N2 1.314(4) . ?
C6 C7 1.493(5) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 N5 1.327(4) . ?
C11 N6 1.331(4) . ?
C11 H11 0.95 . ?
C12 C13 1.348(4) . ?
C12 N5 1.378(4) . ?
C12 H12 0.95 . ?
C13 N6 1.362(4) . ?
C13 H13 0.95 . ?
C14 N6 1.470(4) . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 N7 1.315(4) . ?
C15 N8 1.344(4) . ?
C15 H15 0.95 . ?
C16 C17 1.342(4) . ?
C16 N7 1.389(4) . ?
C16 H16 0.95 . ?
C17 N8 1.360(4) . ?
C17 H17 0.95 . ?
C18 N8 1.463(4) . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C19 N9 1.306(4) . ?
C19 C20 1.472(4) . ?
C19 C28 1.489(4) . ?
C20 N11 1.281(4) . ?
C20 C27 1.487(4) . ?
C21 N11 1.473(4) . ?
C21 C22 1.539(4) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C22 N12 1.470(4) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C23 N12 1.290(4) . ?
C23 C24 1.467(4) . ?
C23 C26 1.485(4) . ?
C24 N10 1.308(4) . ?
C24 C25 1.480(4) . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
C28 H28A 0.98 . ?
C28 H28B 0.98 . ?
C28 H28C 0.98 . ?
C29 N13 1.319(4) . ?
C29 N14 1.337(4) . ?
C29 H29 0.95 . ?
C30 C31 1.356(4) . ?
C30 N13 1.387(4) . ?
C30 H30 0.95 . ?
C31 N14 1.363(4) . ?
C31 H31 0.95 . ?
C32 N14 1.469(4) . ?
C32 H32A 0.98 . ?
C32 H32B 0.98 . ?
C32 H32C 0.98 . ?
C33 N15 1.331(4) . ?
C33 N16 1.333(4) . ?
C33 H33 0.95 . ?
C34 C35 1.358(4) . ?
C34 N15 1.374(4) . ?
C34 H34 0.95 . ?
C35 N16 1.366(4) . ?
C35 H35 0.95 . ?
C36 N16 1.466(4) . ?
C36 H36A 0.98 . ?
C36 H36B 0.98 . ?
C36 H36C 0.98 . ?
C37 O5 1.424(4) . ?
C37 H37A 0.98 . ?
C37 H37B 0.98 . ?
C37 H37C 0.98 . ?
N1 O1 1.320(3) . ?
N1 Co1 1.914(2) . ?
N2 O2 1.304(3) . ?
N2 Co1 1.898(2) . ?
N3 Co1 1.862(2) . ?
N4 Co1 1.867(2) . ?
N5 Co1 1.943(2) . ?
N7 Co1 1.929(2) . ?
N9 O3 1.322(3) . ?
N9 Co2 1.913(2) . ?
N10 O4 1.310(3) . ?
N10 Co2 1.904(2) . ?
N11 Co2 1.867(2) . ?
N12 Co2 1.862(2) . ?
N13 Co2 1.945(2) . ?
N15 Co2 1.941(2) . ?
O1 Zn1 2.018(2) . ?
O2 Zn1 2.046(2) . ?
O3 Zn1 1.982(2) . ?
O4 Zn1 2.040(2) . ?
O5 H5 0.84 . ?
O6 Cl1 1.397(4) . ?
O7 Cl1 1.390(4) . ?
O8 Cl1 1.466(4) . ?
O9 Cl1 1.422(4) . ?
Cl1 O8B 1.359(12) . ?
Cl1 O9B 1.367(14) . ?
Cl1 O6B 1.416(14) . ?
Cl1 O7B 1.542(11) . ?
O10 Cl2 1.427(4) . ?
O11 Cl2 1.460(4) . ?
O12 Cl2 1.433(5) . ?
O13 Cl2 1.459(6) . ?
Cl2 O12B 1.372(13) . ?
Cl2 O13B 1.393(14) . ?
Cl2 O11B 1.432(9) . ?
Cl2 O10B 1.433(10) . ?
O14 Cl3 1.425(2) . ?
O15 Cl3 1.435(2) . ?
O16 Cl3 1.428(2) . ?
O17 Cl3 1.445(2) . ?
O18 Cl4 1.441(10) . ?
O19 Cl4 1.508(4) . ?
O20 Cl4 1.445(11) . ?
O21 Cl4 1.491(6) . ?
Cl4 O21B 1.327(9) . ?
Cl4 O20B 1.406(15) . ?
Cl4 O19B 1.436(5) . ?
Cl4 O18B 1.449(14) . ?
O22 H22P 0.800(5) . ?
O22 H22O 0.800(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
N1 C1 C2 112.7(3) . . ?
N1 C1 C10 123.7(3) . . ?
C2 C1 C10 123.6(3) . . ?
N3 C2 C1 113.5(3) . . ?
N3 C2 C9 123.6(3) . . ?
C1 C2 C9 122.8(3) . . ?
N3 C3 C4 109.0(2) . . ?
N3 C3 H3A 109.9 . . ?
C4 C3 H3A 109.9 . . ?
N3 C3 H3B 109.9 . . ?
C4 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
N4 C4 C3 108.1(2) . . ?
N4 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
N4 C4 H4B 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
N4 C5 C6 113.4(3) . . ?
N4 C5 C8 125.0(3) . . ?
C6 C5 C8 121.6(3) . . ?
N2 C6 C5 113.1(3) . . ?
N2 C6 C7 121.7(3) . . ?
C5 C6 C7 125.3(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C9 H9A 109.5 . . ?
C2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 N6 110.8(3) . . ?
N5 C11 H11 124.6 . . ?
N6 C11 H11 124.6 . . ?
C13 C12 N5 108.5(3) . . ?
C13 C12 H12 125.8 . . ?
N5 C12 H12 125.8 . . ?
C12 C13 N6 107.2(3) . . ?
C12 C13 H13 126.4 . . ?
N6 C13 H13 126.4 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 N8 109.9(3) . . ?
N7 C15 H15 125.1 . . ?
N8 C15 H15 125.1 . . ?
C17 C16 N7 108.5(3) . . ?
C17 C16 H16 125.7 . . ?
N7 C16 H16 125.7 . . ?
C16 C17 N8 106.8(3) . . ?
C16 C17 H17 126.6 . . ?
N8 C17 H17 126.6 . . ?
N8 C18 H18A 109.5 . . ?
N8 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N8 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N9 C19 C20 112.5(3) . . ?
N9 C19 C28 123.4(3) . . ?
C20 C19 C28 124.1(3) . . ?
N11 C20 C19 113.7(3) . . ?
N11 C20 C27 124.8(3) . . ?
C19 C20 C27 121.4(3) . . ?
N11 C21 C22 107.8(2) . . ?
N11 C21 H21A 110.1 . . ?
C22 C21 H21A 110.1 . . ?
N11 C21 H21B 110.1 . . ?
C22 C21 H21B 110.1 . . ?
H21A C21 H21B 108.5 . . ?
N12 C22 C21 108.4(2) . . ?
N12 C22 H22A 110 . . ?
C21 C22 H22A 110 . . ?
N12 C22 H22B 110 . . ?
C21 C22 H22B 110 . . ?
H22A C22 H22B 108.4 . . ?
N12 C23 C24 113.0(2) . . ?
N12 C23 C26 125.1(3) . . ?
C24 C23 C26 121.9(3) . . ?
N10 C24 C23 113.3(2) . . ?
N10 C24 C25 121.3(3) . . ?
C23 C24 C25 125.4(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C20 C27 H27A 109.5 . . ?
C20 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C20 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C19 C28 H28A 109.5 . . ?
C19 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C19 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N13 C29 N14 110.8(3) . . ?
N13 C29 H29 124.6 . . ?
N14 C29 H29 124.6 . . ?
C31 C30 N13 108.3(3) . . ?
C31 C30 H30 125.8 . . ?
N13 C30 H30 125.8 . . ?
C30 C31 N14 106.8(3) . . ?
C30 C31 H31 126.6 . . ?
N14 C31 H31 126.6 . . ?
N14 C32 H32A 109.5 . . ?
N14 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N14 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N15 C33 N16 110.5(3) . . ?
N15 C33 H33 124.8 . . ?
N16 C33 H33 124.8 . . ?
C35 C34 N15 108.9(3) . . ?
C35 C34 H34 125.5 . . ?
N15 C34 H34 125.5 . . ?
C34 C35 N16 106.4(3) . . ?
C34 C35 H35 126.8 . . ?
N16 C35 H35 126.8 . . ?
N16 C36 H36A 109.5 . . ?
N16 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N16 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O5 C37 H37A 109.5 . . ?
O5 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O5 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C1 N1 O1 119.4(2) . . ?
C1 N1 Co1 114.0(2) . . ?
O1 N1 Co1 126.40(17) . . ?
O2 N2 C6 119.0(3) . . ?
O2 N2 Co1 126.91(18) . . ?
C6 N2 Co1 114.1(2) . . ?
C2 N3 C3 128.3(3) . . ?
C2 N3 Co1 116.8(2) . . ?
C3 N3 Co1 114.3(2) . . ?
C5 N4 C4 127.4(3) . . ?
C5 N4 Co1 116.3(2) . . ?
C4 N4 Co1 115.5(2) . . ?
C11 N5 C12 106.0(2) . . ?
C11 N5 Co1 127.7(2) . . ?
C12 N5 Co1 126.2(2) . . ?
C11 N6 C13 107.5(3) . . ?
C11 N6 C14 126.1(3) . . ?
C13 N6 C14 126.4(3) . . ?
C15 N7 C16 106.6(2) . . ?
C15 N7 Co1 128.6(2) . . ?
C16 N7 Co1 124.7(2) . . ?
C15 N8 C17 108.2(3) . . ?
C15 N8 C18 125.7(3) . . ?
C17 N8 C18 126.1(3) . . ?
C19 N9 O3 118.8(2) . . ?
C19 N9 Co2 114.8(2) . . ?
O3 N9 Co2 126.43(19) . . ?
C24 N10 O4 118.2(2) . . ?
C24 N10 Co2 114.31(19) . . ?
O4 N10 Co2 127.44(18) . . ?
C20 N11 C21 127.7(3) . . ?
C20 N11 Co2 116.6(2) . . ?
C21 N11 Co2 114.45(18) . . ?
C23 N12 C22 128.6(2) . . ?
C23 N12 Co2 116.67(19) . . ?
C22 N12 Co2 114.48(18) . . ?
C29 N13 C30 106.2(2) . . ?
C29 N13 Co2 127.5(2) . . ?
C30 N13 Co2 125.6(2) . . ?
C29 N14 C31 107.8(3) . . ?
C29 N14 C32 125.5(3) . . ?
C31 N14 C32 126.6(3) . . ?
C33 N15 C34 106.1(2) . . ?
C33 N15 Co2 128.3(2) . . ?
C34 N15 Co2 125.36(19) . . ?
C33 N16 C35 108.1(2) . . ?
C33 N16 C36 126.8(3) . . ?
C35 N16 C36 125.1(3) . . ?
N1 O1 Zn1 125.99(17) . . ?
N2 O2 Zn1 127.11(17) . . ?
N9 O3 Zn1 128.10(17) . . ?
N10 O4 Zn1 126.42(17) . . ?
C37 O5 H5 109.5 . . ?
O8B Cl1 O9B 116.6(14) . . ?
O8B Cl1 O7 98.4(9) . . ?
O9B Cl1 O7 65.5(11) . . ?
O8B Cl1 O6 76.4(9) . . ?
O9B Cl1 O6 167.0(12) . . ?
O7 Cl1 O6 114.2(3) . . ?
O8B Cl1 O6B 117.1(13) . . ?
O9B Cl1 O6B 111.1(15) . . ?
O7 Cl1 O6B 138.7(9) . . ?
O6 Cl1 O6B 59.8(12) . . ?
O8B Cl1 O9 142.3(9) . . ?
O9B Cl1 O9 61.9(12) . . ?
O7 Cl1 O9 112.1(4) . . ?
O6 Cl1 O9 108.4(3) . . ?
O6B Cl1 O9 49.2(12) . . ?
O8B Cl1 O8 42.5(8) . . ?
O9B Cl1 O8 83.4(11) . . ?
O7 Cl1 O8 109.1(3) . . ?
O6 Cl1 O8 108.3(3) . . ?
O6B Cl1 O8 111.3(9) . . ?
O9 Cl1 O8 104.3(3) . . ?
O8B Cl1 O7B 111.7(11) . . ?
O9B Cl1 O7B 98.3(11) . . ?
O7 Cl1 O7B 45.4(6) . . ?
O6 Cl1 O7B 75.3(7) . . ?
O6B Cl1 O7B 98.9(10) . . ?
O9 Cl1 O7B 105.5(7) . . ?
O8 Cl1 O7B 146.9(7) . . ?
O12B Cl2 O13B 113.2(12) . . ?
O12B Cl2 O10 135.2(9) . . ?
O13B Cl2 O10 104.9(11) . . ?
O12B Cl2 O11B 111.1(9) . . ?
O13B Cl2 O11B 106.5(9) . . ?
O10 Cl2 O11B 78.0(5) . . ?
O12B Cl2 O10B 109.3(9) . . ?
O13B Cl2 O10B 107.7(12) . . ?
O10 Cl2 O10B 33.6(5) . . ?
O11B Cl2 O10B 108.8(6) . . ?
O12B Cl2 O12 24.9(8) . . ?
O13B Cl2 O12 120.9(9) . . ?
O10 Cl2 O12 113.1(4) . . ?
O11B Cl2 O12 124.1(5) . . ?
O10B Cl2 O12 84.6(6) . . ?
O12B Cl2 O13 103.5(10) . . ?
O13B Cl2 O13 13.2(10) . . ?
O10 Cl2 O13 109.5(4) . . ?
O11B Cl2 O13 119.4(5) . . ?
O10B Cl2 O13 104.3(7) . . ?
O12 Cl2 O13 108.2(4) . . ?
O12B Cl2 O11 88.7(7) . . ?
O13B Cl2 O11 99.4(11) . . ?
O10 Cl2 O11 107.8(3) . . ?
O11B Cl2 O11 29.9(4) . . ?
O10B Cl2 O11 137.1(5) . . ?
O12 Cl2 O11 109.3(3) . . ?
O13 Cl2 O11 108.9(4) . . ?
O21B Cl4 O20B 110.2(11) . . ?
O21B Cl4 O19B 119.0(4) . . ?
O20B Cl4 O19B 105.9(12) . . ?
O21B Cl4 O18 114.4(9) . . ?
O20B Cl4 O18 117.9(18) . . ?
O19B Cl4 O18 87.9(5) . . ?
O21B Cl4 O20 121.3(9) . . ?
O20B Cl4 O20 12.1(16) . . ?
O19B Cl4 O20 95.1(8) . . ?
O18 Cl4 O20 112.9(11) . . ?
O21B Cl4 O18B 109.9(10) . . ?
O20B Cl4 O18B 106.6(17) . . ?
O19B Cl4 O18B 104.4(6) . . ?
O18 Cl4 O18B 17.6(8) . . ?
O20 Cl4 O18B 104.8(16) . . ?
O21B Cl4 O21 21.5(3) . . ?
O20B Cl4 O21 97.9(10) . . ?
O19B Cl4 O21 140.5(3) . . ?
O18 Cl4 O21 108.4(7) . . ?
O20 Cl4 O21 109.9(7) . . ?
O18B Cl4 O21 98.2(9) . . ?
O21B Cl4 O19 81.1(3) . . ?
O20B Cl4 O19 117.5(16) . . ?
O19B Cl4 O19 38.4(3) . . ?
O18 Cl4 O19 110.2(4) . . ?
O20 Cl4 O19 112.4(11) . . ?
O18B Cl4 O19 127.4(6) . . ?
O21 Cl4 O19 102.5(3) . . ?
O14 Cl3 O16 110.71(16) . . ?
O14 Cl3 O15 110.47(14) . . ?
O16 Cl3 O15 109.54(14) . . ?
O14 Cl3 O17 108.84(16) . . ?
O16 Cl3 O17 108.09(17) . . ?
O15 Cl3 O17 109.13(14) . . ?
N3 Co1 N4 86.33(11) . . ?
N3 Co1 N2 168.90(11) . . ?
N4 Co1 N2 82.65(11) . . ?
N3 Co1 N1 82.83(11) . . ?
N4 Co1 N1 168.48(11) . . ?
N2 Co1 N1 108.26(10) . . ?
N3 Co1 N7 92.84(10) . . ?
N4 Co1 N7 91.28(10) . . ?
N2 Co1 N7 88.70(11) . . ?
N1 Co1 N7 85.43(10) . . ?
N3 Co1 N5 90.00(10) . . ?
N4 Co1 N5 92.55(10) . . ?
N2 Co1 N5 89.21(10) . . ?
N1 Co1 N5 91.31(10) . . ?
N7 Co1 N5 175.37(10) . . ?
N12 Co2 N11 86.67(10) . . ?
N12 Co2 N10 82.70(10) . . ?
N11 Co2 N10 169.07(10) . . ?
N12 Co2 N9 168.82(10) . . ?
N11 Co2 N9 82.27(10) . . ?
N10 Co2 N9 108.43(10) . . ?
N12 Co2 N15 89.42(10) . . ?
N11 Co2 N15 93.88(10) . . ?
N10 Co2 N15 88.55(10) . . ?
N9 Co2 N15 89.73(10) . . ?
N12 Co2 N13 91.78(10) . . ?
N11 Co2 N13 90.71(10) . . ?
N10 Co2 N13 87.11(10) . . ?
N9 Co2 N13 89.97(10) . . ?
N15 Co2 N13 175.32(10) . . ?
O3 Zn1 O1 118.28(9) . . ?
O3 Zn1 O4 103.14(8) . . ?
O1 Zn1 O4 84.15(8) . . ?
O3 Zn1 O2 85.67(9) . . ?
O1 Zn1 O2 100.80(8) . . ?
O4 Zn1 O2 166.52(9) . . ?
H22P O22 H22O 105.2(9) . . ?


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.500 192 44 'H2O, methanol'
2 0.375 0.083 0.512 7 0 ' '
3 0.625 0.917 0.488 7 0 ' '
_platon_squeeze_details          
;
;

# start Validation Reply Form 
_vrf_PLAT420_I                   
; 

RESPONSE: delocalized solvent serves as acceptor, but 
was removed with the help of squeeze. 
;
# end Validation Reply Form





# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dh_183_0ma
_database_code_depnum_ccdc_archive 'CCDC 1038280'
_audit_update_record             
;
2015-10-27 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_date             2013-08-16T10:35:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
Complex 3-Mn
;
_chemical_name_common            dh_183
_chemical_formula_moiety         'C54 H84 Co3 Mn N24 O6, 5(Cl O4), 6(H2 O)'
_chemical_formula_sum            'C54 H96 Cl5 Co3 Mn N24 O32'
_chemical_formula_weight         2002.53

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_Int_Tables_number      167
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'



_cell_length_a                   28.810(3)
_cell_length_b                   28.810(3)
_cell_length_c                   16.9308(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     12170(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    325
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6210
_exptl_special_details           
;
 10 sec., 0.5 deg., 40mm
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.8923
_exptl_absorpt_correction_T_max  0.9457

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.1074
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_number            141055
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         28.4
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             3409
_reflns_number_gt                2381
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0550P)²+60.1006P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3409
_refine_ls_number_parameters     261
_refine_ls_number_restraints     83
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_ref         0.1417
_refine_ls_wR_factor_gt          0.1252
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.077

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.43617(17) 0.09914(19) 0.0382(2) 0.0729(16) Uani 1 1 d . A .
H1A H 0.4292 0.0637 0.0236 0.087 Uiso 1 1 calc R . .
H1B H 0.4097 0.1054 0.0127 0.087 Uiso 1 1 calc R . .
C2 C 0.51256(15) 0.14363(13) -0.0545(2) 0.0421(8) Uani 1 1 d . A .
C3 C 0.56565(13) 0.19121(12) -0.06233(18) 0.0318(7) Uani 1 1 d . A .
C4 C 0.60191(14) 0.20308(14) -0.13102(19) 0.0385(8) Uani 1 1 d . . .
H4A H 0.623 0.2412 -0.1382 0.058 Uiso 1 1 calc R . .
H4B H 0.581 0.187 -0.1776 0.058 Uiso 1 1 calc R . .
H4C H 0.6251 0.1887 -0.1217 0.058 Uiso 1 1 calc R . .
C5 C 0.48721(18) 0.10473(17) -0.1207(3) 0.0655(13) Uani 1 1 d . . .
H5A H 0.4593 0.0712 -0.1002 0.098 Uiso 1 1 calc R . .
H5B H 0.5138 0.0992 -0.1464 0.098 Uiso 1 1 calc R . .
H5C H 0.4722 0.1187 -0.158 0.098 Uiso 1 1 calc R . .
C6 C 0.61628(13) 0.18486(12) 0.15540(18) 0.0321(7) Uani 1 1 d . A .
H6 H 0.637 0.2213 0.166 0.038 Uiso 1 1 calc R . .
N4 N 0.5969(4) 0.1025(3) 0.1353(5) 0.046(2) Uani 0.5 1 d PDU A 1
C8 C 0.5599(4) 0.1112(3) 0.1051(5) 0.0438(19) Uani 0.5 1 d PDU A 1
H8 H 0.5316 0.086 0.0747 0.053 Uiso 0.5 1 calc PR A 1
C9 C 0.6007(5) 0.0535(4) 0.1355(7) 0.069(2) Uani 0.5 1 d PDU A 1
H9A H 0.5654 0.0227 0.1367 0.103 Uiso 0.5 1 calc PR A 1
H9B H 0.6204 0.0533 0.1812 0.103 Uiso 0.5 1 calc PR A 1
H9C H 0.619 0.0525 0.0886 0.103 Uiso 0.5 1 calc PR A 1
C7 C 0.63110(17) 0.14812(14) 0.17052(19) 0.0424(8) Uani 1 1 d D . .
H7 H 0.6637 0.1544 0.1935 0.051 Uiso 1 1 d R A .
N3 N 0.56664(12) 0.16070(10) 0.12232(16) 0.0367(7) Uani 1 1 d D . .
N4B N 0.5834(4) 0.0993(3) 0.1576(5) 0.046(2) Uani 0.5 1 d PD A 2
C8B C 0.5447(4) 0.1077(3) 0.1312(5) 0.0438(19) Uani 0.5 1 d PD A 2
H8B H 0.5094 0.0818 0.1209 0.053 Uiso 0.5 1 calc PR A 2
C9B C 0.5751(5) 0.0448(3) 0.1697(7) 0.069(2) Uani 0.5 1 d PD A 2
H9B1 H 0.5434 0.0241 0.2008 0.103 Uiso 0.5 1 calc PR A 2
H9B2 H 0.6055 0.0472 0.1968 0.103 Uiso 0.5 1 calc PR A 2
H9B3 H 0.5711 0.0277 0.1195 0.103 Uiso 0.5 1 calc PR A 2
N1 N 0.49012(12) 0.13959(11) 0.01267(18) 0.0449(8) Uani 1 1 d . . .
N2 N 0.57957(9) 0.22297(9) -0.00010(14) 0.0254(5) Uani 1 1 d . . .
O1 O 0.62596(7) 0.26662(7) 0.00113(11) 0.0238(4) Uani 1 1 d . A .
O2 O 0.5785(6) 0.0812(5) -0.0570(11) 0.1040(15) Uani 0.44553(2) 1 d PD B 1
O3 O 0.5349(4) 0.0068(4) -0.1389(7) 0.1040(15) Uani 0.44553(2) 1 d PD B 1
O4 O 0.6233(5) 0.0355(4) -0.1118(7) 0.1040(15) Uani 0.44553(2) 1 d PD B 1
O5 O 0.5926(4) 0.0815(3) -0.1958(6) 0.1040(15) Uani 0.44553(2) 1 d PD B 1
Cl1 Cl 0.58107(12) 0.04988(10) -0.1239(2) 0.0633(7) Uani 0.44553(2) 1 d PD B 1
O6 O 0.5473(7) -0.0032(6) -0.0326(9) 0.1040(15) Uani 0.29253(3) 1 d PD C 2
O7 O 0.6323(6) 0.0442(7) -0.0755(12) 0.1040(15) Uani 0.29253(3) 1 d PD C 2
O8 O 0.5704(7) 0.0249(6) -0.1704(9) 0.1040(15) Uani 0.29253(3) 1 d PD C 2
O9 O 0.5914(10) 0.0902(7) -0.0614(18) 0.1040(15) Uani 0.29253(3) 1 d PD C 2
Cl2 Cl 0.5853(2) 0.04005(16) -0.0812(3) 0.0633(7) Uani 0.29253(3) 1 d PD C 2
Co1 Co 0.528618(19) 0.195285(19) 0.0833 0.03092(18) Uani 1 2 d S A .
Mn1 Mn 0.6667 0.3333 0.0833 0.0190(2) Uani 1 6 d S . .
O14 O 0.6657(5) 0.0087(5) -0.2312(8) 0.077(4) Uani 0.3162 1 d PU . 1
H14O H 0.6579 0.0167 -0.1899 0.116 Uiso 0.3162 1 d PR . 1
H14P H 0.6926 0.0084 -0.2226 0.116 Uiso 0.3162 1 d PR . 1
O10 O 0.5068(10) 0.0114(14) -0.009(2) 0.1040(15) Uani 0.0950(2) 1 d PD . 3
O11 O 0.5780(14) 0.0905(7) -0.057(2) 0.1040(15) Uani 0.0950(2) 1 d PD . 3
O12 O 0.5617(17) 0.0129(16) -0.1198(16) 0.1040(15) Uani 0.0950(2) 1 d PD . 3
O13 O 0.5991(13) 0.0392(15) 0.0099(19) 0.1040(15) Uani 0.0950(2) 1 d PD . 3
Cl3 Cl 0.5603(6) 0.0393(4) -0.0453(9) 0.0633(7) Uani 0.0950(2) 1 d PD . 3
O14B O 0.6627(12) 0.0226(12) -0.122(2) 0.053(7) Uani 0.1 1 d PU D 3
H14R H 0.6782 0.0085 -0.0903 0.079 Uiso 0.1 1 d PR D 3
H14S H 0.6706 0.0512 -0.0956 0.079 Uiso 0.1 1 d PR D 3
O15 O 0.6707(10) 0.0203(9) -0.1703(17) 0.085(7) Uani 0.167 1 d PU E 4
H15O H 0.6793 -0.0017 -0.166 0.127 Uiso 0.167 1 d PR E 4
H15P H 0.6869 0.0419 -0.2066 0.127 Uiso 0.167 1 d PR E 4
O16 O 0.5993(12) 0.0970(11) -0.1039(18) 0.094(8) Uani 0.1667 1 d PU F 4
H16O H 0.5966 0.1036 -0.149 0.142 Uiso 0.1667 1 d PR F 4
H16P H 0.6165 0.0821 -0.1053 0.142 Uiso 0.1667 1 d PR F 4
O17 O 0.5341(10) 0.0096(11) -0.0587(17) 0.090(8) Uani 0.1667 1 d PU G 4
H17O H 0.5351 0.0375 -0.067 0.135 Uiso 0.1667 1 d PR G 4
H17P H 0.5127 -0.0114 -0.0947 0.135 Uiso 0.1667 1 d PR G 4
O18 O 0.628(2) 0.0468(19) -0.023(3) 0.083(13) Uani 0.0834 1 d PU H 4
H18O H 0.6549 0.0644 -0.0483 0.125 Uiso 0.0834 1 d PR H 4
H18P H 0.6078 0.0561 -0.0373 0.125 Uiso 0.0834 1 d PR H 4



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.466(5) . ?
C1 C1 1.540(8) 18_544 ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C2 N1 1.284(5) . ?
C2 C3 1.463(4) . ?
C2 C5 1.493(5) . ?
C3 N2 1.320(4) . ?
C3 C4 1.484(5) . ?
C4 H4A 0.96 . ?
C4 H4B 0.96 . ?
C4 H4C 0.96 . ?
C5 H5A 0.96 . ?
C5 H5B 0.96 . ?
C5 H5C 0.96 . ?
C6 C7 1.349(5) . ?
C6 N3 1.359(4) . ?
C6 H6 0.93 . ?
N4 C8 1.316(11) . ?
N4 C7 1.325(9) . ?
N4 C9 1.470(10) . ?
C8 N3 1.370(9) . ?
C8 H8 0.93 . ?
C9 H9A 0.96 . ?
C9 H9B 0.96 . ?
C9 H9C 0.96 . ?
C7 N4B 1.408(10) . ?
C7 H7 0.9461 . ?
N3 C8B 1.338(9) . ?
N3 Co1 1.929(3) . ?
N4B C8B 1.332(11) . ?
N4B C9B 1.479(10) . ?
C8B H8B 0.93 . ?
C9B H9B1 0.96 . ?
C9B H9B2 0.96 . ?
C9B H9B3 0.96 . ?
N1 Co1 1.859(3) . ?
N2 O1 1.299(3) . ?
N2 Co1 1.901(2) . ?
O1 Mn1 2.1800(19) . ?
O2 Cl1 1.472(15) . ?
O3 Cl1 1.313(10) . ?
O4 Cl1 1.483(12) . ?
O5 Cl1 1.457(10) . ?
O6 Cl2 1.438(14) . ?
O7 Cl2 1.303(15) . ?
O8 Cl2 1.569(14) . ?
O9 Cl2 1.406(17) . ?
Co1 N1 1.859(3) 18_544 ?
Co1 N2 1.901(2) 18_544 ?
Co1 N3 1.929(3) 18_544 ?
Mn1 O1 2.1799(19) 16_554 ?
Mn1 O1 2.1799(19) 18_544 ?
Mn1 O1 2.1800(19) 2_655 ?
Mn1 O1 2.1800(19) 3_665 ?
Mn1 O1 2.1801(19) 17_654 ?
O14 H14O 0.8022 . ?
O14 H14P 0.7961 . ?
O10 O10 0.65(6) 19_655 ?
O10 Cl3 1.472(15) . ?
O10 Cl3 1.97(3) 19_655 ?
O11 Cl3 1.313(10) . ?
O12 Cl3 1.484(12) . ?
O13 Cl3 1.457(10) . ?
Cl3 O10 1.97(3) 19_655 ?
O14B H14R 0.9173 . ?
O14B H14S 0.8605 . ?
O15 H15O 0.7906 . ?
O15 H15P 0.8318 . ?
O16 H16O 0.8001 . ?
O16 H16P 0.8001 . ?
O17 H17O 0.8025 . ?
O17 H17P 0.863 . ?
O18 H18O 0.8 . ?
O18 H18P 0.8 . ?

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 C1 C1 108.7(2) . 18_544 ?
N1 C1 H1A 110 . . ?
C1 C1 H1A 110 18_544 . ?
N1 C1 H1B 110 . . ?
C1 C1 H1B 110 18_544 . ?
H1A C1 H1B 108.3 . . ?
N1 C2 C3 114.1(3) . . ?
N1 C2 C5 124.2(3) . . ?
C3 C2 C5 121.7(3) . . ?
N2 C3 C2 113.0(3) . . ?
N2 C3 C4 122.1(3) . . ?
C2 C3 C4 124.9(3) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N3 109.9(3) . . ?
C7 C6 H6 125 . . ?
N3 C6 H6 125 . . ?
C8 N4 C7 104.9(7) . . ?
C8 N4 C9 129.8(9) . . ?
C7 N4 C9 125.2(9) . . ?
N4 C8 N3 114.1(8) . . ?
N4 C8 H8 122.9 . . ?
N3 C8 H8 122.9 . . ?
N4 C7 C6 108.8(5) . . ?
C6 C7 N4B 102.8(5) . . ?
N4 C7 H7 123.3 . . ?
C6 C7 H7 126.9 . . ?
N4B C7 H7 129.3 . . ?
C8B N3 C6 108.3(5) . . ?
C6 N3 C8 100.7(5) . . ?
C8B N3 Co1 124.2(5) . . ?
C6 N3 Co1 126.9(2) . . ?
C8 N3 Co1 130.0(5) . . ?
C8B N4B C7 110.9(7) . . ?
C8B N4B C9B 122.3(9) . . ?
C7 N4B C9B 126.8(9) . . ?
N4B C8B N3 106.6(8) . . ?
N4B C8B H8B 126.7 . . ?
N3 C8B H8B 126.7 . . ?
N4B C9B H9B1 109.5 . . ?
N4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
N4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C2 N1 C1 128.2(3) . . ?
C2 N1 Co1 115.8(2) . . ?
C1 N1 Co1 115.7(3) . . ?
O1 N2 C3 119.5(3) . . ?
O1 N2 Co1 126.79(18) . . ?
C3 N2 Co1 113.5(2) . . ?
N2 O1 Mn1 134.70(17) . . ?
H16P O2 H17O 109 . . ?
Cl1 O4 H14S 147.2 . . ?
H14S O4 H16P 106.4 . . ?
Cl1 O4 H18O 108.9 . . ?
H16P O4 H18O 74.9 . . ?
O3 Cl1 O5 103.6(6) . . ?
O3 Cl1 O2 113.0(7) . . ?
O5 Cl1 O2 109.0(8) . . ?
O3 Cl1 O4 110.4(7) . . ?
O5 Cl1 O4 109.1(7) . . ?
O2 Cl1 O4 111.4(8) . . ?
O7 Cl2 O9 107.3(13) . . ?
O7 Cl2 O6 110.1(11) . . ?
O9 Cl2 O6 113.9(13) . . ?
O7 Cl2 O8 102.9(11) . . ?
O9 Cl2 O8 113.0(15) . . ?
O6 Cl2 O8 109.1(9) . . ?
O6 Cl2 H16P 164 . . ?
O7 Cl2 H17O 165.9 . . ?
O8 Cl2 H18P 157 . . ?
N1 Co1 N1 86.25(19) 18_544 . ?
N1 Co1 N2 83.47(12) 18_544 18_544 ?
N1 Co1 N2 169.51(12) . 18_544 ?
N1 Co1 N2 169.51(12) 18_544 . ?
N1 Co1 N2 83.47(12) . . ?
N2 Co1 N2 106.87(14) 18_544 . ?
N1 Co1 N3 91.28(13) 18_544 18_544 ?
N1 Co1 N3 90.87(13) . 18_544 ?
N2 Co1 N3 87.26(11) 18_544 18_544 ?
N2 Co1 N3 90.99(10) . 18_544 ?
N1 Co1 N3 90.87(13) 18_544 . ?
N1 Co1 N3 91.27(13) . . ?
N2 Co1 N3 90.99(10) 18_544 . ?
N2 Co1 N3 87.26(11) . . ?
N3 Co1 N3 177.06(16) 18_544 . ?
O1 Mn1 O1 83.61(8) 16_554 18_544 ?
O1 Mn1 O1 104.44(10) 16_554 2_655 ?
O1 Mn1 O1 168.84(10) 18_544 2_655 ?
O1 Mn1 O1 168.85(10) 16_554 . ?
O1 Mn1 O1 89.55(10) 18_544 . ?
O1 Mn1 O1 83.61(7) 2_655 . ?
O1 Mn1 O1 89.56(10) 16_554 3_665 ?
O1 Mn1 O1 104.44(10) 18_544 3_665 ?
O1 Mn1 O1 83.61(8) 2_655 3_665 ?
O1 Mn1 O1 83.61(8) . 3_665 ?
O1 Mn1 O1 83.61(8) 16_554 17_654 ?
O1 Mn1 O1 83.61(8) 18_544 17_654 ?
O1 Mn1 O1 89.55(10) 2_655 17_654 ?
O1 Mn1 O1 104.44(10) . 17_654 ?
O1 Mn1 O1 168.85(10) 3_665 17_654 ?
H14O O14 H14P 104.9 . . ?
O11 Cl3 O13 103.6(7) . . ?
O11 Cl3 O10 113.0(8) . . ?
O13 Cl3 O10 109.0(8) . . ?
O11 Cl3 O12 110.5(7) . . ?
O13 Cl3 O12 109.1(7) . . ?
O10 Cl3 O12 111.4(9) . . ?
H14R O14B H14S 99.5 . . ?
H15O O15 H15P 112.6 . . ?
H16O O16 H16P 105.1 . . ?
H17O O17 H17P 103.4 . . ?
H18O O18 H18P 105.1 . . ?


# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_twin4a
_database_code_depnum_ccdc_archive 'CCDC 1038281'
_audit_update_record             
;
2015-10-27 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_date             2013-08-26T12:00:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 Complex 3-Cd
;
_chemical_name_common            dh_184
_chemical_formula_moiety         'C54 H84 Cd Co3 N24 O6, 5(Cl O4), 6(H2 O)'
_chemical_formula_sum            'C54 H96 Cd Cl5 Co3 N24 O32'
_chemical_formula_weight         2059.99

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_Int_Tables_number      167
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'



_cell_length_a                   28.981(3)
_cell_length_b                   28.981(3)
_cell_length_c                   16.838(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     12247(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    232
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6347.4
_exptl_special_details           
;
 60 sec., 0.5 deg., 40 mm
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.7915
_exptl_absorpt_correction_T_max  0.9457

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_number            9984
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.992
_reflns_number_total             3421
_reflns_number_gt                2407
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0583P)²+0.0628P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3421
_refine_ls_number_parameters     261
_refine_ls_number_restraints     83
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0789
_refine_ls_wR_factor_ref         0.1474
_refine_ls_wR_factor_gt          0.1311
_refine_ls_goodness_of_fit_ref   1.19
_refine_ls_restrained_S_all      1.194
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.43
_refine_diff_density_rms         0.083

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.4349(2) 0.0979(2) 0.0376(3) 0.0657(19) Uani 1 1 d . A .
H1A H 0.4278 0.0619 0.0225 0.079 Uiso 1 1 calc R . .
H1B H 0.4081 0.1044 0.0113 0.079 Uiso 1 1 calc R . .
C2 C 0.51082(19) 0.14103(19) -0.0544(3) 0.0387(12) Uani 1 1 d . A .
C3 C 0.56389(18) 0.18889(18) -0.0632(3) 0.0314(10) Uani 1 1 d . A .
C4 C 0.5995(2) 0.1997(2) -0.1325(3) 0.0405(11) Uani 1 1 d . . .
H4A H 0.6157 0.2373 -0.1475 0.061 Uiso 1 1 calc R . .
H4B H 0.5788 0.1772 -0.1772 0.061 Uiso 1 1 calc R . .
H4C H 0.6276 0.1917 -0.1185 0.061 Uiso 1 1 calc R . .
C5 C 0.4857(2) 0.1021(2) -0.1207(3) 0.0591(16) Uani 1 1 d . . .
H5A H 0.453 0.071 -0.1018 0.089 Uiso 1 1 calc R . .
H5B H 0.5105 0.0909 -0.1397 0.089 Uiso 1 1 calc R . .
H5C H 0.4772 0.119 -0.1643 0.089 Uiso 1 1 calc R . .
C6 C 0.61522(19) 0.18476(18) 0.1549(3) 0.0311(10) Uani 1 1 d . A .
H6 H 0.6362 0.2219 0.1648 0.037 Uiso 1 1 calc R . .
N4 N 0.5943(6) 0.1020(4) 0.1357(12) 0.054(4) Uani 0.5 1 d PDU A 1
C8 C 0.5576(6) 0.1108(4) 0.1047(8) 0.046(3) Uani 0.5 1 d PDU A 1
H8 H 0.529 0.0856 0.0729 0.056 Uiso 0.5 1 calc PR A 1
C9 C 0.6000(7) 0.0535(5) 0.1349(9) 0.070(4) Uani 0.5 1 d PDU A 1
H9A H 0.5789 0.0301 0.0912 0.105 Uiso 0.5 1 calc PR A 1
H9B H 0.5872 0.0345 0.1854 0.105 Uiso 0.5 1 calc PR A 1
H9C H 0.6376 0.0641 0.1276 0.105 Uiso 0.5 1 calc PR A 1
C7 C 0.6303(2) 0.1483(2) 0.1698(3) 0.0433(13) Uani 1 1 d D . .
H7 H 0.6629 0.1546 0.1928 0.052 Uiso 1 1 d R A .
N3 N 0.56504(15) 0.15968(14) 0.1232(2) 0.0346(9) Uani 1 1 d D . .
N4B N 0.5844(6) 0.0999(4) 0.1557(12) 0.054(4) Uani 0.5 1 d PD A 2
C8B C 0.5453(5) 0.1077(4) 0.1307(8) 0.046(3) Uani 0.5 1 d PD A 2
H8B H 0.5096 0.0808 0.1201 0.056 Uiso 0.5 1 calc PR A 2
C9B C 0.5759(6) 0.0449(5) 0.1656(9) 0.070(4) Uani 0.5 1 d PD A 2
H9B1 H 0.5499 0.0265 0.2079 0.105 Uiso 0.5 1 calc PR A 2
H9B2 H 0.6098 0.0471 0.1795 0.105 Uiso 0.5 1 calc PR A 2
H9B3 H 0.5626 0.0252 0.1157 0.105 Uiso 0.5 1 calc PR A 2
N1 N 0.48854(16) 0.13801(15) 0.0126(2) 0.0413(10) Uani 1 1 d . . .
N2 N 0.57806(13) 0.22087(14) -0.00157(19) 0.0257(8) Uani 1 1 d . . .
O1 O 0.62420(10) 0.26397(11) -0.00292(16) 0.0259(7) Uani 1 1 d . A .
O2 O 0.5789(8) 0.0806(6) -0.0551(13) 0.1032(18) Uani 0.4204(30) 1 d PD B 1
O3 O 0.5343(5) 0.0063(5) -0.1367(9) 0.1032(18) Uani 0.4204(30) 1 d PD B 1
O4 O 0.6244(5) 0.0347(6) -0.1170(9) 0.1032(18) Uani 0.4204(30) 1 d PD B 1
O5 O 0.5921(5) 0.0802(5) -0.1958(8) 0.1032(18) Uani 0.4204(30) 1 d PD B 1
Cl1 Cl 0.5829(2) 0.05073(19) -0.1248(3) 0.0619(11) Uani 0.4204(30) 1 d PD B 1
O6 O 0.5471(7) -0.0021(6) -0.0355(10) 0.1032(18) Uani 0.360(4) 1 d PD C 2
O7 O 0.6341(6) 0.0447(7) -0.0794(12) 0.1032(18) Uani 0.360(4) 1 d PD C 2
O8 O 0.5698(7) 0.0284(7) -0.1728(9) 0.1032(18) Uani 0.360(4) 1 d PD C 2
O9 O 0.5931(10) 0.0908(7) -0.0616(18) 0.1032(18) Uani 0.360(4) 1 d PD C 2
Cl2 Cl 0.5861(3) 0.0414(2) -0.0855(4) 0.0619(11) Uani 0.360(4) 1 d PD C 2
Co1 Co 0.52724(3) 0.19390(3) 0.0833 0.0309(2) Uani 1 2 d S A .
Cd1 Cd 0.6667 0.3333 0.0833 0.0206(2) Uani 1 6 d S . .
O14 O 0.6632(7) 0.0071(8) -0.2312(9) 0.069(5) Uani 0.29 1 d PU . 1
H14O H 0.6554 0.015 -0.1899 0.103 Uiso 0.29 1 d PR . 1
H14P H 0.6902 0.0067 -0.2226 0.103 Uiso 0.29 1 d PR . 1
O10 O 0.509(2) 0.016(3) -0.013(5) 0.1032(18) Uani 0.053(4) 1 d PD . 3
O11 O 0.585(3) 0.0895(15) -0.063(5) 0.1032(18) Uani 0.053(4) 1 d PD . 3
O12 O 0.564(3) 0.008(3) -0.121(3) 0.1032(18) Uani 0.053(4) 1 d PD . 3
O13 O 0.598(3) 0.034(3) 0.009(4) 0.1032(18) Uani 0.053(4) 1 d PD . 3
Cl3 Cl 0.5628(14) 0.0363(11) -0.048(2) 0.0619(11) Uani 0.053(4) 1 d PD . 3
O14B O 0.6701(15) 0.0216(14) -0.132(2) 0.069(10) Uani 0.12 1 d PU D 3
H14R H 0.6857 0.0075 -0.0999 0.103 Uiso 0.12 1 d PR D 3
H14S H 0.678 0.0501 -0.1055 0.103 Uiso 0.12 1 d PR D 3
O15 O 0.681(2) 0.017(2) -0.187(4) 0.069(16) Uani 0.08 1 d PU E 4
H15O H 0.6896 -0.0054 -0.1822 0.103 Uiso 0.08 1 d PR E 4
H15P H 0.6972 0.0382 -0.2229 0.103 Uiso 0.08 1 d PR E 4
O16 O 0.6030(17) 0.0954(18) -0.104(2) 0.115(14) Uani 0.17 1 d PU F 4
H16O H 0.6003 0.1021 -0.1489 0.173 Uiso 0.17 1 d PR F 4
H16P H 0.6202 0.0806 -0.1053 0.173 Uiso 0.17 1 d PR F 4
O17 O 0.5359(12) 0.0093(14) -0.062(2) 0.076(9) Uani 0.17 1 d PU G 4
H17O H 0.5368 0.0372 -0.07 0.115 Uiso 0.17 1 d PR G 4
H17P H 0.5145 -0.0117 -0.0977 0.115 Uiso 0.17 1 d PR G 4
O18 O 0.626(2) 0.045(2) -0.028(3) 0.152(18) Uani 0.17 1 d PU H 4
H18O H 0.6528 0.0629 -0.0532 0.227 Uiso 0.17 1 d PR H 4
H18P H 0.6057 0.0546 -0.0422 0.227 Uiso 0.17 1 d PR H 4



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.462(6) . ?
C1 C1 1.551(11) 18_544 ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 N1 1.281(6) . ?
C2 C3 1.476(6) . ?
C2 C5 1.492(7) . ?
C3 N2 1.313(5) . ?
C3 C4 1.484(6) . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.353(7) . ?
C6 N3 1.368(6) . ?
C6 H6 0.95 . ?
N4 C8 1.318(12) . ?
N4 C7 1.349(12) . ?
N4 C9 1.495(12) . ?
C8 N3 1.360(11) . ?
C8 H8 0.95 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C7 N4B 1.388(12) . ?
C7 H7 0.9499 . ?
N3 C8B 1.323(11) . ?
N3 Co1 1.929(4) . ?
N4B C8B 1.330(12) . ?
N4B C9B 1.495(12) . ?
C8B H8B 0.95 . ?
C9B H9B1 0.98 . ?
C9B H9B2 0.98 . ?
C9B H9B3 0.98 . ?
N1 Co1 1.867(4) . ?
N2 O1 1.295(4) . ?
N2 Co1 1.916(3) . ?
O1 Cd1 2.278(3) . ?
O2 Cl1 1.496(17) . ?
O3 Cl1 1.367(13) . ?
O4 Cl1 1.494(14) . ?
O5 Cl1 1.415(13) . ?
O6 Cl2 1.466(16) . ?
O7 Cl2 1.351(16) . ?
O8 Cl2 1.532(15) . ?
O9 Cl2 1.398(18) . ?
Co1 N1 1.866(4) 18_544 ?
Co1 N2 1.916(3) 18_544 ?
Co1 N3 1.929(4) 18_544 ?
Cd1 O1 2.278(3) 16_554 ?
Cd1 O1 2.278(3) 18_544 ?
Cd1 O1 2.278(3) 2_655 ?
Cd1 O1 2.278(3) 3_665 ?
Cd1 O1 2.278(3) 17_654 ?
O14 O14 0.72(3) 4_554 ?
O14 H14O 0.8 . ?
O14 H14P 0.8005 . ?
O10 O10 0.93(14) 19_655 ?
O10 Cl3 1.496(17) . ?
O10 Cl3 2.12(8) 19_655 ?
O11 Cl3 1.367(13) . ?
O12 Cl3 1.494(14) . ?
O13 Cl3 1.415(13) . ?
Cl3 O10 2.12(8) 19_655 ?
O14B H14R 0.9192 . ?
O14B H14S 0.863 . ?
O15 H15O 0.8100 . ?
O15 H15P 0.8200 . ?
O16 H16O 0.7966 . ?
O16 H16P 0.8049 . ?
O17 H17O 0.807 . ?
O17 H17P 0.8632 . ?
O18 H18O 0.8022 . ?
O18 H18P 0.8039 . ?

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 C1 H1A 110 . . ?
C1 C1 H1A 110 18_544 . ?
N1 C1 H1B 110 . . ?
C1 C1 H1B 110 18_544 . ?
H1A C1 H1B 108.4 . . ?
N1 C2 C3 113.9(4) . . ?
N1 C2 C5 124.7(5) . . ?
C3 C2 C5 121.3(5) . . ?
N2 C3 C2 113.3(4) . . ?
N2 C3 C4 122.2(4) . . ?
C2 C3 C4 124.4(4) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N3 109.2(4) . . ?
C7 C6 H6 125.4 . . ?
N3 C6 H6 125.4 . . ?
C8 N4 C7 105.8(10) . . ?
C8 N4 C9 131.1(11) . . ?
C7 N4 C9 123.1(11) . . ?
N4 C8 N3 112.9(10) . . ?
N4 C8 H8 123.6 . . ?
N3 C8 H8 123.6 . . ?
N4 C7 C6 107.9(7) . . ?
C6 C7 N4B 103.7(7) . . ?
N4 C7 H7 124.3 . . ?
C6 C7 H7 127.1 . . ?
N4B C7 H7 128.5 . . ?
C8B N3 C6 107.9(7) . . ?
C8 N3 C6 102.4(7) . . ?
C8B N3 Co1 125.8(6) . . ?
C8 N3 Co1 128.5(6) . . ?
C6 N3 Co1 126.1(3) . . ?
C8B N4B C7 110.5(10) . . ?
C8B N4B C9B 121.1(11) . . ?
C7 N4B C9B 128.4(11) . . ?
N3 C8B N4B 107.6(10) . . ?
N3 C8B H8B 126.2 . . ?
N4B C8B H8B 126.2 . . ?
N4B C9B H9B1 109.5 . . ?
N4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
N4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C2 N1 C1 127.4(4) . . ?
C2 N1 Co1 116.0(3) . . ?
C1 N1 Co1 116.4(3) . . ?
O1 N2 C3 118.3(3) . . ?
O1 N2 Co1 128.2(2) . . ?
C3 N2 Co1 113.4(3) . . ?
N2 O1 Cd1 132.9(2) . . ?
Cl1 O2 H17O 65.5 . . ?
H16P O2 H17O 105.6 . . ?
Cl1 O2 H18P 64.5 . . ?
H16P O2 H18P 52.6 . . ?
H17O O2 H18P 91 . . ?
Cl1 O3 H17O 65.5 . . ?
Cl1 O3 H17P 121.5 . . ?
H17O O3 H17P 65.3 . . ?
Cl1 O4 H14S 148.1 . . ?
H14S O4 H16P 106.5 . . ?
Cl1 O4 H18O 102.9 . . ?
H14S O4 H18O 56.8 . . ?
H16P O4 H18O 68.4 . . ?
Cl1 O5 H16O 67.4 . . ?
O3 Cl1 O5 103.8(9) . . ?
O3 Cl1 O4 109.3(8) . . ?
O5 Cl1 O4 109.0(9) . . ?
O3 Cl1 O2 108.6(9) . . ?
O5 Cl1 O2 111.0(10) . . ?
O4 Cl1 O2 114.7(11) . . ?
O3 Cl1 H16O 128.6 . . ?
O4 Cl1 H16O 116.6 . . ?
O2 Cl1 H16O 72.4 . . ?
O3 Cl1 H16P 168.3 . . ?
O5 Cl1 H16P 87.8 . . ?
O4 Cl1 H16P 64.6 . . ?
O2 Cl1 H16P 67.7 . . ?
H16O Cl1 H16P 61.8 . . ?
O3 Cl1 H17O 58.8 . . ?
O5 Cl1 H17O 123.2 . . ?
O4 Cl1 H17O 127.7 . . ?
H16O Cl1 H17O 105.1 . . ?
H16P Cl1 H17O 116.1 . . ?
O3 Cl1 H18P 114.2 . . ?
O5 Cl1 H18P 141.7 . . ?
H16O Cl1 H18P 106.3 . . ?
Cl2 O6 H17O 57.4 . . ?
Cl2 O6 H17P 83.7 . . ?
H17O O6 H17P 56.3 . . ?
Cl2 O7 H14S 155.3 . . ?
H14S O7 H16P 116.8 . . ?
Cl2 O7 H18O 119.2 . . ?
H14S O7 H18O 76.8 . . ?
H16P O7 H18O 92.3 . . ?
H14S O7 H18P 157.7 . . ?
H18O O7 H18P 81.6 . . ?
O7 Cl2 O9 106.8(13) . . ?
O7 Cl2 O6 109.9(11) . . ?
O9 Cl2 O6 111.8(13) . . ?
O7 Cl2 O8 105.6(11) . . ?
O9 Cl2 O8 113.4(15) . . ?
O6 Cl2 O8 109.2(10) . . ?
N1 Co1 N1 85.5(3) 18_544 . ?
N1 Co1 N2 83.33(16) 18_544 18_544 ?
N1 Co1 N2 168.59(17) . 18_544 ?
N1 Co1 N2 168.58(17) 18_544 . ?
N1 Co1 N2 83.32(16) . . ?
N2 Co1 N2 107.9(2) 18_544 . ?
N1 Co1 N3 91.45(17) 18_544 18_544 ?
N1 Co1 N3 90.82(17) . 18_544 ?
N2 Co1 N3 87.20(15) 18_544 18_544 ?
N2 Co1 N3 90.99(15) . 18_544 ?
N1 Co1 N3 90.82(17) 18_544 . ?
N1 Co1 N3 91.44(17) . . ?
N2 Co1 N3 90.99(15) 18_544 . ?
N2 Co1 N3 87.19(15) . . ?
N3 Co1 N3 176.9(2) 18_544 . ?
O1 Cd1 O1 83.72(11) 16_554 18_544 ?
O1 Cd1 O1 168.63(14) 16_554 . ?
O1 Cd1 O1 89.32(14) 18_544 . ?
O1 Cd1 O1 104.50(14) 16_554 2_655 ?
O1 Cd1 O1 168.63(14) 18_544 2_655 ?
O1 Cd1 O1 83.71(10) . 2_655 ?
O1 Cd1 O1 89.33(14) 16_554 3_665 ?
O1 Cd1 O1 104.51(14) 18_544 3_665 ?
O1 Cd1 O1 83.71(10) . 3_665 ?
O1 Cd1 O1 83.71(10) 2_655 3_665 ?
O1 Cd1 O1 83.71(10) 16_554 17_654 ?
O1 Cd1 O1 83.71(10) 18_544 17_654 ?
O1 Cd1 O1 104.50(14) . 17_654 ?
O1 Cd1 O1 89.32(14) 2_655 17_654 ?
O1 Cd1 O1 168.63(14) 3_665 17_654 ?
O14 O14 H14O 151.7 4_554 . ?
O14 O14 H14P 98.8 4_554 . ?
H14O O14 H14P 105.3 . . ?
O10 O10 Cl3 120(9) 19_655 . ?
Cl3 O10 Cl3 158(5) . 19_655 ?
Cl3 O10 H17O 156 19_655 . ?
Cl3 O11 H16P 81.9 . . ?
H17O O11 H18P 79 . . ?
Cl3 O12 H17P 70.9 . . ?
O11 Cl3 O13 103.8(9) . . ?
O11 Cl3 O12 109.3(9) . . ?
O13 Cl3 O12 109.0(9) . . ?
O11 Cl3 O10 108.6(10) . . ?
O13 Cl3 O10 111.0(10) . . ?
O12 Cl3 O10 114.7(11) . . ?
O11 Cl3 O10 130(5) . 19_655 ?
O13 Cl3 O10 96(5) . 19_655 ?
O12 Cl3 O10 106(5) . 19_655 ?
H17O Cl3 H17P 53.3 . . ?
H14R O14B H14S 99.9 . . ?
H15O O15 H15P 112.7 . . ?
H17O O17 H17P 103.7 . . ?
H18O O18 H18P 105.4 . . ?


# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dh_177_0ma
_database_code_depnum_ccdc_archive 'CCDC 1038282'
_audit_update_record             
;
2015-10-27 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_date             2013-08-27T10:06:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
complex 3-Zn
;
_chemical_name_common            dh_177
_chemical_formula_moiety         'C54 H84 Co3 N24 O6 Zn, 5(Cl O4), 6(H2 O)'
_chemical_formula_sum            'C54 H96 Cl5 Co3 N24 O32 Zn'
_chemical_formula_weight         2012.96

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_Int_Tables_number      167
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'



_cell_length_a                   28.732(3)
_cell_length_b                   28.732(3)
_cell_length_c                   17.5558(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     12551.0(19)
_cell_formula_units_Z            6
_cell_measurement_temperature    292(2)
_cell_measurement_reflns_used    312
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6240
_exptl_special_details           
;
 10 sec., 0.5 deg., 40 mm
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.7955
_exptl_absorpt_correction_T_max  0.8617

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      292(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.1365
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_number            133666
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         25.57
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_reflns_number_total             2588
_reflns_number_gt                1670
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0647P)²+29.7273P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2588
_refine_ls_number_parameters     260
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1394
_refine_ls_wR_factor_gt          0.1081
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.059

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.43791(18) 0.10113(19) 0.0405(3) 0.0876(15) Uani 1 1 d . B .
H1A H 0.4307 0.0655 0.0262 0.105 Uiso 1 1 calc R . .
H1B H 0.4113 0.1075 0.0163 0.105 Uiso 1 1 calc R . .
C2 C 0.51443(17) 0.14602(16) -0.0497(3) 0.0676(12) Uani 1 1 d . B .
C3 C 0.56744(15) 0.19368(15) -0.0567(2) 0.0579(10) Uani 1 1 d . B .
C4 C 0.60309(18) 0.20551(19) -0.1239(2) 0.0720(12) Uani 1 1 d . . .
H4A H 0.6238 0.2437 -0.1314 0.108 Uiso 1 1 calc R . .
H4B H 0.5816 0.1889 -0.1683 0.108 Uiso 1 1 calc R . .
H4C H 0.6268 0.1915 -0.1154 0.108 Uiso 1 1 calc R . .
C5 C 0.4890(2) 0.1071(2) -0.1136(3) 0.1007(18) Uani 1 1 d . . .
H5A H 0.4536 0.0781 -0.0974 0.151 Uiso 0.83 1 d PRD A 1
H5B H 0.5117 0.092 -0.1277 0.151 Uiso 0.83 1 d PR A 1
H5C H 0.4847 0.1256 -0.1576 0.151 Uiso 0.83 1 d PR A 1
H5D H 0.5131 0.1191 -0.1577 0.151 Uiso 0.17 1 d PR A 3
H5E H 0.455 0.1051 -0.1274 0.151 Uiso 0.17 1 d PR A 3
H5F H 0.482 0.0715 -0.0975 0.151 Uiso 0.17 1 d PR A 3
C6 C 0.61634(16) 0.18533(16) 0.1570(2) 0.0600(10) Uani 1 1 d . B .
H6 H 0.6366 0.2217 0.169 0.072 Uiso 1 1 calc R . .
N4 N 0.5959(5) 0.1033(4) 0.1340(8) 0.070(3) Uani 0.5 1 d PDU B 1
C8 C 0.5598(5) 0.1126(4) 0.1001(6) 0.064(3) Uani 0.5 1 d PDU B 1
H8 H 0.5331 0.089 0.067 0.077 Uiso 0.5 1 calc PR B 1
C9 C 0.5970(7) 0.0525(5) 0.1310(9) 0.101(4) Uani 0.5 1 d PDU B 1
H9A H 0.5804 0.0338 0.0847 0.151 Uiso 0.5 1 calc PR B 1
H9B H 0.5777 0.0305 0.1738 0.151 Uiso 0.5 1 calc PR B 1
H9C H 0.6336 0.0602 0.1325 0.151 Uiso 0.5 1 calc PR B 1
C7 C 0.63051(18) 0.14849(17) 0.1725(2) 0.0665(11) Uani 1 1 d D . .
H7 H 0.6631 0.1548 0.1954 0.08 Uiso 1 1 d R B .
N3 N 0.56803(12) 0.16170(12) 0.12112(19) 0.0572(8) Uani 1 1 d D . .
N4B N 0.5867(5) 0.1001(4) 0.1581(9) 0.070(3) Uani 0.5 1 d PD B 2
C8B C 0.5489(5) 0.1091(4) 0.1304(6) 0.064(3) Uani 0.5 1 d PD B 2
H8B H 0.5139 0.0825 0.1192 0.077 Uiso 0.5 1 calc PR B 2
C9B C 0.5811(7) 0.0467(5) 0.1702(9) 0.101(4) Uani 0.5 1 d PD B 2
H9B1 H 0.559 0.0301 0.2141 0.151 Uiso 0.5 1 calc PR B 2
H9B2 H 0.6159 0.0507 0.1783 0.151 Uiso 0.5 1 calc PR B 2
H9B3 H 0.5648 0.0247 0.1262 0.151 Uiso 0.5 1 calc PR B 2
N1 N 0.49192(13) 0.14157(13) 0.0153(2) 0.0649(9) Uani 1 1 d . . .
N2 N 0.58152(11) 0.22506(11) 0.00316(17) 0.0479(7) Uani 1 1 d . . .
O1 O 0.62835(9) 0.26893(10) 0.00439(15) 0.0519(6) Uani 1 1 d . B .
O2 O 0.5823(10) 0.0825(8) -0.0563(14) 0.197(4) Uani 0.3734(40) 1 d PD C 1
O3 O 0.5373(7) 0.0043(7) -0.1372(15) 0.197(4) Uani 0.3734(40) 1 d PD C 1
O4 O 0.6265(7) 0.0325(7) -0.1231(14) 0.197(4) Uani 0.3734(40) 1 d PD C 1
O5 O 0.5864(7) 0.0792(7) -0.1932(12) 0.197(4) Uani 0.3734(40) 1 d PD C 1
Cl1 Cl 0.5840(4) 0.0487(3) -0.1272(5) 0.125(2) Uani 0.3734(40) 1 d PDU C 1
O6 O 0.5357(9) 0.0053(8) -0.0396(17) 0.197(4) Uani 0.322(6) 1 d PD D 2
O7 O 0.6317(9) 0.0469(8) -0.0829(19) 0.197(4) Uani 0.322(6) 1 d PD D 2
O8 O 0.5738(10) 0.0292(9) -0.1771(16) 0.197(4) Uani 0.322(6) 1 d PD D 2
O9 O 0.5930(12) 0.0952(8) -0.079(2) 0.197(4) Uani 0.322(6) 1 d PD D 2
Cl2 Cl 0.5851(5) 0.0425(3) -0.0901(8) 0.125(2) Uani 0.322(6) 1 d PD D 2
Co1 Co 0.53048(2) 0.19715(2) 0.0833 0.0517(3) Uani 1 2 d S B .
Zn1 Zn 0.6667 0.3333 0.0833 0.0454(3) Uani 1 6 d S . .
O14 O 0.6641(11) 0.0067(15) -0.2285(17) 0.235(12) Uani 0.32 1 d PU . 1
H14O H 0.6564 0.0147 -0.1872 0.352 Uiso 0.32 1 d PR . 1
H14P H 0.6911 0.0064 -0.2198 0.352 Uiso 0.32 1 d PR . 1
O10 O 0.5199(13) 0.0331(16) -0.006(2) 0.197(4) Uani 0.138(6) 1 d PD . 3
O11 O 0.6006(16) 0.0896(11) -0.077(3) 0.197(4) Uani 0.138(6) 1 d PD . 3
O12 O 0.5587(18) 0.0024(17) -0.118(3) 0.197(4) Uani 0.138(6) 1 d PD . 3
O13 O 0.6059(16) 0.0382(16) 0.006(3) 0.197(4) Uani 0.138(6) 1 d PD . 3
Cl3 Cl 0.5710(8) 0.0401(5) -0.0509(15) 0.125(2) Uani 0.138(6) 1 d PD . 3
O14B O 0.525(4) -0.022(4) -0.270(8) 0.29(5) Uani 0.1 1 d PU . 3
H14R H 0.5401 -0.036 -0.2379 0.431 Uiso 0.1 1 d PR . 3
H14S H 0.5324 0.0066 -0.2436 0.431 Uiso 0.1 1 d PR . 3
O15 O 0.678(3) 0.025(3) -0.121(4) 0.18(3) Uani 0.082 1 d PU E 4
H15O H 0.6861 0.0035 -0.1165 0.273 Uiso 0.082 1 d PR E 4
H15P H 0.6936 0.047 -0.1572 0.273 Uiso 0.082 1 d PR E 4
O16 O 0.6069(15) 0.1008(16) -0.146(3) 0.166(13) Uani 0.166 1 d PU F 4
H16O H 0.6042 0.1075 -0.1911 0.24 Uiso 0.166 1 d PR F 4
H16P H 0.6241 0.086 -0.1474 0.24 Uiso 0.166 1 d PR F 4
O17 O 0.545(2) 0.006(3) -0.071(3) 0.20(2) Uani 0.166 1 d PU G 4
H17O H 0.5456 0.0337 -0.079 0.307 Uiso 0.166 1 d PRD G 4
H17P H 0.5233 -0.0152 -0.1067 0.307 Uiso 0.166 1 d PR G 4
O18 O 0.612(3) 0.032(3) -0.038(4) 0.24(3) Uani 0.166 1 d PU G 4
H18O H 0.6384 0.0497 -0.0631 0.362 Uiso 0.166 1 d PR G 4
H18P H 0.5913 0.0414 -0.0521 0.362 Uiso 0.166 1 d PR G 4



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.467(5) . ?
C1 C1 1.513(10) 18_544 ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C2 N1 1.285(6) . ?
C2 C3 1.457(6) . ?
C2 C5 1.492(6) . ?
C3 N2 1.310(5) . ?
C3 C4 1.487(6) . ?
C4 H4A 0.96 . ?
C4 H4B 0.96 . ?
C4 H4C 0.96 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C5 H5D 0.98 . ?
C5 H5E 0.98 . ?
C5 H5F 0.98 . ?
C6 C7 1.338(5) . ?
C6 N3 1.357(5) . ?
C6 H6 0.93 . ?
N4 C8 1.333(11) . ?
N4 C7 1.355(11) . ?
N4 C9 1.476(11) . ?
C8 N3 1.360(10) . ?
C8 H8 0.93 . ?
C9 H9A 0.96 . ?
C9 H9B 0.96 . ?
C9 H9C 0.96 . ?
C7 N4B 1.353(11) . ?
C7 H7 0.95 . ?
N3 C8B 1.334(10) . ?
N3 Co1 1.934(3) . ?
N4B C8B 1.329(11) . ?
N4B C9B 1.476(11) . ?
C8B H8B 0.93 . ?
C9B H9B1 0.96 . ?
C9B H9B2 0.96 . ?
C9B H9B3 0.96 . ?
N1 Co1 1.854(4) . ?
N2 O1 1.305(4) . ?
N2 Co1 1.897(3) . ?
O1 Zn1 2.126(2) . ?
O2 Cl1 1.59(2) . ?
O3 Cl1 1.323(19) . ?
O4 Cl1 1.51(2) . ?
O5 Cl1 1.432(18) . ?
O6 Cl2 1.56(3) . ?
O7 Cl2 1.29(2) . ?
O8 Cl2 1.57(2) . ?
O9 Cl2 1.43(2) . ?
Co1 N1 1.854(4) 18_544 ?
Co1 N2 1.897(3) 18_544 ?
Co1 N3 1.934(3) 18_544 ?
Zn1 O1 2.126(2) 16_554 ?
Zn1 O1 2.126(2) 18_544 ?
Zn1 O1 2.126(2) 2_655 ?
Zn1 O1 2.126(2) 3_665 ?
Zn1 O1 2.126(2) 17_654 ?
O14 O14 0.83(6) 4_554 ?
O14 H14O 0.8243 . ?
O14 H14P 0.7951 . ?
O10 Cl3 1.59(2) . ?
O11 Cl3 1.323(19) . ?
O12 Cl3 1.51(2) . ?
O13 Cl3 1.432(18) . ?
O14B H14R 0.9277 . ?
O14B H14S 0.8674 . ?
O15 H15O 0.7700 . ?
O15 H15P 0.8477 . ?
O16 H16O 0.8268 . ?
O16 H16P 0.798 . ?
O17 O18 1.78(8) . ?
O17 H17O 0.8013 . ?
O17 H17P 0.8779 . ?
O18 H18O 0.8071 . ?
O18 H18P 0.8008 . ?

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 C1 C1 109.1(3) . 18_544 ?
N1 C1 H1A 109.9 . . ?
C1 C1 H1A 109.9 18_544 . ?
N1 C1 H1B 109.9 . . ?
C1 C1 H1B 109.9 18_544 . ?
H1A C1 H1B 108.3 . . ?
N1 C2 C3 113.9(4) . . ?
N1 C2 C5 124.0(4) . . ?
C3 C2 C5 122.1(5) . . ?
N2 C3 C2 113.4(4) . . ?
N2 C3 C4 122.6(4) . . ?
C2 C3 C4 124.0(4) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.4 . . ?
C2 C5 H5B 109.6 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C5 H5D 109.6 . . ?
H5A C5 H5D 141.1 . . ?
C2 C5 H5E 109.4 . . ?
H5B C5 H5E 141.1 . . ?
H5D C5 H5E 109.5 . . ?
C2 C5 H5F 109.5 . . ?
H5C C5 H5F 141.1 . . ?
H5D C5 H5F 109.5 . . ?
H5E C5 H5F 109.5 . . ?
C7 C6 N3 109.8(4) . . ?
C7 C6 H6 125.1 . . ?
N3 C6 H6 125.1 . . ?
C8 N4 C7 107.6(9) . . ?
C8 N4 C9 125.7(11) . . ?
C7 N4 C9 126.6(11) . . ?
N4 C8 N3 109.7(9) . . ?
N4 C8 H8 125.2 . . ?
N3 C8 H8 125.2 . . ?
C6 C7 N4B 106.3(6) . . ?
C6 C7 N4 106.8(6) . . ?
C6 C7 H7 126.6 . . ?
N4B C7 H7 126.6 . . ?
N4 C7 H7 125 . . ?
C8B N3 C6 104.4(6) . . ?
C6 N3 C8 104.4(6) . . ?
C8B N3 Co1 128.0(6) . . ?
C6 N3 Co1 126.6(2) . . ?
C8 N3 Co1 126.9(6) . . ?
C8B N4B C7 107.4(9) . . ?
C8B N4B C9B 125.5(11) . . ?
C7 N4B C9B 127.1(11) . . ?
N4B C8B N3 110.5(9) . . ?
N4B C8B H8B 124.7 . . ?
N3 C8B H8B 124.7 . . ?
N4B C9B H9B1 109.5 . . ?
N4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
N4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C2 N1 C1 128.9(4) . . ?
C2 N1 Co1 115.6(3) . . ?
C1 N1 Co1 115.3(3) . . ?
O1 N2 C3 119.5(3) . . ?
O1 N2 Co1 127.0(2) . . ?
C3 N2 Co1 113.4(2) . . ?
N2 O1 Zn1 133.4(2) . . ?
Cl1 O3 H17P 123.2 . . ?
H17O O3 H17P 76.6 . . ?
Cl1 O4 H18O 91.3 . . ?
Cl1 O5 H16O 116.3 . . ?
Cl1 O5 H16P 50.6 . . ?
O3 Cl1 O5 101.5(13) . . ?
O3 Cl1 O4 107.1(11) . . ?
O5 Cl1 O4 115.3(13) . . ?
O3 Cl1 O2 111.5(14) . . ?
O5 Cl1 O2 105.5(12) . . ?
O4 Cl1 O2 115.2(13) . . ?
O7 Cl2 O9 106.1(17) . . ?
O7 Cl2 O6 124.0(18) . . ?
O9 Cl2 O6 104.9(16) . . ?
O7 Cl2 O8 101.4(18) . . ?
O9 Cl2 O8 107.1(17) . . ?
O6 Cl2 O8 112.3(15) . . ?
N1 Co1 N1 86.3(2) 18_544 . ?
N1 Co1 N2 83.61(15) 18_544 18_544 ?
N1 Co1 N2 169.67(15) . 18_544 ?
N1 Co1 N2 169.67(15) 18_544 . ?
N1 Co1 N2 83.60(15) . . ?
N2 Co1 N2 106.56(17) 18_544 . ?
N1 Co1 N3 91.04(14) 18_544 18_544 ?
N1 Co1 N3 90.27(14) . 18_544 ?
N2 Co1 N3 87.73(13) 18_544 18_544 ?
N2 Co1 N3 91.21(12) . 18_544 ?
N1 Co1 N3 90.27(14) 18_544 . ?
N1 Co1 N3 91.03(14) . . ?
N2 Co1 N3 91.20(12) 18_544 . ?
N2 Co1 N3 87.72(13) . . ?
N3 Co1 N3 178.21(18) 18_544 . ?
O1 Zn1 O1 82.10(10) 16_554 18_544 ?
O1 Zn1 O1 104.61(13) 16_554 2_655 ?
O1 Zn1 O1 170.51(12) 18_544 2_655 ?
O1 Zn1 O1 170.52(12) 16_554 . ?
O1 Zn1 O1 92.08(13) 18_544 . ?
O1 Zn1 O1 82.10(10) 2_655 . ?
O1 Zn1 O1 92.08(13) 16_554 3_665 ?
O1 Zn1 O1 104.61(13) 18_544 3_665 ?
O1 Zn1 O1 82.10(10) 2_655 3_665 ?
O1 Zn1 O1 82.10(10) . 3_665 ?
O1 Zn1 O1 82.10(10) 16_554 17_654 ?
O1 Zn1 O1 82.10(10) 18_544 17_654 ?
O1 Zn1 O1 92.08(13) 2_655 17_654 ?
O1 Zn1 O1 104.61(13) . 17_654 ?
O1 Zn1 O1 170.52(12) 3_665 17_654 ?
O14 O14 H14O 154.4 4_554 . ?
O14 O14 H14P 99.8 4_554 . ?
H14O O14 H14P 103.7 . . ?
Cl3 O10 O10 105(3) . 19_655 ?
O11 Cl3 O13 101.5(13) . . ?
O11 Cl3 O12 107.1(12) . . ?
O13 Cl3 O12 115.3(13) . . ?
O11 Cl3 O10 111.5(14) . . ?
O13 Cl3 O10 105.5(12) . . ?
O12 Cl3 O10 115.2(13) . . ??
H14R O14B H14S 97.8 . . ?
H16O O16 H16P 104.4 . . ?
H17O O17 H17P 102.6 . . ?
H17O O17 H18P 75.1 . . ?
H18O O18 H18P 104.1 . . ?



# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_twin5
_database_code_depnum_ccdc_archive 'CCDC 1425227'
_audit_update_record             
;
2015-10-27 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_date             2014-12-08T14:51:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
[(DO)2en(ImMe)2CoNa-15crown5][BPh4]2
;
_chemical_name_common            dh3_29
_chemical_formula_moiety         'C28 H48 Co N8 Na O7, 2(C24 H20 B)'
_chemical_formula_sum            'C76 H88 B2 Co N8 Na O7'
_chemical_formula_weight         1329.08
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_Int_Tables_number      1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'



_cell_length_a                   11.8905(14)
_cell_length_b                   12.4560(16)
_cell_length_c                   13.6113(17)
_cell_angle_alpha                72.344(5)
_cell_angle_beta                 66.193(4)
_cell_angle_gamma                73.679(4)
_cell_volume                     1728.2(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    161
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       shard
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             704
_exptl_special_details           
;
 120 seconds, 1 degree, 40 mm
 179.8 degree twin about (0.005  1.000  0.991) or [-0.719  1.000  0.908]
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.8897
_exptl_absorpt_correction_T_max  0.9745

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.1023
_diffrn_reflns_av_unetI/netI     0.1648
_diffrn_reflns_number            57397
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.991
_reflns_number_total             33864
_reflns_number_gt                21543
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0313P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         33864
_refine_ls_number_parameters     865
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.0677
_refine_ls_wR_factor_ref         0.1303
_refine_ls_wR_factor_gt          0.1102
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.036(12)
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.111

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.3801(4) -0.3827(4) 0.7872(4) 0.0230(12) Uani 1 1 d . . .
H1A H 0.3684 -0.3002 0.7812 0.035 Uiso 1 1 calc R . .
H1B H 0.3093 -0.4131 0.8477 0.035 Uiso 1 1 calc R . .
H1C H 0.3851 -0.3963 0.7182 0.035 Uiso 1 1 calc R . .
C2 C 0.4992(4) -0.4417(4) 0.8094(4) 0.0149(11) Uani 1 1 d . . .
C3 C 0.5100(4) -0.5384(4) 0.9000(4) 0.0202(12) Uani 1 1 d U . .
C4 C 0.4054(4) -0.6003(4) 0.9751(4) 0.0264(12) Uani 1 1 d . . .
H4A H 0.3719 -0.5796 1.0469 0.04 Uiso 1 1 calc R . .
H4B H 0.4363 -0.6831 0.9843 0.04 Uiso 1 1 calc R . .
H4C H 0.3392 -0.579 0.9436 0.04 Uiso 1 1 calc R . .
C5 C 0.6581(4) -0.6539(4) 0.9930(4) 0.0291(13) Uani 1 1 d . . .
H5A H 0.6309 -0.7258 1.003 0.035 Uiso 1 1 calc R . .
H5B H 0.6175 -0.6285 1.0636 0.035 Uiso 1 1 calc R . .
C6 C 0.7992(4) -0.6759(4) 0.9622(4) 0.0211(12) Uani 1 1 d . . .
H6A H 0.8202 -0.6763 1.0257 0.025 Uiso 1 1 calc R . .
H6B H 0.8356 -0.7517 0.9427 0.025 Uiso 1 1 calc R . .
C7 C 1.0669(4) -0.6415(4) 0.8703(4) 0.0253(12) Uani 1 1 d . . .
H7A H 1.0315 -0.6592 0.9508 0.038 Uiso 1 1 calc R . .
H7B H 1.1343 -0.5984 0.846 0.038 Uiso 1 1 calc R . .
H7C H 1.1002 -0.713 0.8438 0.038 Uiso 1 1 calc R . .
C8 C 0.9662(4) -0.5705(4) 0.8245(4) 0.0171(11) Uani 1 1 d . . .
C9 C 0.9917(4) -0.4796(4) 0.7273(4) 0.0192(12) Uani 1 1 d . . .
C10 C 1.1150(4) -0.4442(4) 0.6622(4) 0.0289(13) Uani 1 1 d . . .
H10A H 1.1532 -0.4745 0.5951 0.043 Uiso 1 1 calc R . .
H10B H 1.1697 -0.4745 0.7061 0.043 Uiso 1 1 calc R . .
H10C H 1.1036 -0.3604 0.6425 0.043 Uiso 1 1 calc R . .
C11 C 0.7610(4) -0.5615(4) 0.6063(4) 0.0155(11) Uani 1 1 d . . .
H11 H 0.7201 -0.4884 0.5781 0.019 Uiso 1 1 calc R . .
C12 C 0.8424(5) -0.7014(4) 0.7102(5) 0.0396(16) Uani 1 1 d . . .
H12 H 0.8694 -0.7455 0.7697 0.047 Uiso 1 1 calc R . .
C13 C 0.8568(5) -0.7393(4) 0.6219(4) 0.0384(15) Uani 1 1 d . . .
H13 H 0.8959 -0.8135 0.6077 0.046 Uiso 1 1 calc R . .
C14 C 0.7926(4) -0.6543(4) 0.4554(4) 0.0264(13) Uani 1 1 d . . .
H14A H 0.8724 -0.6914 0.409 0.04 Uiso 1 1 calc R . .
H14B H 0.7698 -0.5762 0.416 0.04 Uiso 1 1 calc R . .
H14C H 0.7275 -0.6981 0.4732 0.04 Uiso 1 1 calc R . .
C15 C 0.7244(4) -0.3859(4) 0.9729(4) 0.0131(11) Uani 1 1 d . . .
H15 H 0.747 -0.4575 1.0172 0.016 Uiso 1 1 calc R . .
C16 C 0.6765(4) -0.2566(4) 0.8407(4) 0.0219(12) Uani 1 1 d . . .
H16 H 0.6596 -0.2212 0.7744 0.026 Uiso 1 1 calc R . .
C17 C 0.6732(4) -0.2016(4) 0.9147(4) 0.0221(12) Uani 1 1 d . . .
H17 H 0.6532 -0.1212 0.9098 0.027 Uiso 1 1 calc R . .
C18 C 0.7066(4) -0.2639(4) 1.0958(4) 0.0209(12) Uani 1 1 d . . .
H18A H 0.622 -0.2576 1.1508 0.031 Uiso 1 1 calc R . .
H18B H 0.7376 -0.1928 1.078 0.031 Uiso 1 1 calc R . .
H18C H 0.762 -0.3282 1.1255 0.031 Uiso 1 1 calc R . .
C19 C 0.9480(4) -0.3398(4) 0.3428(4) 0.0340(13) Uani 1 1 d . . .
H19A H 0.9483 -0.3964 0.4119 0.041 Uiso 1 1 calc R . .
H19B H 1.0263 -0.3606 0.2827 0.041 Uiso 1 1 calc R . .
C20 C 0.8376(4) -0.3373(5) 0.3166(4) 0.0329(13) Uani 1 1 d . . .
H20A H 0.8365 -0.2784 0.249 0.039 Uiso 1 1 calc R . .
H20B H 0.8418 -0.4126 0.3037 0.039 Uiso 1 1 calc R . .
C21 C 0.6253(5) -0.2435(4) 0.3730(4) 0.0329(15) Uani 1 1 d . . .
H21A H 0.5852 -0.2929 0.3571 0.04 Uiso 1 1 calc R . .
H21B H 0.6564 -0.1859 0.3049 0.04 Uiso 1 1 calc R . .
C22 C 0.5313(4) -0.1842(4) 0.4623(4) 0.0297(13) Uani 1 1 d . . .
H22A H 0.4579 -0.1406 0.4412 0.036 Uiso 1 1 calc R . .
H22B H 0.5025 -0.2412 0.5316 0.036 Uiso 1 1 calc R . .
C23 C 0.5099(4) -0.0469(4) 0.5610(4) 0.0339(14) Uani 1 1 d . . .
H23A H 0.4738 -0.1013 0.6301 0.041 Uiso 1 1 calc R . .
H23B H 0.4406 0.0056 0.5384 0.041 Uiso 1 1 calc R . .
C24 C 0.5848(5) 0.0201(4) 0.5782(4) 0.0372(15) Uani 1 1 d . . .
H24A H 0.6289 0.068 0.5073 0.045 Uiso 1 1 calc R . .
H24B H 0.5291 0.071 0.6291 0.045 Uiso 1 1 calc R . .
C25 C 0.7644(4) -0.0086(4) 0.6282(4) 0.0299(13) Uani 1 1 d . . .
H25A H 0.7991 -0.0589 0.6851 0.036 Uiso 1 1 calc R . .
H25B H 0.7231 0.0657 0.6501 0.036 Uiso 1 1 calc R . .
C26 C 0.8693(5) 0.0108(4) 0.5201(4) 0.0372(15) Uani 1 1 d . . .
H26A H 0.8384 0.07 0.4649 0.045 Uiso 1 1 calc R . .
H26B H 0.9357 0.0368 0.5285 0.045 Uiso 1 1 calc R . .
C27 C 1.0159(4) -0.0922(4) 0.3833(4) 0.0322(13) Uani 1 1 d . . .
H27A H 1.0897 -0.0739 0.3871 0.039 Uiso 1 1 calc R . .
H27B H 0.9898 -0.0327 0.3254 0.039 Uiso 1 1 calc R . .
C28 C 1.0476(4) -0.2069(4) 0.3573(4) 0.0340(14) Uani 1 1 d . . .
H28A H 1.1158 -0.2083 0.2852 0.041 Uiso 1 1 calc R . .
H28B H 1.0752 -0.2664 0.4143 0.041 Uiso 1 1 calc R . .
C29 C 0.4195(4) -0.4533(4) 0.2928(4) 0.0165(11) Uani 1 1 d . . .
C30 C 0.4330(4) -0.4154(4) 0.1801(4) 0.0202(11) Uani 1 1 d . . .
H30 H 0.4588 -0.4718 0.1378 0.024 Uiso 1 1 calc R . .
C31 C 0.4112(4) -0.3019(4) 0.1275(4) 0.0249(12) Uani 1 1 d . . .
H31 H 0.4229 -0.2824 0.0514 0.03 Uiso 1 1 calc R . .
C32 C 0.3729(4) -0.2179(4) 0.1851(4) 0.0268(13) Uani 1 1 d . . .
H32 H 0.3575 -0.1396 0.1498 0.032 Uiso 1 1 calc R . .
C33 C 0.3566(4) -0.2485(4) 0.2964(4) 0.0243(13) Uani 1 1 d . . .
H33 H 0.3302 -0.1908 0.3374 0.029 Uiso 1 1 calc R . .
C34 C 0.3789(4) -0.3639(4) 0.3482(4) 0.0220(11) Uani 1 1 d . . .
H34 H 0.3658 -0.3824 0.4246 0.026 Uiso 1 1 calc R . .
C35 C 0.5946(4) -0.6452(4) 0.2914(4) 0.0160(11) Uani 1 1 d U . .
C36 C 0.6392(4) -0.7637(4) 0.3068(4) 0.0196(11) Uani 1 1 d . . .
H36 H 0.5807 -0.814 0.3445 0.023 Uiso 1 1 calc R . .
C37 C 0.7671(4) -0.8108(4) 0.2689(4) 0.0245(12) Uani 1 1 d . . .
H37 H 0.7939 -0.8915 0.2781 0.029 Uiso 1 1 calc R . .
C38 C 0.8543(4) -0.7380(5) 0.2174(4) 0.0259(13) Uani 1 1 d . . .
H38 H 0.9411 -0.7692 0.1926 0.031 Uiso 1 1 calc R . .
C39 C 0.8152(4) -0.6221(4) 0.2026(4) 0.0249(12) Uani 1 1 d . . .
H39 H 0.8748 -0.5727 0.1678 0.03 Uiso 1 1 calc R . .
C40 C 0.6867(4) -0.5757(4) 0.2389(3) 0.0177(11) Uani 1 1 d . . .
H40 H 0.6612 -0.4949 0.2276 0.021 Uiso 1 1 calc R . .
C41 C 0.3504(4) -0.6446(4) 0.3211(4) 0.0184(11) Uani 1 1 d . . .
C42 C 0.2213(4) -0.6001(4) 0.3612(4) 0.0241(12) Uani 1 1 d . . .
H42 H 0.1939 -0.542 0.4019 0.029 Uiso 1 1 calc R . .
C43 C 0.1322(4) -0.6374(4) 0.3440(4) 0.0307(13) Uani 1 1 d . . .
H43 H 0.0467 -0.6025 0.3698 0.037 Uiso 1 1 calc R . .
C44 C 0.1683(4) -0.7258(4) 0.2890(4) 0.0293(14) Uani 1 1 d . . .
H44 H 0.1079 -0.7535 0.2789 0.035 Uiso 1 1 calc R . .
C45 C 0.2942(4) -0.7727(4) 0.2492(4) 0.0281(13) Uani 1 1 d . . .
H45 H 0.321 -0.8328 0.2109 0.034 Uiso 1 1 calc R . .
C46 C 0.3812(4) -0.7315(4) 0.2656(4) 0.0216(12) Uani 1 1 d . . .
H46 H 0.4669 -0.7649 0.237 0.026 Uiso 1 1 calc R . .
C47 C 0.4205(4) -0.6217(4) 0.4780(4) 0.0186(11) Uani 1 1 d . . .
C48 C 0.4759(4) -0.5729(4) 0.5232(4) 0.0189(11) Uani 1 1 d . . .
H48 H 0.5208 -0.5131 0.4774 0.023 Uiso 1 1 calc R . .
C49 C 0.4674(4) -0.6090(4) 0.6333(4) 0.0243(12) Uani 1 1 d . . .
H49 H 0.5071 -0.5746 0.661 0.029 Uiso 1 1 calc R . .
C50 C 0.4016(4) -0.6939(4) 0.7011(4) 0.0279(13) Uani 1 1 d . . .
H50 H 0.3948 -0.7175 0.7762 0.034 Uiso 1 1 calc R . .
C51 C 0.3459(4) -0.7451(4) 0.6621(4) 0.0242(12) Uani 1 1 d . . .
H51 H 0.3014 -0.8047 0.7093 0.029 Uiso 1 1 calc R . .
C52 C 0.3551(4) -0.7086(4) 0.5516(4) 0.0207(12) Uani 1 1 d . . .
H52 H 0.3153 -0.7444 0.5253 0.025 Uiso 1 1 calc R . .
C53 C 1.1097(4) -0.0482(4) 0.7689(4) 0.0215(12) Uani 1 1 d . . .
C54 C 1.1471(4) -0.1317(4) 0.7073(4) 0.0262(12) Uani 1 1 d . . .
H54 H 1.1479 -0.2095 0.7455 0.031 Uiso 1 1 calc R . .
C55 C 1.1832(4) -0.1075(5) 0.5937(4) 0.0323(14) Uani 1 1 d . . .
H55 H 1.2075 -0.1674 0.5557 0.039 Uiso 1 1 calc R . .
C56 C 1.1835(4) 0.0059(5) 0.5360(4) 0.0338(14) Uani 1 1 d . . .
H56 H 1.2079 0.024 0.4581 0.041 Uiso 1 1 calc R . .
C57 C 1.1485(4) 0.0906(5) 0.5921(4) 0.0357(15) Uani 1 1 d . . .
H57 H 1.1477 0.1682 0.5532 0.043 Uiso 1 1 calc R . .
C58 C 1.1139(4) 0.0642(4) 0.7063(4) 0.0306(14) Uani 1 1 d . . .
H58 H 1.0923 0.1247 0.7432 0.037 Uiso 1 1 calc R . .
C59 C 1.1566(4) -0.0149(4) 0.9306(4) 0.0216(11) Uani 1 1 d . . .
C60 C 1.2868(4) -0.0428(4) 0.8796(4) 0.0251(12) Uani 1 1 d . . .
H60 H 1.318 -0.093 0.8303 0.03 Uiso 1 1 calc R . .
C61 C 1.3729(4) -0.0009(4) 0.8971(4) 0.0289(14) Uani 1 1 d . . .
H61 H 1.46 -0.0227 0.8604 0.035 Uiso 1 1 calc R . .
C62 C 1.3305(4) 0.0726(4) 0.9686(4) 0.0283(13) Uani 1 1 d . . .
H62 H 1.3878 0.1023 0.9811 0.034 Uiso 1 1 calc R . .
C63 C 1.2035(4) 0.1017(4) 1.0213(4) 0.0297(13) Uani 1 1 d . . .
H63 H 1.1732 0.1505 1.0718 0.036 Uiso 1 1 calc R . .
C64 C 1.1185(4) 0.0603(4) 1.0012(4) 0.0264(12) Uani 1 1 d . . .
H64 H 1.0316 0.0842 1.0369 0.032 Uiso 1 1 calc R . .
C65 C 0.9162(4) -0.0192(4) 0.9570(4) 0.0221(12) Uani 1 1 d . . .
C66 C 0.8581(4) -0.0259(4) 1.0700(4) 0.0294(13) Uani 1 1 d . . .
H66 H 0.9081 -0.0573 1.1152 0.035 Uiso 1 1 calc R . .
C67 C 0.7301(4) 0.0112(4) 1.1201(4) 0.0333(13) Uani 1 1 d . . .
H67 H 0.6954 0.0071 1.1971 0.04 Uiso 1 1 calc R . .
C68 C 0.6544(5) 0.0539(4) 1.0574(5) 0.0361(14) Uani 1 1 d U . .
H68 H 0.567 0.078 1.091 0.043 Uiso 1 1 calc R . .
C69 C 0.7062(5) 0.0612(4) 0.9464(5) 0.0367(16) Uani 1 1 d . . .
H69 H 0.6549 0.091 0.9024 0.044 Uiso 1 1 calc R . .
C70 C 0.8350(4) 0.0248(4) 0.8973(4) 0.0254(12) Uani 1 1 d . . .
H70 H 0.8686 0.0303 0.8201 0.03 Uiso 1 1 calc R . .
C71 C 1.0789(4) -0.2094(4) 0.9615(4) 0.0176(11) Uani 1 1 d . . .
C72 C 1.1490(4) -0.2655(4) 1.0301(4) 0.0224(12) Uani 1 1 d . . .
H72 H 1.1938 -0.2225 1.0436 0.027 Uiso 1 1 calc R . .
C73 C 1.1555(4) -0.3807(4) 1.0792(4) 0.0209(11) Uani 1 1 d . . .
H73 H 1.2024 -0.4146 1.1269 0.025 Uiso 1 1 calc R . .
C74 C 1.0943(4) -0.4474(4) 1.0594(4) 0.0244(12) Uani 1 1 d . . .
H74 H 1.1003 -0.527 1.0916 0.029 Uiso 1 1 calc R . .
C75 C 1.0241(4) -0.3951(4) 0.9918(4) 0.0219(12) Uani 1 1 d . . .
H75 H 0.981 -0.4391 0.9775 0.026 Uiso 1 1 calc R . .
C76 C 1.0165(4) -0.2789(4) 0.9448(4) 0.0215(12) Uani 1 1 d . . .
H76 H 0.9669 -0.245 0.8995 0.026 Uiso 1 1 calc R . .
B1 B 0.4451(5) -0.5909(4) 0.3454(4) 0.0197(13) Uani 1 1 d . . .
B2 B 1.0655(5) -0.0717(4) 0.9042(5) 0.0203(13) Uani 1 1 d . . .
O1 O 0.6100(2) -0.3185(2) 0.6646(2) 0.0172(7) Uani 1 1 d . . .
O2 O 0.9013(3) -0.3498(2) 0.6102(2) 0.0199(8) Uani 1 1 d . . .
O3 O 0.9368(2) -0.2271(3) 0.3544(3) 0.0243(8) Uani 1 1 d . . .
O4 O 0.7268(3) -0.3112(3) 0.4068(2) 0.0243(8) Uani 1 1 d . . .
O5 O 0.5915(3) -0.1076(3) 0.4770(3) 0.0270(9) Uani 1 1 d . . .
O6 O 0.6733(3) -0.0599(2) 0.6238(3) 0.0260(8) Uani 1 1 d . . .
O7 O 0.9169(3) -0.0946(3) 0.4862(2) 0.0256(8) Uani 1 1 d . . .
N1 N 0.6053(3) -0.4043(3) 0.7477(3) 0.0158(9) Uani 1 1 d . . .
N2 N 0.8928(3) -0.4299(3) 0.6985(3) 0.0145(9) Uani 1 1 d . . .
N3 N 0.8518(3) -0.5866(3) 0.8688(3) 0.0153(9) Uani 1 1 d . . .
N4 N 0.6195(3) -0.5662(3) 0.9076(3) 0.0146(9) Uani 1 1 d . . .
N5 N 0.7829(3) -0.5899(3) 0.7000(3) 0.0151(9) Uani 1 1 d . . .
N6 N 0.8045(3) -0.6503(3) 0.5575(3) 0.0157(9) Uani 1 1 d . . .
N7 N 0.7087(3) -0.3729(3) 0.8789(3) 0.0143(9) Uani 1 1 d . . .
N8 N 0.7038(3) -0.2834(3) 0.9971(3) 0.0138(9) Uani 1 1 d . . .
Co1 Co 0.74336(5) -0.48779(5) 0.79675(5) 0.01448(16) Uani 1 1 d . . .
Na1 Na 0.76733(14) -0.21956(14) 0.52948(14) 0.0185(4) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.504(5) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 N1 1.324(5) . ?
C2 C3 1.459(6) . ?
C3 N4 1.287(5) . ?
C3 C4 1.491(5) . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 N4 1.461(5) . ?
C5 C6 1.519(5) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 N3 1.461(5) . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C7 C8 1.508(5) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 N3 1.293(5) . ?
C8 C9 1.445(6) . ?
C9 N2 1.318(5) . ?
C9 C10 1.486(6) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 N5 1.327(5) . ?
C11 N6 1.333(5) . ?
C11 H11 0.95 . ?
C12 C13 1.351(6) . ?
C12 N5 1.364(6) . ?
C12 H12 0.95 . ?
C13 N6 1.360(5) . ?
C13 H13 0.95 . ?
C14 N6 1.469(5) . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 N7 1.323(5) . ?
C15 N8 1.345(5) . ?
C15 H15 0.95 . ?
C16 C17 1.364(6) . ?
C16 N7 1.381(5) . ?
C16 H16 0.95 . ?
C17 N8 1.362(5) . ?
C17 H17 0.95 . ?
C18 N8 1.451(5) . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C19 O3 1.423(5) . ?
C19 C20 1.483(6) . ?
C19 Na1 3.068(5) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C20 O4 1.430(5) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 O4 1.422(5) . ?
C21 C22 1.502(7) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C22 O5 1.442(5) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C23 O5 1.427(6) . ?
C23 C24 1.500(6) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C24 O6 1.431(5) . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
C25 O6 1.432(5) . ?
C25 C26 1.501(6) . ?
C25 H25A 0.99 . ?
C25 H25B 0.99 . ?
C26 O7 1.412(5) . ?
C26 H26A 0.99 . ?
C26 H26B 0.99 . ?
C27 O7 1.418(5) . ?
C27 C28 1.485(6) . ?
C27 H27A 0.99 . ?
C27 H27B 0.99 . ?
C28 O3 1.427(5) . ?
C28 H28A 0.99 . ?
C28 H28B 0.99 . ?
C29 C34 1.398(6) . ?
C29 C30 1.417(6) . ?
C29 B1 1.637(6) . ?
C30 C31 1.381(6) . ?
C30 H30 0.95 . ?
C31 C32 1.363(6) . ?
C31 H31 0.95 . ?
C32 C33 1.389(6) . ?
C32 H32 0.95 . ?
C33 C34 1.398(6) . ?
C33 H33 0.95 . ?
C34 H34 0.95 . ?
C35 C36 1.402(6) . ?
C35 C40 1.410(5) . ?
C35 B1 1.652(6) . ?
C36 C37 1.404(6) . ?
C36 H36 0.95 . ?
C37 C38 1.395(6) . ?
C37 H37 0.95 . ?
C38 C39 1.365(6) . ?
C38 H38 0.95 . ?
C39 C40 1.407(6) . ?
C39 H39 0.95 . ?
C40 H40 0.95 . ?
C41 C46 1.388(6) . ?
C41 C42 1.411(6) . ?
C41 B1 1.638(6) . ?
C42 C43 1.392(5) . ?
C42 H42 0.95 . ?
C43 C44 1.390(7) . ?
C43 H43 0.95 . ?
C44 C45 1.387(6) . ?
C44 H44 0.95 . ?
C45 C46 1.392(5) . ?
C45 H45 0.95 . ?
C46 H46 0.95 . ?
C47 C48 1.400(5) . ?
C47 C52 1.403(6) . ?
C47 B1 1.645(7) . ?
C48 C49 1.397(6) . ?
C48 H48 0.95 . ?
C49 C50 1.369(6) . ?
C49 H49 0.95 . ?
C50 C51 1.361(6) . ?
C50 H50 0.95 . ?
C51 C52 1.401(6) . ?
C51 H51 0.95 . ?
C52 H52 0.95 . ?
C53 C54 1.396(6) . ?
C53 C58 1.404(6) . ?
C53 B2 1.652(7) . ?
C54 C55 1.386(6) . ?
C54 H54 0.95 . ?
C55 C56 1.392(6) . ?
C55 H55 0.95 . ?
C56 C57 1.363(7) . ?
C56 H56 0.95 . ?
C57 C58 1.394(7) . ?
C57 H57 0.95 . ?
C58 H58 0.95 . ?
C59 C64 1.401(6) . ?
C59 C60 1.406(6) . ?
C59 B2 1.644(6) . ?
C60 C61 1.397(6) . ?
C60 H60 0.95 . ?
C61 C62 1.387(7) . ?
C61 H61 0.95 . ?
C62 C63 1.379(6) . ?
C62 H62 0.95 . ?
C63 C64 1.400(5) . ?
C63 H63 0.95 . ?
C64 H64 0.95 . ?
C65 C66 1.396(6) . ?
C65 C70 1.399(6) . ?
C65 B2 1.642(7) . ?
C66 C67 1.397(6) . ?
C66 H66 0.95 . ?
C67 C68 1.378(6) . ?
C67 H67 0.95 . ?
C68 C69 1.366(7) . ?
C68 H68 0.95 . ?
C69 C70 1.401(6) . ?
C69 H69 0.95 . ?
C70 H70 0.95 . ?
C71 C72 1.401(6) . ?
C71 C76 1.402(5) . ?
C71 B2 1.647(6) . ?
C72 C73 1.382(6) . ?
C72 H72 0.95 . ?
C73 C74 1.387(5) . ?
C73 H73 0.95 . ?
C74 C75 1.385(6) . ?
C74 H74 0.95 . ?
C75 C76 1.387(6) . ?
C75 H75 0.95 . ?
C76 H76 0.95 . ?
O1 N1 1.293(4) . ?
O1 Na1 2.355(3) . ?
O2 N2 1.296(4) . ?
O2 Na1 2.292(3) . ?
O3 Na1 2.430(4) . ?
O4 Na1 2.538(3) . ?
O5 Na1 2.406(3) . ?
O6 Na1 2.448(4) . ?
O7 Na1 2.467(3) . ?
N1 Co1 1.930(3) . ?
N2 Co1 1.919(3) . ?
N3 Co1 1.880(3) . ?
N4 Co1 1.876(3) . ?
N5 Co1 1.937(4) . ?
N7 Co1 1.932(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 . . ?
N1 C2 C3 113.8(4) . . ?
N1 C2 C1 120.8(4) . . ?
C3 C2 C1 125.4(4) . . ?
N4 C3 C2 113.4(4) . . ?
N4 C3 C4 123.3(4) . . ?
C2 C3 C4 123.3(4) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C5 C6 110.7(3) . . ?
N4 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N3 C6 C5 109.8(3) . . ?
N3 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
N3 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C9 115.3(4) . . ?
N3 C8 C7 122.8(4) . . ?
C9 C8 C7 121.9(4) . . ?
N2 C9 C8 112.9(4) . . ?
N2 C9 C10 121.6(4) . . ?
C8 C9 C10 125.5(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 N6 110.3(4) . . ?
N5 C11 H11 124.8 . . ?
N6 C11 H11 124.8 . . ?
C13 C12 N5 109.1(4) . . ?
C13 C12 H12 125.4 . . ?
N5 C12 H12 125.4 . . ?
C12 C13 N6 106.5(4) . . ?
C12 C13 H13 126.8 . . ?
N6 C13 H13 126.8 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 N8 110.5(4) . . ?
N7 C15 H15 124.7 . . ?
N8 C15 H15 124.7 . . ?
C17 C16 N7 108.0(4) . . ?
C17 C16 H16 126 . . ?
N7 C16 H16 126 . . ?
N8 C17 C16 107.2(4) . . ?
N8 C17 H17 126.4 . . ?
C16 C17 H17 126.4 . . ?
N8 C18 H18A 109.5 . . ?
N8 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N8 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O3 C19 C20 105.7(4) . . ?
O3 C19 Na1 50.7(2) . . ?
C20 C19 Na1 87.3(3) . . ?
O3 C19 H19A 110.6 . . ?
C20 C19 H19A 110.6 . . ?
Na1 C19 H19A 74.2 . . ?
O3 C19 H19B 110.6 . . ?
C20 C19 H19B 110.6 . . ?
Na1 C19 H19B 158.4 . . ?
H19A C19 H19B 108.7 . . ?
O4 C20 C19 108.9(4) . . ?
O4 C20 H20A 109.9 . . ?
C19 C20 H20A 109.9 . . ?
O4 C20 H20B 109.9 . . ?
C19 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
O4 C21 C22 109.7(4) . . ?
O4 C21 H21A 109.7 . . ?
C22 C21 H21A 109.7 . . ?
O4 C21 H21B 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
O5 C22 C21 107.6(4) . . ?
O5 C22 H22A 110.2 . . ?
C21 C22 H22A 110.2 . . ?
O5 C22 H22B 110.2 . . ?
C21 C22 H22B 110.2 . . ?
H22A C22 H22B 108.5 . . ?
O5 C23 C24 107.9(4) . . ?
O5 C23 H23A 110.1 . . ?
C24 C23 H23A 110.1 . . ?
O5 C23 H23B 110.1 . . ?
C24 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
O6 C24 C23 107.8(4) . . ?
O6 C24 H24A 110.1 . . ?
C23 C24 H24A 110.1 . . ?
O6 C24 H24B 110.1 . . ?
C23 C24 H24B 110.1 . . ?
H24A C24 H24B 108.5 . . ?
O6 C25 C26 112.5(4) . . ?
O6 C25 H25A 109.1 . . ?
C26 C25 H25A 109.1 . . ?
O6 C25 H25B 109.1 . . ?
C26 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
O7 C26 C25 107.3(4) . . ?
O7 C26 H26A 110.3 . . ?
C25 C26 H26A 110.3 . . ?
O7 C26 H26B 110.3 . . ?
C25 C26 H26B 110.3 . . ?
H26A C26 H26B 108.5 . . ?
O7 C27 C28 108.0(4) . . ?
O7 C27 H27A 110.1 . . ?
C28 C27 H27A 110.1 . . ?
O7 C27 H27B 110.1 . . ?
C28 C27 H27B 110.1 . . ?
H27A C27 H27B 108.4 . . ?
O3 C28 C27 106.6(4) . . ?
O3 C28 H28A 110.4 . . ?
C27 C28 H28A 110.4 . . ?
O3 C28 H28B 110.4 . . ?
C27 C28 H28B 110.4 . . ?
H28A C28 H28B 108.6 . . ?
C34 C29 C30 113.3(4) . . ?
C34 C29 B1 127.2(4) . . ?
C30 C29 B1 119.4(4) . . ?
C31 C30 C29 124.5(5) . . ?
C31 C30 H30 117.8 . . ?
C29 C30 H30 117.8 . . ?
C32 C31 C30 119.9(5) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C31 C32 C33 119.0(5) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
C32 C33 C34 120.3(5) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C29 C34 C33 123.1(4) . . ?
C29 C34 H34 118.5 . . ?
C33 C34 H34 118.5 . . ?
C36 C35 C40 115.7(4) . . ?
C36 C35 B1 122.1(4) . . ?
C40 C35 B1 121.8(4) . . ?
C35 C36 C37 122.6(4) . . ?
C35 C36 H36 118.7 . . ?
C37 C36 H36 118.7 . . ?
C38 C37 C36 119.3(5) . . ?
C38 C37 H37 120.3 . . ?
C36 C37 H37 120.3 . . ?
C39 C38 C37 120.1(4) . . ?
C39 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C38 C39 C40 120.0(4) . . ?
C38 C39 H39 120 . . ?
C40 C39 H39 120 . . ?
C39 C40 C35 122.2(4) . . ?
C39 C40 H40 118.9 . . ?
C35 C40 H40 118.9 . . ?
C46 C41 C42 114.4(4) . . ?
C46 C41 B1 127.8(4) . . ?
C42 C41 B1 117.9(4) . . ?
C43 C42 C41 123.1(5) . . ?
C43 C42 H42 118.5 . . ?
C41 C42 H42 118.5 . . ?
C44 C43 C42 120.0(5) . . ?
C44 C43 H43 120 . . ?
C42 C43 H43 120 . . ?
C45 C44 C43 118.7(4) . . ?
C45 C44 H44 120.7 . . ?
C43 C44 H44 120.7 . . ?
C44 C45 C46 119.8(5) . . ?
C44 C45 H45 120.1 . . ?
C46 C45 H45 120.1 . . ?
C41 C46 C45 124.0(4) . . ?
C41 C46 H46 118 . . ?
C45 C46 H46 118 . . ?
C48 C47 C52 115.0(4) . . ?
C48 C47 B1 122.3(4) . . ?
C52 C47 B1 122.2(4) . . ?
C49 C48 C47 122.4(4) . . ?
C49 C48 H48 118.8 . . ?
C47 C48 H48 118.8 . . ?
C50 C49 C48 119.8(4) . . ?
C50 C49 H49 120.1 . . ?
C48 C49 H49 120.1 . . ?
C51 C50 C49 120.7(4) . . ?
C51 C50 H50 119.7 . . ?
C49 C50 H50 119.7 . . ?
C50 C51 C52 119.2(4) . . ?
C50 C51 H51 120.4 . . ?
C52 C51 H51 120.4 . . ?
C51 C52 C47 122.9(4) . . ?
C51 C52 H52 118.5 . . ?
C47 C52 H52 118.5 . . ?
C54 C53 C58 114.6(5) . . ?
C54 C53 B2 126.0(4) . . ?
C58 C53 B2 119.4(4) . . ?
C55 C54 C53 123.7(5) . . ?
C55 C54 H54 118.2 . . ?
C53 C54 H54 118.2 . . ?
C54 C55 C56 119.2(5) . . ?
C54 C55 H55 120.4 . . ?
C56 C55 H55 120.4 . . ?
C57 C56 C55 119.5(5) . . ?
C57 C56 H56 120.3 . . ?
C55 C56 H56 120.3 . . ?
C56 C57 C58 120.4(5) . . ?
C56 C57 H57 119.8 . . ?
C58 C57 H57 119.8 . . ?
C57 C58 C53 122.6(5) . . ?
C57 C58 H58 118.7 . . ?
C53 C58 H58 118.7 . . ?
C64 C59 C60 114.4(4) . . ?
C64 C59 B2 126.7(4) . . ?
C60 C59 B2 118.9(4) . . ?
C61 C60 C59 123.8(5) . . ?
C61 C60 H60 118.1 . . ?
C59 C60 H60 118.1 . . ?
C62 C61 C60 119.6(5) . . ?
C62 C61 H61 120.2 . . ?
C60 C61 H61 120.2 . . ?
C63 C62 C61 118.7(4) . . ?
C63 C62 H62 120.6 . . ?
C61 C62 H62 120.6 . . ?
C62 C63 C64 120.9(5) . . ?
C62 C63 H63 119.6 . . ?
C64 C63 H63 119.6 . . ?
C63 C64 C59 122.6(5) . . ?
C63 C64 H64 118.7 . . ?
C59 C64 H64 118.7 . . ?
C66 C65 C70 114.5(4) . . ?
C66 C65 B2 120.9(4) . . ?
C70 C65 B2 124.4(4) . . ?
C65 C66 C67 123.3(5) . . ?
C65 C66 H66 118.4 . . ?
C67 C66 H66 118.4 . . ?
C68 C67 C66 119.8(5) . . ?
C68 C67 H67 120.1 . . ?
C66 C67 H67 120.1 . . ?
C69 C68 C67 119.3(5) . . ?
C69 C68 H68 120.4 . . ?
C67 C68 H68 120.4 . . ?
C68 C69 C70 120.2(5) . . ?
C68 C69 H69 119.9 . . ?
C70 C69 H69 119.9 . . ?
C65 C70 C69 122.9(5) . . ?
C65 C70 H70 118.5 . . ?
C69 C70 H70 118.5 . . ?
C72 C71 C76 115.2(4) . . ?
C72 C71 B2 124.2(4) . . ?
C76 C71 B2 120.6(4) . . ?
C73 C72 C71 122.7(4) . . ?
C73 C72 H72 118.7 . . ?
C71 C72 H72 118.7 . . ?
C72 C73 C74 120.5(4) . . ?
C72 C73 H73 119.7 . . ?
C74 C73 H73 119.7 . . ?
C75 C74 C73 118.5(4) . . ?
C75 C74 H74 120.8 . . ?
C73 C74 H74 120.8 . . ?
C74 C75 C76 120.3(4) . . ?
C74 C75 H75 119.8 . . ?
C76 C75 H75 119.8 . . ?
C75 C76 C71 122.7(4) . . ?
C75 C76 H76 118.6 . . ?
C71 C76 H76 118.6 . . ?
C29 B1 C41 105.4(3) . . ?
C29 B1 C47 113.7(4) . . ?
C41 B1 C47 110.5(4) . . ?
C29 B1 C35 109.9(4) . . ?
C41 B1 C35 114.2(4) . . ?
C47 B1 C35 103.3(3) . . ?
C65 B2 C59 113.4(4) . . ?
C65 B2 C71 104.8(4) . . ?
C59 B2 C71 109.5(4) . . ?
C65 B2 C53 110.4(4) . . ?
C59 B2 C53 106.8(4) . . ?
C71 B2 C53 112.0(4) . . ?
N1 O1 Na1 135.4(2) . . ?
N2 O2 Na1 137.2(2) . . ?
C19 O3 C28 113.4(3) . . ?
C19 O3 Na1 102.4(3) . . ?
C28 O3 Na1 110.7(3) . . ?
C21 O4 C20 112.9(3) . . ?
C21 O4 Na1 111.1(3) . . ?
C20 O4 Na1 111.8(2) . . ?
C23 O5 C22 112.2(3) . . ?
C23 O5 Na1 108.3(2) . . ?
C22 O5 Na1 108.3(2) . . ?
C24 O6 C25 113.7(3) . . ?
C24 O6 Na1 110.2(3) . . ?
C25 O6 Na1 112.8(3) . . ?
C26 O7 C27 115.3(4) . . ?
C26 O7 Na1 117.8(3) . . ?
C27 O7 Na1 116.2(3) . . ?
O1 N1 C2 120.8(3) . . ?
O1 N1 Co1 125.8(3) . . ?
C2 N1 Co1 113.4(3) . . ?
O2 N2 C9 120.5(4) . . ?
O2 N2 Co1 125.4(3) . . ?
C9 N2 Co1 114.1(3) . . ?
C8 N3 C6 128.2(4) . . ?
C8 N3 Co1 115.0(3) . . ?
C6 N3 Co1 116.6(3) . . ?
C3 N4 C5 126.8(4) . . ?
C3 N4 Co1 117.0(3) . . ?
C5 N4 Co1 116.3(3) . . ?
C11 N5 C12 106.2(4) . . ?
C11 N5 Co1 125.5(3) . . ?
C12 N5 Co1 128.2(3) . . ?
C11 N6 C13 107.8(4) . . ?
C11 N6 C14 126.6(4) . . ?
C13 N6 C14 125.5(4) . . ?
C15 N7 C16 106.8(4) . . ?
C15 N7 Co1 128.4(3) . . ?
C16 N7 Co1 124.4(3) . . ?
C15 N8 C17 107.5(4) . . ?
C15 N8 C18 126.3(4) . . ?
C17 N8 C18 126.2(4) . . ?
N4 Co1 N3 85.36(15) . . ?
N4 Co1 N2 168.04(16) . . ?
N3 Co1 N2 82.69(16) . . ?
N4 Co1 N1 82.28(15) . . ?
N3 Co1 N1 167.64(16) . . ?
N2 Co1 N1 109.67(16) . . ?
N4 Co1 N7 92.77(15) . . ?
N3 Co1 N7 91.73(15) . . ?
N2 Co1 N7 88.08(15) . . ?
N1 Co1 N7 88.88(15) . . ?
N4 Co1 N5 92.54(15) . . ?
N3 Co1 N5 92.04(15) . . ?
N2 Co1 N5 87.42(15) . . ?
N1 Co1 N5 88.51(15) . . ?
N7 Co1 N5 173.72(17) . . ?
O2 Na1 O1 85.97(11) . . ?
O2 Na1 O5 166.81(13) . . ?
O1 Na1 O5 80.84(11) . . ?
O2 Na1 O3 87.04(11) . . ?
O1 Na1 O3 142.71(13) . . ?
O5 Na1 O3 103.40(12) . . ?
O2 Na1 O6 109.12(12) . . ?
O1 Na1 O6 88.28(11) . . ?
O5 Na1 O6 70.79(11) . . ?
O3 Na1 O6 128.46(12) . . ?
O2 Na1 O7 82.24(10) . . ?
O1 Na1 O7 147.69(12) . . ?
O5 Na1 O7 109.15(12) . . ?
O3 Na1 O7 66.63(11) . . ?
O6 Na1 O7 67.69(11) . . ?
O2 Na1 O4 108.93(12) . . ?
O1 Na1 O4 81.37(10) . . ?
O5 Na1 O4 69.07(11) . . ?
O3 Na1 O4 66.49(10) . . ?
O6 Na1 O4 139.63(11) . . ?
O7 Na1 O4 130.92(12) . . ?
O2 Na1 C19 77.83(13) . . ?
O1 Na1 C19 116.06(13) . . ?
O5 Na1 C19 107.90(13) . . ?
O3 Na1 C19 26.95(11) . . ?
O6 Na1 C19 155.40(13) . . ?
O7 Na1 C19 90.68(12) . . ?
O4 Na1 C19 48.92(11) . . ?


# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dh2_135c_0ma
_database_code_depnum_ccdc_archive 'CCDC 1433671'
_audit_update_record             
;
2015-10-27 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_date             2014-02-25T14:35:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
Complex 4
;
_chemical_name_common            dh2_135c
_chemical_formula_moiety         '16(C38 H44 Co N12 O2 Ru), C8 H12 N4, 48(F6 P)'
_chemical_formula_sum            'C616 H716 Co16 F288 N196 O32 P48 Ru16'
_chemical_formula_weight         20896.41

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_Int_Tables_number      88
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'



_cell_length_a                   40.556(22)
_cell_length_b                   40.556(22)
_cell_length_c                   12.276(10)
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_volume                     20191(26)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10488
_exptl_special_details           
;
 120 seconds, 0.5 degrees, 40 mm
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.7934
_exptl_absorpt_correction_T_max  0.9452

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.3615
_diffrn_reflns_av_unetI/netI     0.2667
_diffrn_reflns_number            90430
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_reflns_number_total             9314
_reflns_number_gt                3292
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0913P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9314
_refine_ls_number_parameters     791
_refine_ls_number_restraints     546
_refine_ls_R_factor_all          0.27
_refine_ls_R_factor_gt           0.0861
_refine_ls_wR_factor_ref         0.2331
_refine_ls_wR_factor_gt          0.1621
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.105

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.8400(3) 0.3609(3) 0.0645(11) 0.059(4) Uani 1 1 d . . .
H1 H 0.8628 0.3552 0.0666 0.071 Uiso 1 1 calc R . .
C2 C 0.8205(3) 0.3444(3) -0.0088(11) 0.052(3) Uani 1 1 d . . .
H2 H 0.8295 0.3283 -0.0564 0.062 Uiso 1 1 calc R . .
C3 C 0.7875(3) 0.3519(3) -0.0112(12) 0.062(4) Uani 1 1 d . . .
H3 H 0.7728 0.3398 -0.0562 0.074 Uiso 1 1 calc R . .
C4 C 0.7762(3) 0.3776(3) 0.0540(10) 0.052(3) Uani 1 1 d . . .
H4 H 0.7539 0.3845 0.0495 0.063 Uiso 1 1 calc R . .
C5 C 0.7975(3) 0.3931(3) 0.1252(10) 0.048(3) Uani 1 1 d . . .
C6 C 0.7882(3) 0.4220(3) 0.1920(11) 0.051(3) Uani 1 1 d . . .
C7 C 0.7569(3) 0.4339(3) 0.2020(11) 0.059(4) Uani 1 1 d . . .
H7 H 0.7387 0.4231 0.1684 0.07 Uiso 1 1 calc R . .
C8 C 0.7524(4) 0.4624(4) 0.2632(12) 0.074(4) Uani 1 1 d . . .
H8 H 0.7309 0.4714 0.2704 0.089 Uiso 1 1 calc R . .
C9 C 0.7780(4) 0.4778(4) 0.3131(13) 0.076(4) Uani 1 1 d . . .
H9 H 0.7751 0.498 0.3511 0.091 Uiso 1 1 calc R . .
C10 C 0.8077(3) 0.4634(3) 0.3065(10) 0.060(4) Uani 1 1 d . . .
H10 H 0.8253 0.473 0.3463 0.072 Uiso 1 1 calc R . .
C11 C 0.8766(3) 0.4377(3) 0.4691(11) 0.056(4) Uani 1 1 d . . .
H11 H 0.8581 0.4267 0.4997 0.067 Uiso 1 1 calc R . .
C12 C 0.8967(3) 0.4550(3) 0.5358(10) 0.057(4) Uani 1 1 d . . .
H12 H 0.8918 0.457 0.6112 0.069 Uiso 1 1 calc R . .
C13 C 0.9241(3) 0.4695(3) 0.4928(13) 0.055(4) Uani 1 1 d . . .
H13 H 0.9391 0.4806 0.5395 0.066 Uiso 1 1 calc R . .
C14 C 0.9303(3) 0.4682(3) 0.3838(11) 0.049(3) Uani 1 1 d . . .
H14 H 0.9493 0.4785 0.3537 0.059 Uiso 1 1 calc R . .
C15 C 0.9083(3) 0.4515(3) 0.3186(10) 0.039(3) Uani 1 1 d . . .
C16 C 0.9096(3) 0.4521(3) 0.1979(11) 0.046(3) Uani 1 1 d . . .
C17 C 0.9337(3) 0.4685(3) 0.1360(12) 0.054(3) Uani 1 1 d . . .
H17 H 0.9515 0.4793 0.1712 0.065 Uiso 1 1 calc R . .
C18 C 0.9313(3) 0.4689(3) 0.0254(12) 0.062(4) Uani 1 1 d . . .
H18 H 0.9482 0.4787 -0.0171 0.074 Uiso 1 1 calc R . .
C19 C 0.9041(3) 0.4548(3) -0.0246(10) 0.055(4) Uani 1 1 d . . .
H19 H 0.9015 0.4561 -0.1014 0.066 Uiso 1 1 calc R . .
C20 C 0.8807(3) 0.4385(3) 0.0399(12) 0.050(3) Uani 1 1 d . . .
H20 H 0.8623 0.4284 0.0057 0.06 Uiso 1 1 calc R . .
C21 C 0.9502(3) 0.3423(3) 0.1662(11) 0.064(4) Uani 1 1 d . . .
H21A H 0.9378 0.3479 0.1003 0.097 Uiso 1 1 calc R . .
H21B H 0.9659 0.3246 0.1498 0.097 Uiso 1 1 calc R . .
H21C H 0.9622 0.3618 0.1918 0.097 Uiso 1 1 calc R . .
C22 C 0.9272(3) 0.3312(3) 0.2517(13) 0.058(4) Uani 1 1 d . . .
C23 C 0.9299(4) 0.3000(3) 0.3144(15) 0.075(5) Uani 1 1 d . . .
C24 C 0.9556(3) 0.2757(3) 0.2872(15) 0.099(6) Uani 1 1 d . . .
H24A H 0.9772 0.2844 0.3084 0.149 Uiso 1 1 calc R . .
H24B H 0.9553 0.2715 0.2086 0.149 Uiso 1 1 calc R . .
H24C H 0.9513 0.2551 0.3264 0.149 Uiso 1 1 calc R . .
C25 C 0.9008(4) 0.2693(4) 0.4582(17) 0.106(6) Uani 1 1 d . . .
H25A H 0.9217 0.2596 0.4844 0.128 Uiso 1 1 calc R . .
H25B H 0.8885 0.2521 0.4176 0.128 Uiso 1 1 calc R . .
C26 C 0.8804(4) 0.2816(3) 0.5542(14) 0.082(5) Uani 1 1 d . . .
H26A H 0.8669 0.2633 0.5842 0.098 Uiso 1 1 calc R . .
H26B H 0.8951 0.2898 0.6125 0.098 Uiso 1 1 calc R . .
C27 C 0.8212(4) 0.3106(3) 0.6750(10) 0.085(5) Uani 1 1 d . . .
H27A H 0.8347 0.2923 0.702 0.128 Uiso 1 1 calc R . .
H27B H 0.7982 0.3034 0.6691 0.128 Uiso 1 1 calc R . .
H27C H 0.8226 0.3292 0.7257 0.128 Uiso 1 1 calc R . .
C28 C 0.8335(4) 0.3212(4) 0.5645(12) 0.065(4) Uani 1 1 d . . .
C29 C 0.8198(4) 0.3504(3) 0.5090(12) 0.062(4) Uani 1 1 d . . .
C30 C 0.7881(3) 0.3658(3) 0.5316(10) 0.065(4) Uani 1 1 d . . .
H30A H 0.789 0.3892 0.5119 0.097 Uiso 1 1 calc R . .
H30B H 0.783 0.3637 0.6094 0.097 Uiso 1 1 calc R . .
H30C H 0.7709 0.3549 0.4888 0.097 Uiso 1 1 calc R . .
N9 N 0.9035(2) 0.3572(2) 0.4970(10) 0.054(3) Uani 1 1 d D A .
N10 N 0.9204(3) 0.3820(2) 0.6460(10) 0.060(3) Uani 1 1 d D . .
C31 C 0.8965(3) 0.3642(3) 0.5969(12) 0.062(4) Uani 1 1 d D . .
H31 H 0.8766 0.3577 0.6319 0.074 Uiso 1 1 calc R . .
C32 C 0.9346(3) 0.3698(3) 0.4787(12) 0.075(5) Uani 1 1 d D . .
H32 H 0.9469 0.3677 0.4132 0.09 Uiso 1 1 calc R . .
C33 C 0.9445(3) 0.3855(3) 0.5700(13) 0.075(5) Uani 1 1 d D . .
H33 H 0.9647 0.397 0.5793 0.09 Uiso 1 1 calc R . .
C34 C 0.9208(3) 0.3938(3) 0.7590(11) 0.084(5) Uani 1 1 d D . .
H34A H 0.8987 0.3917 0.7903 0.125 Uiso 1 1 calc R . .
H34B H 0.9276 0.4169 0.7605 0.125 Uiso 1 1 calc R . .
H34C H 0.9364 0.3805 0.8017 0.125 Uiso 1 1 calc R . .
N11 N 0.8471(7) 0.3093(13) 0.297(3) 0.056(5) Uani 0.71(4) 1 d PD A 1
N12 N 0.8301(6) 0.2783(11) 0.161(2) 0.050(5) Uani 0.71(4) 1 d PD A 1
C35 C 0.8559(6) 0.2915(17) 0.214(4) 0.067(8) Uani 0.71(4) 1 d PD A 1
H35 H 0.8782 0.2883 0.1923 0.081 Uiso 0.71(4) 1 calc PR A 1
C36 C 0.8131(5) 0.3110(8) 0.2890(15) 0.054(7) Uani 0.71(4) 1 d PD A 1
H36 H 0.7992 0.3244 0.3327 0.064 Uiso 0.71(4) 1 calc PR A 1
C37 C 0.8028(5) 0.2906(7) 0.2092(16) 0.050(7) Uani 0.71(4) 1 d PD A 1
H37 H 0.7806 0.2858 0.1906 0.061 Uiso 0.71(4) 1 calc PR A 1
C38 C 0.8309(8) 0.2566(8) 0.065(3) 0.067(9) Uani 0.71(4) 1 d PD A 1
H38A H 0.8519 0.2593 0.0269 0.101 Uiso 0.71(4) 1 calc PR A 1
H38B H 0.8127 0.2623 0.0158 0.101 Uiso 0.71(4) 1 calc PR A 1
H38C H 0.8285 0.2336 0.0883 0.101 Uiso 0.71(4) 1 calc PR A 1
N11B N 0.8500(17) 0.305(3) 0.277(8) 0.056(5) Uani 0.29(4) 1 d PD A 2
N12B N 0.8363(16) 0.276(3) 0.133(6) 0.050(5) Uani 0.29(4) 1 d PD A 2
C35B C 0.8607(14) 0.291(4) 0.189(9) 0.067(8) Uani 0.29(4) 1 d PD A 2
H35B H 0.8832 0.2911 0.1666 0.081 Uiso 0.29(4) 1 calc PR A 2
C36B C 0.8192(14) 0.2914(17) 0.293(4) 0.054(7) Uani 0.29(4) 1 d PD A 2
H36B H 0.8066 0.2927 0.3576 0.064 Uiso 0.29(4) 1 calc PR A 2
C37B C 0.8100(12) 0.2758(16) 0.201(4) 0.054(7) Uani 0.29(4) 1 d PD A 2
H37B H 0.7891 0.2661 0.1866 0.064 Uiso 0.29(4) 1 calc PR A 2
C38B C 0.838(2) 0.262(2) 0.024(5) 0.067(9) Uani 0.29(4) 1 d PD A 2
H38D H 0.8568 0.2712 -0.0162 0.101 Uiso 0.29(4) 1 calc PR A 2
H38E H 0.8176 0.2662 -0.0162 0.101 Uiso 0.29(4) 1 calc PR A 2
H38F H 0.8411 0.2378 0.0302 0.101 Uiso 0.29(4) 1 calc PR A 2
N1 N 0.8297(2) 0.3845(2) 0.1334(7) 0.040(2) Uani 1 1 d . . .
N2 N 0.8142(2) 0.4364(2) 0.2478(8) 0.050(3) Uani 1 1 d . . .
N3 N 0.8817(2) 0.4353(2) 0.3613(8) 0.041(2) Uani 1 1 d . . .
N4 N 0.8835(2) 0.4369(2) 0.1496(9) 0.043(2) Uani 1 1 d . . .
N5 N 0.9011(2) 0.3497(2) 0.2793(7) 0.043(3) Uani 1 1 d . A .
N6 N 0.9074(3) 0.2980(2) 0.3871(11) 0.072(4) Uani 1 1 d . A .
N7 N 0.8588(3) 0.3082(3) 0.5156(10) 0.066(3) Uani 1 1 d . A .
N8 N 0.8397(2) 0.3592(2) 0.4260(9) 0.048(3) Uani 1 1 d . A .
O1 O 0.89685(16) 0.37791(17) 0.2315(6) 0.042(2) Uani 1 1 d . . .
O2 O 0.82838(17) 0.3833(2) 0.3666(6) 0.050(2) Uani 1 1 d . . .
P1 P 0.77914(7) 0.23950(6) 0.5005(3) 0.0441(8) Uani 1 1 d D . .
F1 F 0.79919(17) 0.23786(15) 0.6078(6) 0.092(3) Uani 1 1 d D . .
F2 F 0.76019(14) 0.24317(14) 0.3840(5) 0.062(2) Uani 1 1 d D . .
F3 F 0.81358(14) 0.23991(15) 0.4360(6) 0.087(3) Uani 1 1 d D . .
F4 F 0.78046(14) 0.27902(12) 0.5053(5) 0.065(2) Uani 1 1 d D . .
F5 F 0.74540(15) 0.24008(14) 0.5615(5) 0.073(2) Uani 1 1 d D . .
F6 F 0.77694(14) 0.20016(11) 0.4899(5) 0.0567(18) Uani 1 1 d D . .
P2 P 0.81318(16) 0.42891(12) 0.7587(5) 0.107(3) Uani 0.750(7) 1 d PDU B 3
F7 F 0.8310(2) 0.39539(19) 0.7522(8) 0.101(3) Uani 0.750(7) 1 d PDU B 3
F8 F 0.7943(2) 0.46472(19) 0.7675(8) 0.111(4) Uani 0.750(7) 1 d PDU B 3
F9 F 0.8112(2) 0.4251(2) 0.8885(6) 0.083(3) Uani 0.750(7) 1 d PDU B 3
F10 F 0.84756(18) 0.44756(18) 0.7710(9) 0.072(3) Uani 0.750(7) 1 d PDU B 3
F11 F 0.8141(2) 0.4342(2) 0.6321(6) 0.125(5) Uani 0.750(7) 1 d PDU B 3
F12 F 0.77679(19) 0.4129(2) 0.7461(8) 0.114(5) Uani 0.750(7) 1 d PDU B 3
P3 P 0.9176(2) 0.2954(2) -0.1203(9) 0.0781(14) Uani 0.50(2) 1 d PDU C 4
F13 F 0.8938(3) 0.3212(4) -0.0710(17) 0.103(8) Uani 0.50(2) 1 d PDU C 4
F14 F 0.9442(4) 0.2685(4) -0.1664(14) 0.165(11) Uani 0.50(2) 1 d PDU C 4
F15 F 0.9220(6) 0.2803(4) -0.0005(10) 0.109(8) Uani 0.50(2) 1 d PDU C 4
F16 F 0.9480(3) 0.3196(5) -0.0973(12) 0.101(8) Uani 0.50(2) 1 d PDU C 4
F17 F 0.9144(5) 0.3097(3) -0.2380(10) 0.079(6) Uani 0.50(2) 1 d PDU C 4
F18 F 0.8888(4) 0.2693(4) -0.1465(16) 0.121(6) Uani 0.50(2) 1 d PDU C 4
P4 P 0.9181(2) 0.2969(2) -0.1068(9) 0.0781(14) Uani 0.50(2) 1 d PDU C 5
F19 F 0.9035(5) 0.2624(3) -0.1289(15) 0.121(6) Uani 0.50(2) 1 d PDU C 5
F20 F 0.9356(5) 0.3327(3) -0.0844(16) 0.137(10) Uani 0.50(2) 1 d PDU C 5
F21 F 0.9431(5) 0.2911(7) -0.2061(15) 0.201(13) Uani 0.50(2) 1 d PDU C 5
F22 F 0.9446(4) 0.2811(4) -0.0258(17) 0.120(9) Uani 0.50(2) 1 d PDU C 5
F23 F 0.8947(4) 0.3037(5) -0.0080(14) 0.117(8) Uani 0.50(2) 1 d PDU C 5
F24 F 0.8926(6) 0.3155(4) -0.1864(18) 0.146(10) Uani 0.50(2) 1 d PDU C 5
P5 P 0.8287(4) 0.4188(4) 0.7792(14) 0.107(3) Uani 0.250(7) 1 d PDU B 6
F25 F 0.8499(5) 0.3910(5) 0.830(2) 0.101(3) Uani 0.250(7) 1 d PDU B 6
F26 F 0.8075(7) 0.4483(6) 0.721(2) 0.111(4) Uani 0.250(7) 1 d PDU B 6
F27 F 0.8389(6) 0.4053(7) 0.6612(16) 0.101(3) Uani 0.250(7) 1 d PDU B 6
F28 F 0.8600(6) 0.4427(5) 0.778(3) 0.072(3) Uani 0.250(7) 1 d PDU B 6
F29 F 0.8183(7) 0.4328(7) 0.8929(16) 0.083(3) Uani 0.250(7) 1 d PDU B 6
F30 F 0.7958(5) 0.3965(6) 0.777(2) 0.101(3) Uani 0.250(7) 1 d PDU B 6
Co1 Co 0.87596(4) 0.33139(4) 0.39707(15) 0.0570(6) Uani 1 1 d . . .
Ru1 Ru 0.85603(2) 0.40846(2) 0.24894(8) 0.0401(3) Uani 1 1 d . . .
N13 N 0.984(2) 0.2301(14) -0.334(5) 0.15(2) Uani 0.25 1 d PD . 7
C39 C 0.981(2) 0.2548(14) -0.378(7) 0.15(2) Uani 0.25 1 d PD . 7
C40 C 0.976(2) 0.2884(13) -0.420(7) 0.15(2) Uani 0.25 1 d PD D 7
H40A H 0.9852 0.3031 -0.3637 0.218 Uiso 0.25 1 d PR D 7
H40B H 0.9529 0.2929 -0.431 0.218 Uiso 0.25 1 d PR D 7
H40C H 0.9883 0.2921 -0.4885 0.218 Uiso 0.25 1 d PR D 7



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.345(14) . ?
C1 C2 1.373(16) . ?
C1 H1 0.95 . ?
C2 C3 1.372(15) . ?
C2 H2 0.95 . ?
C3 C4 1.393(16) . ?
C3 H3 0.95 . ?
C4 C5 1.379(15) . ?
C4 H4 0.95 . ?
C5 N1 1.354(13) . ?
C5 C6 1.480(16) . ?
C6 C7 1.365(15) . ?
C6 N2 1.385(14) . ?
C7 C8 1.391(17) . ?
C7 H7 0.95 . ?
C8 C9 1.359(18) . ?
C8 H8 0.95 . ?
C9 C10 1.340(17) . ?
C9 H9 0.95 . ?
C10 N2 1.338(14) . ?
C10 H10 0.95 . ?
C11 N3 1.342(14) . ?
C11 C12 1.351(15) . ?
C11 H11 0.95 . ?
C12 C13 1.366(16) . ?
C12 H12 0.95 . ?
C13 C14 1.362(16) . ?
C13 H13 0.95 . ?
C14 C15 1.376(14) . ?
C14 H14 0.95 . ?
C15 N3 1.369(13) . ?
C15 C16 1.484(15) . ?
C16 N4 1.360(13) . ?
C16 C17 1.403(16) . ?
C17 C18 1.361(16) . ?
C17 H17 0.95 . ?
C18 C19 1.385(16) . ?
C18 H18 0.95 . ?
C19 C20 1.403(15) . ?
C19 H19 0.95 . ?
C20 N4 1.354(14) . ?
C20 H20 0.95 . ?
C21 C22 1.475(17) . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 N5 1.341(14) . ?
C22 C23 1.484(18) . ?
C23 N6 1.278(18) . ?
C23 C24 1.471(19) . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 N6 1.482(18) . ?
C25 C26 1.52(2) . ?
C25 H25A 0.99 . ?
C25 H25B 0.99 . ?
C26 N7 1.469(16) . ?
C26 H26A 0.99 . ?
C26 H26B 0.99 . ?
C27 C28 1.508(18) . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
C28 N7 1.300(16) . ?
C28 C29 1.474(19) . ?
C29 N8 1.347(15) . ?
C29 C30 1.458(17) . ?
C30 H30A 0.98 . ?
C30 H30B 0.98 . ?
C30 H30C 0.98 . ?
N9 C31 1.291(13) . ?
N9 C32 1.379(14) . ?
N9 Co1 1.961(9) . ?
N10 C31 1.351(12) . ?
N10 C33 1.358(14) . ?
N10 C34 1.468(14) . ?
C31 H31 0.95 . ?
C32 C33 1.351(15) . ?
C32 H32 0.95 . ?
C33 H33 0.95 . ?
C34 H34A 0.98 . ?
C34 H34B 0.98 . ?
C34 H34C 0.98 . ?
N11 C35 1.306(16) . ?
N11 C36 1.38(2) . ?
N11 Co1 1.92(2) . ?
N12 C35 1.344(14) . ?
N12 C37 1.351(18) . ?
N12 C38 1.469(16) . ?
C35 H35 0.95 . ?
C36 C37 1.348(16) . ?
C36 H36 0.95 . ?
C37 H37 0.95 . ?
C38 H38A 0.98 . ?
C38 H38B 0.98 . ?
C38 H38C 0.98 . ?
N11B C35B 1.305(19) . ?
N11B C36B 1.38(2) . ?
N11B Co1 2.10(5) . ?
N12B C35B 1.347(18) . ?
N12B C37B 1.36(2) . ?
N12B C38B 1.468(19) . ?
C35B H35B 0.95 . ?
C36B C37B 1.35(2) . ?
C36B H36B 0.95 . ?
C37B H37B 0.95 . ?
C38B H38D 0.98 . ?
C38B H38E 0.98 . ?
C38B H38F 0.98 . ?
N1 Ru1 2.023(9) . ?
N2 Ru1 2.040(9) . ?
N3 Ru1 2.042(9) . ?
N4 Ru1 2.015(9) . ?
N5 O1 1.297(10) . ?
N5 Co1 1.919(9) . ?
N6 Co1 1.865(12) . ?
N7 Co1 1.867(11) . ?
N8 O2 1.305(10) . ?
N8 Co1 1.887(10) . ?
O1 Ru1 2.079(7) . ?
O2 Ru1 2.094(7) . ?
P1 F1 1.550(6) . ?
P1 F5 1.561(6) . ?
P1 F6 1.603(5) . ?
P1 F3 1.605(6) . ?
P1 F4 1.605(5) . ?
P1 F2 1.630(6) . ?
P2 F7 1.541(7) . ?
P2 F11 1.570(7) . ?
P2 F10 1.593(6) . ?
P2 F9 1.602(7) . ?
P2 F12 1.620(6) . ?
P2 F8 1.646(7) . ?
P3 F13 1.544(7) . ?
P3 F17 1.563(7) . ?
P3 F16 1.601(6) . ?
P3 F15 1.603(7) . ?
P3 F18 1.608(6) . ?
P3 F14 1.638(7) . ?
P4 F19 1.542(7) . ?
P4 F23 1.564(7) . ?
P4 F22 1.600(6) . ?
P4 F21 1.603(7) . ?
P4 F24 1.609(6) . ?
P4 F20 1.640(7) . ?
P5 F25 1.546(7) . ?
P5 F29 1.564(7) . ?
P5 F28 1.598(6) . ?
P5 F27 1.604(7) . ?
P5 F30 1.613(6) . ?
P5 F26 1.637(7) . ?
N13 C39 0.67(9) 16_644 ?
N13 C40 0.90(10) 16_644 ?
N13 C39 1.142(5) . ?
N13 C39 1.64(10) 2_755 ?
N13 N13 1.80(8) 15_664 ?
N13 N13 1.80(8) 16_644 ?
N13 C39 1.85(6) 15_664 ?
C39 N13 0.67(9) 15_664 ?
C39 C39 1.11(13) 15_664 ?
C39 C39 1.11(13) 16_644 ?
C39 C40 1.472(5) . ?
C39 C40 1.51(11) 16_644 ?
C39 C39 1.57(18) 2_755 ?
C39 N13 1.64(10) 2_755 ?
C39 N13 1.85(6) 16_644 ?
C40 N13 0.90(10) 15_664 ?
C40 C39 1.51(11) 15_664 ?
C40 H40A 0.98 . ?
C40 H40B 0.98 . ?
C40 H40C 0.98 . ?

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 C1 C2 125.4(12) . . ?
N1 C1 H1 117.3 . . ?
C2 C1 H1 117.3 . . ?
C3 C2 C1 118.0(13) . . ?
C3 C2 H2 121 . . ?
C1 C2 H2 121 . . ?
C2 C3 C4 118.2(12) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C5 C4 C3 120.0(12) . . ?
C5 C4 H4 120 . . ?
C3 C4 H4 120 . . ?
N1 C5 C4 122.3(12) . . ?
N1 C5 C6 114.1(11) . . ?
C4 C5 C6 123.5(12) . . ?
C7 C6 N2 121.0(13) . . ?
C7 C6 C5 124.6(13) . . ?
N2 C6 C5 114.4(11) . . ?
C6 C7 C8 117.6(13) . . ?
C6 C7 H7 121.2 . . ?
C8 C7 H7 121.2 . . ?
C9 C8 C7 121.8(13) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C10 C9 C8 117.3(14) . . ?
C10 C9 H9 121.4 . . ?
C8 C9 H9 121.4 . . ?
N2 C10 C9 124.5(14) . . ?
N2 C10 H10 117.7 . . ?
C9 C10 H10 117.7 . . ?
N3 C11 C12 122.9(11) . . ?
N3 C11 H11 118.6 . . ?
C12 C11 H11 118.6 . . ?
C11 C12 C13 118.7(13) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C14 C13 C12 121.0(12) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 118.0(12) . . ?
C13 C14 H14 121 . . ?
C15 C14 H14 121 . . ?
N3 C15 C14 121.7(11) . . ?
N3 C15 C16 114.7(11) . . ?
C14 C15 C16 123.4(12) . . ?
N4 C16 C17 121.3(12) . . ?
N4 C16 C15 113.6(12) . . ?
C17 C16 C15 124.9(12) . . ?
C18 C17 C16 119.7(12) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C19 119.6(13) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C20 118.9(12) . . ?
C18 C19 H19 120.6 . . ?
C20 C19 H19 120.6 . . ?
N4 C20 C19 121.8(11) . . ?
N4 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C21 120.4(11) . . ?
N5 C22 C23 113.9(13) . . ?
C21 C22 C23 125.6(13) . . ?
N6 C23 C24 128.3(14) . . ?
N6 C23 C22 111.3(14) . . ?
C24 C23 C22 120.3(16) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N6 C25 C26 107.3(13) . . ?
N6 C25 H25A 110.3 . . ?
C26 C25 H25A 110.3 . . ?
N6 C25 H25B 110.3 . . ?
C26 C25 H25B 110.3 . . ?
H25A C25 H25B 108.5 . . ?
N7 C26 C25 108.4(13) . . ?
N7 C26 H26A 110 . . ?
C25 C26 H26A 110 . . ?
N7 C26 H26B 110 . . ?
C25 C26 H26B 110 . . ?
H26A C26 H26B 108.4 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N7 C28 C29 114.0(14) . . ?
N7 C28 C27 124.2(15) . . ?
C29 C28 C27 121.3(15) . . ?
N8 C29 C30 123.9(12) . . ?
N8 C29 C28 109.8(14) . . ?
C30 C29 C28 126.0(14) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C31 N9 C32 106.0(10) . . ?
C31 N9 Co1 125.8(9) . . ?
C32 N9 Co1 128.1(10) . . ?
C31 N10 C33 105.5(11) . . ?
C31 N10 C34 127.0(12) . . ?
C33 N10 C34 127.4(11) . . ?
N9 C31 N10 112.4(12) . . ?
N9 C31 H31 123.8 . . ?
N10 C31 H31 123.8 . . ?
C33 C32 N9 108.1(12) . . ?
C33 C32 H32 125.9 . . ?
N9 C32 H32 125.9 . . ?
C32 C33 N10 107.9(11) . . ?
C32 C33 H33 126.1 . . ?
N10 C33 H33 126.1 . . ?
N10 C34 H34A 109.5 . . ?
N10 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N10 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 N11 C36 104.0(15) . . ?
C35 N11 Co1 126.4(17) . . ?
C36 N11 Co1 129.3(18) . . ?
C35 N12 C37 106.1(15) . . ?
C35 N12 C38 127.4(16) . . ?
C37 N12 C38 126.3(15) . . ?
N11 C35 N12 112.8(14) . . ?
N11 C35 H35 123.6 . . ?
N12 C35 H35 123.6 . . ?
C37 C36 N11 109.4(13) . . ?
C37 C36 H36 125.3 . . ?
N11 C36 H36 125.3 . . ?
C36 C37 N12 107.0(12) . . ?
C36 C37 H37 126.5 . . ?
N12 C37 H37 126.5 . . ?
C35B N11B C36B 104(3) . . ?
C35B N11B Co1 130(4) . . ?
C36B N11B Co1 124(4) . . ?
C35B N12B C37B 106(2) . . ?
C35B N12B C38B 128(3) . . ?
C37B N12B C38B 127(2) . . ?
N11B C35B N12B 112(2) . . ?
N11B C35B H35B 124 . . ?
N12B C35B H35B 124 . . ?
C37B C36B N11B 109(2) . . ?
C37B C36B H36B 125.4 . . ?
N11B C36B H36B 125.4 . . ?
C36B C37B N12B 106.9(18) . . ?
C36B C37B H37B 126.6 . . ?
N12B C37B H37B 126.6 . . ?
N12B C38B H38D 109.5 . . ?
N12B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
N12B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C1 N1 C5 115.9(10) . . ?
C1 N1 Ru1 128.1(8) . . ?
C5 N1 Ru1 116.0(8) . . ?
C10 N2 C6 117.5(11) . . ?
C10 N2 Ru1 127.9(9) . . ?
C6 N2 Ru1 113.8(8) . . ?
C11 N3 C15 117.6(10) . . ?
C11 N3 Ru1 128.8(8) . . ?
C15 N3 Ru1 113.5(8) . . ?
C20 N4 C16 118.5(11) . . ?
C20 N4 Ru1 125.6(9) . . ?
C16 N4 Ru1 115.2(9) . . ?
O1 N5 C22 119.1(10) . . ?
O1 N5 Co1 127.7(8) . . ?
C22 N5 Co1 113.1(9) . . ?
C23 N6 C25 126.3(14) . . ?
C23 N6 Co1 119.2(10) . . ?
C25 N6 Co1 114.1(11) . . ?
C28 N7 C26 128.2(14) . . ?
C28 N7 Co1 116.9(10) . . ?
C26 N7 Co1 113.5(11) . . ?
O2 N8 C29 114.3(10) . . ?
O2 N8 Co1 128.1(8) . . ?
C29 N8 Co1 116.8(9) . . ?
N5 O1 Ru1 125.8(6) . . ?
N8 O2 Ru1 124.3(7) . . ?
F1 P1 F5 93.0(4) . . ?
F1 P1 F6 93.2(3) . . ?
F5 P1 F6 90.3(3) . . ?
F1 P1 F3 87.9(4) . . ?
F5 P1 F3 178.3(4) . . ?
F6 P1 F3 91.1(3) . . ?
F1 P1 F4 89.6(3) . . ?
F5 P1 F4 89.8(3) . . ?
F6 P1 F4 177.2(4) . . ?
F3 P1 F4 88.8(3) . . ?
F1 P1 F2 175.6(4) . . ?
F5 P1 F2 90.4(3) . . ?
F6 P1 F2 89.6(3) . . ?
F3 P1 F2 88.7(4) . . ?
F4 P1 F2 87.5(3) . . ?
F7 P2 F11 93.4(5) . . ?
F7 P2 F10 90.8(4) . . ?
F11 P2 F10 90.5(4) . . ?
F7 P2 F9 89.4(5) . . ?
F11 P2 F9 177.2(6) . . ?
F10 P2 F9 89.8(4) . . ?
F7 P2 F12 93.8(4) . . ?
F11 P2 F12 88.9(4) . . ?
F10 P2 F12 175.4(5) . . ?
F9 P2 F12 90.6(4) . . ?
F7 P2 F8 179.2(6) . . ?
F11 P2 F8 87.3(5) . . ?
F10 P2 F8 89.0(4) . . ?
F9 P2 F8 89.8(5) . . ?
F12 P2 F8 86.4(4) . . ?
F13 P3 F17 93.4(5) . . ?
F13 P3 F16 89.8(5) . . ?
F17 P3 F16 89.9(5) . . ?
F13 P3 F15 88.3(6) . . ?
F17 P3 F15 178.1(6) . . ?
F16 P3 F15 89.3(5) . . ?
F13 P3 F18 94.0(5) . . ?
F17 P3 F18 90.0(5) . . ?
F16 P3 F18 176.2(6) . . ?
F15 P3 F18 90.7(5) . . ?
F13 P3 F14 176.6(6) . . ?
F17 P3 F14 89.0(5) . . ?
F16 P3 F14 87.8(5) . . ?
F15 P3 F14 89.3(5) . . ?
F18 P3 F14 88.4(5) . . ?
F19 P4 F23 93.7(5) . . ?
F19 P4 F22 90.1(5) . . ?
F23 P4 F22 89.8(5) . . ?
F19 P4 F21 88.6(6) . . ?
F23 P4 F21 177.5(6) . . ?
F22 P4 F21 89.3(5) . . ?
F19 P4 F24 94.1(5) . . ?
F23 P4 F24 90.0(5) . . ?
F22 P4 F24 175.8(6) . . ?
F21 P4 F24 90.8(5) . . ?
F19 P4 F20 176.9(6) . . ?
F23 P4 F20 88.6(5) . . ?
F22 P4 F20 87.7(5) . . ?
F21 P4 F20 89.0(5) . . ?
F24 P4 F20 88.0(5) . . ?
F25 P5 F29 93.3(6) . . ?
F25 P5 F28 90.2(5) . . ?
F29 P5 F28 90.3(5) . . ?
F25 P5 F27 88.2(6) . . ?
F29 P5 F27 178.5(7) . . ?
F28 P5 F27 89.4(5) . . ?
F25 P5 F30 93.3(5) . . ?
F29 P5 F30 89.8(5) . . ?
F28 P5 F30 176.4(6) . . ?
F27 P5 F30 90.4(5) . . ?
F25 P5 F26 177.1(6) . . ?
F29 P5 F26 89.2(5) . . ?
F28 P5 F26 88.2(5) . . ?
F27 P5 F26 89.3(5) . . ?
F30 P5 F26 88.2(5) . . ?
N6 Co1 N7 86.6(6) . . ?
N6 Co1 N8 168.4(5) . . ?
N7 Co1 N8 82.1(6) . . ?
N6 Co1 N11 92.1(15) . . ?
N7 Co1 N11 91.9(16) . . ?
N8 Co1 N11 85.6(13) . . ?
N6 Co1 N5 82.4(5) . . ?
N7 Co1 N5 168.6(5) . . ?
N8 Co1 N5 109.0(5) . . ?
N11 Co1 N5 91.5(14) . . ?
N6 Co1 N9 92.2(4) . . ?
N7 Co1 N9 89.6(4) . . ?
N8 Co1 N9 90.5(4) . . ?
N11 Co1 N9 175.5(17) . . ?
N5 Co1 N9 87.8(4) . . ?
N6 Co1 N11B 86(3) . . ?
N7 Co1 N11B 96(3) . . ?
N8 Co1 N11B 92(3) . . ?
N11 Co1 N11B 8(3) . . ?
N5 Co1 N11B 86(3) . . ?
N9 Co1 N11B 174(3) . . ?
N4 Ru1 N1 98.2(4) . . ?
N4 Ru1 N2 98.0(4) . . ?
N1 Ru1 N2 79.7(4) . . ?
N4 Ru1 N3 79.7(4) . . ?
N1 Ru1 N3 176.5(4) . . ?
N2 Ru1 N3 97.6(4) . . ?
N4 Ru1 O1 80.7(3) . . ?
N1 Ru1 O1 93.6(3) . . ?
N2 Ru1 O1 173.0(4) . . ?
N3 Ru1 O1 88.9(3) . . ?
N4 Ru1 O2 173.0(4) . . ?
N1 Ru1 O2 88.1(3) . . ?
N2 Ru1 O2 80.2(3) . . ?
N3 Ru1 O2 93.8(3) . . ?
O1 Ru1 O2 102.0(3) . . ?
C39 N13 C40 137(10) 16_644 16_644 ?
C39 N13 C39 70(10) 16_644 . ?
C40 N13 C39 95(10) 16_644 . ?
C39 N13 C39 30(10) 16_644 2_755 ?
C40 N13 C39 159(9) 16_644 2_755 ?
C39 N13 C39 66(8) . 2_755 ?
C39 N13 N13 66(10) 16_644 15_664 ?
C40 N13 N13 95(9) 16_644 15_664 ?
C39 N13 N13 6(5) . 15_664 ?
C39 N13 N13 65(2) 2_755 15_664 ?
C39 N13 N13 11(8) 16_644 16_644 ?
C40 N13 N13 148(10) 16_644 16_644 ?
C39 N13 N13 74(4) . 16_644 ?
C39 N13 N13 22(2) 2_755 16_644 ?
N13 N13 N13 71(5) 15_664 16_644 ?
C39 N13 C39 56(10) 16_644 15_664 ?
C40 N13 C39 127(9) 16_644 15_664 ?
C39 N13 C39 34(6) . 15_664 ?
C39 N13 C39 37(4) 2_755 15_664 ?
N13 N13 C39 36.4(11) 15_664 15_664 ?
N13 N13 C39 54(3) 16_644 15_664 ?
N13 C39 C39 75(9) 15_664 15_664 ?
N13 C39 C39 133(10) 15_664 16_644 ?
C39 C39 C39 89.8(9) 15_664 16_644 ?
N13 C39 N13 163(10) 15_664 . ?
C39 C39 N13 110(8) 15_664 . ?
C39 C39 N13 35(6) 16_644 . ?
N13 C39 C40 25(10) 15_664 . ?
C39 C39 C40 70(8) 15_664 . ?
C39 C39 C40 152(6) 16_644 . ?
N13 C39 C40 172(5) . . ?
N13 C39 C40 140(10) 15_664 16_644 ?
C39 C39 C40 145(9) 15_664 16_644 ?
C39 C39 C40 66(4) 16_644 16_644 ?
N13 C39 C40 37(6) . 16_644 ?
C40 C39 C40 140(6) . 16_644 ?
N13 C39 C39 104(10) 15_664 2_755 ?
C39 C39 C39 45.1(5) 15_664 2_755 ?
C39 C39 C39 45.1(5) 16_644 2_755 ?
N13 C39 C39 73(6) . 2_755 ?
C40 C39 C39 111(8) . 2_755 ?
C40 C39 C39 109(4) 16_644 2_755 ?
N13 C39 N13 92(9) 15_664 2_755 ?
C39 C39 N13 18(6) 15_664 2_755 ?
C39 C39 N13 82(6) 16_644 2_755 ?
N13 C39 N13 96(10) . 2_755 ?
C40 C39 N13 83(6) . 2_755 ?
C40 C39 N13 128(7) 16_644 2_755 ?
C39 C39 N13 41(3) 2_755 2_755 ?
N13 C39 N13 101(10) 15_664 16_644 ?
C39 C39 N13 62(4) 15_664 16_644 ?
C39 C39 N13 35(3) 16_644 16_644 ?
N13 C39 N13 69(4) . 16_644 ?
C40 C39 N13 117(6) . 16_644 ?
C40 C39 N13 101(4) 16_644 16_644 ?
C39 C39 N13 21(2) 2_755 16_644 ?
N13 C39 N13 61(4) 2_755 16_644 ?
N13 C40 C39 18(8) 15_664 . ?
N13 C40 C39 49(6) 15_664 15_664 ?
C39 C40 C39 44(6) . 15_664 ?
N13 C40 H40A 120.3 15_664 . ?
C39 C40 H40A 105.3 . . ?
C39 C40 H40A 76.8 15_664 . ?
N13 C40 H40B 110.5 15_664 . ?
C39 C40 H40B 110.4 . . ?
C39 C40 H40B 152.7 15_664 . ?
H40A C40 H40B 109.5 . . ?
N13 C40 H40C 96.7 15_664 . ?
C39 C40 H40C 112.6 . . ?
C39 C40 H40C 92.3 15_664 . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?



# start Validation Reply Form 
_vrf_RINTA01_I                   
; 
PROBLEM: The value of Rint is greater than 0.25 
RESPONSE: When samples are extremely small, data variance becomes large.
Rint does not improve with more data, just becomes more certain in
its value. Our sample was very small indeed, yet for the sake of 
quality the best we could do.
;
_vrf_PLAT020_I                   
; 
PROBLEM: The value of Rint is greater than 0.12 ......... 0.361 
RESPONSE: See above
;
# end Validation Reply Form


# END of CIF
