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

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_Co4
_audit_creation_method           SHELXL-97
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H60 Cl8 Co4 N4 O4 S4'
_chemical_formula_sum            'C44 H60 Cl8 Co4 N4 O4 S4'
_chemical_formula_weight         1356.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+3/4'
'y+1/4, -x+1/4, z+1/4'
'-x, -y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+5/4'
'y+3/4, -x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-3/4'
'-y-1/4, x-1/4, -z-1/4'
'x, y-1/2, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z-1/4'
'-y+1/4, x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'

_cell_length_a                   19.2769(8)
_cell_length_b                   19.2769(8)
_cell_length_c                   18.5886(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6907.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6849
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      29.99

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2768
_exptl_absorpt_coefficient_mu    1.410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_T_max  0.6771
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14447
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         29.99
_reflns_number_total             5026
_reflns_number_gt                3748
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_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)+(0.0560P)²+15.6078P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5026
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1284
_refine_ls_wR_factor_gt          0.1184
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.50967(18) 0.65231(15) 0.34290(15) 0.0369(6) Uani 1 1 d . . .
H1 H 0.5517 0.6428 0.3182 0.044 Uiso 1 1 calc R . .
C2 C 0.5110(2) 0.65668(18) 0.41689(16) 0.0455(8) Uani 1 1 d . . .
H2 H 0.5531 0.6499 0.4426 0.055 Uiso 1 1 calc R . .
C3 C 0.4503(2) 0.67097(19) 0.45273(17) 0.0511(9) Uani 1 1 d . . .
H3 H 0.4501 0.6750 0.5037 0.061 Uiso 1 1 calc R . .
C4 C 0.39013(19) 0.67936(16) 0.41425(16) 0.0405(7) Uani 1 1 d . . .
H4 H 0.3479 0.6894 0.4384 0.049 Uiso 1 1 calc R . .
C5 C 0.39131(16) 0.67312(13) 0.33937(14) 0.0315(6) Uani 1 1 d . . .
C6 C 0.32497(16) 0.67924(14) 0.29713(15) 0.0326(6) Uani 1 1 d . . .
H6A H 0.3256 0.7240 0.2710 0.039 Uiso 1 1 calc R . .
H6B H 0.2858 0.6808 0.3315 0.039 Uiso 1 1 calc R . .
C7 C 0.31080(14) 0.62106(13) 0.24250(14) 0.0273(5) Uani 1 1 d . . .
C8 C 0.23531(15) 0.62684(16) 0.21724(17) 0.0370(6) Uani 1 1 d . . .
H8A H 0.2046 0.6242 0.2598 0.044 Uiso 1 1 calc R . .
H8B H 0.2285 0.6730 0.1950 0.044 Uiso 1 1 calc R . .
C9 C 0.21304(16) 0.57154(18) 0.16362(18) 0.0426(7) Uani 1 1 d . . .
H9A H 0.2425 0.5747 0.1201 0.051 Uiso 1 1 calc R . .
H9B H 0.1645 0.5802 0.1489 0.051 Uiso 1 1 calc R . .
C10 C 0.31033(16) 0.48969(15) 0.22442(17) 0.0361(6) Uani 1 1 d . . .
H10A H 0.3238 0.4458 0.2483 0.043 Uiso 1 1 calc R . .
H10B H 0.3381 0.4939 0.1798 0.043 Uiso 1 1 calc R . .
C11 C 0.32780(15) 0.54979(13) 0.27367(14) 0.0302(5) Uani 1 1 d . . .
H11A H 0.3779 0.5481 0.2850 0.036 Uiso 1 1 calc R . .
H11B H 0.3021 0.5440 0.3194 0.036 Uiso 1 1 calc R . .
N1 N 0.45169(12) 0.66094(11) 0.30434(11) 0.0281(4) Uani 1 1 d . . .
O1 O 0.35650(9) 0.63007(10) 0.18041(9) 0.0274(4) Uani 1 1 d . . .
S1 S 0.21970(5) 0.48525(5) 0.20078(5) 0.0469(2) Uani 1 1 d . . .
Cl1 Cl 0.42177(3) 0.78658(3) 0.19020(3) 0.02206(12) Uani 1 1 d . . .
Cl2 Cl 0.51118(3) 0.54683(3) 0.18668(3) 0.02974(15) Uani 1 1 d . . .
Co1 Co 0.460712(17) 0.658026(17) 0.191494(17) 0.02259(10) Uani 1 1 d . . .
H1A H 0.3345 0.6552 0.1500 0.050 Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0493(17) 0.0332(14) 0.0282(13) 0.0055(11) 0.0002(12) -0.0003(12)
C2 0.067(2) 0.0429(17) 0.0267(13) 0.0067(12) -0.0072(14) -0.0084(16)
C3 0.083(3) 0.0456(18) 0.0246(13) -0.0002(12) 0.0076(15) -0.0162(18)
C4 0.0563(19) 0.0351(15) 0.0302(13) -0.0064(11) 0.0151(13) -0.0118(14)
C5 0.0474(16) 0.0213(11) 0.0258(11) -0.0019(9) 0.0103(11) -0.0066(11)
C6 0.0407(15) 0.0243(12) 0.0328(13) -0.0030(10) 0.0141(11) 0.0010(11)
C7 0.0293(12) 0.0254(11) 0.0273(11) 0.0018(9) 0.0119(10) 0.0009(10)
C8 0.0287(13) 0.0357(14) 0.0465(16) 0.0009(12) 0.0096(12) 0.0067(12)
C9 0.0293(14) 0.0509(18) 0.0476(17) -0.0008(14) 0.0013(13) 0.0010(13)
C10 0.0415(15) 0.0259(13) 0.0408(15) -0.0047(11) 0.0095(12) 0.0002(11)
C11 0.0369(14) 0.0244(12) 0.0292(12) 0.0000(10) 0.0090(10) 0.0003(10)
N1 0.0383(12) 0.0235(10) 0.0226(9) 0.0042(8) 0.0027(8) 0.0015(9)
O1 0.0270(9) 0.0304(9) 0.0247(8) 0.0009(7) 0.0030(7) 0.0055(7)
S1 0.0401(4) 0.0422(4) 0.0583(5) -0.0115(4) 0.0127(4) -0.0129(3)
Cl1 0.0242(3) 0.0219(2) 0.0201(2) 0.00084(19) 0.00172(19) 0.0015(2)
Cl2 0.0351(3) 0.0226(3) 0.0315(3) 0.0003(2) 0.0047(2) 0.0037(2)
Co1 0.02489(17) 0.02235(16) 0.02053(16) 0.00036(11) 0.00346(12) 0.00138(12)

_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 1.338(4) . ?
C1 C2 1.378(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.374(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.373(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.397(4) . ?
C4 H4 0.9500 . ?
C5 N1 1.354(4) . ?
C5 C6 1.505(4) . ?
C6 C7 1.537(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O1 1.462(3) . ?
C7 C11 1.526(4) . ?
C7 C8 1.533(4) . ?
C8 C9 1.521(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 S1 1.806(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.515(4) . ?
C10 S1 1.804(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N1 Co1 2.105(2) . ?
O1 Co1 2.0901(19) . ?
O1 H1A 0.8569 . ?
Cl1 Co1 2.4629(6) 10_576 ?
Cl1 Co1 2.5046(7) 4_665 ?
Cl1 Co1 2.5896(6) . ?
Cl2 Co1 2.3558(7) . ?
Co1 Cl1 2.4629(6) 15_655 ?
Co1 Cl1 2.5046(7) 4_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.9(3) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 118.7(3) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C4 C3 C2 119.4(3) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 120.5(3) . . ?
N1 C5 C6 119.5(2) . . ?
C4 C5 C6 119.9(3) . . ?
C5 C6 C7 116.0(2) . . ?
C5 C6 H6A 108.3 . . ?
C7 C6 H6A 108.3 . . ?
C5 C6 H6B 108.3 . . ?
C7 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
O1 C7 C11 106.09(19) . . ?
O1 C7 C8 108.7(2) . . ?
C11 C7 C8 112.7(2) . . ?
O1 C7 C6 109.1(2) . . ?
C11 C7 C6 111.6(2) . . ?
C8 C7 C6 108.5(2) . . ?
C9 C8 C7 114.7(2) . . ?
C9 C8 H8A 108.6 . . ?
C7 C8 H8A 108.6 . . ?
C9 C8 H8B 108.6 . . ?
C7 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
C8 C9 S1 112.0(2) . . ?
C8 C9 H9A 109.2 . . ?
S1 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
S1 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C11 C10 S1 113.5(2) . . ?
C11 C10 H10A 108.9 . . ?
S1 C10 H10A 108.9 . . ?
C11 C10 H10B 108.9 . . ?
S1 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C10 C11 C7 114.3(2) . . ?
C10 C11 H11A 108.7 . . ?
C7 C11 H11A 108.7 . . ?
C10 C11 H11B 108.7 . . ?
C7 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C1 N1 C5 118.8(2) . . ?
C1 N1 Co1 117.48(19) . . ?
C5 N1 Co1 123.69(19) . . ?
C7 O1 Co1 122.13(15) . . ?
C7 O1 H1A 106.8 . . ?
Co1 O1 H1A 113.3 . . ?
C10 S1 C9 96.80(14) . . ?
Co1 Cl1 Co1 95.61(2) 10_576 4_665 ?
Co1 Cl1 Co1 93.48(2) 10_576 . ?
Co1 Cl1 Co1 98.38(2) 4_665 . ?
O1 Co1 N1 91.47(8) . . ?
O1 Co1 Cl2 99.12(5) . . ?
N1 Co1 Cl2 95.52(6) . . ?
O1 Co1 Cl1 87.14(5) . 15_655 ?
N1 Co1 Cl1 171.53(6) . 15_655 ?
Cl2 Co1 Cl1 92.94(2) . 15_655 ?
O1 Co1 Cl1 168.06(5) . 4_665 ?
N1 Co1 Cl1 94.18(7) . 4_665 ?
Cl2 Co1 Cl1 90.80(2) . 4_665 ?
Cl1 Co1 Cl1 85.73(2) 15_655 4_665 ?
O1 Co1 Cl1 88.12(5) . . ?
N1 Co1 Cl1 87.70(6) . . ?
Cl2 Co1 Cl1 171.97(3) . . ?
Cl1 Co1 Cl1 83.91(2) 15_655 . ?
Cl1 Co1 Cl1 81.61(2) 4_665 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -0.4(5) . . . . ?
C1 C2 C3 C4 1.0(5) . . . . ?
C2 C3 C4 C5 0.1(5) . . . . ?
C3 C4 C5 N1 -2.0(4) . . . . ?
C3 C4 C5 C6 177.4(3) . . . . ?
N1 C5 C6 C7 49.5(3) . . . . ?
C4 C5 C6 C7 -129.8(3) . . . . ?
C5 C6 C7 O1 -74.0(3) . . . . ?
C5 C6 C7 C11 42.9(3) . . . . ?
C5 C6 C7 C8 167.7(2) . . . . ?
O1 C7 C8 C9 62.4(3) . . . . ?
C11 C7 C8 C9 -54.9(3) . . . . ?
C6 C7 C8 C9 -179.0(2) . . . . ?
C7 C8 C9 S1 61.0(3) . . . . ?
S1 C10 C11 C7 -59.7(3) . . . . ?
O1 C7 C11 C10 -65.3(3) . . . . ?
C8 C7 C11 C10 53.6(3) . . . . ?
C6 C7 C11 C10 176.0(2) . . . . ?
C2 C1 N1 C5 -1.4(4) . . . . ?
C2 C1 N1 Co1 176.6(2) . . . . ?
C4 C5 N1 C1 2.6(4) . . . . ?
C6 C5 N1 C1 -176.8(2) . . . . ?
C4 C5 N1 Co1 -175.3(2) . . . . ?
C6 C5 N1 Co1 5.3(3) . . . . ?
C11 C7 O1 Co1 -78.7(2) . . . . ?
C8 C7 O1 Co1 159.85(17) . . . . ?
C6 C7 O1 Co1 41.6(3) . . . . ?
C11 C10 S1 C9 56.3(2) . . . . ?
C8 C9 S1 C10 -56.3(2) . . . . ?
C7 O1 Co1 N1 0.10(18) . . . . ?
C7 O1 Co1 Cl2 95.93(17) . . . . ?
C7 O1 Co1 Cl1 -171.54(17) . . . 15_655 ?
C7 O1 Co1 Cl1 -118.2(2) . . . 4_665 ?
C7 O1 Co1 Cl1 -87.55(17) . . . . ?
C1 N1 Co1 O1 156.2(2) . . . . ?
C5 N1 Co1 O1 -25.9(2) . . . . ?
C1 N1 Co1 Cl2 56.9(2) . . . . ?
C5 N1 Co1 Cl2 -125.2(2) . . . . ?
C1 N1 Co1 Cl1 -34.3(2) . . . 4_665 ?
C5 N1 Co1 Cl1 143.6(2) . . . 4_665 ?
C1 N1 Co1 Cl1 -115.7(2) . . . . ?
C5 N1 Co1 Cl1 62.2(2) . . . . ?
Co1 Cl1 Co1 O1 -78.79(5) 10_576 . . . ?
Co1 Cl1 Co1 O1 -174.99(5) 4_665 . . . ?
Co1 Cl1 Co1 N1 -170.34(7) 10_576 . . . ?
Co1 Cl1 Co1 N1 93.46(7) 4_665 . . . ?
Co1 Cl1 Co1 Cl1 8.53(2) 10_576 . . 15_655 ?
Co1 Cl1 Co1 Cl1 -87.67(2) 4_665 . . 15_655 ?
Co1 Cl1 Co1 Cl1 95.087(19) 10_576 . . 4_665 ?
Co1 Cl1 Co1 Cl1 -1.11(3) 4_665 . . 4_665 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A Cl2 0.86 2.39 3.2335(19) 167.3 10_576

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        29.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.091

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
1 -0.002 -0.004 -0.003 1820.5 287.7
_platon_squeeze_details          
;
 The residual electron density was assigned to half a molecule of the 
 dichloromethane solvent [288/16 = 18 e per asymmetric unit; half a molecule
 of CH2Cl2 would give 21e].
;
_database_code_depnum_ccdc_archive 'CCDC 964328'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ni4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H60 Cl8 N4 Ni4 O4 S4'
_chemical_formula_sum            'C44 H60 Cl8 N4 Ni4 O4 S4'
_chemical_formula_weight         1355.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+3/4'
'y+1/4, -x+1/4, z+1/4'
'-x, -y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+5/4'
'y+3/4, -x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-3/4'
'-y-1/4, x-1/4, -z-1/4'
'x, y-1/2, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z-1/4'
'-y+1/4, x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'

_cell_length_a                   19.091(1)
_cell_length_b                   19.091(1)
_cell_length_c                   18.729(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6826.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3152
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      26.022

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2784
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_T_max  0.6968
_exptl_absorpt_process_details   
'R.H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38'


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39794
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0110
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3351
_reflns_number_gt                2860
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
A dichloromethane molecule was found heavily disordered on, 
at least, four positions, 
with no atoms in common.A PLATON SQUEEZE procedure was then applied. 
The calculation, performed on the complete model, 
omitting the disordered dichlorometane, 
risulted in an estimated missing electron density of 519 e/cell, compatible with
 circa ten dichlorometane molecules per cell. The OH hydrogen atom was found in 
the difference maps and was refined with a restrained O-H distance of 0.9 A

;

_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)+(0.0412P)²+55.7097P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3351
_refine_ls_number_parameters     158
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1257
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_restrained_S_all      1.167
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.45921(2) 0.66101(2) 0.19037(2) 0.02017(16) Uani 1 1 d . . .
Cl1A Cl 0.46311(4) 0.67238(4) 0.06140(4) 0.0196(2) Uani 1 1 d . . .
Cl2A Cl 0.50766(5) 0.54812(5) 0.18534(5) 0.0268(2) Uani 1 1 d . . .
N1 N 0.45088(17) 0.66166(16) 0.29961(18) 0.0254(7) Uani 1 1 d . . .
O1 O 0.35612(14) 0.62967(14) 0.17698(14) 0.0246(6) Uani 1 1 d D . .
C1 C 0.3091(2) 0.6210(2) 0.2378(2) 0.0260(8) Uani 1 1 d . . .
C2 C 0.3229(2) 0.6800(2) 0.2920(2) 0.0285(8) Uani 1 1 d . . .
H2A H 0.3238 0.7251 0.2659 0.034 Uiso 1 1 calc R . .
H2B H 0.2830 0.6817 0.3257 0.034 Uiso 1 1 calc R . .
C3 C 0.3895(2) 0.6741(2) 0.3347(2) 0.0285(8) Uani 1 1 d . . .
C4 C 0.3884(3) 0.6797(2) 0.4082(2) 0.0360(10) Uani 1 1 d . . .
H4 H 0.3457 0.6899 0.4322 0.043 Uiso 1 1 calc R . .
C5 C 0.4485(3) 0.6707(3) 0.4463(2) 0.0449(12) Uani 1 1 d . . .
H5 H 0.4479 0.6747 0.4969 0.054 Uiso 1 1 calc R . .
C6 C 0.5104(3) 0.6557(2) 0.4114(2) 0.0382(10) Uani 1 1 d . . .
H6 H 0.5526 0.6482 0.4371 0.046 Uiso 1 1 calc R . .
C7 C 0.5088(2) 0.6519(2) 0.3380(2) 0.0327(9) Uani 1 1 d . . .
H7 H 0.5512 0.6418 0.3135 0.039 Uiso 1 1 calc R . .
C8 C 0.2335(2) 0.6266(2) 0.2106(2) 0.0324(9) Uani 1 1 d . . .
H8A H 0.2014 0.6242 0.2520 0.039 Uiso 1 1 calc R . .
H8B H 0.2272 0.6731 0.1880 0.039 Uiso 1 1 calc R . .
C9 C 0.2122(2) 0.5706(2) 0.1572(3) 0.0389(10) Uani 1 1 d . . .
H9A H 0.2432 0.5734 0.1149 0.047 Uiso 1 1 calc R . .
H9B H 0.1636 0.5795 0.1411 0.047 Uiso 1 1 calc R . .
C10 C 0.3085(2) 0.4874(2) 0.2204(3) 0.0353(10) Uani 1 1 d . . .
H10A H 0.3213 0.4432 0.2448 0.042 Uiso 1 1 calc R . .
H10B H 0.3376 0.4911 0.1768 0.042 Uiso 1 1 calc R . .
C11 C 0.3252(2) 0.5490(2) 0.2697(2) 0.0296(9) Uani 1 1 d . . .
H11A H 0.3756 0.5472 0.2823 0.036 Uiso 1 1 calc R . .
H11B H 0.2981 0.5435 0.3144 0.036 Uiso 1 1 calc R . .
S1 S 0.21751(7) 0.48357(6) 0.19498(7) 0.0439(3) Uani 1 1 d . . .
H1O H 0.339(2) 0.660(2) 0.1448(19) 0.035(13) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0220(3) 0.0200(3) 0.0185(3) 0.00012(17) 0.00211(18) 0.00121(17)
Cl1A 0.0198(4) 0.0224(4) 0.0166(4) -0.0012(3) 0.0007(3) -0.0016(3)
Cl2A 0.0323(5) 0.0195(4) 0.0285(5) 0.0002(3) 0.0038(4) 0.0026(3)
N1 0.0294(17) 0.0201(15) 0.0266(17) 0.0048(13) 0.0038(13) 0.0013(13)
O1 0.0280(14) 0.0250(14) 0.0208(13) -0.0027(11) 0.0002(11) 0.0056(11)
C1 0.028(2) 0.028(2) 0.0222(18) -0.0002(15) 0.0121(15) 0.0012(15)
C2 0.034(2) 0.0242(19) 0.028(2) -0.0032(16) 0.0095(17) 0.0001(16)
C3 0.041(2) 0.0204(18) 0.0239(19) -0.0014(15) 0.0049(17) -0.0046(16)
C4 0.045(3) 0.033(2) 0.030(2) -0.0025(18) 0.0092(19) -0.0078(19)
C5 0.069(3) 0.044(3) 0.022(2) -0.0007(19) 0.005(2) -0.013(2)
C6 0.055(3) 0.033(2) 0.026(2) 0.0045(18) -0.007(2) -0.004(2)
C7 0.041(2) 0.031(2) 0.026(2) 0.0015(17) -0.0001(18) 0.0010(18)
C8 0.023(2) 0.032(2) 0.042(2) 0.0012(18) 0.0083(17) 0.0028(16)
C9 0.030(2) 0.044(3) 0.043(3) -0.008(2) 0.0053(19) 0.0005(19)
C10 0.039(2) 0.026(2) 0.041(2) -0.0047(18) 0.0054(19) -0.0010(17)
C11 0.034(2) 0.029(2) 0.027(2) -0.0006(16) 0.0080(17) -0.0004(17)
S1 0.0392(6) 0.0367(6) 0.0557(8) -0.0106(5) 0.0126(5) -0.0124(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.052(3) . ?
Ni1 O1 2.072(3) . ?
Ni1 Cl2A 2.3472(10) . ?
Ni1 Cl1A 2.4263(10) . ?
Ni1 Cl1A 2.4700(10) 15_655 ?
Ni1 Cl1A 2.5042(9) 10_576 ?
Cl1A Ni1 2.4700(10) 10_576 ?
Cl1A Ni1 2.5042(9) 15_655 ?
N1 C7 1.332(6) . ?
N1 C3 1.364(5) . ?
O1 C1 1.459(4) . ?
O1 H1O 0.896(10) . ?
C1 C11 1.530(6) . ?
C1 C8 1.536(6) . ?
C1 C2 1.539(5) . ?
C2 C3 1.505(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.382(6) . ?
C4 C5 1.363(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.519(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 S1 1.809(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.530(6) . ?
C10 S1 1.803(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?

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 Ni1 O1 92.79(12) . . ?
N1 Ni1 Cl2A 94.36(9) . . ?
O1 Ni1 Cl2A 95.99(8) . . ?
N1 Ni1 Cl1A 173.90(9) . . ?
O1 Ni1 Cl1A 86.25(8) . . ?
Cl2A Ni1 Cl1A 91.73(3) . . ?
N1 Ni1 Cl1A 94.70(10) . 15_655 ?
O1 Ni1 Cl1A 169.70(8) . 15_655 ?
Cl2A Ni1 Cl1A 90.49(3) . 15_655 ?
Cl1A Ni1 Cl1A 85.56(3) . 15_655 ?
N1 Ni1 Cl1A 89.17(9) . 10_576 ?
O1 Ni1 Cl1A 90.50(8) . 10_576 ?
Cl2A Ni1 Cl1A 172.44(4) . 10_576 ?
Cl1A Ni1 Cl1A 84.81(3) . 10_576 ?
Cl1A Ni1 Cl1A 82.55(3) 15_655 10_576 ?
Ni1 Cl1A Ni1 94.75(3) . 10_576 ?
Ni1 Cl1A Ni1 93.88(3) . 15_655 ?
Ni1 Cl1A Ni1 97.43(3) 10_576 15_655 ?
C7 N1 C3 118.6(4) . . ?
C7 N1 Ni1 118.2(3) . . ?
C3 N1 Ni1 123.2(3) . . ?
C1 O1 Ni1 121.5(2) . . ?
C1 O1 H1O 112(3) . . ?
Ni1 O1 H1O 104(3) . . ?
O1 C1 C11 106.4(3) . . ?
O1 C1 C8 108.1(3) . . ?
C11 C1 C8 112.4(3) . . ?
O1 C1 C2 109.1(3) . . ?
C11 C1 C2 111.5(3) . . ?
C8 C1 C2 109.2(3) . . ?
C3 C2 C1 116.0(3) . . ?
C3 C2 H2A 108.3 . . ?
C1 C2 H2A 108.3 . . ?
C3 C2 H2B 108.3 . . ?
C1 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?
N1 C3 C4 120.4(4) . . ?
N1 C3 C2 118.9(3) . . ?
C4 C3 C2 120.7(4) . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 117.8(5) . . ?
C7 C6 H6 121.1 . . ?
C5 C6 H6 121.1 . . ?
N1 C7 C6 123.3(4) . . ?
N1 C7 H7 118.3 . . ?
C6 C7 H7 118.3 . . ?
C9 C8 C1 114.9(3) . . ?
C9 C8 H8A 108.6 . . ?
C1 C8 H8A 108.6 . . ?
C9 C8 H8B 108.6 . . ?
C1 C8 H8B 108.6 . . ?
H8A C8 H8B 107.5 . . ?
C8 C9 S1 112.0(3) . . ?
C8 C9 H9A 109.2 . . ?
S1 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
S1 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C11 C10 S1 113.0(3) . . ?
C11 C10 H10A 109.0 . . ?
S1 C10 H10A 109.0 . . ?
C11 C10 H10B 109.0 . . ?
S1 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C10 C11 C1 114.4(4) . . ?
C10 C11 H11A 108.7 . . ?
C1 C11 H11A 108.7 . . ?
C10 C11 H11B 108.7 . . ?
C1 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C10 S1 C9 96.9(2) . . ?


_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.104
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 -0.004 -0.004 -0.003 1825 519 ' '
_platon_squeeze_details          
;


;

_database_code_depnum_ccdc_archive 'CCDC 964329'
