# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


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#                                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. 
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data_n0009
_database_code_depnum_ccdc_archive 'CCDC 893527'
#TrackingRef 'n0009forpub.txt'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C160 H80 N8 O48 Zn8, 13(C3 H4 N O)'
_chemical_formula_sum            'C199 H219 N21 O61 Zn8'
_chemical_formula_weight         4403.91
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/m
_symmetry_space_group_name_Hall  '-C 2y'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
_cell_length_a                   14.8149(18)
_cell_length_b                   54.114(6)
_cell_length_c                   9.2584(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.055(9)
_cell_angle_gamma                90.00
_cell_volume                     6972.3(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    810
_cell_measurement_theta_min      6.92
_cell_measurement_theta_max      61.68
_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.036
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2288
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8491
_exptl_absorpt_correction_T_max  0.9700
_exptl_absorpt_process_details   'Face-indexed XPREP'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16614
_diffrn_reflns_av_R_equivalents  0.3128
_diffrn_reflns_av_sigmaI/netI    0.4783
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_k_max       64
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         6.92
_diffrn_reflns_theta_max         67.85
_reflns_number_total             6017
_reflns_number_gt                1187
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Various distance restraints were applied to the atoms of the disordered
benzenecarboxylate groups. The phenyl rings were subjected to FLAT
restraints. An isotropic restraint was used to keep the displacement
parameter for O7 reasonable.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1062P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6017
_refine_ls_number_parameters     357
_refine_ls_number_restraints     419
_refine_ls_R_factor_all          0.2304
_refine_ls_R_factor_gt           0.0953
_refine_ls_wR_factor_ref         0.2623
_refine_ls_wR_factor_gt          0.2167
_refine_ls_goodness_of_fit_ref   0.622
_refine_ls_restrained_S_all      0.618
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn -0.08344(10) 0.32452(3) -0.17761(13) 0.0558(5) Uani 1 1 d U . .
O1 O -0.1509(5) 0.32116(15) -0.3957(6) 0.068(2) Uani 1 1 d U . .
O2 O -0.1826(5) 0.28304(14) -0.3327(7) 0.064(2) Uani 1 1 d U . .
O3 O -0.0312(6) 0.35802(12) -0.1309(8) 0.078(2) Uani 1 1 d U . .
O4 O -0.1532(4) 0.31534(12) -0.0395(6) 0.0536(18) Uani 1 1 d U . .
O5 O 0.0294(4) 0.30382(12) -0.1626(7) 0.0550(18) Uani 1 1 d U . .
N1 N -0.4281(5) 0.27069(16) -0.9181(7) 0.049(2) Uani 1 1 d U . .
C1 C -0.1835(8) 0.2993(3) -0.4272(12) 0.065(3) Uani 1 1 d U . .
C2 C -0.2177(7) 0.29384(18) -0.5964(10) 0.050(2) Uani 1 1 d U . .
C3 C -0.3085(7) 0.28283(19) -0.6741(10) 0.054(3) Uani 1 1 d U . .
C4 C -0.3350(7) 0.28029(18) -0.8324(9) 0.050(2) Uani 1 1 d U . .
C5 C -0.2736(7) 0.28609(18) -0.9188(9) 0.050(2) Uani 1 1 d U . .
C6 C -0.1850(7) 0.29699(18) -0.8350(9) 0.049(2) Uani 1 1 d U . .
C7 C -0.1563(7) 0.29960(18) -0.6798(9) 0.056(3) Uani 1 1 d U . .
H7A H -0.0933 0.3055 -0.6257 0.067 Uiso 1 1 calc R . .
C8 C -0.3761(7) 0.27570(19) -0.5943(10) 0.058(3) Uani 1 1 d U . .
H8A H -0.4408 0.2816 -0.6534 0.087 Uiso 1 1 calc R . .
H8B H -0.3551 0.2831 -0.4915 0.087 Uiso 1 1 calc R . .
H8C H -0.3770 0.2577 -0.5852 0.087 Uiso 1 1 calc R . .
C9 C -0.3100(7) 0.28146(19) -1.0922(8) 0.057(3) Uani 1 1 d U . .
H9A H -0.3411 0.2652 -1.1139 0.086 Uiso 1 1 calc R . .
H9B H -0.2558 0.2819 -1.1300 0.086 Uiso 1 1 calc R . .
H9C H -0.3565 0.2943 -1.1440 0.086 Uiso 1 1 calc R . .
C10 C -0.4549(6) 0.2458(2) -0.9480(9) 0.058(3) Uani 1 1 d U . .
H10A H -0.4171 0.2317 -0.9039 0.087 Uiso 1 1 calc R . .
C11 C -0.5000 0.2871(3) -1.0000 0.050(3) Uani 1 2 d SU . .
C12 C 0.0000 0.3676(3) 0.0000 0.085(5) Uani 1 2 d SU . .
C13 C 0.0000 0.3950(3) 0.0000 0.109(7) Uani 1 2 d SU . .
C14 C -0.0384(12) 0.4080(2) -0.1387(13) 0.133(6) Uani 1 1 d U . .
H14A H -0.0638 0.3995 -0.2339 0.159 Uiso 1 1 calc R . .
C15 C -0.0380(14) 0.4338(3) -0.1327(15) 0.165(7) Uani 1 1 d U . .
H15A H -0.0654 0.4429 -0.2252 0.198 Uiso 1 1 calc R . .
C16 C 0.0000 0.4459(4) 0.0000 0.144(8) Uani 1 2 d SU . .
C17 C 0.0000 0.4745(4) 0.0000 0.127(7) Uani 1 2 d SU . .
C18 C -0.086(3) 0.4867(5) -0.078(4) 0.137(9) Uani 0.50 1 d PU . 1
C18' C -0.044(3) 0.4856(5) 0.079(3) 0.122(8) Uani 0.50 1 d PU . 2
C19 C -0.1176(7) 0.30562(19) 0.0899(10) 0.055(3) Uani 1 1 d U . .
C20 C -0.174(2) 0.4779(10) -0.138(5) 0.189(16) Uani 0.25 1 d PGDU . 1
C21 C -0.244(3) 0.4941(6) -0.227(5) 0.207(18) Uani 0.25 1 d PGDU . 1
C22 C -0.329(3) 0.4848(5) -0.329(5) 0.204(19) Uani 0.25 1 d PGDU . 1
C23 C -0.3452(16) 0.4595(5) -0.342(3) 0.206(17) Uani 0.25 1 d PGDU . 1
C24 C -0.275(2) 0.4433(5) -0.252(5) 0.27(2) Uani 0.25 1 d PGDU . 1
C25 C -0.189(2) 0.4526(9) -0.150(5) 0.26(2) Uani 0.25 1 d PGDU . 1
C26 C -0.4137(14) 0.4396(5) -0.423(5) 0.200(16) Uani 0.25 1 d PDU . 1
O6 O -0.5000 0.4476(5) -0.5000 0.236(15) Uani 0.50 2 d SPDU . 1
O7 O -0.3810(15) 0.4201(4) -0.449(3) 0.066(7) Uani 0.25 1 d PDU . 1
C20' C -0.107(3) 0.4711(7) 0.152(4) 0.140(11) Uani 0.25 1 d PGDU . 2
C21' C -0.079(2) 0.4790(6) 0.304(5) 0.146(13) Uani 0.25 1 d PGDU . 2
C22' C -0.126(2) 0.4700(6) 0.401(4) 0.147(13) Uani 0.25 1 d PGDU . 2
C23' C -0.2005(18) 0.4531(4) 0.345(3) 0.147(13) Uani 0.25 1 d PGDU . 2
C24' C -0.228(2) 0.4452(5) 0.193(3) 0.138(12) Uani 0.25 1 d PGDU . 2
C25' C -0.182(3) 0.4542(7) 0.097(3) 0.148(13) Uani 0.25 1 d PGDU . 2
C26' C -0.269(2) 0.4392(6) 0.401(4) 0.148(15) Uani 0.25 1 d PGDU . 2
O6' O -0.324(2) 0.4240(7) 0.303(5) 0.22(2) Uani 0.25 1 d PDU . 2
O7' O -0.264(3) 0.4418(9) 0.534(4) 0.23(2) Uani 0.25 1 d PDU . 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0567(8) 0.0786(10) 0.0257(6) -0.0039(8) 0.0058(5) -0.0057(9)
O1 0.080(5) 0.090(5) 0.014(3) -0.004(4) -0.011(3) 0.004(5)
O2 0.066(5) 0.093(6) 0.027(3) 0.000(4) 0.006(4) 0.007(4)
O3 0.126(7) 0.040(4) 0.057(5) -0.005(3) 0.014(5) -0.023(4)
O4 0.053(4) 0.080(5) 0.027(3) 0.000(3) 0.013(3) -0.007(3)
O5 0.034(4) 0.066(4) 0.049(4) -0.001(4) -0.006(3) 0.009(3)
N1 0.058(5) 0.070(5) 0.009(3) -0.002(4) -0.003(3) -0.011(4)
C1 0.065(7) 0.092(8) 0.033(5) -0.005(5) 0.010(5) 0.012(6)
C2 0.061(6) 0.052(6) 0.020(4) 0.000(4) -0.006(4) 0.015(5)
C3 0.052(6) 0.071(7) 0.027(4) 0.009(5) -0.002(4) 0.007(5)
C4 0.053(5) 0.063(6) 0.014(4) -0.004(4) -0.015(3) -0.003(5)
C5 0.061(6) 0.054(6) 0.020(4) -0.006(5) -0.006(4) 0.004(5)
C6 0.048(5) 0.064(7) 0.020(4) -0.006(5) -0.007(4) 0.008(5)
C7 0.058(6) 0.070(7) 0.019(4) 0.014(5) -0.013(4) -0.003(5)
C8 0.062(6) 0.080(8) 0.025(5) -0.007(5) 0.005(5) -0.002(6)
C9 0.051(6) 0.095(9) 0.013(4) 0.009(5) -0.005(4) -0.010(6)
C10 0.066(7) 0.076(6) 0.025(6) -0.009(5) 0.005(5) -0.008(5)
C11 0.041(7) 0.097(9) 0.005(6) 0.000 0.000(5) 0.000
C12 0.122(14) 0.068(7) 0.044(8) 0.000 0.002(10) 0.000
C13 0.178(17) 0.067(7) 0.040(8) 0.000 -0.018(11) 0.000
C14 0.233(15) 0.067(6) 0.047(7) 0.000(5) -0.018(9) -0.022(10)
C15 0.303(18) 0.063(7) 0.062(9) 0.007(6) -0.024(11) 0.002(12)
C16 0.26(2) 0.063(9) 0.058(10) 0.000 -0.007(14) 0.000
C17 0.208(18) 0.066(9) 0.089(15) 0.000 0.026(13) 0.000
C18 0.196(19) 0.088(14) 0.115(19) 0.003(15) 0.038(18) 0.010(11)
C18' 0.18(2) 0.067(14) 0.099(17) 0.023(12) 0.027(14) 0.018(13)
C19 0.059(7) 0.074(8) 0.017(4) -0.012(5) -0.007(4) 0.004(6)
C20 0.20(2) 0.13(2) 0.21(3) -0.07(3) 0.03(3) 0.008(18)
C21 0.18(3) 0.15(2) 0.25(4) -0.09(3) 0.02(3) 0.02(2)
C22 0.18(3) 0.15(2) 0.24(4) -0.09(3) 0.03(3) 0.01(2)
C23 0.16(2) 0.14(2) 0.29(4) -0.13(2) 0.04(3) 0.034(18)
C24 0.23(3) 0.15(2) 0.31(4) -0.05(3) -0.04(3) -0.02(2)
C25 0.26(3) 0.14(2) 0.28(4) -0.04(3) -0.04(3) -0.03(2)
C26 0.10(2) 0.14(2) 0.35(4) -0.08(2) 0.06(3) 0.023(12)
O6 0.070(16) 0.18(2) 0.46(4) 0.000 0.09(2) 0.000
O7 0.066(7) 0.066(7) 0.066(7) 0.0005(10) 0.023(3) -0.0006(10)
C20' 0.20(3) 0.08(2) 0.12(2) 0.04(2) 0.034(19) 0.014(18)
C21' 0.22(3) 0.09(3) 0.12(2) 0.06(2) 0.04(2) 0.00(2)
C22' 0.20(3) 0.09(3) 0.15(2) 0.03(2) 0.06(2) 0.00(2)
C23' 0.17(3) 0.09(3) 0.16(2) 0.06(2) 0.03(2) 0.024(19)
C24' 0.16(3) 0.06(3) 0.17(3) 0.04(2) 0.03(2) 0.039(19)
C25' 0.21(3) 0.06(3) 0.16(3) 0.04(2) 0.04(2) 0.017(19)
C26' 0.11(3) 0.14(3) 0.17(3) 0.01(3) 0.02(3) 0.02(2)
O6' 0.13(4) 0.11(3) 0.32(4) 0.00(3) -0.04(3) 0.02(2)
O7' 0.14(3) 0.36(6) 0.13(3) 0.12(3) -0.01(2) 0.04(4)
_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
Zn1 O1 1.930(5) . ?
Zn1 O3 1.960(7) . ?
Zn1 O4 1.964(6) . ?
Zn1 O5 1.978(6) . ?
O1 C1 1.272(13) . ?
O2 C1 1.239(12) . ?
O3 C12 1.252(9) . ?
O4 C19 1.247(10) . ?
O5 C19 1.251(10) 2 ?
N1 C11 1.395(11) . ?
N1 C10 1.406(11) . ?
N1 C4 1.432(10) . ?
C1 C2 1.501(12) . ?
C2 C7 1.415(12) . ?
C2 C3 1.421(12) . ?
C3 C4 1.387(11) . ?
C3 C8 1.485(12) . ?
C4 C5 1.439(13) . ?
C5 C6 1.405(12) . ?
C5 C9 1.529(10) . ?
C6 C7 1.359(11) . ?
C6 C19 1.474(13) 1_554 ?
C7 H7A 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C10 1.354(16) 2_453 ?
C10 H10A 0.9500 . ?
C11 N1 1.395(11) 2_453 ?
C12 O3 1.252(9) 2 ?
C12 C13 1.48(2) . ?
C13 C14 1.401(13) . ?
C13 C14 1.401(13) 2 ?
C14 C15 1.398(16) . ?
C14 H14A 0.9500 . ?
C15 C16 1.336(14) . ?
C15 H15A 0.9500 . ?
C16 C15 1.336(14) 2 ?
C16 C17 1.55(3) . ?
C17 C18' 1.29(3) . ?
C17 C18' 1.29(3) 2 ?
C17 C18 1.39(3) . ?
C17 C18 1.39(3) 2 ?
C18 C20 1.32(4) . ?
C18 C18 1.44(5) 6_565 ?
C18' C20' 1.54(4) . ?
C18' C18' 1.56(5) 6_565 ?
C19 O5 1.251(10) 2 ?
C19 C6 1.475(13) 1_556 ?
C20 C21 1.3900 . ?
C20 C25 1.3900 . ?
C20 C21 1.86(5) 6_565 ?
C21 C21 0.64(7) 6_565 ?
C21 C22 1.3900 . ?
C21 C22 1.73(3) 6_565 ?
C21 C20 1.86(6) 6_565 ?
C22 C23 1.3900 . ?
C22 C22 1.64(5) 6_565 ?
C22 C21 1.73(4) 6_565 ?
C23 C24 1.3900 . ?
C23 C26 1.492(12) . ?
C24 C25 1.3900 . ?
C26 O7 1.223(14) . ?
C26 O6 1.305(15) . ?
O6 C26 1.305(15) 2_454 ?
C20' C21' 1.3900 . ?
C20' C25' 1.3900 . ?
C21' C22' 1.3900 . ?
C22' C23' 1.3900 . ?
C23' C24' 1.3900 . ?
C23' C26' 1.4886 . ?
C24' C25' 1.3900 . ?
C26' O7' 1.216(13) . ?
C26' O6' 1.292(14) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O3 110.0(3) . . ?
O1 Zn1 O4 117.3(3) . . ?
O3 Zn1 O4 110.3(3) . . ?
O1 Zn1 O5 98.2(3) . . ?
O3 Zn1 O5 104.3(3) . . ?
O4 Zn1 O5 115.6(3) . . ?
C1 O1 Zn1 110.3(7) . . ?
C12 O3 Zn1 125.7(9) . . ?
C19 O4 Zn1 126.0(7) . . ?
C19 O5 Zn1 134.0(7) 2 . ?
C11 N1 C10 113.2(8) . . ?
C11 N1 C4 118.7(9) . . ?
C10 N1 C4 127.6(8) . . ?
O2 C1 O1 126.0(10) . . ?
O2 C1 C2 121.0(11) . . ?
O1 C1 C2 112.9(10) . . ?
C7 C2 C3 119.4(8) . . ?
C7 C2 C1 118.4(9) . . ?
C3 C2 C1 122.3(10) . . ?
C4 C3 C2 116.9(10) . . ?
C4 C3 C8 120.3(9) . . ?
C2 C3 C8 122.6(9) . . ?
C3 C4 N1 119.4(10) . . ?
C3 C4 C5 124.2(9) . . ?
N1 C4 C5 116.4(7) . . ?
C6 C5 C4 115.7(8) . . ?
C6 C5 C9 125.1(9) . . ?
C4 C5 C9 119.0(8) . . ?
C7 C6 C5 121.4(10) . . ?
C7 C6 C19 116.7(9) . 1_554 ?
C5 C6 C19 121.8(8) . 1_554 ?
C6 C7 C2 121.9(9) . . ?
C6 C7 H7A 119.1 . . ?
C2 C7 H7A 119.1 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 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 . . ?
C10 C10 N1 106.4(5) 2_453 . ?
C10 C10 H10A 126.8 2_453 . ?
N1 C10 H10A 126.8 . . ?
N1 C11 N1 100.8(12) 2_453 . ?
O3 C12 O3 131.0(17) 2 . ?
O3 C12 C13 114.5(8) 2 . ?
O3 C12 C13 114.5(8) . . ?
C14 C13 C14 120.0(17) . 2 ?
C14 C13 C12 120.0(9) . . ?
C14 C13 C12 120.0(9) 2 . ?
C15 C14 C13 117.9(13) . . ?
C15 C14 H14A 121.0 . . ?
C13 C14 H14A 121.0 . . ?
C16 C15 C14 121.5(15) . . ?
C16 C15 H15A 119.2 . . ?
C14 C15 H15A 119.2 . . ?
C15 C16 C15 121(2) 2 . ?
C15 C16 C17 119.5(10) 2 . ?
C15 C16 C17 119.5(10) . . ?
C18' C17 C18' 125(4) . 2 ?
C18' C17 C18 61.6(17) . . ?
C18' C17 C18 92(2) 2 . ?
C18' C17 C18 92(2) . 2 ?
C18' C17 C18 61.6(17) 2 2 ?
C18 C17 C18 124(3) . 2 ?
C18' C17 C16 117.7(18) . . ?
C18' C17 C16 117.7(18) 2 . ?
C18 C17 C16 118.1(16) . . ?
C18 C17 C16 118.1(16) 2 . ?
C20 C18 C17 130(4) . . ?
C20 C18 C18 111(3) . 6_565 ?
C17 C18 C18 118.1(16) . 6_565 ?
C17 C18' C20' 121(3) . . ?
C17 C18' C18' 117.7(18) . 6_565 ?
C20' C18' C18' 120.6(17) . 6_565 ?
O4 C19 O5 124.7(11) . 2 ?
O4 C19 C6 117.0(9) . 1_556 ?
O5 C19 C6 118.2(8) 2 1_556 ?
C18 C20 C21 117(4) . . ?
C18 C20 C25 120(4) . . ?
C21 C20 C25 120.0 . . ?
C18 C20 C21 102(5) . 6_565 ?
C21 C20 C21 15.6(12) . 6_565 ?
C25 C20 C21 135.6(12) . 6_565 ?
C21 C21 C20 128.88(6) 6_565 . ?
C21 C21 C22 111.07(7) 6_565 . ?
C20 C21 C22 120.0 . . ?
C21 C21 C22 48.6(13) 6_565 6_565 ?
C20 C21 C22 176.8(10) . 6_565 ?
C22 C21 C22 62.5(13) . 6_565 ?
C21 C21 C20 36(3) 6_565 6_565 ?
C20 C21 C20 93(3) . 6_565 ?
C22 C21 C20 147(3) . 6_565 ?
C22 C21 C20 84(3) 6_565 6_565 ?
C23 C22 C21 120.0 . . ?
C23 C22 C22 170.8 . 6_565 ?
C21 C22 C22 68.9 . 6_565 ?
C23 C22 C21 140.3(16) . 6_565 ?
C21 C22 C21 20.3(17) . 6_565 ?
C22 C22 C21 48.6(17) 6_565 6_565 ?
C22 C23 C24 120.0 . . ?
C22 C23 C26 144.9(17) . . ?
C24 C23 C26 95.0(17) . . ?
C25 C24 C23 120.0 . . ?
C24 C25 C20 120.0 . . ?
O7 C26 O6 123.9(18) . . ?
O7 C26 C23 118.4(15) . . ?
O6 C26 C23 114.0(17) . . ?
C26 O6 C26 141(3) 2_454 . ?
C21' C20' C25' 120.0 . . ?
C21' C20' C18' 106(3) . . ?
C25' C20' C18' 134(3) . . ?
C22' C21' C20' 120.0 . . ?
C21' C22' C23' 120.0 . . ?
C24' C23' C22' 120.0 . . ?
C24' C23' C26' 101.2 . . ?
C22' C23' C26' 138.8 . . ?
C25' C24' C23' 120.0 . . ?
C24' C25' C20' 120.0 . . ?
O7' C26' O6' 125.7(15) . . ?
O7' C26' C23' 119.3(14) . . ?
O6' C26' C23' 114.8(16) . . ?
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
O3 Zn1 O1 C1 178.8(7) . . . . ?
O4 Zn1 O1 C1 -54.2(8) . . . . ?
O5 Zn1 O1 C1 70.2(8) . . . . ?
O1 Zn1 O3 C12 165.6(7) . . . . ?
O4 Zn1 O3 C12 34.7(8) . . . . ?
O5 Zn1 O3 C12 -90.0(8) . . . . ?
O1 Zn1 O4 C19 145.4(8) . . . . ?
O3 Zn1 O4 C19 -87.7(8) . . . . ?
O5 Zn1 O4 C19 30.3(8) . . . . ?
O1 Zn1 O5 C19 139.6(9) . . . 2 ?
O3 Zn1 O5 C19 26.5(9) . . . 2 ?
O4 Zn1 O5 C19 -94.8(9) . . . 2 ?
Zn1 O1 C1 O2 7.6(15) . . . . ?
Zn1 O1 C1 C2 -167.6(7) . . . . ?
O2 C1 C2 C7 -126.1(12) . . . . ?
O1 C1 C2 C7 49.3(13) . . . . ?
O2 C1 C2 C3 53.0(15) . . . . ?
O1 C1 C2 C3 -131.6(11) . . . . ?
C7 C2 C3 C4 -5.3(14) . . . . ?
C1 C2 C3 C4 175.6(10) . . . . ?
C7 C2 C3 C8 178.5(9) . . . . ?
C1 C2 C3 C8 -0.5(16) . . . . ?
C2 C3 C4 N1 -176.3(9) . . . . ?
C8 C3 C4 N1 -0.1(15) . . . . ?
C2 C3 C4 C5 5.5(15) . . . . ?
C8 C3 C4 C5 -178.3(9) . . . . ?
C11 N1 C4 C3 102.2(10) . . . . ?
C10 N1 C4 C3 -86.8(12) . . . . ?
C11 N1 C4 C5 -79.5(10) . . . . ?
C10 N1 C4 C5 91.5(11) . . . . ?
C3 C4 C5 C6 -5.7(15) . . . . ?
N1 C4 C5 C6 176.0(9) . . . . ?
C3 C4 C5 C9 177.5(9) . . . . ?
N1 C4 C5 C9 -0.7(14) . . . . ?
C4 C5 C6 C7 6.0(15) . . . . ?
C9 C5 C6 C7 -177.5(9) . . . . ?
C4 C5 C6 C19 -175.5(9) . . . 1_554 ?
C9 C5 C6 C19 1.0(15) . . . 1_554 ?
C5 C6 C7 C2 -6.5(16) . . . . ?
C19 C6 C7 C2 174.9(9) 1_554 . . . ?
C3 C2 C7 C6 6.1(15) . . . . ?
C1 C2 C7 C6 -174.8(10) . . . . ?
C11 N1 C10 C10 0.6(13) . . . 2_453 ?
C4 N1 C10 C10 -170.8(9) . . . 2_453 ?
C10 N1 C11 N1 -0.2(5) . . . 2_453 ?
C4 N1 C11 N1 172.0(9) . . . 2_453 ?
Zn1 O3 C12 O3 22.5(5) . . . 2 ?
Zn1 O3 C12 C13 -157.5(5) . . . . ?
O3 C12 C13 C14 -176.3(9) 2 . . . ?
O3 C12 C13 C14 3.7(9) . . . . ?
O3 C12 C13 C14 3.7(9) 2 . . 2 ?
O3 C12 C13 C14 -176.3(9) . . . 2 ?
C14 C13 C14 C15 -0.9(13) 2 . . . ?
C12 C13 C14 C15 179.1(13) . . . . ?
C13 C14 C15 C16 2(3) . . . . ?
C14 C15 C16 C15 -1.0(14) . . . 2 ?
C14 C15 C16 C17 179.0(14) . . . . ?
C15 C16 C17 C18' -59.8(19) 2 . . . ?
C15 C16 C17 C18' 120.2(19) . . . . ?
C15 C16 C17 C18' 120.2(19) 2 . . 2 ?
C15 C16 C17 C18' -59.8(19) . . . 2 ?
C15 C16 C17 C18 -131(2) 2 . . . ?
C15 C16 C17 C18 49(2) . . . . ?
C15 C16 C17 C18 49(2) 2 . . 2 ?
C15 C16 C17 C18 -131(2) . . . 2 ?
C18' C17 C18 C20 -97(5) . . . . ?
C18' C17 C18 C20 134(5) 2 . . . ?
C18 C17 C18 C20 -169(5) 2 . . . ?
C16 C17 C18 C20 11(5) . . . . ?
C18' C17 C18 C18 72(2) . . . 6_565 ?
C18' C17 C18 C18 -56.8(17) 2 . . 6_565 ?
C18 C17 C18 C18 0.000(7) 2 . . 6_565 ?
C16 C17 C18 C18 180.000(7) . . . 6_565 ?
C18' C17 C18' C20' 171(3) 2 . . . ?
C18 C17 C18' C20' 100(4) . . . . ?
C18 C17 C18' C20' -132(3) 2 . . . ?
C16 C17 C18' C20' -9(3) . . . . ?
C18' C17 C18' C18' 0.004(7) 2 . . 6_565 ?
C18 C17 C18' C18' -71.2(18) . . . 6_565 ?
C18 C17 C18' C18' 56.5(16) 2 . . 6_565 ?
C16 C17 C18' C18' 180.002(8) . . . 6_565 ?
Zn1 O4 C19 O5 12.2(14) . . . 2 ?
Zn1 O4 C19 C6 -171.5(6) . . . 1_556 ?
C17 C18 C20 C21 -172(3) . . . . ?
C18 C18 C20 C21 18(4) 6_565 . . . ?
C17 C18 C20 C25 -11(5) . . . . ?
C18 C18 C20 C25 179.0(16) 6_565 . . . ?
C17 C18 C20 C21 -178(3) . . . 6_565 ?
C18 C18 C20 C21 12(3) 6_565 . . 6_565 ?
C18 C20 C21 C21 -22(4) . . . 6_565 ?
C25 C20 C21 C21 177.1 . . . 6_565 ?
C18 C20 C21 C22 161(4) . . . . ?
C25 C20 C21 C22 0.0 . . . . ?
C21 C20 C21 C22 -177.1 6_565 . . . ?
C18 C20 C21 C22 -60(17) . . . 6_565 ?
C25 C20 C21 C22 139(17) . . . 6_565 ?
C21 C20 C21 C22 -38(17) 6_565 . . 6_565 ?
C18 C20 C21 C20 -22(4) . . . 6_565 ?
C25 C20 C21 C20 177.1(19) . . . 6_565 ?
C21 C20 C21 C20 0.0(18) 6_565 . . 6_565 ?
C21 C21 C22 C23 -177.6 6_565 . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C22 C21 C22 C23 -177.6 6_565 . . . ?
C20 C21 C22 C23 -175(3) 6_565 . . . ?
C21 C21 C22 C22 0.0 6_565 . . 6_565 ?
C20 C21 C22 C22 177.6 . . . 6_565 ?
C20 C21 C22 C22 3(3) 6_565 . . 6_565 ?
C20 C21 C22 C21 177.62(6) . . . 6_565 ?
C22 C21 C22 C21 0.00(6) 6_565 . . 6_565 ?
C20 C21 C22 C21 3(3) 6_565 . . 6_565 ?
C21 C22 C23 C24 0.0 . . . . ?
C22 C22 C23 C24 -165.94(11) 6_565 . . . ?
C21 C22 C23 C24 -1.29(15) 6_565 . . . ?
C21 C22 C23 C26 -179(3) . . . . ?
C22 C22 C23 C26 15(3) 6_565 . . . ?
C21 C22 C23 C26 -180(3) 6_565 . . . ?
C22 C23 C24 C25 0.0 . . . . ?
C26 C23 C24 C25 179.2(17) . . . . ?
C23 C24 C25 C20 0.0 . . . . ?
C18 C20 C25 C24 -160(4) . . . . ?
C21 C20 C25 C24 0.0 . . . . ?
C21 C20 C25 C24 1.10(10) 6_565 . . . ?
C22 C23 C26 O7 145(3) . . . . ?
C24 C23 C26 O7 -33(4) . . . . ?
C22 C23 C26 O6 -14(6) . . . . ?
C24 C23 C26 O6 167(3) . . . . ?
O7 C26 O6 C26 30(4) . . . 2_454 ?
C23 C26 O6 C26 -172(4) . . . 2_454 ?
C17 C18' C20' C21' 132(3) . . . . ?
C18' C18' C20' C21' -57(2) 6_565 . . . ?
C17 C18' C20' C25' -52(4) . . . . ?
C18' C18' C20' C25' 119(2) 6_565 . . . ?
C25' C20' C21' C22' 0.0 . . . . ?
C18' C20' C21' C22' 177(2) . . . . ?
C20' C21' C22' C23' 0.0 . . . . ?
C21' C22' C23' C24' 0.0 . . . . ?
C21' C22' C23' C26' -179.3 . . . . ?
C22' C23' C24' C25' 0.0 . . . . ?
C26' C23' C24' C25' 179.5 . . . . ?
C23' C24' C25' C20' 0.0 . . . . ?
C21' C20' C25' C24' 0.0 . . . . ?
C18' C20' C25' C24' -176(3) . . . . ?
C24' C23' C26' O7' 180(3) . . . . ?
C22' C23' C26' O7' -1(3) . . . . ?
C24' C23' C26' O6' 4(2) . . . . ?
C22' C23' C26' O6' -176(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.938
_diffrn_reflns_theta_full        67.85
_diffrn_measured_fraction_theta_full 0.938
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.087
# 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 0.000 0.000 -0.014 1435 262 ' '
2 0.468 0.500 -0.010 1435 262 ' '
3 0.500 0.240 0.500 14 4 ' '
4 1.000 0.260 0.500 14 3 ' '
5 1.000 0.740 0.500 14 4 ' '
6 0.500 0.760 0.500 14 3 ' '
_platon_squeeze_details          
;
The proposed model was refined with contributions from the solvate,
dimethylformamide, removed from the diffraction data using the bypass
procedure in Platon (Spek, 1990). The total potential solvent accessible
void Volume was 2929.3 Ang^3^ and the electron count / cell = 538. This
corresponded to about 13 dimethylformamide molecules for the unit cell.
The "Squeeze" data are reported here.
;
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The reported formula reflects 13 DMF molecules removed via the
SQUEEZE program.
;
_vrf_RINTA01_I                   
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: Despite the poor quality of these data we are confident in our
model which is supported by other spectroscopic techniques.
;
_vrf_PLAT020_I                   
;
PROBLEM: The value of Rint is greater than 0.12 ......... 0.313
RESPONSE: see above.
;
_vrf_PLAT026_I                   
;
PROBLEM: Ratio Observed / Unique Reflections too Low .... 20 Perc.
RESPONSE: see above
;
_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.938
RESPONSE: see above
;
_vrf_PLAT043_I                   
;
PROBLEM: Check Reported Molecular Weight ................ 4403.91
RESPONSE: This value is off due to the use of SQUEEZE.
;
_vrf_PLAT044_I                   
;
PROBLEM: Calculated and Reported Dx Differ .............. ?
RESPONSE: This value is off due to the use of SQUEEZE.
;
_vrf_PLAT051_I                   
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 10.79 Perc.
RESPONSE: This value is off due to the use of SQUEEZE.
;
_vrf_PLAT430_I                   
;
PROBLEM: Short Inter D...A Contact O6 .. O7 .. 2.23 Ang.
RESPONSE: This is involving two atoms from different symmetry-generated parts.
This close contact is not present in the structure as is evidenced by the
disorder.
;


data_n0035s
_database_code_depnum_ccdc_archive 'CCDC 893528'
#TrackingRef 'n0035sforpub.txt'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H24 Br N2 O13 Zn2, 5(C3 H7 N O)'
_chemical_formula_sum            'C55 H59 Br N7 O18 Zn2'
_chemical_formula_weight         1316.74
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   9.2506(6)
_cell_length_b                   14.4032(10)
_cell_length_c                   27.384(2)
_cell_angle_alpha                97.587(6)
_cell_angle_beta                 93.139(6)
_cell_angle_gamma                106.920(5)
_cell_volume                     3443.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3258
_cell_measurement_theta_min      5.09
_cell_measurement_theta_max      49.60
_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1354
_exptl_absorpt_coefficient_mu    2.094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.709182
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13343
_diffrn_reflns_av_R_equivalents  0.0838
_diffrn_reflns_av_sigmaI/netI    0.1604
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.24
_diffrn_reflns_theta_max         50.26
_reflns_number_total             6665
_reflns_number_gt                3559
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Data were scaled for absorption and other effects using the program SADABS
(v2.03, Bruker).
Data for this compound were very weak and, though collected to a resolution of
at least 0.83Ang, no reflections above 3 sigma were evident past approximately
1.0Ang.
The thermal parameters for the tetra-acid group are large an indicate some
degree of disorder. Attempts to model this disorder did not result in any
significant improvement in the refinement. While the thermal parameters of
the other portions of this structure were subject to isotropic restraints,
the thermal parameters of the tetra-acid moiety were restrained only with
DELU and SIMU so as to better represent the suggested disorder.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0033(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6665
_refine_ls_number_parameters     516
_refine_ls_number_restraints     692
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0903
_refine_ls_wR_factor_ref         0.2452
_refine_ls_wR_factor_gt          0.2221
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_restrained_S_all      0.906
_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
Zn1 Zn 0.29683(13) 0.11710(9) 0.84991(5) 0.0336(5) Uani 1 1 d U . .
Zn2 Zn 0.11104(14) 0.28793(9) 0.84581(5) 0.0394(5) Uani 1 1 d U . .
Br1 Br 0.3376(3) 0.1376(3) 0.54973(9) 0.1977(15) Uani 1 1 d U . .
O1 O 0.4101(7) 0.2430(4) 0.8900(2) 0.0350(16) Uani 1 1 d U . .
O2 O 0.3256(7) 0.3618(4) 0.8655(3) 0.0382(16) Uani 1 1 d U . .
O3 O 0.2671(8) 0.1383(6) 0.7824(3) 0.062(2) Uani 1 1 d U . .
O4 O 0.0789(9) 0.2084(7) 0.7821(3) 0.071(2) Uani 1 1 d U . .
O5 O 0.0956(7) 0.0523(4) 0.8663(3) 0.0376(17) Uani 1 1 d U . .
O6 O 0.0279(7) 0.1859(5) 0.8893(2) 0.0383(16) Uani 1 1 d U . .
O7 O 0.4493(7) 0.0518(5) 0.8548(3) 0.0436(18) Uani 1 1 d U . .
O8 O 0.3768(7) 0.0448(4) 0.9315(3) 0.0373(18) Uani 1 1 d U . .
O9 O -0.0407(7) 0.3545(5) 0.8552(3) 0.0460(18) Uani 1 1 d U . .
O10 O 0.0812(7) 0.4139(4) 0.9308(2) 0.0350(17) Uani 1 1 d U . .
O11 O 0.1608(13) 0.3927(9) 0.7853(4) 0.125(3) Uani 1 1 d U . .
O12 O -0.592(3) -0.263(2) 0.6643(10) 0.295(13) Uani 1 1 d U . .
O13 O -0.702(2) -0.1625(17) 0.6519(9) 0.248(10) Uani 1 1 d U . .
N1 N 0.7469(8) 0.6670(5) 0.9598(3) 0.0247(17) Uani 1 1 d U . .
N2 N 0.7263(8) 0.8097(5) 0.9603(3) 0.0215(16) Uani 1 1 d U . .
C1 C 0.4242(11) 0.3309(7) 0.8862(4) 0.029(2) Uani 1 1 d U . .
C2 C 0.5709(10) 0.4037(6) 0.9050(3) 0.025(2) Uani 1 1 d U . .
C3 C 0.5870(10) 0.5038(6) 0.9260(3) 0.025(2) Uani 1 1 d U . .
C4 C 0.7355(10) 0.5644(6) 0.9393(4) 0.028(2) Uani 1 1 d U . .
C5 C 0.8666(10) 0.5373(7) 0.9346(3) 0.025(2) Uani 1 1 d U . .
C6 C 0.8492(11) 0.4437(7) 0.9125(4) 0.033(2) Uani 1 1 d U . .
C7 C 0.6975(10) 0.3774(7) 0.8983(4) 0.031(2) Uani 1 1 d U . .
H7A H 0.6867 0.3120 0.8834 0.037 Uiso 1 1 calc R . .
C8 C 0.4522(10) 0.5406(7) 0.9362(4) 0.033(3) Uani 1 1 d U . .
H8A H 0.4720 0.5819 0.9687 0.050 Uiso 1 1 calc R . .
H8B H 0.3613 0.4845 0.9357 0.050 Uiso 1 1 calc R . .
H8C H 0.4359 0.5792 0.9106 0.050 Uiso 1 1 calc R . .
C9 C 1.0192(11) 0.6114(7) 0.9497(4) 0.038(3) Uani 1 1 d U . .
H9A H 1.0945 0.5933 0.9298 0.057 Uiso 1 1 calc R . .
H9B H 1.0483 0.6128 0.9848 0.057 Uiso 1 1 calc R . .
H9C H 1.0146 0.6764 0.9443 0.057 Uiso 1 1 calc R . .
C10 C 0.7292(10) 0.7292(7) 0.9303(3) 0.024(2) Uani 1 1 d U . .
C11 C 0.7553(10) 0.7058(7) 1.0081(4) 0.026(2) Uani 1 1 d U . .
H11A H 0.7652 0.6748 1.0362 0.032 Uiso 1 1 calc R . .
C12 C 0.7467(9) 0.7988(6) 1.0081(4) 0.025(2) Uani 1 1 d U . .
H12A H 0.7538 0.8466 1.0363 0.030 Uiso 1 1 calc R . .
C13 C 0.7311(10) 0.8984(6) 0.9412(3) 0.0229(19) Uani 1 1 d U . .
C14 C 0.5946(10) 0.9217(7) 0.9349(3) 0.026(2) Uani 1 1 d U . .
C15 C 0.6036(10) 1.0035(7) 0.9132(4) 0.028(2) Uani 1 1 d U . .
C16 C 0.7376(11) 1.0591(7) 0.8988(4) 0.031(2) Uani 1 1 d U . .
H16A H 0.7389 1.1153 0.8839 0.037 Uiso 1 1 calc R . .
C17 C 0.8743(10) 1.0339(6) 0.9057(3) 0.027(2) Uani 1 1 d U . .
C18 C 0.8684(10) 0.9510(6) 0.9279(3) 0.023(2) Uani 1 1 d U . .
C19 C 0.4523(11) 0.8586(7) 0.9513(4) 0.039(3) Uani 1 1 d U . .
H19A H 0.3675 0.8834 0.9429 0.059 Uiso 1 1 calc R . .
H19B H 0.4651 0.8602 0.9872 0.059 Uiso 1 1 calc R . .
H19C H 0.4309 0.7909 0.9345 0.059 Uiso 1 1 calc R . .
C20 C 1.0110(10) 0.9207(7) 0.9376(4) 0.036(3) Uani 1 1 d U . .
H20A H 1.0137 0.9014 0.9706 0.054 Uiso 1 1 calc R . .
H20B H 1.1011 0.9761 0.9359 0.054 Uiso 1 1 calc R . .
H20C H 1.0099 0.8651 0.9126 0.054 Uiso 1 1 calc R . .
C21 C 0.1598(15) 0.1585(11) 0.7588(5) 0.069(3) Uani 1 1 d U . .
C22 C 0.1222(16) 0.1228(12) 0.7075(5) 0.082(4) Uani 1 1 d U . .
C23 C 0.0381(18) 0.1555(14) 0.6804(5) 0.106(5) Uani 1 1 d U . .
H23A H -0.0009 0.2050 0.6958 0.127 Uiso 1 1 calc R . .
C24 C 0.000(2) 0.1242(15) 0.6302(6) 0.126(6) Uani 1 1 d U . .
H24A H -0.0698 0.1476 0.6122 0.151 Uiso 1 1 calc R . .
C25 C 0.0629(19) 0.0603(15) 0.6078(5) 0.109(5) Uani 1 1 d U . .
C26 C 0.1393(18) 0.0138(14) 0.6356(6) 0.110(5) Uani 1 1 d U . .
H26A H 0.1684 -0.0407 0.6208 0.133 Uiso 1 1 calc R . .
C27 C 0.1722(16) 0.0471(13) 0.6845(5) 0.095(5) Uani 1 1 d U . .
H27A H 0.2308 0.0183 0.7038 0.114 Uiso 1 1 calc R . .
C28 C 0.028(2) 0.0312(18) 0.5522(6) 0.135(5) Uani 1 1 d U . .
C29 C -0.123(2) -0.0303(17) 0.5315(6) 0.127(5) Uani 1 1 d U . .
C30 C 0.150(2) 0.0661(19) 0.5210(6) 0.146(7) Uani 1 1 d U . .
C31 C -0.2391(14) -0.0725(11) 0.5647(4) 0.131(5) Uani 1 1 d GU . .
C32 C -0.3539(17) -0.0295(9) 0.5729(5) 0.143(6) Uani 1 1 d GU . .
H32A H -0.3524 0.0284 0.5597 0.172 Uiso 1 1 calc R . .
C33 C -0.4707(14) -0.0714(12) 0.6005(5) 0.145(6) Uani 1 1 d GU . .
H33A H -0.5491 -0.0420 0.6061 0.174 Uiso 1 1 calc R . .
C34 C -0.4728(15) -0.1562(12) 0.6198(5) 0.173(7) Uani 1 1 d GU . .
C35 C -0.3581(19) -0.1992(10) 0.6116(6) 0.181(7) Uani 1 1 d GU . .
H35A H -0.3595 -0.2571 0.6249 0.217 Uiso 1 1 calc R . .
C36 C -0.2412(15) -0.1573(12) 0.5841(5) 0.158(7) Uani 1 1 d GU . .
H36A H -0.1628 -0.1867 0.5784 0.190 Uiso 1 1 calc R . .
C37 C -0.589(4) -0.192(3) 0.6492(15) 0.226(10) Uani 1 1 d U . .
C38 C 1.0052(11) 1.0938(8) 0.8858(4) 0.031(2) Uani 1 1 d U . .
C39 C 0.4621(12) 0.0363(7) 0.9007(5) 0.036(2) Uani 1 1 d U . .
C40 C -0.0231(11) 0.4026(7) 0.9001(4) 0.030(2) Uani 1 1 d U . .
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
Zn1 0.0077(8) 0.0280(8) 0.0704(11) 0.0077(7) 0.0069(7) 0.0129(6)
Zn2 0.0084(8) 0.0301(9) 0.0817(12) -0.0007(7) 0.0026(7) 0.0133(6)
Br1 0.150(2) 0.304(4) 0.1062(19) -0.010(2) -0.0020(16) 0.038(2)
O1 0.019(4) 0.021(3) 0.064(4) 0.011(3) 0.002(3) 0.003(2)
O2 0.009(3) 0.026(3) 0.083(5) 0.006(3) 0.012(3) 0.010(2)
O3 0.032(4) 0.092(5) 0.060(4) 0.002(3) 0.001(3) 0.023(4)
O4 0.040(5) 0.121(5) 0.055(4) -0.007(3) -0.007(3) 0.041(4)
O5 0.013(3) 0.025(3) 0.074(5) 0.001(3) 0.007(3) 0.007(3)
O6 0.024(4) 0.022(4) 0.068(4) -0.001(3) -0.003(3) 0.010(3)
O7 0.026(4) 0.042(4) 0.070(4) -0.001(4) 0.009(3) 0.025(3)
O8 0.018(4) 0.027(4) 0.076(5) 0.004(3) 0.011(3) 0.021(3)
O9 0.025(4) 0.054(4) 0.067(4) 0.002(3) -0.014(3) 0.031(3)
O10 0.021(4) 0.034(4) 0.056(4) 0.009(3) 0.006(3) 0.017(3)
O11 0.118(7) 0.146(6) 0.122(6) 0.071(5) 0.018(4) 0.031(6)
O12 0.31(3) 0.35(3) 0.36(3) 0.21(2) 0.23(2) 0.20(2)
O13 0.197(18) 0.29(2) 0.34(2) 0.164(19) 0.170(18) 0.124(16)
N1 0.007(4) 0.022(3) 0.045(4) 0.001(3) -0.002(4) 0.006(3)
N2 0.0203(19) 0.0213(17) 0.0232(18) 0.0024(10) 0.0022(10) 0.0070(11)
C1 0.017(4) 0.027(3) 0.048(6) 0.005(4) 0.009(4) 0.011(3)
C2 0.020(3) 0.019(3) 0.041(5) 0.008(4) 0.003(4) 0.012(3)
C3 0.014(3) 0.021(4) 0.044(5) 0.005(4) 0.003(4) 0.011(3)
C4 0.015(3) 0.021(3) 0.052(5) 0.005(3) 0.004(4) 0.010(3)
C5 0.013(4) 0.025(4) 0.040(5) 0.004(4) 0.002(4) 0.009(3)
C6 0.023(4) 0.025(4) 0.055(6) 0.002(4) -0.001(5) 0.015(3)
C7 0.019(4) 0.019(4) 0.059(6) 0.004(4) 0.004(4) 0.012(3)
C8 0.014(4) 0.032(5) 0.058(6) 0.003(4) 0.004(5) 0.014(4)
C9 0.018(4) 0.032(5) 0.067(6) 0.005(5) 0.003(5) 0.013(4)
C10 0.008(5) 0.022(4) 0.044(4) 0.002(3) 0.003(4) 0.009(4)
C11 0.015(5) 0.033(4) 0.038(4) 0.013(3) 0.005(4) 0.015(4)
C12 0.008(5) 0.023(4) 0.040(4) 0.000(3) 0.003(4) 0.002(4)
C13 0.013(3) 0.016(4) 0.040(5) 0.001(3) 0.001(4) 0.007(3)
C14 0.017(4) 0.022(4) 0.042(5) -0.004(4) 0.006(4) 0.014(3)
C15 0.018(4) 0.023(4) 0.047(6) -0.003(4) 0.000(4) 0.018(4)
C16 0.022(4) 0.020(5) 0.053(6) 0.006(4) -0.006(4) 0.012(3)
C17 0.021(4) 0.015(4) 0.049(6) 0.003(4) 0.009(4) 0.012(3)
C18 0.014(4) 0.017(4) 0.040(5) 0.001(3) -0.002(4) 0.008(3)
C19 0.016(4) 0.035(5) 0.069(6) 0.004(4) 0.006(5) 0.012(4)
C20 0.021(4) 0.030(5) 0.061(6) 0.006(5) -0.006(5) 0.017(4)
C21 0.061(9) 0.103(10) 0.057(5) 0.003(6) 0.000(6) 0.049(7)
C22 0.062(9) 0.147(12) 0.057(5) 0.000(7) 0.001(6) 0.069(8)
C23 0.108(12) 0.191(15) 0.052(6) 0.006(8) 0.000(8) 0.103(11)
C24 0.124(13) 0.220(17) 0.065(7) -0.025(10) -0.024(9) 0.124(12)
C25 0.099(11) 0.197(15) 0.058(6) -0.002(7) 0.011(7) 0.095(9)
C26 0.094(11) 0.161(14) 0.084(7) -0.038(8) -0.028(9) 0.081(10)
C27 0.071(10) 0.160(13) 0.068(6) -0.016(7) -0.005(8) 0.073(9)
C28 0.119(7) 0.239(17) 0.060(6) -0.019(8) 0.003(6) 0.095(8)
C29 0.131(8) 0.213(16) 0.055(9) 0.031(9) -0.004(6) 0.077(8)
C30 0.115(8) 0.29(2) 0.038(8) 0.004(11) -0.013(6) 0.089(10)
C31 0.145(9) 0.208(14) 0.066(10) 0.024(9) 0.021(9) 0.091(8)
C32 0.107(13) 0.199(16) 0.141(15) 0.044(12) 0.009(9) 0.067(11)
C33 0.137(14) 0.192(17) 0.125(15) 0.030(11) 0.031(10) 0.073(13)
C34 0.173(15) 0.218(18) 0.177(17) 0.064(13) 0.090(12) 0.108(13)
C35 0.175(18) 0.207(17) 0.211(19) 0.070(13) 0.096(13) 0.104(14)
C36 0.163(15) 0.215(18) 0.145(16) 0.060(12) 0.070(11) 0.107(13)
C37 0.20(2) 0.28(3) 0.27(3) 0.129(18) 0.140(17) 0.123(18)
C38 0.021(4) 0.029(5) 0.040(6) 0.005(4) -0.007(4) 0.004(4)
C39 0.020(6) 0.023(6) 0.071(6) -0.001(6) 0.005(5) 0.021(5)
C40 0.011(6) 0.016(5) 0.066(6) 0.010(5) 0.004(4) 0.007(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
Zn1 O7 1.918(6) . ?
Zn1 O3 1.931(8) . ?
Zn1 O5 1.931(7) . ?
Zn1 O1 1.958(6) . ?
Zn2 O4 1.914(8) . ?
Zn2 O9 1.927(6) . ?
Zn2 O2 1.966(6) . ?
Zn2 O6 2.019(7) . ?
Zn2 O11 2.361(10) . ?
Br1 C30 1.81(2) . ?
O1 C1 1.254(10) . ?
O2 C1 1.264(11) . ?
O3 C21 1.279(13) . ?
O4 C21 1.313(13) . ?
O5 C38 1.264(11) 1_445 ?
O6 C38 1.270(11) 1_445 ?
O7 C39 1.310(12) . ?
O8 C39 1.204(12) . ?
O9 C40 1.305(11) . ?
O10 C40 1.203(11) . ?
O12 C37 1.15(3) . ?
O13 C37 1.24(3) . ?
N1 C10 1.320(11) . ?
N1 C11 1.357(11) . ?
N1 C4 1.481(11) . ?
N2 C10 1.339(10) . ?
N2 C12 1.348(11) . ?
N2 C13 1.433(11) . ?
C1 C2 1.469(13) . ?
C2 C7 1.347(12) . ?
C2 C3 1.442(12) . ?
C3 C4 1.395(13) . ?
C3 C8 1.516(12) . ?
C4 C5 1.385(12) . ?
C5 C6 1.363(12) . ?
C5 C9 1.497(13) . ?
C6 C7 1.447(13) . ?
C6 C40 1.504(13) 1_655 ?
C7 H7A 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.365(12) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 C18 1.372(12) . ?
C13 C14 1.405(12) . ?
C14 C15 1.371(12) . ?
C14 C19 1.495(13) . ?
C15 C16 1.377(13) . ?
C15 C39 1.551(13) 1_565 ?
C16 C17 1.423(13) . ?
C16 H16A 0.9500 . ?
C17 C18 1.400(12) . ?
C17 C38 1.448(13) . ?
C18 C20 1.526(12) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.420(17) . ?
C22 C23 1.272(17) . ?
C22 C27 1.393(18) . ?
C23 C24 1.382(18) . ?
C23 H23A 0.9500 . ?
C24 C25 1.331(19) . ?
C24 H24A 0.9500 . ?
C25 C26 1.37(2) . ?
C25 C28 1.52(2) . ?
C26 C27 1.348(18) . ?
C26 H26A 0.9500 . ?
C27 H27A 0.9500 . ?
C28 C29 1.45(3) . ?
C28 C30 1.46(3) . ?
C29 C30 1.44(2) 2_556 ?
C29 C31 1.49(2) . ?
C30 C29 1.44(2) 2_556 ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C32 C33 1.3900 . ?
C32 H32A 0.9500 . ?
C33 C34 1.3900 . ?
C33 H33A 0.9500 . ?
C34 C35 1.3900 . ?
C34 C37 1.39(3) . ?
C35 C36 1.3900 . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C38 O5 1.264(11) 1_665 ?
C38 O6 1.270(11) 1_665 ?
C39 C15 1.551(13) 1_545 ?
C40 C6 1.504(13) 1_455 ?
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
O7 Zn1 O3 109.2(3) . . ?
O7 Zn1 O5 118.4(3) . . ?
O3 Zn1 O5 104.6(3) . . ?
O7 Zn1 O1 98.0(3) . . ?
O3 Zn1 O1 108.4(3) . . ?
O5 Zn1 O1 117.9(3) . . ?
O4 Zn2 O9 112.1(3) . . ?
O4 Zn2 O2 113.0(3) . . ?
O9 Zn2 O2 119.0(3) . . ?
O4 Zn2 O6 101.4(3) . . ?
O9 Zn2 O6 96.0(3) . . ?
O2 Zn2 O6 112.7(3) . . ?
O4 Zn2 O11 71.6(4) . . ?
O9 Zn2 O11 78.8(4) . . ?
O2 Zn2 O11 78.8(4) . . ?
O6 Zn2 O11 168.4(4) . . ?
C1 O1 Zn1 133.8(6) . . ?
C1 O2 Zn2 126.5(6) . . ?
C21 O3 Zn1 132.0(8) . . ?
C21 O4 Zn2 132.5(8) . . ?
C38 O5 Zn1 126.2(6) 1_445 . ?
C38 O6 Zn2 135.0(7) 1_445 . ?
C39 O7 Zn1 107.0(6) . . ?
C40 O9 Zn2 111.1(6) . . ?
C10 N1 C11 111.5(7) . . ?
C10 N1 C4 120.6(8) . . ?
C11 N1 C4 127.3(8) . . ?
C10 N2 C12 110.5(7) . . ?
C10 N2 C13 120.8(8) . . ?
C12 N2 C13 127.5(7) . . ?
O1 C1 O2 125.7(9) . . ?
O1 C1 C2 117.2(8) . . ?
O2 C1 C2 117.0(8) . . ?
C7 C2 C3 118.4(8) . . ?
C7 C2 C1 117.7(8) . . ?
C3 C2 C1 123.6(8) . . ?
C4 C3 C2 115.9(8) . . ?
C4 C3 C8 121.3(8) . . ?
C2 C3 C8 122.7(8) . . ?
C5 C4 C3 126.4(8) . . ?
C5 C4 N1 119.6(8) . . ?
C3 C4 N1 114.0(7) . . ?
C6 C5 C4 116.8(8) . . ?
C6 C5 C9 122.7(8) . . ?
C4 C5 C9 120.4(8) . . ?
C5 C6 C7 119.1(8) . . ?
C5 C6 C40 125.1(9) . 1_655 ?
C7 C6 C40 115.8(8) . 1_655 ?
C2 C7 C6 123.3(8) . . ?
C2 C7 H7A 118.3 . . ?
C6 C7 H7A 118.3 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 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 . . ?
N1 C10 N2 105.6(8) . . ?
N1 C11 C12 105.5(8) . . ?
N1 C11 H11A 127.2 . . ?
C12 C11 H11A 127.2 . . ?
N2 C12 C11 106.8(8) . . ?
N2 C12 H12A 126.6 . . ?
C11 C12 H12A 126.6 . . ?
C18 C13 C14 125.3(8) . . ?
C18 C13 N2 116.6(7) . . ?
C14 C13 N2 118.0(8) . . ?
C15 C14 C13 115.5(8) . . ?
C15 C14 C19 124.4(8) . . ?
C13 C14 C19 120.1(8) . . ?
C14 C15 C16 122.1(8) . . ?
C14 C15 C39 122.4(9) . 1_565 ?
C16 C15 C39 115.4(8) . 1_565 ?
C15 C16 C17 121.1(8) . . ?
C15 C16 H16A 119.4 . . ?
C17 C16 H16A 119.4 . . ?
C18 C17 C16 117.9(8) . . ?
C18 C17 C38 126.0(9) . . ?
C16 C17 C38 116.0(8) . . ?
C13 C18 C17 118.0(8) . . ?
C13 C18 C20 121.1(8) . . ?
C17 C18 C20 120.9(8) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 O4 120.7(11) . . ?
O3 C21 C22 119.9(12) . . ?
O4 C21 C22 119.3(11) . . ?
C23 C22 C27 116.6(14) . . ?
C23 C22 C21 122.2(14) . . ?
C27 C22 C21 121.1(13) . . ?
C22 C23 C24 124.6(15) . . ?
C22 C23 H23A 117.7 . . ?
C24 C23 H23A 117.7 . . ?
C25 C24 C23 117.9(15) . . ?
C25 C24 H24A 121.1 . . ?
C23 C24 H24A 121.1 . . ?
C24 C25 C26 119.7(15) . . ?
C24 C25 C28 117.6(15) . . ?
C26 C25 C28 122.1(15) . . ?
C27 C26 C25 118.4(15) . . ?
C27 C26 H26A 120.8 . . ?
C25 C26 H26A 120.8 . . ?
C26 C27 C22 121.6(14) . . ?
C26 C27 H27A 119.2 . . ?
C22 C27 H27A 119.2 . . ?
C29 C28 C30 122.2(15) . . ?
C29 C28 C25 119.8(18) . . ?
C30 C28 C25 118.0(17) . . ?
C30 C29 C28 119.0(17) 2_556 . ?
C30 C29 C31 119.4(19) 2_556 . ?
C28 C29 C31 120.4(15) . . ?
C29 C30 C28 118.5(18) 2_556 . ?
C29 C30 Br1 121.3(15) 2_556 . ?
C28 C30 Br1 119.6(12) . . ?
C32 C31 C36 120.0 . . ?
C32 C31 C29 118.4(13) . . ?
C36 C31 C29 121.4(13) . . ?
C31 C32 C33 120.0 . . ?
C31 C32 H32A 120.0 . . ?
C33 C32 H32A 120.0 . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33A 120.0 . . ?
C34 C33 H33A 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 C37 118(2) . . ?
C35 C34 C37 122(2) . . ?
C36 C35 C34 120.0 . . ?
C36 C35 H35A 120.0 . . ?
C34 C35 H35A 120.0 . . ?
C35 C36 C31 120.0 . . ?
C35 C36 H36A 120.0 . . ?
C31 C36 H36A 120.0 . . ?
O12 C37 O13 118(4) . . ?
O12 C37 C34 117(3) . . ?
O13 C37 C34 123(3) . . ?
O5 C38 O6 122.0(9) 1_665 1_665 ?
O5 C38 C17 118.3(9) 1_665 . ?
O6 C38 C17 119.7(9) 1_665 . ?
O8 C39 O7 126.4(9) . . ?
O8 C39 C15 120.8(10) . 1_545 ?
O7 C39 C15 112.9(9) . 1_545 ?
O10 C40 O9 126.0(9) . . ?
O10 C40 C6 120.1(10) . 1_455 ?
O9 C40 C6 113.9(9) . 1_455 ?
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
O7 Zn1 O1 C1 139.3(8) . . . . ?
O3 Zn1 O1 C1 25.9(9) . . . . ?
O5 Zn1 O1 C1 -92.5(9) . . . . ?
O4 Zn2 O2 C1 -84.9(8) . . . . ?
O9 Zn2 O2 C1 140.4(7) . . . . ?
O6 Zn2 O2 C1 29.2(8) . . . . ?
O11 Zn2 O2 C1 -149.3(8) . . . . ?
O7 Zn1 O3 C21 162.7(11) . . . . ?
O5 Zn1 O3 C21 35.0(12) . . . . ?
O1 Zn1 O3 C21 -91.6(12) . . . . ?
O9 Zn2 O4 C21 173.1(12) . . . . ?
O2 Zn2 O4 C21 35.3(13) . . . . ?
O6 Zn2 O4 C21 -85.6(12) . . . . ?
O11 Zn2 O4 C21 103.9(13) . . . . ?
O7 Zn1 O5 C38 146.9(7) . . . 1_445 ?
O3 Zn1 O5 C38 -91.3(8) . . . 1_445 ?
O1 Zn1 O5 C38 29.1(9) . . . 1_445 ?
O4 Zn2 O6 C38 22.5(9) . . . 1_445 ?
O9 Zn2 O6 C38 136.5(9) . . . 1_445 ?
O2 Zn2 O6 C38 -98.5(9) . . . 1_445 ?
O11 Zn2 O6 C38 74(2) . . . 1_445 ?
O3 Zn1 O7 C39 -178.1(6) . . . . ?
O5 Zn1 O7 C39 -58.7(7) . . . . ?
O1 Zn1 O7 C39 69.2(7) . . . . ?
O4 Zn2 O9 C40 175.4(6) . . . . ?
O2 Zn2 O9 C40 -49.6(7) . . . . ?
O6 Zn2 O9 C40 70.6(6) . . . . ?
O11 Zn2 O9 C40 -119.9(7) . . . . ?
Zn1 O1 C1 O2 29.2(15) . . . . ?
Zn1 O1 C1 C2 -147.4(7) . . . . ?
Zn2 O2 C1 O1 13.3(14) . . . . ?
Zn2 O2 C1 C2 -170.1(6) . . . . ?
O1 C1 C2 C7 37.8(13) . . . . ?
O2 C1 C2 C7 -139.2(9) . . . . ?
O1 C1 C2 C3 -148.2(9) . . . . ?
O2 C1 C2 C3 34.9(13) . . . . ?
C7 C2 C3 C4 -2.3(13) . . . . ?
C1 C2 C3 C4 -176.3(9) . . . . ?
C7 C2 C3 C8 -178.6(9) . . . . ?
C1 C2 C3 C8 7.3(14) . . . . ?
C2 C3 C4 C5 -0.6(15) . . . . ?
C8 C3 C4 C5 175.8(9) . . . . ?
C2 C3 C4 N1 178.9(8) . . . . ?
C8 C3 C4 N1 -4.7(13) . . . . ?
C10 N1 C4 C5 102.4(10) . . . . ?
C11 N1 C4 C5 -86.8(11) . . . . ?
C10 N1 C4 C3 -77.2(11) . . . . ?
C11 N1 C4 C3 93.6(11) . . . . ?
C3 C4 C5 C6 3.7(15) . . . . ?
N1 C4 C5 C6 -175.8(9) . . . . ?
C3 C4 C5 C9 178.8(9) . . . . ?
N1 C4 C5 C9 -0.7(14) . . . . ?
C4 C5 C6 C7 -3.8(14) . . . . ?
C9 C5 C6 C7 -178.8(9) . . . . ?
C4 C5 C6 C40 174.6(10) . . . 1_655 ?
C9 C5 C6 C40 -0.4(16) . . . 1_655 ?
C3 C2 C7 C6 2.1(15) . . . . ?
C1 C2 C7 C6 176.5(9) . . . . ?
C5 C6 C7 C2 1.1(15) . . . . ?
C40 C6 C7 C2 -177.5(9) 1_655 . . . ?
C11 N1 C10 N2 0.0(10) . . . . ?
C4 N1 C10 N2 172.2(7) . . . . ?
C12 N2 C10 N1 1.9(10) . . . . ?
C13 N2 C10 N1 170.7(7) . . . . ?
C10 N1 C11 C12 -1.8(10) . . . . ?
C4 N1 C11 C12 -173.4(8) . . . . ?
C10 N2 C12 C11 -3.1(10) . . . . ?
C13 N2 C12 C11 -170.9(8) . . . . ?
N1 C11 C12 N2 2.9(9) . . . . ?
C10 N2 C13 C18 -74.2(11) . . . . ?
C12 N2 C13 C18 92.5(11) . . . . ?
C10 N2 C13 C14 102.3(10) . . . . ?
C12 N2 C13 C14 -91.0(11) . . . . ?
C18 C13 C14 C15 0.6(14) . . . . ?
N2 C13 C14 C15 -175.6(8) . . . . ?
C18 C13 C14 C19 -179.6(9) . . . . ?
N2 C13 C14 C19 4.2(13) . . . . ?
C13 C14 C15 C16 -0.1(13) . . . . ?
C19 C14 C15 C16 -179.9(9) . . . . ?
C13 C14 C15 C39 176.3(9) . . . 1_565 ?
C19 C14 C15 C39 -3.5(15) . . . 1_565 ?
C14 C15 C16 C17 0.0(15) . . . . ?
C39 C15 C16 C17 -176.7(9) 1_565 . . . ?
C15 C16 C17 C18 -0.3(14) . . . . ?
C15 C16 C17 C38 175.8(9) . . . . ?
C14 C13 C18 C17 -0.9(14) . . . . ?
N2 C13 C18 C17 175.3(8) . . . . ?
C14 C13 C18 C20 178.5(9) . . . . ?
N2 C13 C18 C20 -5.3(13) . . . . ?
C16 C17 C18 C13 0.7(13) . . . . ?
C38 C17 C18 C13 -174.9(9) . . . . ?
C16 C17 C18 C20 -178.7(8) . . . . ?
C38 C17 C18 C20 5.7(14) . . . . ?
Zn1 O3 C21 O4 29(2) . . . . ?
Zn1 O3 C21 C22 -147.5(11) . . . . ?
Zn2 O4 C21 O3 16(2) . . . . ?
Zn2 O4 C21 C22 -166.8(11) . . . . ?
O3 C21 C22 C23 -166.1(17) . . . . ?
O4 C21 C22 C23 17(2) . . . . ?
O3 C21 C22 C27 16(2) . . . . ?
O4 C21 C22 C27 -160.8(15) . . . . ?
C27 C22 C23 C24 -3(3) . . . . ?
C21 C22 C23 C24 179.2(18) . . . . ?
C22 C23 C24 C25 -5(3) . . . . ?
C23 C24 C25 C26 12(3) . . . . ?
C23 C24 C25 C28 -176.2(19) . . . . ?
C24 C25 C26 C27 -12(3) . . . . ?
C28 C25 C26 C27 176.9(18) . . . . ?
C25 C26 C27 C22 4(3) . . . . ?
C23 C22 C27 C26 3(3) . . . . ?
C21 C22 C27 C26 -178.8(16) . . . . ?
C24 C25 C28 C29 -71(3) . . . . ?
C26 C25 C28 C29 100(2) . . . . ?
C24 C25 C28 C30 110(2) . . . . ?
C26 C25 C28 C30 -79(3) . . . . ?
C30 C28 C29 C30 6(3) . . . 2_556 ?
C25 C28 C29 C30 -173.4(18) . . . 2_556 ?
C30 C28 C29 C31 173.9(19) . . . . ?
C25 C28 C29 C31 -6(3) . . . . ?
C29 C28 C30 C29 -6(3) . . . 2_556 ?
C25 C28 C30 C29 173.4(18) . . . 2_556 ?
C29 C28 C30 Br1 -176.9(17) . . . . ?
C25 C28 C30 Br1 3(3) . . . . ?
C30 C29 C31 C32 -89.0(19) 2_556 . . . ?
C28 C29 C31 C32 103.3(17) . . . . ?
C30 C29 C31 C36 86.0(18) 2_556 . . . ?
C28 C29 C31 C36 -82(2) . . . . ?
C36 C31 C32 C33 0.0 . . . . ?
C29 C31 C32 C33 175.1(14) . . . . ?
C31 C32 C33 C34 0.0 . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C32 C33 C34 C37 177(2) . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C37 C34 C35 C36 -177(3) . . . . ?
C34 C35 C36 C31 0.0 . . . . ?
C32 C31 C36 C35 0.0 . . . . ?
C29 C31 C36 C35 -174.9(15) . . . . ?
C33 C34 C37 O12 178(4) . . . . ?
C35 C34 C37 O12 -5(6) . . . . ?
C33 C34 C37 O13 12(5) . . . . ?
C35 C34 C37 O13 -171(3) . . . . ?
C18 C17 C38 O5 33.6(14) . . . 1_665 ?
C16 C17 C38 O5 -142.1(9) . . . 1_665 ?
C18 C17 C38 O6 -145.1(9) . . . 1_665 ?
C16 C17 C38 O6 39.2(13) . . . 1_665 ?
Zn1 O7 C39 O8 12.2(12) . . . . ?
Zn1 O7 C39 C15 -168.1(6) . . . 1_545 ?
Zn2 O9 C40 O10 7.3(12) . . . . ?
Zn2 O9 C40 C6 -171.3(6) . . . 1_455 ?
_diffrn_measured_fraction_theta_max 0.929
_diffrn_reflns_theta_full        50.26
_diffrn_measured_fraction_theta_full 0.929
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.116
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 0.008 0.464 0.500 1840 442 ' '
2 0.229 0.777 0.023 14 4 ' '
3 0.770 0.223 0.977 14 5 ' '
_platon_squeeze_details          
;
The proposed model was refined with contributions from the solvate,
dimethylformamide, removed from the diffraction data using the bypass
procedure in Platon (Spek, 1990). The total potential solvent accessible void
Volume was 1872.1 Ang^3^ and the electron count / cell = 451. This
corresponded to about 10 dimethylformamide molecules for the unit cell.
The "Squeeze" data are reported here.
;
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The reported formula includes solvent molecules that had been
"removed" via SQUEEZE.
;
_vrf_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Despite long exposure times, no significant intensity was observed
beyond approximately 1.0Ang resolution.
;
_vrf_PLAT023_I                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 50.26 Deg.
RESPONSE: see above.
;
_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.929
RESPONSE: see above.
;
_vrf_PLAT043_I                   
;
PROBLEM: Check Reported Molecular Weight ................ 1316.74
RESPONSE: The reported formula includes solvent molecules that had been
"removed" via SQUEEZE.
;
_vrf_PLAT044_I                   
;
PROBLEM: Calculated and Reported Dx Differ .............. ?
RESPONSE: The reported formula includes solvent molecules that had been
"removed" via SQUEEZE.
;
_vrf_PLAT051_I                   
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 10.44 Perc.
RESPONSE: The reported formula includes solvent molecules that had been
"removed" via SQUEEZE.
;
_vrf_PLAT213_I                   
;
PROBLEM: Atom Zn1 has ADP max/min Ratio ..... 6.4 prola
RESPONSE: Due to disorder inherent in this structure.
;