# 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_csh75
_database_code_depnum_ccdc_archive 'CCDC 1040598'
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_audit_creation_date             2014-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        '4-(3,5-dimethyl-1H-pyrazol-4-yl)benzoic acid'
_chemical_formula_moiety         'C12 H12 N2 O2'
_chemical_formula_sum            'C12 H12 N2 O2'
_chemical_formula_weight         216.24
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_symmetry_int_tables_number      ?
_cell_length_a                   9.6538(5)
_cell_length_b                   10.4193(6)
_cell_length_c                   21.9388(14)
_cell_angle_alpha                91.284(4)
_cell_angle_beta                 101.971(4)
_cell_angle_gamma                102.808(4)
_cell_volume                     2099.6(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2540
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.63
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0680 before and 0.0558 after correction.
The Ratio of minimum to maximum transmission is 0.8540.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.1106
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27642
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.15
_diffrn_reflns_theta_min         0.95
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_reflns_number_gt                5096
_reflns_number_total             10151
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.53A (Bruker, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XLMP (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         10151
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0540
_refine_ls_restrained_S_all      0.937
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0460P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1305
_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. 
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H2(0.045) H1(0.035) H2A(0.028) H3(0.028) H5(0.025) H6(0.025)
 H31D(0.043) H31E(0.043) H31F(0.043) H51D(0.045) H51E(0.045) H51F(0.045)
 H2B(0.05) H1B(0.034) H2BA(0.028) H3B(0.027) H5B(0.026) H6B(0.028) H31A(0.042)
 H31B(0.042) H31C(0.042) H51A(0.047) H51B(0.047) H51C(0.047) H2AA(0.045)
 H1A(0.034) H2AB(0.029) H3A(0.028) H5A(0.031) H6A(0.032) H31J(0.046)
 H31K(0.046) H31L(0.046) H51J(0.047) H51K(0.047) H51L(0.047) H2C(0.051)
 H1C(0.031) H2CA(0.028) H3C(0.028) H5C(0.026) H6C(0.026) H31G(0.039)
 H31H(0.039) H31I(0.039) H51G(0.04) H51H(0.04) H51I(0.04)
 Fixed X: H2A(0.0546) H3(-0.041) H5(0.096) H6(0.1973) H31D(0.1721)
 H31E(0.2271) H31F(0.1396) H51D(-0.3881) H51E(-0.3002) H51F(-0.268) H2BA(0.455)
 H3B(0.4774) H5B(0.4581) H6B(0.4443) H31A(0.5632) H31B(0.7032) H31C(0.6881)
 H51A(0.4277) H51B(0.3123) H51C(0.2854) H2AB(0.4406) H3A(0.345) H5A(0.7532)
 H6A(0.8474) H31J(0.7687) H31K(0.6932) H31L(0.6783) H51J(0.1823) H51K(0.2825)
 H51L(0.1751) H2CA(0.7623) H3C(0.7599) H5C(1.1514) H6C(1.1509) H31G(1.2032)
 H31H(1.051) H31I(1.1037) H51G(0.7323) H51H(0.8857) H51I(0.8172)
 Fixed Y: H2A(0.0421) H3(0.0403) H5(0.4381) H6(0.439) H31D(0.4284)
 H31E(0.3836) H31F(0.498) H51D(0.0504) H51E(0.0784) H51F(-0.03) H2BA(0.933)
 H3B(0.9282) H5B(0.536) H6B(0.5428) H31A(0.4606) H31B(0.531) H31C(0.572)
 H51A(0.9999) H51B(0.9248) H51C(0.8946) H2AB(0.1934) H3A(0.207) H5A(0.3327)
 H6A(0.3272) H31J(0.4191) H31K(0.51) H31L(0.5144) H51J(0.1167) H51K(0.0138)
 H51L(0.0376) H2CA(0.7944) H3C(0.7939) H5C(0.6967) H6C(0.6944) H31G(0.6134)
 H31H(0.5182) H31I(0.5251) H51G(0.9134) H51H(1.0138) H51I(0.9986)
 Fixed Z: H2A(0.2953) H3(0.1889) H5(0.1974) H6(0.3031) H31D(0.0347)
 H31E(0.1031) H31F(0.0943) H51D(0.0726) H51E(0.1437) H51F(0.0992) H2BA(0.2042)
 H3B(0.3114) H5B(0.2986) H6B(0.1918) H31A(0.3967) H31B(0.449) H31C(0.3785)
 H51A(0.4114) H51B(0.4491) H51C(0.3752) H2AB(0.3172) H3A(0.2119) H5A(0.1834)
 H6A(0.289) H31J(0.089) H31K(0.125) H31L(0.051) H51J(0.1198) H51K(0.118)
 H51L(0.0554) H2CA(0.1822) H3C(0.2876) H5C(0.3228) H6C(0.2172) H31G(0.4221)
 H31H(0.3883) H31I(0.4627) H51G(0.3716) H51H(0.3746) H51I(0.4353)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
O1 O 0.16462(17) 0.14442(17) 0.40814(7) 0.0278(4) Uani 1 d . . .
O2 O 0.29128(17) 0.35024(17) 0.40249(8) 0.0299(4) Uani 1 d . . D
H2 H 0.335(2) 0.345(3) 0.4402(6) 0.045 Uiso 1 d . . DR
N1 N -0.1953(2) 0.1901(2) 0.02220(9) 0.0290(5) Uani 1 d . . D
H1 H -0.2692(19) 0.164(2) -0.0104(8) 0.035 Uiso 1 d . . DR
N2 N -0.0807(2) 0.2845(2) 0.01306(9) 0.0280(5) Uani 1 d . . .
C1 C 0.1360(2) 0.2414(2) 0.31017(10) 0.0207(5) Uani 1 d . . .
C2 C 0.0640(2) 0.1226(2) 0.27542(10) 0.0233(5) Uani 1 d . . .
H2A H 0.0546 0.0421 0.2953 0.028 Uiso 1 calc . . R
C3 C 0.0062(2) 0.1220(2) 0.21205(11) 0.0232(5) Uani 1 d . . .
H3 H -0.0410 0.0403 0.1889 0.028 Uiso 1 calc . . R
C3' C 0.0089(2) 0.3139(2) 0.06900(11) 0.0227(6) Uani 1 d . . .
C4 C 0.0155(2) 0.2383(2) 0.18145(10) 0.0194(5) Uani 1 d . . .
C4' C -0.0484(2) 0.2370(2) 0.11403(10) 0.0200(5) Uani 1 d . . .
C5 C 0.0880(2) 0.3572(2) 0.21694(10) 0.0211(5) Uani 1 d . . .
H5 H 0.0960 0.4381 0.1974 0.025 Uiso 1 calc . . R
C5' C -0.1805(2) 0.1585(2) 0.08190(11) 0.0228(6) Uani 1 d . . .
C6 C 0.1477(2) 0.3578(2) 0.28008(10) 0.0210(5) Uani 1 d . . .
H6 H 0.1973 0.4390 0.3031 0.025 Uiso 1 calc . . R
C7 C 0.1976(2) 0.2395(2) 0.37849(11) 0.0214(5) Uani 1 d . . .
C31 C 0.1490(2) 0.4146(2) 0.07588(11) 0.0290(6) Uani 1 d . . .
H31D H 0.1721 0.4284 0.0347 0.043 Uiso 1 calc . . GR
H31E H 0.2271 0.3836 0.1031 0.043 Uiso 1 calc . . GR
H31F H 0.1396 0.4980 0.0943 0.043 Uiso 1 calc . . GR
C51 C -0.2939(2) 0.0555(2) 0.10098(12) 0.0298(6) Uani 1 d . . .
H51D H -0.3881 0.0504 0.0726 0.045 Uiso 1 calc . . GR
H51E H -0.3002 0.0784 0.1437 0.045 Uiso 1 calc . . GR
H51F H -0.2680 -0.0300 0.0992 0.045 Uiso 1 calc . . GR
O1B O 0.41310(17) 0.83962(17) 0.09033(7) 0.0284(4) Uani 1 d . . .
O2B O 0.4676(2) 0.64137(18) 0.09280(8) 0.0335(5) Uani 1 d . . D
H2B H 0.483(3) 0.667(3) 0.0577(7) 0.050 Uiso 1 d . . DR
N1B N 0.4835(2) 0.7739(2) 0.48273(9) 0.0281(5) Uani 1 d . . D
H1B H 0.452(2) 0.789(2) 0.5166(7) 0.034 Uiso 1 d . . DR
N2B N 0.5558(2) 0.6751(2) 0.48452(9) 0.0275(5) Uani 1 d . . .
C1B C 0.4476(2) 0.7383(2) 0.18697(11) 0.0211(5) Uani 1 d . . .
C2B C 0.4570(2) 0.8523(2) 0.22331(11) 0.0236(6) Uani 1 d . . .
H2BA H 0.4550 0.9330 0.2042 0.028 Uiso 1 calc . . R
C3B C 0.4691(2) 0.8490(2) 0.28723(11) 0.0224(5) Uani 1 d . . .
H3B H 0.4774 0.9282 0.3114 0.027 Uiso 1 calc . . R
C3B' C 0.5585(2) 0.6469(2) 0.42519(11) 0.0232(5) Uani 1 d . . .
C4B C 0.4693(2) 0.7315(2) 0.31699(11) 0.0207(5) Uani 1 d . . .
C4B' C 0.4873(2) 0.7292(2) 0.38526(11) 0.0204(5) Uani 1 d . . .
C5B C 0.4588(2) 0.6174(2) 0.27981(11) 0.0217(5) Uani 1 d . . .
H5B H 0.4581 0.5360 0.2986 0.026 Uiso 1 calc . . R
C5B' C 0.4404(2) 0.8089(2) 0.42474(11) 0.0220(5) Uani 1 d . . .
C6B C 0.4495(2) 0.6212(2) 0.21605(11) 0.0231(6) Uani 1 d . . .
H6B H 0.4443 0.5428 0.1918 0.028 Uiso 1 calc . . R
C7B C 0.4400(2) 0.7453(2) 0.11883(11) 0.0226(5) Uani 1 d . . .
C31B C 0.6348(2) 0.5438(2) 0.41112(11) 0.0279(6) Uani 1 d . . .
H31A H 0.5632 0.4606 0.3967 0.042 Uiso 1 calc . . GR
H31B H 0.7032 0.5310 0.4490 0.042 Uiso 1 calc . . GR
H31C H 0.6881 0.5720 0.3785 0.042 Uiso 1 calc . . GR
C51B C 0.3594(3) 0.9163(2) 0.41421(11) 0.0312(6) Uani 1 d . . .
H51A H 0.4277 0.9999 0.4114 0.047 Uiso 1 calc . . GR
H51B H 0.3123 0.9248 0.4491 0.047 Uiso 1 calc . . GR
H51C H 0.2854 0.8946 0.3752 0.047 Uiso 1 calc . . GR
O1A O 0.64106(17) 0.18993(17) 0.41563(7) 0.0287(4) Uani 1 d . . .
O2A O 0.85433(17) 0.30003(18) 0.39777(7) 0.0302(4) Uani 1 d . . D
H2AA H 0.887(3) 0.290(3) 0.4361(5) 0.045 Uiso 1 d . . DR
N1A N 0.3542(2) 0.2204(2) 0.02221(9) 0.0283(5) Uani 1 d . . D
H1A H 0.2786(18) 0.191(2) -0.0097(8) 0.034 Uiso 1 d . . DR
N2A N 0.4688(2) 0.3198(2) 0.01760(9) 0.0298(5) Uani 1 d . . .
C1A C 0.6542(2) 0.2560(2) 0.31351(10) 0.0197(5) Uani 1 d . . .
C2A C 0.5043(2) 0.2218(2) 0.28992(11) 0.0244(6) Uani 1 d . . .
H2AB H 0.4406 0.1934 0.3172 0.029 Uiso 1 calc . . R
C3A C 0.4475(2) 0.2289(2) 0.22703(11) 0.0236(6) Uani 1 d . . .
H3A H 0.3450 0.2070 0.2119 0.028 Uiso 1 calc . . R
C3A' C 0.5485(3) 0.3495(3) 0.07557(11) 0.0256(6) Uani 1 d . . .
C4A C 0.5379(2) 0.2674(2) 0.18531(10) 0.0216(5) Uani 1 d . . .
C4A' C 0.4821(2) 0.2690(2) 0.11784(11) 0.0227(6) Uani 1 d . . .
C5A C 0.6889(2) 0.3043(2) 0.21037(11) 0.0257(6) Uani 1 d . . .
H5A H 0.7532 0.3327 0.1834 0.031 Uiso 1 calc . . R
C5A' C 0.3570(2) 0.1875(3) 0.08117(11) 0.0244(6) Uani 1 d . . .
C6A C 0.7453(2) 0.2999(2) 0.27318(11) 0.0270(6) Uani 1 d . . .
H6A H 0.8474 0.3272 0.2890 0.032 Uiso 1 calc . . R
C7A C 0.7145(2) 0.2457(2) 0.38050(11) 0.0211(5) Uani 1 d . . .
C31A C 0.6838(2) 0.4576(2) 0.08605(11) 0.0306(6) Uani 1 d . . .
H31J H 0.7687 0.4191 0.0890 0.046 Uiso 1 calc . . GR
H31K H 0.6932 0.5100 0.1250 0.046 Uiso 1 calc . . GR
H31L H 0.6783 0.5144 0.0510 0.046 Uiso 1 calc . . GR
C51A C 0.2391(2) 0.0796(2) 0.09475(11) 0.0310(6) Uani 1 d . . .
H51J H 0.1823 0.1167 0.1198 0.047 Uiso 1 calc . . GR
H51K H 0.2825 0.0138 0.1180 0.047 Uiso 1 calc . . GR
H51L H 0.1751 0.0376 0.0554 0.047 Uiso 1 calc . . GR
O1C O 0.87370(17) 0.80243(18) 0.08554(8) 0.0337(5) Uani 1 d . . .
O2C O 1.05549(19) 0.69843(19) 0.10415(8) 0.0339(5) Uani 1 d . . D
H2C H 1.051(3) 0.709(3) 0.0653(5) 0.051 Uiso 1 d . . DR
N1C N 0.9358(2) 0.8187(2) 0.47754(9) 0.0254(5) Uani 1 d . . D
H1C H 0.900(2) 0.840(2) 0.5093(7) 0.031 Uiso 1 d . . DR
N2C N 1.0090(2) 0.7204(2) 0.48754(9) 0.0249(5) Uani 1 d . . .
C1C C 0.9573(2) 0.7461(2) 0.18883(10) 0.0208(5) Uani 1 d . . .
C2C C 0.8419(2) 0.7750(2) 0.21090(11) 0.0237(6) Uani 1 d . . .
H2CA H 0.7623 0.7944 0.1822 0.028 Uiso 1 calc . . R
C3C C 0.8411(2) 0.7759(2) 0.27377(11) 0.0233(6) Uani 1 d . . .
H3C H 0.7599 0.7939 0.2876 0.028 Uiso 1 calc . . R
C3C' C 1.0276(2) 0.6857(2) 0.43168(11) 0.0215(5) Uani 1 d . . .
C4C C 0.9585(2) 0.7506(2) 0.31750(10) 0.0188(5) Uani 1 d . . .
C4C' C 0.9626(2) 0.7594(2) 0.38499(11) 0.0209(5) Uani 1 d . . .
C5C C 1.0723(2) 0.7180(2) 0.29443(10) 0.0216(5) Uani 1 d . . .
H5C H 1.1514 0.6967 0.3228 0.026 Uiso 1 calc . . R
C5C' C 0.9049(2) 0.8444(2) 0.41720(10) 0.0213(5) Uani 1 d . . .
C6C C 1.0721(2) 0.7162(2) 0.23153(11) 0.0216(5) Uani 1 d . . .
H6C H 1.1509 0.6944 0.2172 0.026 Uiso 1 calc . . R
C7C C 0.9569(2) 0.7518(2) 0.12104(11) 0.0230(6) Uani 1 d . . .
C31C C 1.1029(2) 0.5761(2) 0.42568(11) 0.0261(6) Uani 1 d . . .
H31G H 1.2032 0.6134 0.4221 0.039 Uiso 1 calc . . GR
H31H H 1.0510 0.5182 0.3883 0.039 Uiso 1 calc . . GR
H31I H 1.1037 0.5251 0.4627 0.039 Uiso 1 calc . . GR
C51C C 0.8285(2) 0.9518(2) 0.39802(11) 0.0266(6) Uani 1 d . . .
H51G H 0.7323 0.9134 0.3716 0.040 Uiso 1 calc . . GR
H51H H 0.8857 1.0138 0.3746 0.040 Uiso 1 calc . . GR
H51I H 0.8172 0.9986 0.4353 0.040 Uiso 1 calc . . GR


_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
O1 C7 1.217(3) . ?
O2 H2 0.856(10) . ?
O2 C7 1.319(3) . ?
N1 H1 0.887(9) . ?
N1 N2 1.361(3) . ?
N1 C5' 1.344(3) . ?
N2 C3' 1.332(3) . ?
C1 C2 1.398(3) . ?
C1 C6 1.387(3) . ?
C1 C7 1.496(3) . ?
C2 H2A 0.9500 . ?
C2 C3 1.386(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.393(3) . ?
C3' C4' 1.411(3) . ?
C3' C31 1.493(3) . ?
C4 C4' 1.478(3) . ?
C4 C5 1.406(3) . ?
C4' C5' 1.390(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.385(3) . ?
C5' C51 1.488(3) . ?
C6 H6 0.9500 . ?
C31 H31D 0.9800 . ?
C31 H31E 0.9800 . ?
C31 H31F 0.9800 . ?
C51 H51D 0.9800 . ?
C51 H51E 0.9800 . ?
C51 H51F 0.9800 . ?
O1B C7B 1.223(3) . ?
O2B H2B 0.849(10) . ?
O2B C7B 1.317(3) . ?
N1B H1B 0.883(10) . ?
N1B N2B 1.364(3) . ?
N1B C5B' 1.339(3) . ?
N2B C3B' 1.335(3) . ?
C1B C2B 1.391(3) . ?
C1B C6B 1.391(3) . ?
C1B C7B 1.485(3) . ?
C2B H2BA 0.9500 . ?
C2B C3B 1.385(3) . ?
C3B H3B 0.9500 . ?
C3B C4B 1.401(3) . ?
C3B' C4B' 1.422(3) . ?
C3B' C31B 1.491(3) . ?
C4B C4B' 1.473(3) . ?
C4B C5B 1.399(3) . ?
C4B' C5B' 1.393(3) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.385(3) . ?
C5B' C51B 1.497(3) . ?
C6B H6B 0.9500 . ?
C31B H31A 0.9800 . ?
C31B H31B 0.9800 . ?
C31B H31C 0.9800 . ?
C51B H51A 0.9800 . ?
C51B H51B 0.9800 . ?
C51B H51C 0.9800 . ?
O1A C7A 1.224(3) . ?
O2A H2AA 0.853(10) . ?
O2A C7A 1.313(3) . ?
N1A H1A 0.892(9) . ?
N1A N2A 1.361(3) . ?
N1A C5A' 1.342(3) . ?
N2A C3A' 1.333(3) . ?
C1A C2A 1.393(3) . ?
C1A C6A 1.389(3) . ?
C1A C7A 1.480(3) . ?
C2A H2AB 0.9500 . ?
C2A C3A 1.385(3) . ?
C3A H3A 0.9500 . ?
C3A C4A 1.397(3) . ?
C3A' C4A' 1.421(3) . ?
C3A' C31A 1.496(3) . ?
C4A C4A' 1.468(3) . ?
C4A C5A 1.409(3) . ?
C4A' C5A' 1.392(3) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.378(3) . ?
C5A' C51A 1.496(3) . ?
C6A H6A 0.9500 . ?
C31A H31J 0.9800 . ?
C31A H31K 0.9800 . ?
C31A H31L 0.9800 . ?
C51A H51J 0.9800 . ?
C51A H51K 0.9800 . ?
C51A H51L 0.9800 . ?
O1C C7C 1.215(2) . ?
O2C H2C 0.856(10) . ?
O2C C7C 1.313(3) . ?
N1C H1C 0.884(9) . ?
N1C N2C 1.364(3) . ?
N1C C5C' 1.342(3) . ?
N2C C3C' 1.329(3) . ?
C1C C2C 1.390(3) . ?
C1C C6C 1.392(3) . ?
C1C C7C 1.489(3) . ?
C2C H2CA 0.9500 . ?
C2C C3C 1.381(3) . ?
C3C H3C 0.9500 . ?
C3C C4C 1.403(3) . ?
C3C' C4C' 1.420(3) . ?
C3C' C31C 1.500(3) . ?
C4C C4C' 1.473(3) . ?
C4C C5C 1.402(3) . ?
C4C' C5C' 1.396(3) . ?
C5C H5C 0.9500 . ?
C5C C6C 1.379(3) . ?
C5C' C51C 1.494(3) . ?
C6C H6C 0.9500 . ?
C31C H31G 0.9800 . ?
C31C H31H 0.9800 . ?
C31C H31I 0.9800 . ?
C51C H51G 0.9800 . ?
C51C H51H 0.9800 . ?
C51C H51I 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 O2 H2 112.8(18) . . ?
N2 N1 H1 116.8(17) . . ?
C5' N1 H1 130.4(17) . . ?
C5' N1 N2 112.63(19) . . ?
C3' N2 N1 105.29(19) . . ?
C2 C1 C7 119.2(2) . . ?
C6 C1 C2 118.8(2) . . ?
C6 C1 C7 122.0(2) . . ?
C1 C2 H2A 119.9 . . ?
C3 C2 C1 120.2(2) . . ?
C3 C2 H2A 119.9 . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.6(2) . . ?
C4 C3 H3 119.2 . . ?
N2 C3' C4' 110.5(2) . . ?
N2 C3' C31 119.6(2) . . ?
C4' C3' C31 129.9(2) . . ?
C3 C4 C4' 121.3(2) . . ?
C3 C4 C5 117.6(2) . . ?
C5 C4 C4' 121.1(2) . . ?
C3' C4' C4 128.2(2) . . ?
C5' C4' C3' 105.5(2) . . ?
C5' C4' C4 126.3(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 C4 120.8(2) . . ?
C6 C5 H5 119.6 . . ?
N1 C5' C4' 106.1(2) . . ?
N1 C5' C51 120.6(2) . . ?
C4' C5' C51 133.3(2) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 C1 121.0(2) . . ?
C5 C6 H6 119.5 . . ?
O1 C7 O2 124.1(2) . . ?
O1 C7 C1 122.8(2) . . ?
O2 C7 C1 113.0(2) . . ?
C3' C31 H31D 109.5 . . ?
C3' C31 H31E 109.5 . . ?
C3' C31 H31F 109.5 . . ?
H31D C31 H31E 109.5 . . ?
H31D C31 H31F 109.5 . . ?
H31E C31 H31F 109.5 . . ?
C5' C51 H51D 109.5 . . ?
C5' C51 H51E 109.5 . . ?
C5' C51 H51F 109.5 . . ?
H51D C51 H51E 109.5 . . ?
H51D C51 H51F 109.5 . . ?
H51E C51 H51F 109.5 . . ?
C7B O2B H2B 103.1(19) . . ?
N2B N1B H1B 115.8(16) . . ?
C5B' N1B H1B 128.9(16) . . ?
C5B' N1B N2B 112.9(2) . . ?
C3B' N2B N1B 105.26(18) . . ?
C2B C1B C6B 118.7(2) . . ?
C2B C1B C7B 119.4(2) . . ?
C6B C1B C7B 121.9(2) . . ?
C1B C2B H2BA 119.8 . . ?
C3B C2B C1B 120.4(2) . . ?
C3B C2B H2BA 119.8 . . ?
C2B C3B H3B 119.3 . . ?
C2B C3B C4B 121.5(2) . . ?
C4B C3B H3B 119.3 . . ?
N2B C3B' C4B' 110.3(2) . . ?
N2B C3B' C31B 118.8(2) . . ?
C4B' C3B' C31B 130.9(2) . . ?
C3B C4B C4B' 121.3(2) . . ?
C5B C4B C3B 117.5(2) . . ?
C5B C4B C4B' 121.1(2) . . ?
C3B' C4B' C4B 127.4(2) . . ?
C5B' C4B' C3B' 105.2(2) . . ?
C5B' C4B' C4B 127.4(2) . . ?
C4B C5B H5B 119.5 . . ?
C6B C5B C4B 121.0(2) . . ?
C6B C5B H5B 119.5 . . ?
N1B C5B' C4B' 106.4(2) . . ?
N1B C5B' C51B 120.0(2) . . ?
C4B' C5B' C51B 133.7(2) . . ?
C1B C6B H6B 119.6 . . ?
C5B C6B C1B 120.9(2) . . ?
C5B C6B H6B 119.6 . . ?
O1B C7B O2B 123.8(2) . . ?
O1B C7B C1B 123.0(2) . . ?
O2B C7B C1B 113.2(2) . . ?
C3B' C31B H31A 109.5 . . ?
C3B' C31B H31B 109.5 . . ?
C3B' C31B H31C 109.5 . . ?
H31A C31B H31B 109.5 . . ?
H31A C31B H31C 109.5 . . ?
H31B C31B H31C 109.5 . . ?
C5B' C51B H51A 109.5 . . ?
C5B' C51B H51B 109.5 . . ?
C5B' C51B H51C 109.5 . . ?
H51A C51B H51B 109.5 . . ?
H51A C51B H51C 109.5 . . ?
H51B C51B H51C 109.5 . . ?
C7A O2A H2AA 111.6(18) . . ?
N2A N1A H1A 122.3(16) . . ?
C5A' N1A H1A 124.1(16) . . ?
C5A' N1A N2A 112.7(2) . . ?
C3A' N2A N1A 105.6(2) . . ?
C2A C1A C7A 120.3(2) . . ?
C6A C1A C2A 118.9(2) . . ?
C6A C1A C7A 120.9(2) . . ?
C1A C2A H2AB 119.8 . . ?
C3A C2A C1A 120.5(2) . . ?
C3A C2A H2AB 119.8 . . ?
C2A C3A H3A 119.3 . . ?
C2A C3A C4A 121.4(2) . . ?
C4A C3A H3A 119.3 . . ?
N2A C3A' C4A' 110.1(2) . . ?
N2A C3A' C31A 118.4(2) . . ?
C4A' C3A' C31A 131.4(2) . . ?
C3A C4A C4A' 122.9(2) . . ?
C3A C4A C5A 117.2(2) . . ?
C5A C4A C4A' 119.9(2) . . ?
C3A' C4A' C4A 127.2(2) . . ?
C5A' C4A' C3A' 105.4(2) . . ?
C5A' C4A' C4A 127.4(2) . . ?
C4A C5A H5A 119.3 . . ?
C6A C5A C4A 121.4(2) . . ?
C6A C5A H5A 119.3 . . ?
N1A C5A' C4A' 106.2(2) . . ?
N1A C5A' C51A 119.8(2) . . ?
C4A' C5A' C51A 133.9(2) . . ?
C1A C6A H6A 119.7 . . ?
C5A C6A C1A 120.6(2) . . ?
C5A C6A H6A 119.7 . . ?
O1A C7A O2A 123.9(2) . . ?
O1A C7A C1A 122.9(2) . . ?
O2A C7A C1A 113.2(2) . . ?
C3A' C31A H31J 109.5 . . ?
C3A' C31A H31K 109.5 . . ?
C3A' C31A H31L 109.5 . . ?
H31J C31A H31K 109.5 . . ?
H31J C31A H31L 109.5 . . ?
H31K C31A H31L 109.5 . . ?
C5A' C51A H51J 109.5 . . ?
C5A' C51A H51K 109.5 . . ?
C5A' C51A H51L 109.5 . . ?
H51J C51A H51K 109.5 . . ?
H51J C51A H51L 109.5 . . ?
H51K C51A H51L 109.5 . . ?
C7C O2C H2C 107.7(17) . . ?
N2C N1C H1C 114.5(15) . . ?
C5C' N1C H1C 130.8(15) . . ?
C5C' N1C N2C 112.82(19) . . ?
C3C' N2C N1C 105.07(18) . . ?
C2C C1C C6C 118.5(2) . . ?
C2C C1C C7C 119.40(19) . . ?
C6C C1C C7C 122.1(2) . . ?
C1C C2C H2CA 119.4 . . ?
C3C C2C C1C 121.2(2) . . ?
C3C C2C H2CA 119.4 . . ?
C2C C3C H3C 119.6 . . ?
C2C C3C C4C 120.9(2) . . ?
C4C C3C H3C 119.6 . . ?
N2C C3C' C4C' 111.0(2) . . ?
N2C C3C' C31C 119.0(2) . . ?
C4C' C3C' C31C 130.0(2) . . ?
C3C C4C C4C' 121.23(19) . . ?
C3C C4C C5C 117.3(2) . . ?
C5C C4C C4C' 121.43(19) . . ?
C3C' C4C' C4C 128.0(2) . . ?
C5C' C4C' C3C' 104.8(2) . . ?
C5C' C4C' C4C 127.2(2) . . ?
C4C C5C H5C 119.3 . . ?
C6C C5C C4C 121.5(2) . . ?
C6C C5C H5C 119.3 . . ?
N1C C5C' C4C' 106.34(19) . . ?
N1C C5C' C51C 120.0(2) . . ?
C4C' C5C' C51C 133.6(2) . . ?
C1C C6C H6C 119.7 . . ?
C5C C6C C1C 120.6(2) . . ?
C5C C6C H6C 119.7 . . ?
O1C C7C O2C 124.0(2) . . ?
O1C C7C C1C 122.6(2) . . ?
O2C C7C C1C 113.38(19) . . ?
C3C' C31C H31G 109.5 . . ?
C3C' C31C H31H 109.5 . . ?
C3C' C31C H31I 109.5 . . ?
H31G C31C H31H 109.5 . . ?
H31G C31C H31I 109.5 . . ?
H31H C31C H31I 109.5 . . ?
C5C' C51C H51G 109.5 . . ?
C5C' C51C H51H 109.5 . . ?
C5C' C51C H51I 109.5 . . ?
H51G C51C H51H 109.5 . . ?
H51G C51C H51I 109.5 . . ?
H51H C51C H51I 109.5 . . ?

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
O2 H2 N2B 0.856(10) 1.809(10) 2.660(2) 173(2) 2_666
N1 H1 O1B 0.887(9) 1.993(12) 2.852(2) 162(2) 2_565
O2B H2B N2A 0.849(10) 1.810(12) 2.637(3) 164(3) 2_665
N1B H1B O1A 0.883(10) 1.921(10) 2.799(3) 173(2) 2_666
O2A H2AA N2C 0.853(10) 1.784(11) 2.625(2) 169(3) 2_766
N1A H1A O1C 0.892(9) 1.991(13) 2.841(2) 159(2) 2_665
O2C H2C N2 0.856(10) 1.800(12) 2.639(3) 166(3) 2_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 N2 C3' C4' 0.5(2) . . . . ?
N1 N2 C3' C31 179.29(19) . . . . ?
N2 N1 C5' C4' 0.2(3) . . . . ?
N2 N1 C5' C51 -179.0(2) . . . . ?
N2 C3' C4' C4 -180.0(2) . . . . ?
N2 C3' C4' C5' -0.4(3) . . . . ?
C1 C2 C3 C4 -1.1(3) . . . . ?
C2 C1 C6 C5 0.7(3) . . . . ?
C2 C1 C7 O1 -14.7(3) . . . . ?
C2 C1 C7 O2 164.62(19) . . . . ?
C2 C3 C4 C4' -179.0(2) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
C3 C4 C4' C3' -140.8(2) . . . . ?
C3 C4 C4' C5' 39.6(3) . . . . ?
C3 C4 C5 C6 0.0(3) . . . . ?
C3' C4' C5' N1 0.1(2) . . . . ?
C3' C4' C5' C51 179.2(2) . . . . ?
C4 C4' C5' N1 179.7(2) . . . . ?
C4 C4' C5' C51 -1.2(4) . . . . ?
C4 C5 C6 C1 -0.8(3) . . . . ?
C4' C4 C5 C6 180.00(19) . . . . ?
C5 C4 C4' C3' 39.2(3) . . . . ?
C5 C4 C4' C5' -140.3(2) . . . . ?
C5' N1 N2 C3' -0.4(3) . . . . ?
C6 C1 C2 C3 0.3(3) . . . . ?
C6 C1 C7 O1 165.0(2) . . . . ?
C6 C1 C7 O2 -15.6(3) . . . . ?
C7 C1 C2 C3 -179.95(19) . . . . ?
C7 C1 C6 C5 -179.1(2) . . . . ?
C31 C3' C4' C4 1.3(4) . . . . ?
C31 C3' C4' C5' -179.0(2) . . . . ?
N1B N2B C3B' C4B' 0.2(3) . . . . ?
N1B N2B C3B' C31B 178.2(2) . . . . ?
N2B N1B C5B' C4B' -0.3(3) . . . . ?
N2B N1B C5B' C51B -179.9(2) . . . . ?
N2B C3B' C4B' C4B 178.6(2) . . . . ?
N2B C3B' C4B' C5B' -0.4(3) . . . . ?
C1B C2B C3B C4B -1.3(3) . . . . ?
C2B C1B C6B C5B 0.7(3) . . . . ?
C2B C1B C7B O1B -14.7(3) . . . . ?
C2B C1B C7B O2B 164.1(2) . . . . ?
C2B C3B C4B C4B' 177.9(2) . . . . ?
C2B C3B C4B C5B 0.8(3) . . . . ?
C3B C4B C4B' C3B' -146.4(2) . . . . ?
C3B C4B C4B' C5B' 32.3(4) . . . . ?
C3B C4B C5B C6B 0.4(3) . . . . ?
C3B' C4B' C5B' N1B 0.4(3) . . . . ?
C3B' C4B' C5B' C51B 179.9(2) . . . . ?
C4B C4B' C5B' N1B -178.6(2) . . . . ?
C4B C4B' C5B' C51B 1.0(4) . . . . ?
C4B C5B C6B C1B -1.2(3) . . . . ?
C4B' C4B C5B C6B -176.7(2) . . . . ?
C5B C4B C4B' C3B' 30.5(4) . . . . ?
C5B C4B C4B' C5B' -150.7(2) . . . . ?
C5B' N1B N2B C3B' 0.1(3) . . . . ?
C6B C1B C2B C3B 0.5(3) . . . . ?
C6B C1B C7B O1B 167.0(2) . . . . ?
C6B C1B C7B O2B -14.2(3) . . . . ?
C7B C1B C2B C3B -177.8(2) . . . . ?
C7B C1B C6B C5B 179.03(19) . . . . ?
C31B C3B' C4B' C4B 0.9(4) . . . . ?
C31B C3B' C4B' C5B' -178.1(2) . . . . ?
N1A N2A C3A' C4A' -1.0(2) . . . . ?
N1A N2A C3A' C31A -179.66(19) . . . . ?
N2A N1A C5A' C4A' -0.8(3) . . . . ?
N2A N1A C5A' C51A -179.89(19) . . . . ?
N2A C3A' C4A' C4A 177.6(2) . . . . ?
N2A C3A' C4A' C5A' 0.5(3) . . . . ?
C1A C2A C3A C4A 1.4(4) . . . . ?
C2A C1A C6A C5A -2.7(4) . . . . ?
C2A C1A C7A O1A 11.1(4) . . . . ?
C2A C1A C7A O2A -170.1(2) . . . . ?
C2A C3A C4A C4A' 176.5(2) . . . . ?
C2A C3A C4A C5A -2.7(3) . . . . ?
C3A C4A C4A' C3A' 153.6(2) . . . . ?
C3A C4A C4A' C5A' -30.0(4) . . . . ?
C3A C4A C5A C6A 1.3(4) . . . . ?
C3A' C4A' C5A' N1A 0.1(2) . . . . ?
C3A' C4A' C5A' C51A 179.1(2) . . . . ?
C4A C4A' C5A' N1A -176.9(2) . . . . ?
C4A C4A' C5A' C51A 2.1(4) . . . . ?
C4A C5A C6A C1A 1.4(4) . . . . ?
C4A' C4A C5A C6A -177.9(2) . . . . ?
C5A C4A C4A' C3A' -27.3(3) . . . . ?
C5A C4A C4A' C5A' 149.1(2) . . . . ?
C5A' N1A N2A C3A' 1.1(3) . . . . ?
C6A C1A C2A C3A 1.4(4) . . . . ?
C6A C1A C7A O1A -169.0(2) . . . . ?
C6A C1A C7A O2A 9.8(3) . . . . ?
C7A C1A C2A C3A -178.8(2) . . . . ?
C7A C1A C6A C5A 177.4(2) . . . . ?
C31A C3A' C4A' C4A -3.9(4) . . . . ?
C31A C3A' C4A' C5A' 179.0(2) . . . . ?
N1C N2C C3C' C4C' -1.6(3) . . . . ?
N1C N2C C3C' C31C -178.73(19) . . . . ?
N2C N1C C5C' C4C' -0.9(3) . . . . ?
N2C N1C C5C' C51C -178.4(2) . . . . ?
N2C C3C' C4C' C4C -179.8(2) . . . . ?
N2C C3C' C4C' C5C' 1.1(3) . . . . ?
C1C C2C C3C C4C 1.5(4) . . . . ?
C2C C1C C6C C5C -1.3(3) . . . . ?
C2C C1C C7C O1C 13.2(4) . . . . ?
C2C C1C C7C O2C -167.5(2) . . . . ?
C2C C3C C4C C4C' 176.2(2) . . . . ?
C2C C3C C4C C5C -3.1(4) . . . . ?
C3C C4C C4C' C3C' 148.8(2) . . . . ?
C3C C4C C4C' C5C' -32.3(4) . . . . ?
C3C C4C C5C C6C 2.6(3) . . . . ?
C3C' C4C' C5C' N1C -0.1(3) . . . . ?
C3C' C4C' C5C' C51C 176.9(2) . . . . ?
C4C C4C' C5C' N1C -179.3(2) . . . . ?
C4C C4C' C5C' C51C -2.3(4) . . . . ?
C4C C5C C6C C1C -0.4(4) . . . . ?
C4C' C4C C5C C6C -176.7(2) . . . . ?
C5C C4C C4C' C3C' -32.0(4) . . . . ?
C5C C4C C4C' C5C' 146.9(2) . . . . ?
C5C' N1C N2C C3C' 1.6(3) . . . . ?
C6C C1C C2C C3C 0.8(4) . . . . ?
C6C C1C C7C O1C -165.0(2) . . . . ?
C6C C1C C7C O2C 14.3(3) . . . . ?
C7C C1C C2C C3C -177.4(2) . . . . ?
C7C C1C C6C C5C 176.8(2) . . . . ?
C31C C3C' C4C' C4C -3.1(4) . . . . ?
C31C C3C' C4C' C5C' 177.8(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PUBL024_GLOBAL              
;
PROBLEM: The number of authors is greater than 5.
RESPONSE: MRB, SOH, CSH, DK and CR synthesised, characterised and analysed H2L 
and compounds 1-8. CSH, CMF, LLK and MFM collected, solved, refined and prepared
the cif files for H2L H2L.NO3 and 1-8. CR, ADB and PEK conceived and directed 
the research. CR drafted the manuscript with help from CSH, PEK and ADB and 
compiled the supplementary data.
;
####################################################################### 
# 
# 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_csh27
_database_code_depnum_ccdc_archive 'CCDC 1040599'
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_audit_creation_date             2014-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            
'4-(3,5-dimethyl-1H,2H-pyrazolium-4-yl)benzoic acid nitrate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H13 N2 O2, N O3'
_chemical_formula_sum            'C12 H13 N3 O5'
_chemical_formula_weight         279.25
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_symmetry_int_tables_number      ?
_cell_length_a                   7.4272(4)
_cell_length_b                   8.9566(6)
_cell_length_c                   10.4607(6)
_cell_angle_alpha                72.810(4)
_cell_angle_beta                 70.221(4)
_cell_angle_gamma                78.066(4)
_cell_volume                     621.14(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1852
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      22.42
_cell_measurement_theta_min      2.79
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.704295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0961
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14759
_diffrn_reflns_theta_full        28.43
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         2.79
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_reflns_number_gt                1604
_reflns_number_total             3077
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.53A (Bruker, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XLMP (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3077
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0484
_refine_ls_restrained_S_all      0.877
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0550P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1213
_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. 
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H2(0.03) H6(0.029) H3(0.027) H1(0.03) H2B(0.027) H5(0.03)
 H51A(0.044) H51B(0.044) H51C(0.044) H31A(0.048) H31B(0.048) H31C(0.048)
 Fixed X: H6(0.4881) H3(-0.1371) H2B(0.0293) H5(0.3244) H51A(0.2035)
 H51B(0.1021) H51C(0.0086) H31A(-0.3441) H31B(-0.131) H31C(-0.2868)
 Fixed Y: H6(0.3696) H3(0.2432) H2B(0.339) H5(0.2652) H51A(0.2847)
 H51B(0.4325) H51C(0.3806) H31A(0.0557) H31B(-0.035) H31C(-0.1045)
 Fixed Z: H6(0.6453) H3(0.8904) H2B(0.9955) H5(0.5436) H51A(0.335)
 H51B(0.4005) H51C(0.3054) H31A(0.9128) H31B(0.8964) H31C(0.8624)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
O1 O 0.2982(2) 0.43256(19) 1.02639(14) 0.0286(4) Uani 1 d . . .
O3 O 0.5390(2) 0.0987(2) 0.36388(15) 0.0334(4) Uani 1 d . . .
N2 N -0.1679(3) 0.1634(2) 0.48789(18) 0.0252(5) Uani 1 d . . D
H2 H -0.204(3) 0.169(3) 0.4104(15) 0.030 Uiso 1 d . . DR
O2 O 0.5454(2) 0.4665(2) 0.82872(17) 0.0334(4) Uani 1 d . . D
N3 N 0.6431(3) 0.1569(2) 0.24158(19) 0.0300(5) Uani 1 d . . .
C6 C 0.3616(3) 0.3426(3) 0.6958(2) 0.0245(5) Uani 1 d . . .
H6 H 0.4881 0.3696 0.6453 0.029 Uiso 1 calc . . R
C7 C 0.3756(3) 0.4245(3) 0.9019(2) 0.0237(5) Uani 1 d . . .
C4 C 0.0744(3) 0.2451(2) 0.7060(2) 0.0203(5) Uani 1 d . . .
C1 C 0.2756(3) 0.3640(3) 0.8311(2) 0.0215(5) Uani 1 d . . .
C3 C -0.0096(3) 0.2678(3) 0.8405(2) 0.0228(5) Uani 1 d . . .
H3 H -0.1371 0.2432 0.8904 0.027 Uiso 1 calc . . R
N1 N -0.2525(3) 0.0705(2) 0.61421(18) 0.0248(5) Uani 1 d . . D
H1 H -0.347(2) 0.011(2) 0.623(2) 0.030 Uiso 1 d . . DR
C2 C 0.0890(3) 0.3255(3) 0.9031(2) 0.0224(5) Uani 1 d . . .
H2B H 0.0293 0.3390 0.9955 0.027 Uiso 1 calc . . R
O5 O 0.7895(2) 0.2147(2) 0.23106(16) 0.0402(5) Uani 1 d . . .
C5 C 0.2632(3) 0.2820(3) 0.6348(2) 0.0253(5) Uani 1 d . . .
H5 H 0.3244 0.2652 0.5436 0.030 Uiso 1 calc . . R
C4' C -0.0378(3) 0.1887(3) 0.6398(2) 0.0213(5) Uani 1 d . . .
C5' C -0.0343(3) 0.2372(2) 0.5011(2) 0.0166(5) Uani 1 d . . .
C51 C 0.0796(3) 0.3427(3) 0.3749(2) 0.0296(6) Uani 1 d . . .
H51A H 0.2035 0.2847 0.3350 0.044 Uiso 1 calc . . GR
H51B H 0.1021 0.4325 0.4005 0.044 Uiso 1 calc . . GR
H51C H 0.0086 0.3806 0.3054 0.044 Uiso 1 calc . . GR
C31 C -0.2402(3) -0.0079(3) 0.8580(2) 0.0318(6) Uani 1 d . . .
H31A H -0.3441 0.0557 0.9128 0.048 Uiso 1 calc . . GR
H31B H -0.1310 -0.0350 0.8964 0.048 Uiso 1 calc . . GR
H31C H -0.2868 -0.1045 0.8624 0.048 Uiso 1 calc . . GR
O4 O 0.6008(3) 0.1575(3) 0.13800(17) 0.0561(6) Uani 1 d . . .
C3' C -0.1772(3) 0.0840(3) 0.7088(2) 0.0225(5) Uani 1 d . . .
H2A H 0.586(4) 0.506(3) 0.877(3) 0.071(11) Uiso 1 d . . D


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C7 1.250(2) . ?
O3 N3 1.269(2) . ?
N2 H2 0.924(9) . ?
N2 N1 1.356(2) . ?
N2 C5' 1.364(3) . ?
O2 C7 1.300(2) . ?
O2 H2A 0.849(10) . ?
N3 O5 1.257(2) . ?
N3 O4 1.224(2) . ?
C6 H6 0.9500 . ?
C6 C1 1.395(3) . ?
C6 C5 1.385(3) . ?
C7 C1 1.472(3) . ?
C4 C3 1.391(3) . ?
C4 C5 1.404(3) . ?
C4 C4' 1.484(3) . ?
C1 C2 1.395(3) . ?
C3 H3 0.9500 . ?
C3 C2 1.383(3) . ?
N1 H1 0.934(9) . ?
N1 C3' 1.334(3) . ?
C2 H2B 0.9500 . ?
C5 H5 0.9500 . ?
C4' C5' 1.378(3) . ?
C4' C3' 1.403(3) . ?
C5' C51 1.479(3) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C31 C3' 1.496(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 N2 H2 120.3(14) . . ?
N1 N2 C5' 109.25(17) . . ?
C5' N2 H2 130.5(14) . . ?
C7 O2 H2A 108.7(19) . . ?
O5 N3 O3 117.62(18) . . ?
O4 N3 O3 120.85(18) . . ?
O4 N3 O5 121.53(18) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C1 120.23(19) . . ?
O1 C7 O2 123.1(2) . . ?
O1 C7 C1 120.37(18) . . ?
O2 C7 C1 116.56(18) . . ?
C3 C4 C5 118.1(2) . . ?
C3 C4 C4' 119.98(17) . . ?
C5 C4 C4' 121.86(18) . . ?
C6 C1 C7 122.38(18) . . ?
C2 C1 C6 119.1(2) . . ?
C2 C1 C7 118.48(18) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 C4 121.33(18) . . ?
C2 C3 H3 119.3 . . ?
N2 N1 H1 120.3(13) . . ?
C3' N1 N2 108.95(17) . . ?
C3' N1 H1 130.8(13) . . ?
C1 C2 H2B 119.9 . . ?
C3 C2 C1 120.25(19) . . ?
C3 C2 H2B 119.9 . . ?
C6 C5 C4 120.9(2) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5' C4' C4 126.48(18) . . ?
C5' C4' C3' 107.19(19) . . ?
C3' C4' C4 126.20(19) . . ?
N2 C5' C4' 106.88(17) . . ?
N2 C5' C51 118.65(18) . . ?
C4' C5' C51 134.5(2) . . ?
C5' C51 H51A 109.5 . . ?
C5' C51 H51B 109.5 . . ?
C5' C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C3' C31 H31A 109.5 . . ?
C3' C31 H31B 109.5 . . ?
C3' C31 H31C 109.5 . . ?
N1 C3' C4' 107.74(18) . . ?
N1 C3' C31 121.09(19) . . ?
C4' C3' C31 131.1(2) . . ?

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
N2 H2 O5 0.924(9) 1.812(11) 2.705(2) 162(2) 1_455
N1 H1 O3 0.934(9) 1.837(10) 2.770(2) 177(2) 2_556
O2 H2A O1 0.849(10) 1.784(11) 2.627(2) 171(3) 2_667

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
O1 C7 C1 C6 -175.4(2) . . . . ?
O1 C7 C1 C2 3.9(3) . . . . ?
N2 N1 C3' C4' -0.5(2) . . . . ?
N2 N1 C3' C31 -178.8(2) . . . . ?
O2 C7 C1 C6 4.1(3) . . . . ?
O2 C7 C1 C2 -176.6(2) . . . . ?
C6 C1 C2 C3 -0.4(3) . . . . ?
C7 C1 C2 C3 -179.8(2) . . . . ?
C4 C3 C2 C1 0.7(3) . . . . ?
C4 C4' C5' N2 -176.0(2) . . . . ?
C4 C4' C5' C51 5.2(4) . . . . ?
C4 C4' C3' N1 176.4(2) . . . . ?
C4 C4' C3' C31 -5.6(4) . . . . ?
C1 C6 C5 C4 1.7(3) . . . . ?
C3 C4 C5 C6 -1.4(3) . . . . ?
C3 C4 C4' C5' 141.3(2) . . . . ?
C3 C4 C4' C3' -33.9(3) . . . . ?
N1 N2 C5' C4' -0.3(2) . . . . ?
N1 N2 C5' C51 178.69(19) . . . . ?
C5 C6 C1 C7 178.5(2) . . . . ?
C5 C6 C1 C2 -0.8(3) . . . . ?
C5 C4 C3 C2 0.2(3) . . . . ?
C5 C4 C4' C5' -36.5(3) . . . . ?
C5 C4 C4' C3' 148.3(2) . . . . ?
C4' C4 C3 C2 -177.7(2) . . . . ?
C4' C4 C5 C6 176.5(2) . . . . ?
C5' N2 N1 C3' 0.5(2) . . . . ?
C5' C4' C3' N1 0.4(2) . . . . ?
C5' C4' C3' C31 178.4(2) . . . . ?
C3' C4' C5' N2 -0.1(2) . . . . ?
C3' C4' C5' C51 -178.8(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_k08adb02
_database_code_depnum_ccdc_archive 'CCDC 1040600'
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_audit_creation_date             2014-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H30 Co N4 O8, 2 (C3 H7 N O)'
_chemical_formula_sum            'C30 H44 Co N6 O10'
_chemical_formula_weight         707.64
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
#===END
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_symmetry_int_tables_number      14
_cell_length_a                   7.6150(3)
_cell_length_b                   19.8070(7)
_cell_length_c                   11.4480(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.902(2)
_cell_angle_gamma                90.00
_cell_volume                     1683.11(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    75746
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            Pale-pink
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             746
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24010
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.59
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  '95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2693
_reflns_number_total             3862
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3862
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0528
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0397P)²+1.8619P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1252
_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. 

Asymmetric unit contains one half of a cobalt complex molecule and 
one DMF of recrystallisation. Water hydrogens and H1 (attached to N1) 
were located and refined at 0.9Å from the relevant parent atoms.
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H2(0.03) H3(0.031) H5(0.032) H6(0.032) H8(0.052) H9A(0.071)
 H9B(0.071) H9C(0.071) H10A(0.076) H10B(0.076) H10C(0.076) H31A(0.046)
 H31B(0.046) H31C(0.046) H51A(0.049) H51B(0.049) H51C(0.049)
 Fixed X: Co1(0) H2(0.6933) H3(0.5173) H5(0.0947) H6(0.2725) H8(0.7068)
 H9A(0.7834) H9B(0.5838) H9C(0.7423) H10A(0.5069) H10B(0.5542) H10C(0.4017)
 H31A(0.3789) H31B(0.2614) H31C(0.1928) H51A(-0.07) H51B(0.1132) H51C(-0.0672)
 Fixed Y: Co1(0) H2(0.2459) H3(0.1788) H5(0.3053) H6(0.3727) H8(0.4403)
 H9A(0.4829) H9B(0.4626) H9C(0.408) H10A(0.3627) H10B(0.333) H10C(0.3896)
 H31A(0.0661) H31B(0.0914) H31C(0.0294) H51A(0.3052) H51B(0.3048) H51C(0.2746)
 Fixed Z: Co1(1) H2(0.7587) H3(0.8543) H5(0.7422) H6(0.6487) H8(1.1975)
 H9A(0.9264) H9B(0.8573) H9C(0.8754) H10A(1.1017) H10B(0.9823) H10C(0.9733)
 H31A(0.8429) H31B(0.7168) H31C(0.7844) H51A(0.9036) H51B(1.0045) H51C(1.0334)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.0000 1.0000 0.02188(16) Uani 1 2 d S . .
O1 O 0.7770(2) 0.34310(9) 0.64179(18) 0.0277(5) Uani 1 1 d . . .
O2 O 0.5427(3) 0.41117(9) 0.57604(19) 0.0311(5) Uani 1 1 d . . .
O3 O 0.2823(3) -0.01363(9) 1.05727(19) 0.0264(5) Uani 1 1 d D . .
O4 O 0.0059(3) 0.05119(9) 1.15690(18) 0.0266(5) Uani 1 1 d D . .
O5 O 0.8435(4) 0.50233(13) 1.1318(2) 0.0574(7) Uani 1 1 d . . .
N1 N -0.0293(3) 0.15575(11) 0.9606(2) 0.0245(5) Uani 1 1 d D . .
N2 N 0.0379(3) 0.09838(11) 0.9204(2) 0.0247(5) Uani 1 1 d . . .
N3 N 0.6529(4) 0.42590(13) 1.0246(2) 0.0379(6) Uani 1 1 d . . .
C1 C 0.5008(3) 0.31586(13) 0.6936(2) 0.0222(6) Uani 1 1 d . . .
C2 C 0.5716(4) 0.25806(13) 0.7553(3) 0.0250(6) Uani 1 1 d . . .
H2 H 0.6933 0.2459 0.7587 0.030 Uiso 1 1 calc R . .
C3 C 0.4666(4) 0.21795(14) 0.8120(3) 0.0258(6) Uani 1 1 d . . .
H3 H 0.5173 0.1788 0.8543 0.031 Uiso 1 1 calc R . .
C4 C 0.2863(4) 0.23469(13) 0.8075(2) 0.0231(6) Uani 1 1 d . . .
C5 C 0.2163(4) 0.29294(14) 0.7459(3) 0.0267(6) Uani 1 1 d . . .
H5 H 0.0947 0.3053 0.7422 0.032 Uiso 1 1 calc R . .
C6 C 0.3222(4) 0.33309(14) 0.6899(3) 0.0263(6) Uani 1 1 d . . .
H6 H 0.2725 0.3727 0.6487 0.032 Uiso 1 1 calc R . .
C7 C 0.6140(4) 0.35982(13) 0.6322(3) 0.0240(6) Uani 1 1 d . . .
C8 C 0.7343(5) 0.45579(18) 1.1251(3) 0.0435(8) Uani 1 1 d . . .
H8 H 0.7068 0.4403 1.1975 0.052 Uiso 1 1 calc R . .
C9 C 0.6940(5) 0.44653(18) 0.9117(3) 0.0475(9) Uani 1 1 d . . .
H9A H 0.7834 0.4829 0.9264 0.071 Uiso 1 1 calc R . .
H9B H 0.5838 0.4626 0.8573 0.071 Uiso 1 1 calc R . .
H9C H 0.7423 0.4080 0.8754 0.071 Uiso 1 1 calc R . .
C10 C 0.5180(5) 0.37356(18) 1.0201(3) 0.0504(9) Uani 1 1 d . . .
H10A H 0.5069 0.3627 1.1017 0.076 Uiso 1 1 calc R . .
H10B H 0.5542 0.3330 0.9823 0.076 Uiso 1 1 calc R . .
H10C H 0.4017 0.3896 0.9733 0.076 Uiso 1 1 calc R . .
C31 C 0.2563(4) 0.07279(14) 0.7953(3) 0.0305(7) Uani 1 1 d . . .
H31A H 0.3789 0.0661 0.8429 0.046 Uiso 1 1 calc R . .
H31B H 0.2614 0.0914 0.7168 0.046 Uiso 1 1 calc R . .
H31C H 0.1928 0.0294 0.7844 0.046 Uiso 1 1 calc R . .
C51 C 0.0019(4) 0.28000(14) 0.9714(3) 0.0329(7) Uani 1 1 d . . .
H51A H -0.0700 0.3052 0.9036 0.049 Uiso 1 1 calc R . .
H51B H 0.1132 0.3048 1.0045 0.049 Uiso 1 1 calc R . .
H51C H -0.0672 0.2746 1.0334 0.049 Uiso 1 1 calc R . .
C3' C 0.1578(4) 0.12093(14) 0.8591(2) 0.0240(6) Uani 1 1 d . . .
C4' C 0.1691(4) 0.19097(14) 0.8637(2) 0.0244(6) Uani 1 1 d . . .
C5' C 0.0476(4) 0.21177(13) 0.9294(3) 0.0249(6) Uani 1 1 d . . .
H1 H -0.106(4) 0.1530(17) 1.010(2) 0.045(10) Uiso 1 1 d D . .
H3A H 0.352(4) 0.0236(10) 1.070(3) 0.050(11) Uiso 1 1 d D . .
H4A H 0.049(5) 0.036(2) 1.2320(15) 0.075(14) Uiso 1 1 d D . .
H3B H 0.336(4) -0.0365(16) 1.007(3) 0.056(11) Uiso 1 1 d D . .
H4B H -0.075(3) 0.0830(12) 1.164(3) 0.045(10) Uiso 1 1 d D . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O3 2.1199(19) . ?
Co1 O3 2.1198(19) 3_557 ?
Co1 O4 2.0543(19) 3_557 ?
Co1 O4 2.054(2) . ?
Co1 N2 2.197(2) 3_557 ?
Co1 N2 2.197(2) . ?
O1 C7 1.265(3) . ?
O2 C7 1.260(3) . ?
O3 H3A 0.900(3) . ?
O3 H3B 0.900(3) . ?
O4 H4A 0.900(3) . ?
O4 H4B 0.899(3) . ?
O5 C8 1.232(4) . ?
N1 N2 1.367(3) . ?
N1 C5' 1.339(3) . ?
N1 H1 0.900(3) . ?
N2 C3' 1.347(3) . ?
N3 C8 1.319(4) . ?
N3 C9 1.454(4) . ?
N3 C10 1.452(4) . ?
C1 C2 1.390(4) . ?
C1 C6 1.393(4) . ?
C1 C7 1.505(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.387(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.402(4) . ?
C4 C5 1.394(4) . ?
C4 C4' 1.488(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.387(4) . ?
C6 H6 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C31 C3' 1.500(4) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C51 C5' 1.501(4) . ?
C3' C4' 1.390(4) . ?
C4' C5' 1.380(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
O3 Co1 O3 180.00(3) 3_557 . ?
O3 Co1 N2 91.32(8) 3_557 3_557 ?
O3 Co1 N2 91.32(8) . . ?
O3 Co1 N2 88.68(8) . 3_557 ?
O3 Co1 N2 88.68(8) 3_557 . ?
O4 Co1 O3 88.26(8) . . ?
O4 Co1 O3 91.74(8) 3_557 . ?
O4 Co1 O3 91.74(8) . 3_557 ?
O4 Co1 O3 88.26(8) 3_557 3_557 ?
O4 Co1 O4 180.0 3_557 . ?
O4 Co1 N2 86.88(8) 3_557 3_557 ?
O4 Co1 N2 93.12(8) 3_557 . ?
O4 Co1 N2 93.12(8) . 3_557 ?
O4 Co1 N2 86.88(8) . . ?
N2 Co1 N2 180.0 3_557 . ?
Co1 O3 H3A 118(2) . . ?
Co1 O3 H3B 116(2) . . ?
H3A O3 H3B 101(3) . . ?
Co1 O4 H4A 127(3) . . ?
Co1 O4 H4B 123(2) . . ?
H4A O4 H4B 105(3) . . ?
N2 N1 H1 120(2) . . ?
C5' N1 N2 112.3(2) . . ?
C5' N1 H1 127(2) . . ?
N1 N2 Co1 120.26(17) . . ?
C3' N2 Co1 132.66(18) . . ?
C3' N2 N1 104.4(2) . . ?
C8 N3 C9 119.8(3) . . ?
C8 N3 C10 122.9(3) . . ?
C10 N3 C9 117.4(3) . . ?
C2 C1 C6 118.9(2) . . ?
C2 C1 C7 121.0(2) . . ?
C6 C1 C7 120.1(2) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 H3 119.7 . . ?
C2 C3 C4 120.6(3) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C4' 121.5(2) . . ?
C5 C4 C3 118.3(2) . . ?
C5 C4 C4' 120.1(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 C4 120.8(3) . . ?
C6 C5 H5 119.6 . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.6(3) . . ?
C5 C6 H6 119.7 . . ?
O1 C7 C1 117.5(2) . . ?
O2 C7 O1 123.9(2) . . ?
O2 C7 C1 118.6(2) . . ?
O5 C8 N3 124.7(3) . . ?
O5 C8 H8 117.6 . . ?
N3 C8 H8 117.6 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C3' C31 H31A 109.5 . . ?
C3' C31 H31B 109.5 . . ?
C3' C31 H31C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C5' C51 H51A 109.5 . . ?
C5' C51 H51B 109.5 . . ?
C5' C51 H51C 109.5 . . ?
N2 C3' C31 120.9(2) . . ?
N2 C3' C4' 110.8(2) . . ?
C4' C3' C31 128.3(2) . . ?
C3' C4' C4 127.0(2) . . ?
C5' C4' C4 127.0(2) . . ?
C5' C4' C3' 106.0(2) . . ?
N1 C5' C51 121.0(2) . . ?
N1 C5' C4' 106.5(2) . . ?
C4' C5' C51 132.4(2) . . ?

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
Co1 N2 C3' C31 22.2(4) . . . . ?
Co1 N2 C3' C4' -159.0(2) . . . . ?
O3 Co1 N2 N1 -119.1(2) . . . . ?
O3 Co1 N2 N1 60.9(2) 3_557 . . . ?
O3 Co1 N2 C3' -141.0(3) 3_557 . . . ?
O3 Co1 N2 C3' 39.0(3) . . . . ?
O4 Co1 N2 N1 -30.9(2) . . . . ?
O4 Co1 N2 N1 149.1(2) 3_557 . . . ?
O4 Co1 N2 C3' -52.8(3) 3_557 . . . ?
O4 Co1 N2 C3' 127.2(3) . . . . ?
N1 N2 C3' C31 -177.2(3) . . . . ?
N1 N2 C3' C4' 1.6(3) . . . . ?
N2 Co1 N2 N1 62(55) 3_557 . . . ?
N2 Co1 N2 C3' -140(55) 3_557 . . . ?
N2 N1 C5' C51 -176.0(2) . . . . ?
N2 N1 C5' C4' 1.1(3) . . . . ?
N2 C3' C4' C4 179.8(3) . . . . ?
N2 C3' C4' C5' -1.0(3) . . . . ?
C1 C2 C3 C4 0.4(4) . . . . ?
C2 C1 C6 C5 -0.6(4) . . . . ?
C2 C1 C7 O1 -1.9(4) . . . . ?
C2 C1 C7 O2 179.0(3) . . . . ?
C2 C3 C4 C5 -0.7(4) . . . . ?
C2 C3 C4 C4' 177.6(3) . . . . ?
C3 C4 C5 C6 0.4(4) . . . . ?
C3 C4 C4' C3' -43.0(4) . . . . ?
C3 C4 C4' C5' 138.0(3) . . . . ?
C4 C5 C6 C1 0.3(4) . . . . ?
C4 C4' C5' N1 179.1(3) . . . . ?
C4 C4' C5' C51 -4.3(5) . . . . ?
C5 C4 C4' C3' 135.3(3) . . . . ?
C5 C4 C4' C5' -43.7(4) . . . . ?
C6 C1 C2 C3 0.2(4) . . . . ?
C6 C1 C7 O1 177.6(3) . . . . ?
C6 C1 C7 O2 -1.5(4) . . . . ?
C7 C1 C2 C3 179.7(3) . . . . ?
C7 C1 C6 C5 179.9(3) . . . . ?
C9 N3 C8 O5 1.6(5) . . . . ?
C10 N3 C8 O5 -176.7(3) . . . . ?
C31 C3' C4' C4 -1.5(5) . . . . ?
C31 C3' C4' C5' 177.7(3) . . . . ?
C3' C4' C5' N1 -0.1(3) . . . . ?
C3' C4' C5' C51 176.6(3) . . . . ?
C4' C4 C5 C6 -178.0(3) . . . . ?
C5' N1 N2 Co1 161.86(19) . . . . ?
C5' N1 N2 C3' -1.7(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_55cry100
_database_code_depnum_ccdc_archive 'CCDC 1040601'
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_audit_creation_date             2014-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C12 H11 N2 O2 Zn0.5), 0.5(H2 O), 2(C H4 O)'
_chemical_formula_sum            'C50 H53 N8 O10.50 Zn2'
_chemical_formula_weight         1064.74
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_properties_physical    'Loses solvent immediately'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_symmetry_int_tables_number      43
_cell_length_a                   22.3458(7)
_cell_length_b                   29.7691(11)
_cell_length_c                   33.3734(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     22200.5(13)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    6228
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.1560
_cell_measurement_theta_min      3.8910
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.563
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8848
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            17046
_diffrn_reflns_point_group_measured_fraction_full 0.803
_diffrn_reflns_point_group_measured_fraction_max 0.770
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.789
_diffrn_reflns_theta_min         2.805
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -79.00  -42.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.7813  125.0000    0.0000 37

#__ type_ start__ end____ width___ exp.time_
  2 omega  -53.00   -3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.7813  125.0000   60.0000 50

#__ type_ start__ end____ width___ exp.time_
  3 omega -126.00  -92.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -125.0000 -180.0000 34

#__ type_ start__ end____ width___ exp.time_
  4 omega -122.00  -75.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -125.0000   90.0000 47

#__ type_ start__ end____ width___ exp.time_
  5 omega   50.00   98.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000  150.0000 48

#__ type_ start__ end____ width___ exp.time_
  6 omega   42.00   88.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000 -120.0000 46

#__ type_ start__ end____ width___ exp.time_
  7 omega   32.00   85.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  -30.0000 53

#__ type_ start__ end____ width___ exp.time_
  8 omega   61.00   99.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000   90.0000 38

#__ type_ start__ end____ width___ exp.time_
  9 omega   78.00  155.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   61.0000   90.0000 77

#__ type_ start__ end____ width___ exp.time_
 10 omega -114.00  -10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.7813  -57.0000 -180.0000 104

#__ type_ start__ end____ width___ exp.time_
 11 omega   77.00  104.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   61.0000  -90.0000 27
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0202062000
_diffrn_orient_matrix_UB_12      -0.0086272000
_diffrn_orient_matrix_UB_13      0.0434484000
_diffrn_orient_matrix_UB_21      -0.0394400000
_diffrn_orient_matrix_UB_22      -0.0424070000
_diffrn_orient_matrix_UB_23      0.0015125000
_diffrn_orient_matrix_UB_31      0.0527736000
_diffrn_orient_matrix_UB_32      -0.0284155000
_diffrn_orient_matrix_UB_33      -0.0155250000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.550
_reflns_Friedel_fraction_full    0.602
_reflns_Friedel_fraction_max     0.557
_reflns_number_gt                7876
_reflns_number_total             8656
_reflns_odcompleteness_completeness 97.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.63
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.586
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 
;
 Flack x determined using 2607 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         8656
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0763
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1647P)²+137.7684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2192
_refine_ls_wR_factor_ref         0.2287
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O18(0.5) H18A(0.5) H18B(0.5) O17(0.5) H17(0.5) C16(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5) O15(0.5) H15(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 O11(0.5) H11(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) O13(0.5) H13(0.5)
 C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5)
3.a Riding coordinates:
 O17(H17), C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C)
3.b Free rotating group:
 O18(H18A,H18B)
3.c Aromatic/amide H refined with riding coordinates:
 N1C(H1C), C2C(H2C), C3C(H3C), C5C(H5C), C6C(H6C), N1D(H1D), C2D(H2D),
 C3D(H3D), C5D(H5D), C6D(H6D), N1A(H1A), N1B(H1B), C2A(H2A), C2B(H2B), C3A(H3A),
  C3B(H3B), C5A(H5A), C5B(H5B), C6A(H6A), C6B(H6B)
3.d Tetrahedral OH refined with riding coordinates:
 O15(H15), O11(H11), O13(H13)
3.e Idealised Me refined as rotating group:
 C31C(H31G,H31H,H31I), C51C(H51G,H51H,H51I), C31D(H31J,H31K,H31L), C51D(H51J,
 H51K,H51L), C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F), C51A(H51A,H51B,H51C),
 C51B(H51D,H51E,H51F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 1.0000 0.5000 0.38346(5) 0.0304(4) Uani 1 2 d S T P . .
O1C O 0.8571(3) 0.3223(2) 0.6375(2) 0.0490(16) Uani 1 1 d . . . . .
O2C O 0.7902(3) 0.2909(2) 0.59717(19) 0.0393(14) Uani 1 1 d . . . . .
N1C N 0.9015(3) 0.5025(2) 0.4404(2) 0.0359(16) Uani 1 1 d . . . . .
H1C H 0.8953 0.5292 0.4317 0.043 Uiso 1 1 calc R . . . .
N2C N 0.9407(3) 0.4728(3) 0.4233(2) 0.0371(16) Uani 1 1 d . . . . .
C1C C 0.8508(4) 0.3491(3) 0.5709(3) 0.0336(17) Uani 1 1 d . . . . .
C2C C 0.8350(4) 0.3398(3) 0.5317(3) 0.0408(19) Uani 1 1 d . . . . .
H2C H 0.8134 0.3140 0.5256 0.049 Uiso 1 1 calc R . . . .
C3'C C 0.9389(4) 0.4362(3) 0.4464(3) 0.0362(18) Uani 1 1 d . . . . .
C3C C 0.8518(4) 0.3697(3) 0.5011(3) 0.043(2) Uani 1 1 d . . . . .
H3C H 0.8423 0.3629 0.4747 0.051 Uiso 1 1 calc R . . . .
C4'C C 0.8981(4) 0.4414(3) 0.4771(3) 0.0334(17) Uani 1 1 d . . . . .
C4C C 0.8824(4) 0.4092(3) 0.5097(3) 0.0355(18) Uani 1 1 d . . . . .
C5'C C 0.8744(4) 0.4850(3) 0.4719(3) 0.0401(19) Uani 1 1 d . . . . .
C5C C 0.8978(4) 0.4181(3) 0.5494(3) 0.0384(19) Uani 1 1 d . . . . .
H5C H 0.9180 0.4445 0.5558 0.046 Uiso 1 1 calc R . . . .
C6C C 0.8833(4) 0.3881(3) 0.5790(3) 0.0404(19) Uani 1 1 d . . . . .
H6C H 0.8954 0.3938 0.6052 0.049 Uiso 1 1 calc R . . . .
C7C C 0.8322(4) 0.3185(3) 0.6050(3) 0.0381(19) Uani 1 1 d . . . . .
C31C C 0.9781(4) 0.3965(3) 0.4382(3) 0.043(2) Uani 1 1 d . . . . .
H31G H 0.9784 0.3905 0.4099 0.065 Uiso 1 1 calc GR . . . .
H31H H 0.9628 0.3708 0.4522 0.065 Uiso 1 1 calc GR . . . .
H31I H 1.0180 0.4028 0.4471 0.065 Uiso 1 1 calc GR . . . .
C51C C 0.8282(5) 0.5101(4) 0.4953(3) 0.046(2) Uani 1 1 d . . . . .
H51G H 0.8472 0.5330 0.5109 0.069 Uiso 1 1 calc GR . . . .
H51H H 0.8075 0.4897 0.5127 0.069 Uiso 1 1 calc GR . . . .
H51I H 0.8002 0.5237 0.4771 0.069 Uiso 1 1 calc GR . . . .
Zn2 Zn 0.5000 0.5000 0.50050(5) 0.0316(4) Uani 1 2 d S T P . .
O1D O 0.2939(3) 0.7088(3) 0.2853(2) 0.0481(17) Uani 1 1 d . . . . .
O2D O 0.3852(3) 0.7385(3) 0.2903(2) 0.0492(17) Uani 1 1 d . . . . .
N1D N 0.3862(3) 0.5400(3) 0.4779(2) 0.0385(16) Uani 1 1 d . . . . .
H1D H 0.3701 0.5253 0.4973 0.046 Uiso 1 1 calc R . . . .
N2D N 0.4449(3) 0.5369(2) 0.4679(2) 0.0325(15) Uani 1 1 d . . . . .
C1D C 0.3604(4) 0.6771(3) 0.3319(3) 0.0332(17) Uani 1 1 d . . . . .
C2D C 0.3243(4) 0.6400(3) 0.3380(3) 0.044(2) Uani 1 1 d . . . . .
H2D H 0.2916 0.6352 0.3214 0.053 Uiso 1 1 calc R . . . .
C3'D C 0.4523(4) 0.5648(3) 0.4371(3) 0.0356(17) Uani 1 1 d . . . . .
C3D C 0.3364(4) 0.6099(4) 0.3686(3) 0.045(2) Uani 1 1 d . . . . .
H3D H 0.3114 0.5853 0.3725 0.054 Uiso 1 1 calc R . . . .
C4'D C 0.3981(4) 0.5850(3) 0.4265(3) 0.0376(19) Uani 1 1 d . . . . .
C4D C 0.3857(4) 0.6163(3) 0.3936(3) 0.0343(17) Uani 1 1 d . . . . .
C5'D C 0.3562(4) 0.5685(3) 0.4544(3) 0.0394(19) Uani 1 1 d . . . . .
C5D C 0.4224(4) 0.6527(3) 0.3862(3) 0.0369(18) Uani 1 1 d . . . . .
H5D H 0.4558 0.6572 0.4023 0.044 Uiso 1 1 calc R . . . .
C6D C 0.4109(4) 0.6824(3) 0.3557(3) 0.0371(18) Uani 1 1 d . . . . .
H6D H 0.4370 0.7061 0.3509 0.044 Uiso 1 1 calc R . . . .
C7D C 0.3463(4) 0.7111(3) 0.3003(3) 0.0367(18) Uani 1 1 d . . . . .
C31D C 0.5123(4) 0.5703(4) 0.4176(3) 0.051(3) Uani 1 1 d . . . . .
H31J H 0.5173 0.6009 0.4093 0.076 Uiso 1 1 calc GR . . . .
H31K H 0.5149 0.5508 0.3948 0.076 Uiso 1 1 calc GR . . . .
H31L H 0.5432 0.5626 0.4365 0.076 Uiso 1 1 calc GR . . . .
C51D C 0.2919(4) 0.5793(4) 0.4604(4) 0.057(3) Uani 1 1 d . . . . .
H51J H 0.2680 0.5607 0.4432 0.086 Uiso 1 1 calc GR . . . .
H51K H 0.2850 0.6103 0.4541 0.086 Uiso 1 1 calc GR . . . .
H51L H 0.2811 0.5737 0.4878 0.086 Uiso 1 1 calc GR . . . .
Zn3 Zn 0.75206(5) 0.50489(4) 0.68707(3) 0.0315(3) Uani 1 1 d . . . . .
O1A O 0.9496(3) 0.2900(2) 0.90002(18) 0.0359(13) Uani 1 1 d . . . . .
O1B O 0.6244(3) 0.2651(3) 0.4815(2) 0.0501(17) Uani 1 1 d . . . . .
O2A O 0.8674(3) 0.2488(2) 0.8861(2) 0.0467(17) Uani 1 1 d . . . . .
O2B O 0.5349(3) 0.2982(2) 0.47273(19) 0.0391(14) Uani 1 1 d . . . . .
N1A N 0.8546(4) 0.4467(3) 0.6987(3) 0.0471(19) Uani 1 1 d . . . . .
H1A H 0.8679 0.4567 0.6762 0.056 Uiso 1 1 calc R . . . .
N1B N 0.6351(3) 0.4676(3) 0.6657(2) 0.0390(16) Uani 1 1 d . . . . .
H1B H 0.6203 0.4809 0.6863 0.047 Uiso 1 1 calc R . . . .
N2A N 0.8043(3) 0.4617(3) 0.7167(2) 0.0376(16) Uani 1 1 d . . . . .
N2B N 0.6938(3) 0.4708(3) 0.6539(2) 0.0367(16) Uani 1 1 d . . . . .
C1A C 0.8861(4) 0.3148(3) 0.8487(3) 0.0358(18) Uani 1 1 d . . . . .
C1B C 0.6018(4) 0.3308(3) 0.5188(3) 0.0346(18) Uani 1 1 d . . . . .
C2A C 0.9289(4) 0.3459(3) 0.8353(3) 0.0388(19) Uani 1 1 d . . . . .
H2A H 0.9668 0.3461 0.8468 0.047 Uiso 1 1 calc R . . . .
C2B C 0.5654(4) 0.3672(3) 0.5263(3) 0.0369(18) Uani 1 1 d . . . . .
H2B H 0.5308 0.3706 0.5111 0.044 Uiso 1 1 calc R . . . .
C3'A C 0.7983(4) 0.4373(3) 0.7503(3) 0.0374(19) Uani 1 1 d . . . . .
C3'B C 0.6988(4) 0.4454(3) 0.6214(3) 0.041(2) Uani 1 1 d . . . . .
C3A C 0.9155(4) 0.3761(3) 0.8054(3) 0.042(2) Uani 1 1 d . . . . .
H3A H 0.9439 0.3971 0.7976 0.050 Uiso 1 1 calc R . . . .
C3B C 0.5782(4) 0.3986(3) 0.5552(3) 0.0360(18) Uani 1 1 d . . . . .
H3B H 0.5526 0.4228 0.5591 0.043 Uiso 1 1 calc R . . . .
C4'A C 0.8455(4) 0.4075(3) 0.7532(3) 0.043(2) Uani 1 1 d . . . . .
C4'B C 0.6423(4) 0.4253(3) 0.6111(3) 0.0390(19) Uani 1 1 d . . . . .
C4A C 0.8597(4) 0.3755(3) 0.7866(3) 0.0382(19) Uani 1 1 d . . . . .
C4B C 0.6304(4) 0.3941(3) 0.5793(3) 0.0382(19) Uani 1 1 d . . . . .
C5'A C 0.8812(4) 0.4144(4) 0.7199(3) 0.046(2) Uani 1 1 d . . . . .
C5'B C 0.6035(4) 0.4409(3) 0.6410(3) 0.0404(19) Uani 1 1 d . . . . .
C5A C 0.8173(4) 0.3444(4) 0.7996(3) 0.045(2) Uani 1 1 d . . . . .
H5A H 0.7798 0.3436 0.7875 0.054 Uiso 1 1 calc R . . . .
C5B C 0.6677(5) 0.3579(4) 0.5714(3) 0.047(2) Uani 1 1 d . . . . .
H5B H 0.7027 0.3548 0.5862 0.057 Uiso 1 1 calc R . . . .
C6A C 0.8305(4) 0.3147(3) 0.8303(3) 0.041(2) Uani 1 1 d . . . . .
H6A H 0.8015 0.2944 0.8388 0.050 Uiso 1 1 calc R . . . .
C6B C 0.6547(4) 0.3260(3) 0.5422(3) 0.044(2) Uani 1 1 d . . . . .
H6B H 0.6803 0.3018 0.5380 0.053 Uiso 1 1 calc R . . . .
C7A C 0.9011(4) 0.2821(3) 0.8806(3) 0.0362(18) Uani 1 1 d . . . . .
C7B C 0.5865(4) 0.2956(3) 0.4888(3) 0.0393(19) Uani 1 1 d . . . . .
C31A C 0.7466(4) 0.4440(4) 0.7781(3) 0.043(2) Uani 1 1 d . . . . .
H31A H 0.7612 0.4527 0.8040 0.064 Uiso 1 1 calc GR . . . .
H31B H 0.7245 0.4165 0.7804 0.064 Uiso 1 1 calc GR . . . .
H31C H 0.7210 0.4672 0.7678 0.064 Uiso 1 1 calc GR . . . .
C31B C 0.7557(5) 0.4433(5) 0.5992(4) 0.059(3) Uani 1 1 d . . . . .
H31D H 0.7827 0.4233 0.6126 0.089 Uiso 1 1 calc GR . . . .
H31E H 0.7731 0.4728 0.5979 0.089 Uiso 1 1 calc GR . . . .
H31F H 0.7483 0.4326 0.5725 0.089 Uiso 1 1 calc GR . . . .
C51A C 0.9371(5) 0.3913(5) 0.7049(4) 0.061(3) Uani 1 1 d . . . . .
H51A H 0.9684 0.4131 0.7014 0.091 Uiso 1 1 calc GR . . . .
H51B H 0.9289 0.3771 0.6797 0.091 Uiso 1 1 calc GR . . . .
H51C H 0.9496 0.3691 0.7240 0.091 Uiso 1 1 calc GR . . . .
C51B C 0.5390(5) 0.4321(4) 0.6479(4) 0.055(3) Uani 1 1 d . . . . .
H51D H 0.5159 0.4457 0.6269 0.083 Uiso 1 1 calc GR . . . .
H51E H 0.5273 0.4447 0.6732 0.083 Uiso 1 1 calc GR . . . .
H51F H 0.5320 0.4003 0.6481 0.083 Uiso 1 1 calc GR . . . .
O18 O 0.7073(8) 0.5761(7) 0.4976(6) 0.071(5) Uani 0.5 1 d . . . . .
H18A H 0.6784 0.5903 0.4869 0.106 Uiso 0.5 1 d G . . . .
H18B H 0.7101 0.5503 0.4870 0.106 Uiso 0.5 1 d G . . . .
O17 O 0.3431(18) 0.5109(13) 0.3140(10) 0.150(13) Uani 0.5 1 d . . . . .
H17 H 0.3276 0.5337 0.3231 0.225 Uiso 0.5 1 d R . . . .
C16 C 0.4081(13) 0.5019(7) 0.3353(9) 0.063(7) Uani 0.5 1 d . . . . .
H16A H 0.4384 0.5182 0.3211 0.095 Uiso 0.5 1 d R . . . .
H16B H 0.4173 0.4704 0.3348 0.095 Uiso 0.5 1 d R . . . .
H16C H 0.4066 0.5120 0.3626 0.095 Uiso 0.5 1 d R . . . .
O15 O 0.2528(11) 0.5156(8) 0.3775(10) 0.141(16) Uani 0.5 1 d . . . . .
H15 H 0.2499 0.4904 0.3871 0.212 Uiso 0.5 1 calc R . . . .
C14 C 0.1963(7) 0.5301(6) 0.3641(5) 0.038(4) Uani 0.5 1 d . . . . .
H14A H 0.1817 0.5105 0.3434 0.057 Uiso 0.5 1 d R . . . .
H14B H 0.1994 0.5601 0.3538 0.057 Uiso 0.5 1 d R . . . .
H14C H 0.1693 0.5297 0.3864 0.057 Uiso 0.5 1 d R . . . .
O11 O 0.6683(13) 0.6616(10) 0.5097(12) 0.136(12) Uani 0.5 1 d . . . . .
H11 H 0.6686 0.6355 0.5177 0.204 Uiso 0.5 1 calc R . . . .
C10 C 0.6185(12) 0.6697(12) 0.4922(9) 0.078(8) Uani 0.5 1 d . . . . .
H10A H 0.6154 0.6522 0.4681 0.118 Uiso 0.5 1 d R . . . .
H10B H 0.6162 0.7010 0.4857 0.118 Uiso 0.5 1 d R . . . .
H10C H 0.5864 0.6619 0.5100 0.118 Uiso 0.5 1 d R . . . .
O13 O 0.7096(16) 0.5548(8) 0.4180(8) 0.117(10) Uani 0.5 1 d . . . . .
H13 H 0.7008 0.5622 0.4409 0.175 Uiso 0.5 1 calc R . . . .
C12 C 0.7000(17) 0.5897(10) 0.3928(8) 0.083(9) Uani 0.5 1 d . . . . .
H12A H 0.6709 0.5811 0.3731 0.124 Uiso 0.5 1 d R . . . .
H12B H 0.7370 0.5970 0.3797 0.124 Uiso 0.5 1 d R . . . .
H12C H 0.6858 0.6155 0.4072 0.124 Uiso 0.5 1 d R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O2C 1.938(6) 8_554 ?
Zn1 O2C 1.938(6) 11_654 ?
Zn1 N2C 2.044(8) 2_765 ?
Zn1 N2C 2.044(8) . ?
O1C C7C 1.226(12) . ?
O2C Zn1 1.938(6) 15_645 ?
O2C C7C 1.275(12) . ?
N1C H1C 0.8600 . ?
N1C N2C 1.368(11) . ?
N1C C5'C 1.321(12) . ?
N2C C3'C 1.336(12) . ?
C1C C2C 1.384(13) . ?
C1C C6C 1.394(13) . ?
C1C C7C 1.516(12) . ?
C2C H2C 0.9300 . ?
C2C C3C 1.404(14) . ?
C3'C C4'C 1.379(12) . ?
C3'C C31C 1.496(12) . ?
C3C H3C 0.9300 . ?
C3C C4C 1.392(13) . ?
C4'C C4C 1.493(12) . ?
C4'C C5'C 1.412(13) . ?
C4C C5C 1.394(13) . ?
C5'C C51C 1.493(14) . ?
C5C H5C 0.9300 . ?
C5C C6C 1.373(13) . ?
C6C H6C 0.9300 . ?
C31C H31G 0.9600 . ?
C31C H31H 0.9600 . ?
C31C H31I 0.9600 . ?
C51C H51G 0.9600 . ?
C51C H51H 0.9600 . ?
C51C H51I 0.9600 . ?
Zn2 O1D 1.955(7) 4_565 ?
Zn2 O1D 1.955(7) 15_545 ?
Zn2 N2D 1.976(7) . ?
Zn2 N2D 1.976(7) 2_665 ?
O1D Zn2 1.955(7) 11_554 ?
O1D C7D 1.276(11) . ?
O2D C7D 1.236(11) . ?
N1D H1D 0.8600 . ?
N1D N2D 1.358(10) . ?
N1D C5'D 1.335(12) . ?
N2D C3'D 1.332(11) . ?
C1D C2D 1.381(13) . ?
C1D C6D 1.389(13) . ?
C1D C7D 1.496(12) . ?
C2D H2D 0.9300 . ?
C2D C3D 1.385(14) . ?
C3'D C4'D 1.396(13) . ?
C3'D C31D 1.500(13) . ?
C3D H3D 0.9300 . ?
C3D C4D 1.396(13) . ?
C4'D C4D 1.466(13) . ?
C4'D C5'D 1.410(13) . ?
C4D C5D 1.382(13) . ?
C5'D C51D 1.485(13) . ?
C5D H5D 0.9300 . ?
C5D C6D 1.372(13) . ?
C6D H6D 0.9300 . ?
C31D H31J 0.9600 . ?
C31D H31K 0.9600 . ?
C31D H31L 0.9600 . ?
C51D H51J 0.9600 . ?
C51D H51K 0.9600 . ?
C51D H51L 0.9600 . ?
Zn3 O1A 1.947(6) 11_654 ?
Zn3 O2B 1.939(6) 3_655 ?
Zn3 N2A 1.997(7) . ?
Zn3 N2B 1.988(7) . ?
O1A Zn3 1.947(6) 15_645 ?
O1A C7A 1.284(11) . ?
O1B C7B 1.264(12) . ?
O2A C7A 1.258(11) . ?
O2B Zn3 1.939(6) 7_644 ?
O2B C7B 1.276(12) . ?
N1A H1A 0.8600 . ?
N1A N2A 1.351(11) . ?
N1A C5'A 1.334(13) . ?
N1B H1B 0.8600 . ?
N1B N2B 1.373(11) . ?
N1B C5'B 1.344(12) . ?
N2A C3'A 1.343(11) . ?
N2B C3'B 1.325(12) . ?
C1A C2A 1.403(13) . ?
C1A C6A 1.386(13) . ?
C1A C7A 1.484(13) . ?
C1B C2B 1.378(13) . ?
C1B C6B 1.424(13) . ?
C1B C7B 1.488(13) . ?
C2A H2A 0.9300 . ?
C2A C3A 1.375(13) . ?
C2B H2B 0.9300 . ?
C2B C3B 1.375(13) . ?
C3'A C4'A 1.380(14) . ?
C3'A C31A 1.496(13) . ?
C3'B C4'B 1.439(14) . ?
C3'B C31B 1.473(14) . ?
C3A H3A 0.9300 . ?
C3A C4A 1.395(13) . ?
C3B H3B 0.9300 . ?
C3B C4B 1.420(12) . ?
C4'A C4A 1.499(12) . ?
C4'A C5'A 1.384(14) . ?
C4'B C4B 1.437(13) . ?
C4'B C5'B 1.401(13) . ?
C4A C5A 1.394(13) . ?
C4B C5B 1.389(13) . ?
C5'A C51A 1.513(15) . ?
C5'B C51B 1.482(14) . ?
C5A H5A 0.9300 . ?
C5A C6A 1.386(13) . ?
C5B H5B 0.9300 . ?
C5B C6B 1.390(14) . ?
C6A H6A 0.9300 . ?
C6B H6B 0.9300 . ?
C31A H31A 0.9600 . ?
C31A H31B 0.9600 . ?
C31A H31C 0.9600 . ?
C31B H31D 0.9600 . ?
C31B H31E 0.9600 . ?
C31B H31F 0.9600 . ?
C51A H51A 0.9600 . ?
C51A H51B 0.9600 . ?
C51A H51C 0.9600 . ?
C51B H51D 0.9600 . ?
C51B H51E 0.9600 . ?
C51B H51F 0.9600 . ?
O18 H18A 0.8500 . ?
O18 H18B 0.8500 . ?
O17 H17 0.8198 . ?
O17 C16 1.64(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9596 . ?
C16 H16C 0.9593 . ?
O15 H15 0.8200 . ?
O15 C14 1.41(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9602 . ?
C14 H14C 0.9597 . ?
O11 H11 0.8200 . ?
O11 C10 1.28(4) . ?
C10 H10A 0.9598 . ?
C10 H10B 0.9601 . ?
C10 H10C 0.9597 . ?
O13 H13 0.8200 . ?
O13 C12 1.35(3) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9602 . ?
C12 H12C 0.9602 . ?

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
O2C Zn1 O2C 102.6(4) 8_554 11_654 ?
O2C Zn1 N2C 110.8(3) 8_554 2_765 ?
O2C Zn1 N2C 117.3(3) 11_654 2_765 ?
O2C Zn1 N2C 117.3(3) 8_554 . ?
O2C Zn1 N2C 110.8(3) 11_654 . ?
N2C Zn1 N2C 98.9(4) 2_765 . ?
C7C O2C Zn1 128.2(6) . 15_645 ?
N2C N1C H1C 124.1 . . ?
C5'C N1C H1C 124.1 . . ?
C5'C N1C N2C 111.9(7) . . ?
N1C N2C Zn1 115.5(6) . . ?
C3'C N2C Zn1 135.9(6) . . ?
C3'C N2C N1C 105.4(7) . . ?
C2C C1C C6C 118.9(8) . . ?
C2C C1C C7C 121.3(8) . . ?
C6C C1C C7C 119.8(8) . . ?
C1C C2C H2C 120.2 . . ?
C1C C2C C3C 119.5(8) . . ?
C3C C2C H2C 120.2 . . ?
N2C C3'C C4'C 110.9(8) . . ?
N2C C3'C C31C 121.4(8) . . ?
C4'C C3'C C31C 127.8(8) . . ?
C2C C3C H3C 119.4 . . ?
C4C C3C C2C 121.1(9) . . ?
C4C C3C H3C 119.4 . . ?
C3'C C4'C C4C 128.6(8) . . ?
C3'C C4'C C5'C 105.2(8) . . ?
C5'C C4'C C4C 126.2(8) . . ?
C3C C4C C4'C 120.5(8) . . ?
C3C C4C C5C 118.5(9) . . ?
C5C C4C C4'C 120.9(8) . . ?
N1C C5'C C4'C 106.6(8) . . ?
N1C C5'C C51C 122.4(8) . . ?
C4'C C5'C C51C 131.0(8) . . ?
C4C C5C H5C 119.9 . . ?
C6C C5C C4C 120.2(9) . . ?
C6C C5C H5C 119.9 . . ?
C1C C6C H6C 119.2 . . ?
C5C C6C C1C 121.7(9) . . ?
C5C C6C H6C 119.2 . . ?
O1C C7C O2C 125.1(8) . . ?
O1C C7C C1C 119.0(8) . . ?
O2C C7C C1C 115.9(8) . . ?
C3'C C31C H31G 109.5 . . ?
C3'C C31C H31H 109.5 . . ?
C3'C C31C H31I 109.5 . . ?
H31G C31C H31H 109.5 . . ?
H31G C31C H31I 109.5 . . ?
H31H C31C H31I 109.5 . . ?
C5'C C51C H51G 109.5 . . ?
C5'C C51C H51H 109.5 . . ?
C5'C C51C H51I 109.5 . . ?
H51G C51C H51H 109.5 . . ?
H51G C51C H51I 109.5 . . ?
H51H C51C H51I 109.5 . . ?
O1D Zn2 O1D 107.0(5) 4_565 15_545 ?
O1D Zn2 N2D 111.4(3) 15_545 . ?
O1D Zn2 N2D 106.9(3) 4_565 . ?
O1D Zn2 N2D 111.4(3) 4_565 2_665 ?
O1D Zn2 N2D 106.9(3) 15_545 2_665 ?
N2D Zn2 N2D 113.1(4) . 2_665 ?
C7D O1D Zn2 131.2(6) . 11_554 ?
N2D N1D H1D 123.7 . . ?
C5'D N1D H1D 123.7 . . ?
C5'D N1D N2D 112.6(7) . . ?
N1D N2D Zn2 120.3(6) . . ?
C3'D N2D Zn2 134.0(6) . . ?
C3'D N2D N1D 105.5(7) . . ?
C2D C1D C6D 118.7(8) . . ?
C2D C1D C7D 121.6(8) . . ?
C6D C1D C7D 119.7(8) . . ?
C1D C2D H2D 119.6 . . ?
C1D C2D C3D 120.9(9) . . ?
C3D C2D H2D 119.6 . . ?
N2D C3'D C4'D 110.9(8) . . ?
N2D C3'D C31D 120.8(8) . . ?
C4'D C3'D C31D 128.2(8) . . ?
C2D C3D H3D 119.8 . . ?
C2D C3D C4D 120.4(9) . . ?
C4D C3D H3D 119.8 . . ?
C3'D C4'D C4D 128.9(8) . . ?
C3'D C4'D C5'D 105.0(8) . . ?
C5'D C4'D C4D 126.2(8) . . ?
C3D C4D C4'D 120.7(8) . . ?
C5D C4D C3D 117.9(8) . . ?
C5D C4D C4'D 121.4(8) . . ?
N1D C5'D C4'D 106.0(8) . . ?
N1D C5'D C51D 122.9(8) . . ?
C4'D C5'D C51D 131.0(9) . . ?
C4D C5D H5D 119.1 . . ?
C6D C5D C4D 121.8(8) . . ?
C6D C5D H5D 119.1 . . ?
C1D C6D H6D 119.9 . . ?
C5D C6D C1D 120.2(8) . . ?
C5D C6D H6D 119.9 . . ?
O1D C7D C1D 115.5(8) . . ?
O2D C7D O1D 125.3(8) . . ?
O2D C7D C1D 119.2(8) . . ?
C3'D C31D H31J 109.5 . . ?
C3'D C31D H31K 109.5 . . ?
C3'D C31D H31L 109.5 . . ?
H31J C31D H31K 109.5 . . ?
H31J C31D H31L 109.5 . . ?
H31K C31D H31L 109.5 . . ?
C5'D C51D H51J 109.5 . . ?
C5'D C51D H51K 109.5 . . ?
C5'D C51D H51L 109.5 . . ?
H51J C51D H51K 109.5 . . ?
H51J C51D H51L 109.5 . . ?
H51K C51D H51L 109.5 . . ?
O1A Zn3 N2A 109.6(3) 11_654 . ?
O1A Zn3 N2B 106.5(3) 11_654 . ?
O2B Zn3 O1A 105.6(3) 3_655 11_654 ?
O2B Zn3 N2A 111.9(3) 3_655 . ?
O2B Zn3 N2B 113.8(3) 3_655 . ?
N2B Zn3 N2A 109.3(3) . . ?
C7A O1A Zn3 133.6(6) . 15_645 ?
C7B O2B Zn3 127.1(6) . 7_644 ?
N2A N1A H1A 124.1 . . ?
C5'A N1A H1A 124.1 . . ?
C5'A N1A N2A 111.8(8) . . ?
N2B N1B H1B 124.2 . . ?
C5'B N1B H1B 124.2 . . ?
C5'B N1B N2B 111.6(7) . . ?
N1A N2A Zn3 118.6(6) . . ?
C3'A N2A Zn3 134.7(6) . . ?
C3'A N2A N1A 105.9(7) . . ?
N1B N2B Zn3 120.1(6) . . ?
C3'B N2B Zn3 133.7(7) . . ?
C3'B N2B N1B 106.0(7) . . ?
C2A C1A C7A 120.5(8) . . ?
C6A C1A C2A 118.2(8) . . ?
C6A C1A C7A 121.3(8) . . ?
C2B C1B C6B 118.0(8) . . ?
C2B C1B C7B 122.7(8) . . ?
C6B C1B C7B 119.3(8) . . ?
C1A C2A H2A 119.6 . . ?
C3A C2A C1A 120.9(8) . . ?
C3A C2A H2A 119.6 . . ?
C1B C2B H2B 118.7 . . ?
C3B C2B C1B 122.6(8) . . ?
C3B C2B H2B 118.7 . . ?
N2A C3'A C4'A 109.4(8) . . ?
N2A C3'A C31A 121.5(8) . . ?
C4'A C3'A C31A 129.1(9) . . ?
N2B C3'B C4'B 111.0(8) . . ?
N2B C3'B C31B 120.6(9) . . ?
C4'B C3'B C31B 128.2(9) . . ?
C2A C3A H3A 119.6 . . ?
C2A C3A C4A 120.9(8) . . ?
C4A C3A H3A 119.6 . . ?
C2B C3B H3B 119.9 . . ?
C2B C3B C4B 120.3(8) . . ?
C4B C3B H3B 119.9 . . ?
C3'A C4'A C4A 128.6(9) . . ?
C3'A C4'A C5'A 106.7(9) . . ?
C5'A C4'A C4A 124.6(9) . . ?
C4B C4'B C3'B 127.5(9) . . ?
C5'B C4'B C3'B 103.6(8) . . ?
C5'B C4'B C4B 128.7(9) . . ?
C3A C4A C4'A 121.1(8) . . ?
C5A C4A C3A 118.3(8) . . ?
C5A C4A C4'A 120.6(8) . . ?
C3B C4B C4'B 120.6(8) . . ?
C5B C4B C3B 117.3(8) . . ?
C5B C4B C4'B 122.1(8) . . ?
N1A C5'A C4'A 106.2(9) . . ?
N1A C5'A C51A 121.2(9) . . ?
C4'A C5'A C51A 132.5(9) . . ?
N1B C5'B C4'B 107.9(8) . . ?
N1B C5'B C51B 121.2(8) . . ?
C4'B C5'B C51B 130.9(9) . . ?
C4A C5A H5A 119.7 . . ?
C6A C5A C4A 120.7(9) . . ?
C6A C5A H5A 119.7 . . ?
C4B C5B H5B 118.7 . . ?
C4B C5B C6B 122.5(9) . . ?
C6B C5B H5B 118.8 . . ?
C1A C6A H6A 119.5 . . ?
C5A C6A C1A 121.1(9) . . ?
C5A C6A H6A 119.5 . . ?
C1B C6B H6B 120.3 . . ?
C5B C6B C1B 119.3(9) . . ?
C5B C6B H6B 120.3 . . ?
O1A C7A C1A 115.6(8) . . ?
O2A C7A O1A 125.3(8) . . ?
O2A C7A C1A 119.0(8) . . ?
O1B C7B O2B 124.6(9) . . ?
O1B C7B C1B 118.7(8) . . ?
O2B C7B C1B 116.6(8) . . ?
C3'A C31A H31A 109.5 . . ?
C3'A C31A H31B 109.5 . . ?
C3'A C31A H31C 109.5 . . ?
H31A C31A H31B 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C3'B C31B H31D 109.5 . . ?
C3'B C31B H31E 109.5 . . ?
C3'B C31B H31F 109.5 . . ?
H31D C31B H31E 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C5'A C51A H51A 109.5 . . ?
C5'A C51A H51B 109.5 . . ?
C5'A C51A H51C 109.5 . . ?
H51A C51A H51B 109.5 . . ?
H51A C51A H51C 109.5 . . ?
H51B C51A H51C 109.5 . . ?
C5'B C51B H51D 109.5 . . ?
C5'B C51B H51E 109.5 . . ?
C5'B C51B H51F 109.5 . . ?
H51D C51B H51E 109.5 . . ?
H51D C51B H51F 109.5 . . ?
H51E C51B H51F 109.5 . . ?
H18A O18 H18B 109.5 . . ?
C16 O17 H17 110.4 . . ?
O17 C16 H16A 109.1 . . ?
O17 C16 H16B 110.0 . . ?
O17 C16 H16C 109.3 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 O15 H15 109.5 . . ?
O15 C14 H14A 110.4 . . ?
O15 C14 H14B 109.6 . . ?
O15 C14 H14C 108.4 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 O11 H11 109.5 . . ?
O11 C10 H10A 110.1 . . ?
O11 C10 H10B 109.5 . . ?
O11 C10 H10C 108.8 . . ?
H10A C10 H10B 109.4 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 O13 H13 109.5 . . ?
O13 C12 H12A 109.1 . . ?
O13 C12 H12B 108.6 . . ?
O13 C12 H12C 110.8 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.4 . . ?

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
Zn1 O2C C7C O1C 4.1(14) 15_645 . . . ?
Zn1 O2C C7C C1C -174.7(5) 15_645 . . . ?
Zn1 N2C C3'C C4'C 159.8(7) . . . . ?
Zn1 N2C C3'C C31C -19.7(14) . . . . ?
N1C N2C C3'C C4'C 1.9(10) . . . . ?
N1C N2C C3'C C31C -177.5(8) . . . . ?
N2C N1C C5'C C4'C 1.8(10) . . . . ?
N2C N1C C5'C C51C -178.2(8) . . . . ?
N2C C3'C C4'C C4C -179.4(8) . . . . ?
N2C C3'C C4'C C5'C -0.9(10) . . . . ?
C1C C2C C3C C4C -2.1(15) . . . . ?
C2C C1C C6C C5C 2.7(14) . . . . ?
C2C C1C C7C O1C 164.6(9) . . . . ?
C2C C1C C7C O2C -16.4(12) . . . . ?
C2C C3C C4C C4'C -177.8(9) . . . . ?
C2C C3C C4C C5C 1.9(14) . . . . ?
C3'C C4'C C4C C3C -69.1(13) . . . . ?
C3'C C4'C C4C C5C 111.2(11) . . . . ?
C3'C C4'C C5'C N1C -0.6(10) . . . . ?
C3'C C4'C C5'C C51C 179.5(10) . . . . ?
C3C C4C C5C C6C 0.5(13) . . . . ?
C4'C C4C C5C C6C -179.8(8) . . . . ?
C4C C4'C C5'C N1C 178.0(8) . . . . ?
C4C C4'C C5'C C51C -2.0(16) . . . . ?
C4C C5C C6C C1C -2.8(14) . . . . ?
C5'C N1C N2C Zn1 -165.5(6) . . . . ?
C5'C N1C N2C C3'C -2.4(10) . . . . ?
C5'C C4'C C4C C3C 112.7(11) . . . . ?
C5'C C4'C C4C C5C -67.0(12) . . . . ?
C6C C1C C2C C3C -0.2(14) . . . . ?
C6C C1C C7C O1C -16.9(12) . . . . ?
C6C C1C C7C O2C 162.1(8) . . . . ?
C7C C1C C2C C3C 178.3(8) . . . . ?
C7C C1C C6C C5C -175.9(8) . . . . ?
C31C C3'C C4'C C4C 0.0(15) . . . . ?
C31C C3'C C4'C C5'C 178.5(9) . . . . ?
Zn2 O1D C7D O2D -12.1(15) 11_554 . . . ?
Zn2 O1D C7D C1D 169.0(6) 11_554 . . . ?
Zn2 N2D C3'D C4'D -176.0(7) . . . . ?
Zn2 N2D C3'D C31D 5.9(14) . . . . ?
N1D N2D C3'D C4'D -1.8(10) . . . . ?
N1D N2D C3'D C31D -179.9(9) . . . . ?
N2D N1D C5'D C4'D 0.8(11) . . . . ?
N2D N1D C5'D C51D -177.3(10) . . . . ?
N2D C3'D C4'D C4D -177.5(9) . . . . ?
N2D C3'D C4'D C5'D 2.2(10) . . . . ?
C1D C2D C3D C4D -0.6(16) . . . . ?
C2D C1D C6D C5D -3.9(13) . . . . ?
C2D C1D C7D O1D 13.5(13) . . . . ?
C2D C1D C7D O2D -165.5(9) . . . . ?
C2D C3D C4D C4'D 179.0(9) . . . . ?
C2D C3D C4D C5D -1.6(14) . . . . ?
C3'D C4'D C4D C3D 133.0(11) . . . . ?
C3'D C4'D C4D C5D -46.3(14) . . . . ?
C3'D C4'D C5'D N1D -1.8(10) . . . . ?
C3'D C4'D C5'D C51D 176.2(12) . . . . ?
C3D C4D C5D C6D 1.0(13) . . . . ?
C4'D C4D C5D C6D -179.6(8) . . . . ?
C4D C4'D C5'D N1D 178.0(9) . . . . ?
C4D C4'D C5'D C51D -4.1(18) . . . . ?
C4D C5D C6D C1D 1.8(13) . . . . ?
C5'D N1D N2D Zn2 175.8(6) . . . . ?
C5'D N1D N2D C3'D 0.6(10) . . . . ?
C5'D C4'D C4D C3D -46.7(14) . . . . ?
C5'D C4'D C4D C5D 134.0(10) . . . . ?
C6D C1D C2D C3D 3.3(14) . . . . ?
C6D C1D C7D O1D -166.8(8) . . . . ?
C6D C1D C7D O2D 14.2(13) . . . . ?
C7D C1D C2D C3D -176.9(9) . . . . ?
C7D C1D C6D C5D 176.3(8) . . . . ?
C31D C3'D C4'D C4D 0.4(17) . . . . ?
C31D C3'D C4'D C5'D -179.8(10) . . . . ?
Zn3 O1A C7A O2A 10.7(14) 15_645 . . . ?
Zn3 O1A C7A C1A -167.3(6) 15_645 . . . ?
Zn3 O2B C7B O1B 5.4(14) 7_644 . . . ?
Zn3 O2B C7B C1B -173.2(6) 7_644 . . . ?
Zn3 N2A C3'A C4'A 170.3(7) . . . . ?
Zn3 N2A C3'A C31A -9.6(14) . . . . ?
Zn3 N2B C3'B C4'B 175.4(7) . . . . ?
Zn3 N2B C3'B C31B -9.3(15) . . . . ?
N1A N2A C3'A C4'A 0.8(11) . . . . ?
N1A N2A C3'A C31A -179.1(9) . . . . ?
N1B N2B C3'B C4'B 0.7(11) . . . . ?
N1B N2B C3'B C31B 176.1(10) . . . . ?
N2A N1A C5'A C4'A 1.3(12) . . . . ?
N2A N1A C5'A C51A 177.8(10) . . . . ?
N2A C3'A C4'A C4A 176.1(10) . . . . ?
N2A C3'A C4'A C5'A -0.1(12) . . . . ?
N2B N1B C5'B C4'B 0.0(11) . . . . ?
N2B N1B C5'B C51B 179.5(9) . . . . ?
N2B C3'B C4'B C4B -176.6(9) . . . . ?
N2B C3'B C4'B C5'B -0.7(11) . . . . ?
C1A C2A C3A C4A -2.4(14) . . . . ?
C1B C2B C3B C4B -0.7(14) . . . . ?
C2A C1A C6A C5A 0.0(14) . . . . ?
C2A C1A C7A O1A 13.4(13) . . . . ?
C2A C1A C7A O2A -164.7(9) . . . . ?
C2A C3A C4A C4'A -178.4(9) . . . . ?
C2A C3A C4A C5A 1.7(14) . . . . ?
C2B C1B C6B C5B -0.1(15) . . . . ?
C2B C1B C7B O1B 174.7(9) . . . . ?
C2B C1B C7B O2B -6.6(13) . . . . ?
C2B C3B C4B C4'B -176.4(9) . . . . ?
C2B C3B C4B C5B 1.7(14) . . . . ?
C3'A C4'A C4A C3A -125.0(11) . . . . ?
C3'A C4'A C4A C5A 54.9(16) . . . . ?
C3'A C4'A C5'A N1A -0.7(12) . . . . ?
C3'A C4'A C5'A C51A -176.7(12) . . . . ?
C3'B C4'B C4B C3B -137.9(10) . . . . ?
C3'B C4'B C4B C5B 44.1(16) . . . . ?
C3'B C4'B C5'B N1B 0.4(10) . . . . ?
C3'B C4'B C5'B C51B -179.0(11) . . . . ?
C3A C4A C5A C6A -0.3(15) . . . . ?
C3B C4B C5B C6B -2.0(17) . . . . ?
C4'A C4A C5A C6A 179.8(9) . . . . ?
C4'B C4B C5B C6B 176.1(10) . . . . ?
C4A C4'A C5'A N1A -177.0(10) . . . . ?
C4A C4'A C5'A C51A 7(2) . . . . ?
C4A C5A C6A C1A -0.6(16) . . . . ?
C4B C4'B C5'B N1B 176.2(9) . . . . ?
C4B C4'B C5'B C51B -3.1(18) . . . . ?
C4B C5B C6B C1B 1.2(17) . . . . ?
C5'A N1A N2A Zn3 -172.8(7) . . . . ?
C5'A N1A N2A C3'A -1.3(11) . . . . ?
C5'A C4'A C4A C3A 50.5(15) . . . . ?
C5'A C4'A C4A C5A -129.6(12) . . . . ?
C5'B N1B N2B Zn3 -176.0(6) . . . . ?
C5'B N1B N2B C3'B -0.5(10) . . . . ?
C5'B C4'B C4B C3B 47.2(15) . . . . ?
C5'B C4'B C4B C5B -130.9(12) . . . . ?
C6A C1A C2A C3A 1.5(14) . . . . ?
C6A C1A C7A O1A -168.8(9) . . . . ?
C6A C1A C7A O2A 13.1(13) . . . . ?
C6B C1B C2B C3B -0.1(14) . . . . ?
C6B C1B C7B O1B -8.1(13) . . . . ?
C6B C1B C7B O2B 170.5(9) . . . . ?
C7A C1A C2A C3A 179.4(9) . . . . ?
C7A C1A C6A C5A -177.9(9) . . . . ?
C7B C1B C2B C3B 177.0(8) . . . . ?
C7B C1B C6B C5B -177.4(9) . . . . ?
C31A C3'A C4'A C4A -4.0(18) . . . . ?
C31A C3'A C4'A C5'A 179.8(10) . . . . ?
C31B C3'B C4'B C4B 8.5(17) . . . . ?
C31B C3'B C4'B C5'B -175.6(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_csh194
_database_code_depnum_ccdc_archive 'CCDC 1040602'
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_audit_creation_date             2014-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H22 Co N4 O4'
_chemical_formula_sum            'C24 H22 Co N4 O4'
_chemical_formula_weight         489.39
_chemical_absolute_configuration unk
_chemical_melting_point          ?
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'
Co Co -2.3653 3.6143 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 'y, -x, -z'
3 '-x, -y, z'
4 '-y, x, -z'
5 'x, -y+1/2, -z+1/4'
6 '-x, y+1/2, -z+1/4'
7 '-y, -x+1/2, z+1/4'
8 'y, x+1/2, z+1/4'
9 'x+1/2, y+1/2, z+1/2'
10 'y+1/2, -x+1/2, -z+1/2'
11 '-x+1/2, -y+1/2, z+1/2'
12 '-y+1/2, x+1/2, -z+1/2'
13 'x+1/2, -y+1, -z+3/4'
14 '-x+1/2, y+1, -z+3/4'
15 '-y+1/2, -x+1, z+3/4'
16 'y+1/2, x+1, z+3/4'

_symmetry_int_tables_number      122
_cell_length_a                   14.85742(19)
_cell_length_b                   14.85742(19)
_cell_length_c                   39.7127(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8766.3(2)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    5188
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      73.5597
_cell_measurement_theta_min      3.1732
_exptl_absorpt_coefficient_mu    6.476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            13939
_diffrn_reflns_theta_full        65.50
_diffrn_reflns_theta_max         65.50
_diffrn_reflns_theta_min         3.18
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -74.00   21.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313   77.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
  2 omega   54.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0313   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
  3 omega  103.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   77.0000 -120.0000 75

#__ type_ start__ end____ width___ exp.time_
  4 omega  124.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   77.0000  120.0000 54

#__ type_ start__ end____ width___ exp.time_
  5 omega   83.00  139.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   77.0000   30.0000 56

#__ type_ start__ end____ width___ exp.time_
  6 omega  126.00  163.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   77.0000    0.0000 37

#__ type_ start__ end____ width___ exp.time_
  7 omega -114.00  -10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313  -57.0000  150.0000 104

#__ type_ start__ end____ width___ exp.time_
  8 omega -114.00  -10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313  -57.0000  -90.0000 104

#__ type_ start__ end____ width___ exp.time_
  9 omega   33.00  105.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -125.0000  -30.0000 72
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0169132000
_diffrn_orient_matrix_UB_12      -0.0089847000
_diffrn_orient_matrix_UB_13      0.0381158000
_diffrn_orient_matrix_UB_21      -0.0259842000
_diffrn_orient_matrix_UB_22      -0.0995588000
_diffrn_orient_matrix_UB_23      -0.0049057000
_diffrn_orient_matrix_UB_31      0.0989675000
_diffrn_orient_matrix_UB_32      -0.0276145000
_diffrn_orient_matrix_UB_33      0.0051909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_diffrn_standards_number         0
_reflns_number_gt                3286
_reflns_number_total             3736
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         3736
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0418
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0855P)²+3.7978P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1230
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The structure is similar to that reported by Chen et al, Chem Sci 2014, 5,
 4755-4762 for the Zn analogue in the space group I41/acd. These data could
 be satisfactorily modelled in either I-42d or I41/acd, and we found a more
 descriptive model, free from apparant torsional disorder on the phenyl rings,
 could be achieved by modelling the diffraction data in I-42d with Z'=2 and
 the twin law 0 1 0 1 0 0 0 0 -1 (BASF 0.49). As such, the absolute 
 configuration for this compound is a meaningless parameter.
;
_olex2_refinement_description    
;
1. Others
 Fixed U13: Co1(0) Co1A(0)
 Fixed U23: Co1(0) Co1A(0)
 Fixed Uiso: H31A(0.037) H31B(0.037) H31C(0.037) H51D(0.032) H51E(0.032)
 H51F(0.032) H31D(0.034) H31E(0.034) H31F(0.034) H51A(0.033) H51B(0.033)
 H51C(0.033) H2A(0.022) H3A(0.023) H6(0.027) H3(0.023) H5A(0.024) H5(0.024)
 H6A(0.023) H2(0.024) H1A(0.024) H1(0.024)
 Fixed X: Co1(0.5) Co1A(0.5) H31A(0.3255) H31B(0.3817) H31C(0.3795)
 H51D(0.2494) H51E(0.2647) H51F(0.3295) H31D(0.059) H31E(0.1196) H31F(0.0247)
 H51A(0.7047) H51B(0.6343) H51C(0.6784) H2A(0.3239) H3A(0.352) H6(0.4039)
 H3(0.1154) H5A(0.6197) H5(0.3477) H6A(0.5916) H2(0.1765)
 Fixed Y: Co1(1) Co1A(1) H31A(0.6027) H31B(0.5558) H31C(0.5115) H51D(1.2182)
 H51E(1.1859) H51F(1.1501) H31D(0.8499) H31E(0.8372) H31F(0.8876) H51A(0.7492)
 H51B(0.8307) H51C(0.7954) H2A(0.7832) H3A(0.7249) H6(1.0315) H3(0.926)
 H5A(0.7385) H5(1.0472) H6A(0.8041) H2(0.8991)
 Fixed Z: H31A(0.4168) H31B(0.4464) H31C(0.4097) H51D(0.5987) H51E(0.5607)
 H51F(0.59) H31D(0.6039) H31E(0.5709) H31F(0.5684) H51A(0.4263) H51B(0.4256)
 H51C(0.3913) H2A(0.5141) H3A(0.4608) H6(0.4913) H3(0.5179) H5A(0.4785)
 H5(0.5459) H6A(0.5306) H2(0.4644)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 1.0000 0.400051(18) 0.0155(2) Uani 1 2 d S . .
Co1A Co 0.5000 1.0000 0.601149(18) 0.0144(2) Uani 1 2 d S . .
O2A O 0.50132(19) 0.89368(16) 0.57285(6) 0.0215(5) Uani 1 1 d . . .
O2 O 0.40011(18) 1.0017(2) 0.43050(6) 0.0280(6) Uani 1 1 d . . .
N2A N 0.5016(2) 0.60610(18) 0.38283(6) 0.0172(6) Uani 1 1 d . . .
N2 N 0.10396(18) 1.0100(2) 0.61816(6) 0.0159(6) Uani 1 1 d . . .
N1 N 0.15539(19) 1.0848(2) 0.61776(7) 0.0164(6) Uani 1 1 d D . .
N1A N 0.5742(2) 0.6618(2) 0.38152(7) 0.0159(6) Uani 1 1 d D . .
O1A O 0.36126(17) 0.83718(19) 0.57375(6) 0.0257(6) Uani 1 1 d . . .
C1A C 0.4550(2) 0.8018(2) 0.52756(8) 0.0147(7) Uani 1 1 d . . .
C3' C 0.1228(2) 0.9650(2) 0.58947(8) 0.0166(7) Uani 1 1 d . . .
C1 C 0.2951(2) 0.9646(2) 0.47239(8) 0.0154(7) Uani 1 1 d . . .
C7 C 0.3354(3) 0.9496(2) 0.43808(9) 0.0191(7) Uani 1 1 d . . .
C3'A C 0.4606(2) 0.6214(2) 0.41254(8) 0.0150(7) Uani 1 1 d . . .
C4 C 0.2251(2) 0.9923(2) 0.53730(8) 0.0153(7) Uani 1 1 d . . .
C4'A C 0.5081(2) 0.6875(2) 0.43018(8) 0.0150(7) Uani 1 1 d . . .
C4A C 0.4891(2) 0.7252(2) 0.46390(8) 0.0148(7) Uani 1 1 d . . .
C4' C 0.1871(2) 1.0131(2) 0.57071(8) 0.0162(7) Uani 1 1 d . . .
C7A C 0.4369(2) 0.8460(2) 0.56052(8) 0.0176(7) Uani 1 1 d . . .
C5' C 0.2064(2) 1.0903(2) 0.59015(8) 0.0143(7) Uani 1 1 d . . .
O1 O 0.30211(18) 0.89223(18) 0.41896(6) 0.0302(6) Uani 1 1 d . . .
C5'A C 0.5799(2) 0.7114(2) 0.40925(8) 0.0169(7) Uani 1 1 d . . .
C31A C 0.3800(3) 0.5683(3) 0.42217(9) 0.0249(9) Uani 1 1 d . . .
H31A H 0.3255 0.6027 0.4168 0.037 Uiso 1 1 calc R . .
H31B H 0.3817 0.5558 0.4464 0.037 Uiso 1 1 calc R . .
H31C H 0.3795 0.5115 0.4097 0.037 Uiso 1 1 calc R . .
C51 C 0.2677(2) 1.1677(2) 0.58438(10) 0.0213(8) Uani 1 1 d . . .
H51D H 0.2494 1.2182 0.5987 0.032 Uiso 1 1 calc R . .
H51E H 0.2647 1.1859 0.5607 0.032 Uiso 1 1 calc R . .
H51F H 0.3295 1.1501 0.5900 0.032 Uiso 1 1 calc R . .
C31 C 0.0777(3) 0.8775(3) 0.58257(9) 0.0230(8) Uani 1 1 d . . .
H31D H 0.0590 0.8499 0.6039 0.034 Uiso 1 1 calc R . .
H31E H 0.1196 0.8372 0.5709 0.034 Uiso 1 1 calc R . .
H31F H 0.0247 0.8876 0.5684 0.034 Uiso 1 1 calc R . .
C51A C 0.6560(2) 0.7774(2) 0.41346(9) 0.0221(8) Uani 1 1 d . . .
H51A H 0.7047 0.7492 0.4263 0.033 Uiso 1 1 calc R . .
H51B H 0.6343 0.8307 0.4256 0.033 Uiso 1 1 calc R . .
H51C H 0.6784 0.7954 0.3913 0.033 Uiso 1 1 calc R . .
C2A C 0.3842(2) 0.7760(2) 0.50667(8) 0.0186(7) Uani 1 1 d . . .
H2A H 0.3239 0.7832 0.5141 0.022 Uiso 1 1 calc R . .
C3A C 0.4010(2) 0.7399(2) 0.47509(8) 0.0193(7) Uani 1 1 d . . .
H3A H 0.3520 0.7249 0.4608 0.023 Uiso 1 1 calc R . .
C6 C 0.3459(2) 1.0089(2) 0.49671(8) 0.0225(7) Uani 1 1 d . . .
H6 H 0.4039 1.0315 0.4913 0.027 Uiso 1 1 calc R . .
C3 C 0.1743(2) 0.9467(2) 0.51267(8) 0.0193(7) Uani 1 1 d . . .
H3 H 0.1154 0.9260 0.5179 0.023 Uiso 1 1 calc R . .
C5A C 0.5594(2) 0.7489(2) 0.48537(8) 0.0199(7) Uani 1 1 d . . .
H5A H 0.6197 0.7385 0.4785 0.024 Uiso 1 1 calc R . .
C5 C 0.3113(2) 1.0200(2) 0.52907(8) 0.0196(7) Uani 1 1 d . . .
H5 H 0.3477 1.0472 0.5459 0.024 Uiso 1 1 calc R . .
C6A C 0.5425(2) 0.7874(2) 0.51657(8) 0.0188(7) Uani 1 1 d . . .
H6A H 0.5916 0.8041 0.5306 0.023 Uiso 1 1 calc R . .
C2 C 0.2102(2) 0.9318(2) 0.48062(8) 0.0198(7) Uani 1 1 d . . .
H2 H 0.1765 0.8991 0.4644 0.024 Uiso 1 1 calc R . .
H1A H 0.605(2) 0.664(3) 0.3638(7) 0.024 Uiso 1 1 d D . .
H1 H 0.150(3) 1.123(2) 0.6330(8) 0.024 Uiso 1 1 d D . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 1.915(2) . ?
Co1 O2 1.914(2) 3_675 ?
Co1 N2 2.003(3) 16_454 ?
Co1 N2 2.003(3) 15_654 ?
Co1A O2A 1.939(2) . ?
Co1A O2A 1.939(2) 3_675 ?
Co1A N2A 2.017(3) 7_665 ?
Co1A N2A 2.017(3) 8 ?
O2A C7A 1.288(4) . ?
O2 C7 1.271(5) . ?
N2A Co1A 2.017(3) 15_654 ?
N2A N1A 1.361(4) . ?
N2A C3'A 1.347(4) . ?
N2 Co1 2.003(3) 7_665 ?
N2 N1 1.350(4) . ?
N2 C3' 1.350(4) . ?
N1 C5' 1.335(4) . ?
N1 H1 0.837(19) . ?
N1A C5'A 1.327(4) . ?
N1A H1A 0.837(19) . ?
O1A C7A 1.247(4) . ?
C1A C7A 1.489(5) . ?
C1A C2A 1.394(5) . ?
C1A C6A 1.388(5) . ?
C3' C4' 1.406(5) . ?
C3' C31 1.489(5) . ?
C1 C7 1.505(5) . ?
C1 C6 1.391(5) . ?
C1 C2 1.391(5) . ?
C7 O1 1.244(4) . ?
C3'A C4'A 1.398(5) . ?
C3'A C31A 1.484(5) . ?
C4 C4' 1.475(4) . ?
C4 C3 1.410(5) . ?
C4 C5 1.384(5) . ?
C4'A C4A 1.479(4) . ?
C4'A C5'A 1.398(5) . ?
C4A C3A 1.398(5) . ?
C4A C5A 1.393(5) . ?
C4' C5' 1.413(5) . ?
C5' C51 1.484(5) . ?
C5'A C51A 1.506(5) . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C51 H51D 0.9800 . ?
C51 H51E 0.9800 . ?
C51 H51F 0.9800 . ?
C31 H31D 0.9800 . ?
C31 H31E 0.9800 . ?
C31 H31F 0.9800 . ?
C51A H51A 0.9800 . ?
C51A H51B 0.9800 . ?
C51A H51C 0.9800 . ?
C2A H2A 0.9500 . ?
C2A C3A 1.387(5) . ?
C3A H3A 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.394(5) . ?
C3 H3 0.9500 . ?
C3 C2 1.398(5) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.387(5) . ?
C5 H5 0.9500 . ?
C6A H6A 0.9500 . ?
C2 H2 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O2 101.67(17) 3_675 . ?
O2 Co1 N2 110.64(12) . 15_654 ?
O2 Co1 N2 116.50(13) 3_675 15_654 ?
O2 Co1 N2 110.63(12) 3_675 16_454 ?
O2 Co1 N2 116.50(13) . 16_454 ?
N2 Co1 N2 101.57(16) 15_654 16_454 ?
O2A Co1A O2A 109.16(15) 3_675 . ?
O2A Co1A N2A 111.09(12) 3_675 8 ?
O2A Co1A N2A 111.29(13) . 8 ?
O2A Co1A N2A 111.09(12) . 7_665 ?
O2A Co1A N2A 111.29(13) 3_675 7_665 ?
N2A Co1A N2A 102.83(16) 8 7_665 ?
C7A O2A Co1A 131.4(2) . . ?
C7 O2 Co1 136.7(2) . . ?
N1A N2A Co1A 117.4(2) . 15_654 ?
C3'A N2A Co1A 132.3(3) . 15_654 ?
C3'A N2A N1A 106.8(3) . . ?
N1 N2 Co1 120.3(2) . 7_665 ?
N1 N2 C3' 106.3(3) . . ?
C3' N2 Co1 131.0(2) . 7_665 ?
N2 N1 H1 120(3) . . ?
C5' N1 N2 112.4(3) . . ?
C5' N1 H1 127(3) . . ?
N2A N1A H1A 119(3) . . ?
C5'A N1A N2A 110.9(3) . . ?
C5'A N1A H1A 130(3) . . ?
C2A C1A C7A 120.5(3) . . ?
C6A C1A C7A 120.9(3) . . ?
C6A C1A C2A 118.5(3) . . ?
N2 C3' C4' 109.7(3) . . ?
N2 C3' C31 119.6(3) . . ?
C4' C3' C31 130.7(3) . . ?
C6 C1 C7 118.9(3) . . ?
C6 C1 C2 119.6(3) . . ?
C2 C1 C7 121.4(3) . . ?
O2 C7 C1 115.1(3) . . ?
O1 C7 O2 125.0(3) . . ?
O1 C7 C1 119.7(3) . . ?
N2A C3'A C4'A 109.2(3) . . ?
N2A C3'A C31A 120.1(3) . . ?
C4'A C3'A C31A 130.7(3) . . ?
C3 C4 C4' 121.3(3) . . ?
C5 C4 C4' 120.3(3) . . ?
C5 C4 C3 118.4(3) . . ?
C3'A C4'A C4A 128.5(3) . . ?
C3'A C4'A C5'A 105.4(3) . . ?
C5'A C4'A C4A 126.0(3) . . ?
C3A C4A C4'A 121.7(3) . . ?
C5A C4A C4'A 120.4(3) . . ?
C5A C4A C3A 117.8(3) . . ?
C3' C4' C4 129.1(3) . . ?
C3' C4' C5' 105.2(3) . . ?
C5' C4' C4 125.7(3) . . ?
O2A C7A C1A 116.3(3) . . ?
O1A C7A O2A 124.5(3) . . ?
O1A C7A C1A 119.2(3) . . ?
N1 C5' C4' 106.5(3) . . ?
N1 C5' C51 121.5(3) . . ?
C4' C5' C51 132.0(3) . . ?
N1A C5'A C4'A 107.7(3) . . ?
N1A C5'A C51A 120.1(3) . . ?
C4'A C5'A C51A 132.2(3) . . ?
C3'A C31A H31A 109.5 . . ?
C3'A C31A H31B 109.5 . . ?
C3'A C31A H31C 109.5 . . ?
H31A C31A H31B 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C5' C51 H51D 109.5 . . ?
C5' C51 H51E 109.5 . . ?
C5' C51 H51F 109.5 . . ?
H51D C51 H51E 109.5 . . ?
H51D C51 H51F 109.5 . . ?
H51E C51 H51F 109.5 . . ?
C3' C31 H31D 109.5 . . ?
C3' C31 H31E 109.5 . . ?
C3' C31 H31F 109.5 . . ?
H31D C31 H31E 109.5 . . ?
H31D C31 H31F 109.5 . . ?
H31E C31 H31F 109.5 . . ?
C5'A C51A H51A 109.5 . . ?
C5'A C51A H51B 109.5 . . ?
C5'A C51A H51C 109.5 . . ?
H51A C51A H51B 109.5 . . ?
H51A C51A H51C 109.5 . . ?
H51B C51A H51C 109.5 . . ?
C1A C2A H2A 119.7 . . ?
C3A C2A C1A 120.6(3) . . ?
C3A C2A H2A 119.7 . . ?
C4A C3A H3A 119.5 . . ?
C2A C3A C4A 121.1(3) . . ?
C2A C3A H3A 119.5 . . ?
C1 C6 H6 120.1 . . ?
C1 C6 C5 119.8(3) . . ?
C5 C6 H6 120.1 . . ?
C4 C3 H3 119.9 . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 H3 119.9 . . ?
C4A C5A H5A 119.5 . . ?
C6A C5A C4A 121.0(3) . . ?
C6A C5A H5A 119.5 . . ?
C4 C5 C6 121.6(3) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C1A C6A H6A 119.6 . . ?
C5A C6A C1A 120.9(3) . . ?
C5A C6A H6A 119.6 . . ?
C1 C2 C3 120.3(3) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?

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
N1A H1A O1A 0.837(19) 1.85(2) 2.667(4) 166(4) 15_654
N1 H1 O1 0.837(19) 1.91(2) 2.731(4) 165(4) 7_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
Co1 O2 C7 C1 157.3(3) . . . . ?
Co1 O2 C7 O1 -26.2(6) . . . . ?
Co1 N2 N1 C5' -164.5(2) 7_665 . . . ?
Co1 N2 C3' C4' 162.0(3) 7_665 . . . ?
Co1 N2 C3' C31 -18.9(5) 7_665 . . . ?
Co1A O2A C7A O1A -28.5(5) . . . . ?
Co1A O2A C7A C1A 149.2(2) . . . . ?
Co1A N2A N1A C5'A -161.7(2) 15_654 . . . ?
Co1A N2A C3'A C4'A 157.7(3) 15_654 . . . ?
Co1A N2A C3'A C31A -20.1(5) 15_654 . . . ?
O2A Co1A O2A C7A -90.3(3) 3_675 . . . ?
O2 Co1 O2 C7 -114.7(4) 3_675 . . . ?
N2A Co1A O2A C7A 146.7(3) 8 . . . ?
N2A Co1A O2A C7A 32.8(3) 7_665 . . . ?
N2A N1A C5'A C4'A 0.2(4) . . . . ?
N2A N1A C5'A C51A 179.4(3) . . . . ?
N2A C3'A C4'A C4A -179.2(3) . . . . ?
N2A C3'A C4'A C5'A 0.3(4) . . . . ?
N2 Co1 O2 C7 9.6(4) 15_654 . . . ?
N2 Co1 O2 C7 124.9(4) 16_454 . . . ?
N2 N1 C5' C4' 0.2(4) . . . . ?
N2 N1 C5' C51 179.5(3) . . . . ?
N2 C3' C4' C4 -177.3(3) . . . . ?
N2 C3' C4' C5' 0.3(4) . . . . ?
N1 N2 C3' C4' -0.2(4) . . . . ?
N1 N2 C3' C31 178.9(3) . . . . ?
N1A N2A C3'A C4'A -0.1(4) . . . . ?
N1A N2A C3'A C31A -177.9(3) . . . . ?
C1A C2A C3A C4A 2.5(5) . . . . ?
C3' N2 N1 C5' 0.0(4) . . . . ?
C3' C4' C5' N1 -0.3(4) . . . . ?
C3' C4' C5' C51 -179.5(4) . . . . ?
C1 C6 C5 C4 -3.6(5) . . . . ?
C7 C1 C6 C5 -177.2(3) . . . . ?
C7 C1 C2 C3 -180.0(3) . . . . ?
C3'A N2A N1A C5'A -0.1(4) . . . . ?
C3'A C4'A C4A C3A -37.1(5) . . . . ?
C3'A C4'A C4A C5A 144.2(4) . . . . ?
C3'A C4'A C5'A N1A -0.3(4) . . . . ?
C3'A C4'A C5'A C51A -179.3(4) . . . . ?
C4 C4' C5' N1 177.4(3) . . . . ?
C4 C4' C5' C51 -1.8(6) . . . . ?
C4 C3 C2 C1 -2.3(5) . . . . ?
C4'A C4A C3A C2A -179.4(3) . . . . ?
C4'A C4A C5A C6A 177.6(3) . . . . ?
C4A C4'A C5'A N1A 179.2(3) . . . . ?
C4A C4'A C5'A C51A 0.2(6) . . . . ?
C4A C5A C6A C1A 1.3(5) . . . . ?
C4' C4 C3 C2 176.7(3) . . . . ?
C4' C4 C5 C6 -173.8(3) . . . . ?
C7A C1A C2A C3A 176.1(3) . . . . ?
C7A C1A C6A C5A -177.9(3) . . . . ?
C5'A C4'A C4A C3A 143.6(4) . . . . ?
C5'A C4'A C4A C5A -35.1(5) . . . . ?
C31A C3'A C4'A C4A -1.7(6) . . . . ?
C31A C3'A C4'A C5'A 177.7(4) . . . . ?
C31 C3' C4' C4 3.8(6) . . . . ?
C31 C3' C4' C5' -178.6(4) . . . . ?
C2A C1A C7A O2A -157.6(3) . . . . ?
C2A C1A C7A O1A 20.2(5) . . . . ?
C2A C1A C6A C5A 0.6(5) . . . . ?
C3A C4A C5A C6A -1.2(5) . . . . ?
C6 C1 C7 O2 -21.1(5) . . . . ?
C6 C1 C7 O1 162.3(3) . . . . ?
C6 C1 C2 C3 2.9(5) . . . . ?
C3 C4 C4' C3' 31.1(6) . . . . ?
C3 C4 C4' C5' -146.1(4) . . . . ?
C3 C4 C5 C6 4.1(5) . . . . ?
C5A C4A C3A C2A -0.7(5) . . . . ?
C5 C4 C4' C3' -151.1(4) . . . . ?
C5 C4 C4' C5' 31.8(5) . . . . ?
C5 C4 C3 C2 -1.2(5) . . . . ?
C6A C1A C7A O2A 20.8(5) . . . . ?
C6A C1A C7A O1A -161.3(3) . . . . ?
C6A C1A C2A C3A -2.4(5) . . . . ?
C2 C1 C7 O2 161.7(3) . . . . ?
C2 C1 C7 O1 -14.9(5) . . . . ?
C2 C1 C6 C5 0.0(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_h11adb06
_database_code_depnum_ccdc_archive 'CCDC 1040603'
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_audit_creation_date             2014-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C13 H15 Cd0.5 N2 O3, 1.8(C O)'
_chemical_formula_sum            'C14.80 H22.20 Cd0.50 N2 O4.80'
_chemical_formula_weight         361.15
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_properties_physical    'Loses solvent immediately.'
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'
O O 0.0106 0.0060 '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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
# end Validation Reply Form
#===END
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_symmetry_int_tables_number      15
_cell_length_a                   15.2670(4)
_cell_length_b                   21.2820(4)
_cell_length_c                   12.6080(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.841(2)
_cell_angle_gamma                90.00
_cell_volume                     3553.34(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    98871
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1499
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29301
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.83
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  '95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3659
_reflns_number_total             4032
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4032
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0342
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0493P)²+6.2410P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0929
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

The asymmetric unit comprises 1/2 of a Cd centre (located on a 
crystallographic 2 fold rotation axis) one mono-anionic ligand, 
a methanol ligand and some diffuse solvent.

The alcoholic hydrogen in the ligated methanol was readily 
located and refined at a distance of 0.95 Å from O3.

The guest solvent was modelled as a total of 1.8 methanol 
units. The solvent fragments based on C9 and C10 have 
occupancies of 50% with the oxygen in the former disordered 
in a 35:15 ratio. The third solvent moiety containing C8 
has 80% occupancy and  also exhibits disorder of the 
oxygen over 2 sites -- this time in a 50:30 ratio. 
C-O distances in the disordered guest solvent were 
refined subject to being similar. ADP restraints were 
also added for the fractional occupancy O4B, to assist 
convergence. Hydrogens in the disordered solvent region 
could not be reliably located and hence were omitted from 
the refinement.  
;
_olex2_refinement_description    
;
1. Others
 Fixed Sof: O6(0.5) O4A(0.35) O5A(0.5) O4B(0.15) O5B(0.3) C8(0.8) C9(0.5)
 Fixed U12: Cd1(0) C10(0)
 Fixed U23: Cd1(0) C10(0)
 Fixed Uiso: H1(0.032) H2(0.034) H3(0.034) H5(0.04) H6(0.039) H11A(0.08)
 H11B(0.08) H11C(0.08) H31A(0.053) H31B(0.053) H31C(0.053) H51A(0.061)
 H51B(0.061) H51C(0.061)
 Fixed X: Cd1(0.5) H1(0.7375) H2(0.714) H3(0.6709) H5(0.8352) H6(0.8871)
 C10(1) H11A(0.4432) H11B(0.4582) H11C(0.5421) H31A(0.467) H31B(0.5226)
 H31C(0.5237) H51A(0.9057) H51B(0.9269) H51C(0.8996)
 Fixed Y: H1(0.6938) H2(0.4031) H3(0.5037) H5(0.4764) H6(0.3793) H11A(0.7488)
 H11B(0.6742) H11C(0.7181) H31A(0.584) H31B(0.5176) H31C(0.5668) H51A(0.6544)
 H51B(0.5977) H51C(0.5833)
 Fixed Z: Cd1(0.25) H1(0.3979) H2(0.0521) H3(0.0848) H5(0.4504) H6(0.4176)
 C10(0.25) H11A(-0.0879) H11B(-0.0808) H11C(0.0231) H31A(0.1212) H31B(0.1423)
 H31C(0.047) H51A(0.4984) H51B(0.4309) H51C(0.5358)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
Cd1 Cd 0.5000 0.720424(10) 0.2500 0.02159(11) Uani 1 2 d S . .
O1 O 0.78136(14) 0.28929(8) 0.11193(16) 0.0280(4) Uani 1 1 d . . .
O2 O 0.92123(14) 0.29751(9) 0.29342(17) 0.0352(4) Uani 1 1 d . . .
O3 O 0.41901(15) 0.70781(10) 0.03580(18) 0.0363(4) Uani 1 1 d D . .
O6 O 1.0337(7) 0.6021(5) 0.3094(8) 0.139(4) Uani 0.50 1 d PD . .
O4A O 0.8798(7) 0.8211(4) 0.1456(8) 0.078(2) Uani 0.35 1 d PD A 2
O5A O 0.8854(6) 0.6893(5) 0.1580(8) 0.116(3) Uani 0.50 1 d PD B 1
O4B O 0.877(3) 0.8802(19) 0.0587(11) 0.155(13) Uani 0.15 1 d PDU A 1
O5B O 0.7928(10) 0.7114(5) 0.1556(9) 0.101(5) Uani 0.30 1 d PD B 2
N1 N 0.71697(15) 0.65866(10) 0.35589(19) 0.0263(4) Uani 1 1 d . . .
H1 H 0.7375 0.6938 0.3979 0.032 Uiso 1 1 calc R . .
N2 N 0.62071(15) 0.64838(9) 0.26549(19) 0.0263(4) Uani 1 1 d . . .
C1 C 0.80460(18) 0.38115(11) 0.2315(2) 0.0261(5) Uani 1 1 d . . .
C2 C 0.74014(19) 0.41829(11) 0.1331(2) 0.0282(5) Uani 1 1 d . . .
H2 H 0.7140 0.4031 0.0521 0.034 Uiso 1 1 calc R . .
C3 C 0.71362(19) 0.47803(11) 0.1529(2) 0.0286(5) Uani 1 1 d . . .
H3 H 0.6709 0.5037 0.0848 0.034 Uiso 1 1 calc R . .
C4 C 0.74885(18) 0.50083(11) 0.2714(2) 0.0266(5) Uani 1 1 d . . .
C5 C 0.8120(2) 0.46237(12) 0.3691(2) 0.0332(6) Uani 1 1 d . . .
H5 H 0.8352 0.4764 0.4504 0.040 Uiso 1 1 calc R . .
C6 C 0.8414(2) 0.40401(12) 0.3497(2) 0.0327(6) Uani 1 1 d . . .
H6 H 0.8871 0.3793 0.4176 0.039 Uiso 1 1 calc R . .
C7 C 0.83762(18) 0.31781(11) 0.2102(2) 0.0255(5) Uani 1 1 d . . .
C8 C 0.7894(6) 0.6621(4) 0.0808(8) 0.118(3) Uani 0.80 1 d PD . .
C9 C 0.9250(9) 0.8808(5) 0.1884(10) 0.092(3) Uani 0.50 1 d PD . .
C10 C 1.0000 0.5428(5) 0.2500 0.108(3) Uani 1 2 d SD . .
C11 C 0.4695(3) 0.71262(18) -0.0328(3) 0.0533(9) Uani 1 1 d . . .
H11A H 0.4432 0.7488 -0.0879 0.080 Uiso 1 1 calc R . .
H11B H 0.4582 0.6742 -0.0808 0.080 Uiso 1 1 calc R . .
H11C H 0.5421 0.7181 0.0231 0.080 Uiso 1 1 calc R . .
C31 C 0.5252(2) 0.56226(12) 0.1253(3) 0.0356(6) Uani 1 1 d . . .
H31A H 0.4670 0.5840 0.1212 0.053 Uiso 1 1 calc R . .
H31B H 0.5226 0.5176 0.1423 0.053 Uiso 1 1 calc R . .
H31C H 0.5237 0.5668 0.0470 0.053 Uiso 1 1 calc R . .
C51 C 0.8868(2) 0.61134(14) 0.4678(3) 0.0406(7) Uani 1 1 d . . .
H51A H 0.9057 0.6544 0.4984 0.061 Uiso 1 1 calc R . .
H51B H 0.9269 0.5977 0.4309 0.061 Uiso 1 1 calc R . .
H51C H 0.8996 0.5833 0.5358 0.061 Uiso 1 1 calc R . .
C3' C 0.62049(18) 0.59038(11) 0.2249(2) 0.0264(5) Uani 1 1 d . . .
C4' C 0.71783(18) 0.56362(11) 0.2902(2) 0.0255(5) Uani 1 1 d . . .
C5' C 0.77731(19) 0.60931(11) 0.3741(2) 0.0274(5) Uani 1 1 d . . .
H3A H 0.3483(7) 0.7033(19) -0.016(3) 0.066(12) Uiso 1 1 d D . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O2 2.2565(18) 4_655 ?
Cd1 O2 2.2565(18) 3_455 ?
Cd1 O3 2.3604(19) . ?
Cd1 O3 2.3604(19) 2_655 ?
Cd1 N2 2.329(2) 2_655 ?
Cd1 N2 2.329(2) . ?
O1 C7 1.258(3) . ?
O2 Cd1 2.2566(18) 3_545 ?
O2 C7 1.259(3) . ?
O3 C11 1.420(4) . ?
O3 H3A 0.948(5) . ?
O6 O6 1.330(16) 2_755 ?
O6 C10 1.426(5) . ?
O4A C9 1.419(5) . ?
O5A C8 1.418(5) . ?
O4B C9 1.420(5) . ?
O5B C8 1.393(5) . ?
N1 H1 0.8800 . ?
N1 N2 1.356(3) . ?
N1 C5' 1.339(3) . ?
N2 C3' 1.336(3) . ?
C1 C2 1.384(3) . ?
C1 C6 1.393(4) . ?
C1 C7 1.509(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.394(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.399(3) . ?
C4 C5 1.391(3) . ?
C4 C4' 1.476(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.383(3) . ?
C6 H6 0.9500 . ?
C9 C9 2.03(2) 2_755 ?
C10 O6 1.426(5) 2_755 ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C31 C3' 1.494(3) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C51 C5' 1.492(4) . ?
C3' C4' 1.412(3) . ?
C4' C5' 1.390(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
O2 Cd1 O2 86.74(11) 4_655 3_455 ?
O2 Cd1 O3 108.74(7) 4_655 2_655 ?
O2 Cd1 O3 81.03(7) 3_455 2_655 ?
O2 Cd1 O3 81.03(7) 4_655 . ?
O2 Cd1 O3 108.74(7) 3_455 . ?
O2 Cd1 N2 162.36(7) 4_655 2_655 ?
O2 Cd1 N2 90.22(8) 4_655 . ?
O2 Cd1 N2 162.36(7) 3_455 . ?
O2 Cd1 N2 90.22(8) 3_455 2_655 ?
O3 Cd1 O3 166.94(10) . 2_655 ?
N2 Cd1 O3 83.52(7) . 2_655 ?
N2 Cd1 O3 83.52(7) 2_655 . ?
N2 Cd1 O3 87.89(7) 2_655 2_655 ?
N2 Cd1 O3 87.89(7) . . ?
N2 Cd1 N2 97.68(10) 2_655 . ?
C7 O2 Cd1 119.27(16) . 3_545 ?
Cd1 O3 H3A 125(3) . . ?
C11 O3 Cd1 123.66(19) . . ?
C11 O3 H3A 111(3) . . ?
O6 O6 C10 62.2(4) 2_755 . ?
N2 N1 H1 123.7 . . ?
C5' N1 H1 123.7 . . ?
C5' N1 N2 112.5(2) . . ?
N1 N2 Cd1 116.45(14) . . ?
C3' N2 Cd1 136.48(17) . . ?
C3' N2 N1 105.43(19) . . ?
C2 C1 C6 119.2(2) . . ?
C2 C1 C7 120.1(2) . . ?
C6 C1 C7 120.6(2) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.1(2) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 121.1(2) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 C4' 120.1(2) . . ?
C5 C4 C3 118.1(2) . . ?
C5 C4 C4' 121.8(2) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 120.9(2) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.6(2) . . ?
C5 C6 H6 119.7 . . ?
O1 C7 O2 124.6(2) . . ?
O1 C7 C1 118.8(2) . . ?
O2 C7 C1 116.6(2) . . ?
O5B C8 O5A 63.3(7) . . ?
O4A C9 O4B 71.3(17) . . ?
O4A C9 C9 116.2(6) . 2_755 ?
O4B C9 C9 128.3(19) . 2_755 ?
O6 C10 O6 55.6(8) . 2_755 ?
O3 C11 H11A 109.5 . . ?
O3 C11 H11B 109.5 . . ?
O3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C3' C31 H31A 109.5 . . ?
C3' C31 H31B 109.5 . . ?
C3' C31 H31C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C5' C51 H51A 109.5 . . ?
C5' C51 H51B 109.5 . . ?
C5' C51 H51C 109.5 . . ?
N2 C3' C31 120.5(2) . . ?
N2 C3' C4' 110.4(2) . . ?
C4' C3' C31 129.1(2) . . ?
C3' C4' C4 126.9(2) . . ?
C5' C4' C4 128.0(2) . . ?
C5' C4' C3' 105.1(2) . . ?
N1 C5' C51 121.1(2) . . ?
N1 C5' C4' 106.5(2) . . ?
C4' C5' C51 132.3(2) . . ?

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
Cd1 O2 C7 O1 18.2(4) 3_545 . . . ?
Cd1 O2 C7 C1 -161.34(17) 3_545 . . . ?
Cd1 N2 C3' C31 14.8(4) . . . . ?
Cd1 N2 C3' C4' -164.20(19) . . . . ?
O2 Cd1 O3 C11 40.0(2) 4_655 . . . ?
O2 Cd1 O3 C11 123.4(2) 3_455 . . . ?
O2 Cd1 N2 N1 63.43(17) 4_655 . . . ?
O2 Cd1 N2 N1 -16.5(4) 3_455 . . . ?
O2 Cd1 N2 C3' 146.3(3) 3_455 . . . ?
O2 Cd1 N2 C3' -133.8(3) 4_655 . . . ?
O3 Cd1 O3 C11 -99.4(2) 2_655 . . . ?
O3 Cd1 N2 N1 144.45(17) . . . . ?
O3 Cd1 N2 N1 -45.41(17) 2_655 . . . ?
O3 Cd1 N2 C3' 117.4(3) 2_655 . . . ?
O3 Cd1 N2 C3' -52.8(3) . . . . ?
N1 N2 C3' C31 178.8(2) . . . . ?
N1 N2 C3' C4' -0.1(3) . . . . ?
N2 Cd1 O3 C11 -148.6(2) 2_655 . . . ?
N2 Cd1 O3 C11 -50.6(2) . . . . ?
N2 Cd1 N2 N1 -132.38(19) 2_655 . . . ?
N2 Cd1 N2 C3' 30.4(2) 2_655 . . . ?
N2 N1 C5' C51 178.8(2) . . . . ?
N2 N1 C5' C4' 0.5(3) . . . . ?
N2 C3' C4' C4 -179.0(2) . . . . ?
N2 C3' C4' C5' 0.4(3) . . . . ?
C1 C2 C3 C4 -1.9(4) . . . . ?
C2 C1 C6 C5 1.7(4) . . . . ?
C2 C1 C7 O1 -26.1(4) . . . . ?
C2 C1 C7 O2 153.5(3) . . . . ?
C2 C3 C4 C5 0.6(4) . . . . ?
C2 C3 C4 C4' -178.5(2) . . . . ?
C3 C4 C5 C6 1.8(4) . . . . ?
C3 C4 C4' C3' 41.5(4) . . . . ?
C3 C4 C4' C5' -137.8(3) . . . . ?
C4 C5 C6 C1 -3.0(4) . . . . ?
C4 C4' C5' N1 178.9(2) . . . . ?
C4 C4' C5' C51 0.8(5) . . . . ?
C5 C4 C4' C3' -137.6(3) . . . . ?
C5 C4 C4' C5' 43.2(4) . . . . ?
C6 C1 C2 C3 0.7(4) . . . . ?
C6 C1 C7 O1 156.4(3) . . . . ?
C6 C1 C7 O2 -24.0(4) . . . . ?
C7 C1 C2 C3 -176.9(2) . . . . ?
C7 C1 C6 C5 179.3(3) . . . . ?
C31 C3' C4' C4 2.2(5) . . . . ?
C31 C3' C4' C5' -178.4(3) . . . . ?
C3' C4' C5' N1 -0.5(3) . . . . ?
C3' C4' C5' C51 -178.5(3) . . . . ?
C4' C4 C5 C6 -179.1(3) . . . . ?
C5' N1 N2 Cd1 167.60(17) . . . . ?
C5' N1 N2 C3' -0.2(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT430_h11adb06            
;
PROBLEM: Short Inter D...A Contact  O5A    ..  O6      ..       2.15 Ang.  
RESPONSE: O5A, O5B and C8 are a disordered and partially occupied 
guest methanol molecule with 80% occupancy with the oxygen atoms 
disordered in a 50:30 ratio. Similarly O6 and C10 are another partially 
occupied guest methanol molecule with 50% occupancy and with C10 laying 
on a 2 fold screw axis. The result is an artifactual D...A contact from 
the positions of the disordered and partially occupied oxygen atoms and is 
not representative of a true or persistent interaction. As such it can be 
satisfactorily accepted in the model.
;
####################################################################### 
# 
# 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_c2m-sr
_database_code_depnum_ccdc_archive 'CCDC 1040604'
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_audit_creation_date             2014-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H26 Cu2 N4 O10 S'
_chemical_formula_sum            'C24 H26 Cu2 N4 O10 S'
_chemical_formula_weight         689.63
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3280 1.2590 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z'
5 '-x, -y, -z'
6 'x, -y, z'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z'

_symmetry_int_tables_number      12
_cell_length_a                   32.685(7)
_cell_length_b                   29.520(6)
_cell_length_c                   9.7350(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.71(3)
_cell_angle_gamma                90.00
_cell_volume                     9125(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.004
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 Crystals were collected using a single 360 degree phi scan on the 
Australian Synchrotron MX1 beamline. The crystals were extremely 
weakly diffracting and as a result, reflections were only observed 
to a theta value of 22.48 degrees. 
;
_diffrn_reflns_av_R_equivalents  0.1489
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            42241
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.28
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71083
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_reflns_number_gt                3883
_reflns_number_total             5882
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XLMP (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         2.430
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5882
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.1023
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2701
_refine_ls_wR_factor_ref         0.2914
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Others
 Fixed U12: Cu2(0) Cu3(0) O8(0) O9(0)
 Fixed U23: Cu2(0) Cu3(0) O8(0) O9(0)
 Fixed Uiso: H7A(0.163) H7B(0.163) H8A(0.16) H8B(0.16) H9A(0.183) H9B(0.183)
 H1(0.069) H1A(0.072) H2(0.101) H2A(0.082) H3(0.086) H3A(0.092) H5(0.094)
 H5A(0.071) H6(0.102) H6A(0.065) H31A(0.116) H31B(0.116) H31C(0.116)
 H31D(0.134) H31E(0.134) H31F(0.134) H51A(0.085) H51B(0.085) H51C(0.085)
 H51D(0.134) H51E(0.134) H51F(0.134)
 Fixed X: H7A(0.166) H7B(0.2074) H1(0.2762) H1A(0.1531) H2(0.4449) H2A(0.0098)
 H3(0.3967) H3A(0.0462) H5(0.346) H5A(0.1504) H6(0.394) H6A(0.1146)
 H31A(0.2825) H31B(0.3289) H31C(0.2891) H31D(0.2104) H31E(0.1711) H31F(0.2055)
 H51A(0.3205) H51B(0.3672) H51C(0.3372) H51D(0.0895) H51E(0.0784) H51F(0.0574)
 Fixed Y: Cu2(0) Cu3(0) H7A(0.1737) H7B(0.1581) O8(0) H8A(0) H8B(0) O9(0)
 H9A(0) H9B(0) H1(0.257) H1A(0.255) H2(0.0809) H2A(0.1064) H3(0.1338)
 H3A(0.1519) H5(0.1556) H5A(0.1359) H6(0.1114) H6A(0.0885) H31A(0.1204)
 H31B(0.1069) H31C(0.0966) H31D(0.1174) H31E(0.0946) H31F(0.1219) H51A(0.2521)
 H51B(0.2456) H51C(0.2841) H51D(0.2812) H51E(0.2542) H51F(0.2395)
 Fixed Z: H7A(-0.2995) H7B(-0.3396) H1(-0.2718) H1A(-0.0796) H2(-0.1698)
 H2A(0.1508) H3(-0.1091) H3A(0.0171) H5(-0.5188) H5A(0.335) H6(-0.5864)
 H6A(0.4491) H31A(-0.0587) H31B(-0.0717) H31C(-0.1996) H31D(0.0329)
 H31E(0.0776) H31F(0.192) H51A(-0.4975) H51B(-0.4017) H51C(-0.3632) H51D(-
 0.0127) H51E(0.1162) H51F(-0.0432)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.23027(4) 0.20022(4) -0.09435(13) 0.0557(5) Uani 1 d . . 1 . . .
Cu2 Cu 0.47657(5) 0.0000 -0.6304(2) 0.0613(6) Uani 1 d . . 2 S T P
Cu3 Cu 0.03260(5) 0.0000 0.61085(17) 0.0492(5) Uani 1 d . . 2 S T P
S1 S 0.20818(8) 0.30800(8) -0.2139(3) 0.0622(8) Uani 1 d . . 1 . . .
O1 O 0.4845(3) 0.0464(2) -0.3344(9) 0.079(2) Uani 1 d . . 1 . . .
O1A O 0.0003(2) 0.0464(2) 0.3179(8) 0.071(2) Uani 1 d . . 1 . . .
O2 O 0.4439(3) 0.0459(3) -0.5543(11) 0.096(3) Uani 1 d . . 1 . . .
O2A O 0.0563(2) 0.0456(2) 0.5032(8) 0.0664(19) Uani 1 d . . 1 . . .
O3 O 0.2303(2) 0.2787(3) -0.0991(9) 0.084(2) Uani 1 d . . 1 . . .
O4 O 0.2249(2) 0.2976(2) -0.3362(8) 0.075(2) Uani 1 d . . 1 . . .
O5 O 0.2142(3) 0.3543(3) -0.1732(12) 0.108(3) Uani 1 d . . 1 . . .
O6 O 0.1641(2) 0.2944(3) -0.2356(10) 0.092(3) Uani 1 d . . 1 . . .
O7 O 0.1970(3) 0.1740(3) -0.2657(11) 0.108(3) Uani 1 d . . 1 . . .
H7A H 0.1660 0.1737 -0.2995 0.163 Uiso 1 d . . 1 DGR . .
H7B H 0.2074 0.1581 -0.3396 0.163 Uiso 1 d . . 1 DGR . .
O8 O 0.4418(4) 0.0000 -0.8448(16) 0.107(4) Uani 1 d . . 2 DS TU P
H8A H 0.459(5) 0.0000 -0.900(16) 0.160 Uiso 1 d . . 2 DRS T P
H8B H 0.4155(12) 0.0000 -0.882(18) 0.160 Uiso 1 d . . 2 DRS T P
O9 O 0.0865(4) 0.0000 0.7973(18) 0.122(5) Uani 1 d . . 2 DS TU P
H9A H 0.094(3) 0.0000 0.888(3) 0.183 Uiso 1 d . . 2 DRS T P
H9B H 0.103(3) 0.0000 0.741(8) 0.183 Uiso 1 d . . 2 DRS T P
N1 N 0.2895(2) 0.2308(2) -0.2582(8) 0.057(2) Uani 1 d . . 1 . . .
H1 H 0.2762 0.2570 -0.2718 0.069 Uiso 1 calc . . 1 R . .
N1A N 0.1511(2) 0.2296(2) -0.0344(9) 0.060(2) Uani 1 d . . 1 . . .
H1A H 0.1531 0.2550 -0.0796 0.072 Uiso 1 calc . . 1 R . .
N2 N 0.2792(2) 0.1969(2) -0.1822(8) 0.054(2) Uani 1 d . . 1 . . .
N2A N 0.1804(3) 0.1962(2) -0.0162(9) 0.056(2) Uani 1 d . . 1 . . .
C1 C 0.4246(4) 0.0910(4) -0.3863(13) 0.073(3) Uani 1 d . . 1 . . .
C1A C 0.0607(3) 0.0918(3) 0.3120(11) 0.059(2) Uani 1 d . . 1 . . .
C2 C 0.4253(4) 0.0968(4) -0.2412(14) 0.084(4) Uani 1 d . . 1 . . .
H2 H 0.4449 0.0809 -0.1698 0.101 Uiso 1 calc . . 1 R . .
C2A C 0.0392(3) 0.1118(3) 0.1847(12) 0.069(3) Uani 1 d . . 1 . . .
H2A H 0.0098 0.1064 0.1508 0.082 Uiso 1 calc . . 1 R . .
C3 C 0.3954(3) 0.1278(4) -0.2059(13) 0.072(3) Uani 1 d . . 1 . . .
H3 H 0.3967 0.1338 -0.1091 0.086 Uiso 1 calc . . 1 R . .
C3' C 0.3061(3) 0.1643(3) -0.1866(12) 0.067(3) Uani 1 d . . 1 . . .
C3A C 0.0603(3) 0.1396(4) 0.1059(13) 0.077(3) Uani 1 d . . 1 . . .
H3A H 0.0462 0.1519 0.0171 0.092 Uiso 1 calc . . 1 R . .
C3A' C 0.1653(3) 0.1636(3) 0.0534(12) 0.067(3) Uani 1 d . . 1 . . .
C4 C 0.3655(4) 0.1484(3) -0.3054(13) 0.071(3) Uani 1 d . . 1 . . .
C4' C 0.3326(3) 0.1775(3) -0.2692(10) 0.055(2) Uani 1 d . . 1 . . .
C4A C 0.1030(3) 0.1484(3) 0.1644(12) 0.064(3) Uani 1 d . . 1 . . .
C4A' C 0.1285(3) 0.1764(3) 0.0854(10) 0.051(2) Uani 1 d . . 1 . . .
C5 C 0.3666(4) 0.1409(4) -0.4476(12) 0.078(3) Uani 1 d . . 1 . . .
H5 H 0.3460 0.1556 -0.5188 0.094 Uiso 1 calc . . 1 R . .
C5' C 0.3219(3) 0.2205(3) -0.3100(10) 0.050(2) Uani 1 d . . 1 . . .
C5A C 0.1217(3) 0.1293(3) 0.2932(11) 0.059(3) Uani 1 d . . 1 . . .
H5A H 0.1504 0.1359 0.3350 0.071 Uiso 1 calc . . 1 R . .
C5A' C 0.1187(3) 0.2199(3) 0.0232(12) 0.065(3) Uani 1 d . . 1 . . .
C6 C 0.3945(4) 0.1144(4) -0.4889(13) 0.085(4) Uani 1 d . . 1 . . .
H6 H 0.3940 0.1114 -0.5864 0.102 Uiso 1 calc . . 1 R . .
C6A C 0.1002(3) 0.1015(3) 0.3616(10) 0.054(2) Uani 1 d . . 1 . . .
H6A H 0.1146 0.0885 0.4491 0.065 Uiso 1 calc . . 1 R . .
C7 C 0.4530(4) 0.0580(4) -0.4291(14) 0.068(3) Uani 1 d . . 1 . . .
C7A C 0.0373(3) 0.0585(3) 0.3902(13) 0.057(2) Uani 1 d . . 1 . . .
C31 C 0.3012(4) 0.1179(3) -0.1235(13) 0.077(3) Uani 1 d . . 1 . . .
H31A H 0.2825 0.1204 -0.0587 0.116 Uiso 1 calc . . 1 GR . .
H31B H 0.3289 0.1069 -0.0717 0.116 Uiso 1 calc . . 1 GR . .
H31C H 0.2891 0.0966 -0.1996 0.116 Uiso 1 calc . . 1 GR . .
C31A C 0.1903(4) 0.1206(3) 0.0924(15) 0.089(4) Uani 1 d . . 1 . . .
H31D H 0.2104 0.1174 0.0329 0.134 Uiso 1 calc . . 1 GR . .
H31E H 0.1711 0.0946 0.0776 0.134 Uiso 1 calc . . 1 GR . .
H31F H 0.2055 0.1219 0.1920 0.134 Uiso 1 calc . . 1 GR . .
C51 C 0.3381(3) 0.2534(3) -0.4009(11) 0.057(2) Uani 1 d . . 1 . . .
H51A H 0.3205 0.2521 -0.4975 0.085 Uiso 1 calc . . 1 GR . .
H51B H 0.3672 0.2456 -0.4017 0.085 Uiso 1 calc . . 1 GR . .
H51C H 0.3372 0.2841 -0.3632 0.085 Uiso 1 calc . . 1 GR . .
C51A C 0.0830(4) 0.2514(4) 0.0207(17) 0.090(4) Uani 1 d . . 1 . . .
H51D H 0.0895 0.2812 -0.0127 0.134 Uiso 1 calc . . 1 GR . .
H51E H 0.0784 0.2542 0.1162 0.134 Uiso 1 calc . . 1 GR . .
H51F H 0.0574 0.2395 -0.0432 0.134 Uiso 1 calc . . 1 GR . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O3 2.108(9) 7 ?
Cu1 O3 2.316(8) . ?
Cu1 O7 1.924(11) . ?
Cu1 N2 1.987(7) . ?
Cu1 N2A 1.958(7) . ?
Cu2 Cu2 2.637(4) 5_654 ?
Cu2 O1 1.956(7) 5_654 ?
Cu2 O1 1.956(7) 2_654 ?
Cu2 O2 1.974(8) 6 ?
Cu2 O2 1.974(8) . ?
Cu2 O8 2.127(15) . ?
Cu3 Cu3 2.649(3) 5_556 ?
Cu3 O1A 1.967(6) 5_556 ?
Cu3 O1A 1.967(6) 2_556 ?
Cu3 O2A 1.972(6) . ?
Cu3 O2A 1.972(6) 6 ?
Cu3 O9 2.209(17) . ?
S1 O3 1.462(9) . ?
S1 O4 1.455(7) . ?
S1 O5 1.423(8) . ?
S1 O6 1.461(8) . ?
O1 Cu2 1.956(7) 5_654 ?
O1 C7 1.255(13) . ?
O1A Cu3 1.967(6) 5_556 ?
O1A C7A 1.297(12) . ?
O2 C7 1.237(13) . ?
O2A C7A 1.190(12) . ?
O3 Cu1 2.109(9) 7 ?
N1 N2 1.336(9) . ?
N1 C5' 1.312(11) . ?
N1A N2A 1.357(10) . ?
N1A C5A' 1.340(11) . ?
N2 C3' 1.311(11) . ?
N2A C3A' 1.338(11) . ?
C1 C2 1.418(16) . ?
C1 C6 1.407(16) . ?
C1 C7 1.471(15) . ?
C1A C2A 1.402(15) . ?
C1A C6A 1.301(13) . ?
C1A C7A 1.552(13) . ?
C2 C3 1.438(14) . ?
C2A C3A 1.411(14) . ?
C3 C4 1.348(16) . ?
C3' C4' 1.370(12) . ?
C3' C31 1.524(13) . ?
C3A C4A 1.401(15) . ?
C3A' C4A' 1.366(13) . ?
C3A' C31A 1.507(14) . ?
C4 C4' 1.482(13) . ?
C4 C5 1.411(15) . ?
C4' C5' 1.351(13) . ?
C4A C4A' 1.507(13) . ?
C4A C5A 1.378(14) . ?
C4A' C5A' 1.426(13) . ?
C5 C6 1.333(14) . ?
C5' C51 1.493(12) . ?
C5A C6A 1.354(13) . ?
C5A' C51A 1.489(15) . ?

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
O3 Cu1 O3 73.7(3) 7 . ?
O7 Cu1 O3 112.8(3) . . ?
O7 Cu1 O3 173.3(3) . 7 ?
O7 Cu1 N2 87.4(3) . . ?
O7 Cu1 N2A 87.8(3) . . ?
N2 Cu1 O3 92.2(2) . . ?
N2 Cu1 O3 90.8(3) . 7 ?
N2A Cu1 O3 93.4(3) . 7 ?
N2A Cu1 O3 94.1(2) . . ?
N2A Cu1 N2 173.2(3) . . ?
O1 Cu2 Cu2 85.1(3) 2_654 5_654 ?
O1 Cu2 Cu2 85.1(3) 5_654 5_654 ?
O1 Cu2 O1 89.0(5) 2_654 5_654 ?
O1 Cu2 O2 91.0(4) 5_654 6 ?
O1 Cu2 O2 168.2(4) 5_654 . ?
O1 Cu2 O2 168.2(4) 2_654 6 ?
O1 Cu2 O2 91.0(4) 2_654 . ?
O1 Cu2 O8 92.7(4) 5_654 . ?
O1 Cu2 O8 92.7(4) 2_654 . ?
O2 Cu2 Cu2 83.2(3) . 5_654 ?
O2 Cu2 Cu2 83.2(3) 6 5_654 ?
O2 Cu2 O2 86.6(5) . 6 ?
O2 Cu2 O8 99.1(4) . . ?
O2 Cu2 O8 99.1(4) 6 . ?
O8 Cu2 Cu2 176.9(4) . 5_654 ?
O1A Cu3 Cu3 83.4(2) 2_556 5_556 ?
O1A Cu3 Cu3 83.4(2) 5_556 5_556 ?
O1A Cu3 O1A 88.3(4) 5_556 2_556 ?
O1A Cu3 O2A 91.7(3) 5_556 6 ?
O1A Cu3 O2A 168.1(3) 5_556 . ?
O1A Cu3 O2A 91.7(3) 2_556 . ?
O1A Cu3 O2A 168.1(3) 2_556 6 ?
O1A Cu3 O9 96.1(3) 2_556 . ?
O1A Cu3 O9 96.1(3) 5_556 . ?
O2A Cu3 Cu3 84.8(2) 6 5_556 ?
O2A Cu3 Cu3 84.8(2) . 5_556 ?
O2A Cu3 O2A 86.0(4) . 6 ?
O2A Cu3 O9 95.7(3) . . ?
O2A Cu3 O9 95.7(3) 6 . ?
O9 Cu3 Cu3 179.4(3) . 5_556 ?
O4 S1 O3 106.7(4) . . ?
O4 S1 O6 111.8(5) . . ?
O5 S1 O3 110.2(6) . . ?
O5 S1 O4 112.1(5) . . ?
O5 S1 O6 111.7(5) . . ?
O6 S1 O3 103.8(4) . . ?
C7 O1 Cu2 121.1(7) . 5_654 ?
C7A O1A Cu3 121.2(7) . 5_556 ?
C7 O2 Cu2 122.9(8) . . ?
C7A O2A Cu3 121.7(7) . . ?
Cu1 O3 Cu1 106.3(3) 7 . ?
S1 O3 Cu1 127.2(5) . . ?
S1 O3 Cu1 126.5(5) . 7 ?
C5' N1 N2 111.7(7) . . ?
C5A' N1A N2A 113.2(7) . . ?
N1 N2 Cu1 122.3(5) . . ?
C3' N2 Cu1 131.7(6) . . ?
C3' N2 N1 105.9(7) . . ?
N1A N2A Cu1 122.2(5) . . ?
C3A' N2A Cu1 133.0(6) . . ?
C3A' N2A N1A 104.7(7) . . ?
C2 C1 C7 120.0(11) . . ?
C6 C1 C2 119.4(9) . . ?
C6 C1 C7 120.4(11) . . ?
C2A C1A C7A 119.9(9) . . ?
C6A C1A C2A 118.9(9) . . ?
C6A C1A C7A 121.2(10) . . ?
C1 C2 C3 117.6(11) . . ?
C1A C2A C3A 121.2(10) . . ?
C4 C3 C2 122.3(11) . . ?
N2 C3' C4' 109.4(8) . . ?
N2 C3' C31 120.7(8) . . ?
C4' C3' C31 129.3(9) . . ?
C4A C3A C2A 117.0(11) . . ?
N2A C3A' C4A' 111.6(8) . . ?
N2A C3A' C31A 119.3(8) . . ?
C4A' C3A' C31A 129.0(8) . . ?
C3 C4 C4' 122.3(10) . . ?
C3 C4 C5 116.8(9) . . ?
C5 C4 C4' 120.9(10) . . ?
C3' C4' C4 124.7(9) . . ?
C5' C4' C3' 106.6(8) . . ?
C5' C4' C4 128.7(8) . . ?
C3A C4A C4A' 120.7(10) . . ?
C5A C4A C3A 118.7(9) . . ?
C5A C4A C4A' 120.5(9) . . ?
C3A' C4A' C4A 126.0(8) . . ?
C3A' C4A' C5A' 105.8(8) . . ?
C5A' C4A' C4A 128.1(8) . . ?
C6 C5 C4 124.5(11) . . ?
N1 C5' C4' 106.4(8) . . ?
N1 C5' C51 120.5(8) . . ?
C4' C5' C51 133.0(8) . . ?
C6A C5A C4A 121.7(9) . . ?
N1A C5A' C4A' 104.5(8) . . ?
N1A C5A' C51A 123.7(9) . . ?
C4A' C5A' C51A 131.7(8) . . ?
C5 C6 C1 119.2(11) . . ?
C1A C6A C5A 122.4(10) . . ?
O1 C7 C1 115.7(11) . . ?
O2 C7 O1 127.5(11) . . ?
O2 C7 C1 116.8(12) . . ?
O1A C7A C1A 114.3(10) . . ?
O2A C7A O1A 128.9(9) . . ?
O2A C7A C1A 116.6(9) . . ?

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
N1 H1 O4 0.88 2.04 2.857(10) 154.8 .
N1A H1A O6 0.88 2.01 2.842(11) 156.7 .

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
Cu1 N2 C3' C4' 175.7(7) . . . . ?
Cu1 N2 C3' C31 3.9(17) . . . . ?
Cu1 N2A C3A' C4A' -179.1(7) . . . . ?
Cu1 N2A C3A' C31A 4.1(17) . . . . ?
Cu2 Cu2 O2 C7 -1.3(9) 5_654 . . . ?
Cu2 O1 C7 O2 -6.1(16) 5_654 . . . ?
Cu2 O1 C7 C1 176.0(7) 5_654 . . . ?
Cu2 O2 C7 O1 4.8(17) . . . . ?
Cu2 O2 C7 C1 -177.3(7) . . . . ?
Cu3 Cu3 O2A C7A 1.4(8) 5_556 . . . ?
Cu3 O1A C7A O2A -1.2(14) 5_556 . . . ?
Cu3 O1A C7A C1A 174.2(6) 5_556 . . . ?
Cu3 O2A C7A O1A -0.5(15) . . . . ?
Cu3 O2A C7A C1A -175.9(6) . . . . ?
O1 Cu2 O2 C7 -86.2(10) 2_654 . . . ?
O1 Cu2 O2 C7 4(2) 5_654 . . . ?
O1A Cu3 O2A C7A 8(2) 5_556 . . . ?
O1A Cu3 O2A C7A -81.9(8) 2_556 . . . ?
O2 Cu2 O2 C7 82.2(10) 6 . . . ?
O2A Cu3 O2A C7A 86.5(8) 6 . . . ?
O3 Cu1 O3 Cu1 0.0 7 . . 7 ?
O3 Cu1 O3 S1 178.8(6) 7 . . . ?
O3 Cu1 N2 N1 -22.0(8) . . . . ?
O3 Cu1 N2 N1 -95.7(8) 7 . . . ?
O3 Cu1 N2 C3' 160.9(10) . . . . ?
O3 Cu1 N2 C3' 87.1(10) 7 . . . ?
O3 Cu1 N2A N1A 25.3(8) . . . . ?
O3 Cu1 N2A N1A 99.2(8) 7 . . . ?
O3 Cu1 N2A C3A' -85.4(10) 7 . . . ?
O3 Cu1 N2A C3A' -159.3(10) . . . . ?
O4 S1 O3 Cu1 117.3(5) . . . 7 ?
O4 S1 O3 Cu1 -61.3(6) . . . . ?
O5 S1 O3 Cu1 -4.7(6) . . . 7 ?
O5 S1 O3 Cu1 176.8(5) . . . . ?
O6 S1 O3 Cu1 -124.4(5) . . . 7 ?
O6 S1 O3 Cu1 57.0(6) . . . . ?
O7 Cu1 O3 Cu1 -178.3(3) . . . 7 ?
O7 Cu1 O3 S1 0.5(6) . . . . ?
O7 Cu1 N2 N1 90.7(8) . . . . ?
O7 Cu1 N2 C3' -86.4(10) . . . . ?
O7 Cu1 N2A N1A -87.4(8) . . . . ?
O7 Cu1 N2A C3A' 88.1(10) . . . . ?
O8 Cu2 O2 C7 -179.1(9) . . . . ?
O9 Cu3 O2A C7A -178.2(8) . . . . ?
N1 N2 C3' C4' -1.8(12) . . . . ?
N1 N2 C3' C31 -173.6(10) . . . . ?
N1A N2A C3A' C4A' -3.0(12) . . . . ?
N1A N2A C3A' C31A -179.9(10) . . . . ?
N2 Cu1 O3 Cu1 -90.2(3) . . . 7 ?
N2 Cu1 O3 S1 88.5(5) . . . . ?
N2 Cu1 N2A N1A -132(3) . . . . ?
N2 Cu1 N2A C3A' 43(3) . . . . ?
N2 N1 C5' C4' 1.5(11) . . . . ?
N2 N1 C5' C51 178.8(8) . . . . ?
N2 C3' C4' C4 -176.2(10) . . . . ?
N2 C3' C4' C5' 2.7(12) . . . . ?
N2A Cu1 O3 Cu1 92.4(3) . . . 7 ?
N2A Cu1 O3 S1 -88.8(5) . . . . ?
N2A Cu1 N2 N1 135(3) . . . . ?
N2A Cu1 N2 C3' -42(3) . . . . ?
N2A N1A C5A' C4A' 0.5(11) . . . . ?
N2A N1A C5A' C51A 178.5(11) . . . . ?
N2A C3A' C4A' C4A -179.3(9) . . . . ?
N2A C3A' C4A' C5A' 3.4(13) . . . . ?
C1 C2 C3 C4 4.6(17) . . . . ?
C1A C2A C3A C4A -3.4(17) . . . . ?
C2 C1 C6 C5 -1.4(18) . . . . ?
C2 C1 C7 O1 -20.0(15) . . . . ?
C2 C1 C7 O2 161.8(11) . . . . ?
C2 C3 C4 C4' 175.1(10) . . . . ?
C2 C3 C4 C5 -4.3(17) . . . . ?
C2A C1A C6A C5A -1.5(15) . . . . ?
C2A C1A C7A O1A 9.9(13) . . . . ?
C2A C1A C7A O2A -174.1(9) . . . . ?
C2A C3A C4A C4A' 177.8(9) . . . . ?
C2A C3A C4A C5A 0.4(15) . . . . ?
C3 C4 C4' C3' -54.4(16) . . . . ?
C3 C4 C4' C5' 126.9(12) . . . . ?
C3 C4 C5 C6 1.1(18) . . . . ?
C3' C4' C5' N1 -2.5(11) . . . . ?
C3' C4' C5' C51 -179.3(11) . . . . ?
C3A C4A C4A' C3A' -125.4(12) . . . . ?
C3A C4A C4A' C5A' 51.3(15) . . . . ?
C3A C4A C5A C6A 2.1(15) . . . . ?
C3A' C4A' C5A' N1A -2.3(11) . . . . ?
C3A' C4A' C5A' C51A 179.9(13) . . . . ?
C4 C4' C5' N1 176.4(10) . . . . ?
C4 C4' C5' C51 -0.4(18) . . . . ?
C4 C5 C6 C1 2(2) . . . . ?
C4' C4 C5 C6 -178.4(12) . . . . ?
C4A C4A' C5A' N1A -179.5(10) . . . . ?
C4A C4A' C5A' C51A 3(2) . . . . ?
C4A C5A C6A C1A -1.5(16) . . . . ?
C4A' C4A C5A C6A -175.3(9) . . . . ?
C5 C4 C4' C3' 125.0(12) . . . . ?
C5 C4 C4' C5' -53.7(16) . . . . ?
C5' N1 N2 Cu1 -177.7(6) . . . . ?
C5' N1 N2 C3' 0.1(11) . . . . ?
C5A C4A C4A' C3A' 51.9(15) . . . . ?
C5A C4A C4A' C5A' -131.3(11) . . . . ?
C5A' N1A N2A Cu1 178.1(7) . . . . ?
C5A' N1A N2A C3A' 1.5(11) . . . . ?
C6 C1 C2 C3 -1.6(17) . . . . ?
C6 C1 C7 O1 164.9(11) . . . . ?
C6 C1 C7 O2 -13.3(16) . . . . ?
C6A C1A C2A C3A 4.0(16) . . . . ?
C6A C1A C7A O1A -169.4(9) . . . . ?
C6A C1A C7A O2A 6.7(14) . . . . ?
C7 C1 C2 C3 -176.8(10) . . . . ?
C7 C1 C6 C5 173.7(11) . . . . ?
C7A C1A C2A C3A -175.3(10) . . . . ?
C7A C1A C6A C5A 177.8(9) . . . . ?
C31 C3' C4' C4 -5.3(19) . . . . ?
C31 C3' C4' C5' 173.6(12) . . . . ?
C31A C3A' C4A' C4A -2.8(19) . . . . ?
C31A C3A' C4A' C5A' 179.8(12) . . . . ?

_olex2_computing_structure_refinement_long 'SHELXL-97 (Sheldrick, 1997)'
_olex2_computing_structure_solution_long 'SHELXS-97 (Sheldrick, 1997)'
#===END
_olex2_submission_special_instructions 'No special instructions were received'
# SQUEEZE RESULTS
# 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 -0.005 -0.029 -0.005 4312 1180 ' '

_vrf_PLAT023_c2m-sr              
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      22.48 Degree
RESPONSE: As before, the crystals did not diffract past 22.48 degrees and this
leads to the low resolution. We accept that this value is low but all crystals 
exhibited these poor characteristics. We note that we have not made any analyse
s based upon the accuracy of the data obtained. However, we were able to 
develop a sensible structural model.
;
# start Validation Reply Form
_vrf_THETM01_c2m-sr              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: All crystals on which diffraction was attempted were found to exhibit
poor diffraction intensity at wide angle, even using high intensity synchrotron
radiation. As such, reflections were only observed to a theta value of 22.48 
degrees
;
####################################################################### 
# 
# 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_55crw
_database_code_depnum_ccdc_archive 'CCDC 1040605'
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_audit_creation_date             2014-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.13(C192 H176 Cu8 N32 O32), 4(C H4 O), O'
_chemical_formula_sum            'C28 H38 Cu N4 O9'
_chemical_formula_weight         638.16
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_properties_physical    
'Crystals lose solvent and change to another phase.'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_symmetry_int_tables_number      88
_cell_length_a                   23.5927(4)
_cell_length_b                   23.5927(4)
_cell_length_c                   11.7356(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6532.2(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6699
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.7460
_cell_measurement_theta_min      4.1870
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.401
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9018
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.920
_diffrn_reflns_theta_min         4.208
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -49.00   36.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563   37.0000 -120.0000 85

#__ type_ start__ end____ width___ exp.time_
  2 omega   41.00   74.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6563 -125.0000  -90.0000 33

#__ type_ start__ end____ width___ exp.time_
  3 omega -119.00  -92.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -125.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
  4 omega  132.00  168.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  125.0000   30.0000 36

#__ type_ start__ end____ width___ exp.time_
  5 omega   31.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  -90.0000 32

#__ type_ start__ end____ width___ exp.time_
  6 omega   33.00   78.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000 -180.0000 45

#__ type_ start__ end____ width___ exp.time_
  7 omega   80.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   45.0000  150.0000 97

#__ type_ start__ end____ width___ exp.time_
  8 omega -118.00   -6.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563  -77.0000  120.0000 112

#__ type_ start__ end____ width___ exp.time_
  9 omega -116.00  -13.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563  -37.0000 -120.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0569727000
_diffrn_orient_matrix_UB_12      0.0306468000
_diffrn_orient_matrix_UB_13      -0.0178507000
_diffrn_orient_matrix_UB_21      0.0300988000
_diffrn_orient_matrix_UB_22      -0.0455879000
_diffrn_orient_matrix_UB_23      0.0719933000
_diffrn_orient_matrix_UB_31      0.0108123000
_diffrn_orient_matrix_UB_32      -0.0352272000
_diffrn_orient_matrix_UB_33      -0.1083051000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2962
_reflns_number_total             3092
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3092
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0601
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1153P)²+18.7110P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.1831
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Sof: O16(0.5)
 Fixed Uiso: H1(0.027) H6(0.03) H5(0.03) H3(0.03) H14(0.052) H31A(0.043)
 H31B(0.043) H31C(0.043) H2(0.031) H51A(0.048) H51B(0.048) H51C(0.048)
 H10(0.142) H11A(0.127) H11B(0.127) H11C(0.127) H12(0.294) H15A(0.109)
 H15B(0.109) H15C(0.109) H13A(0.155) H13B(0.155) H13C(0.155)
 Fixed X: Cu1(0.5) H1(0.1925) H6(0.3969) H5(0.3405) H3(0.3138) H14(0.3679)
 H31A(0.1591) H31B(0.2029) H31C(0.2065) H2(0.3704) H51A(0.3659) H51B(0.3877)
 H51C(0.3525) H10(0.5244) H11A(0.432) H11B(0.4546) H11C(0.4634) H12(0.4294)
 H15A(0.4536) H15B(0.44) H15C(0.3939) H13A(0.4432) H13B(0.4681) H13C(0.4283)
 Fixed Y: Cu1(0.5) H1(0.6441) H6(0.6164) H5(0.661) H3(0.5116) H14(0.6346)
 H31A(0.5685) H31B(0.5444) H31C(0.5264) H2(0.4672) H51A(0.7234) H51B(0.68)
 H51C(0.7331) H10(0.5768) H11A(0.5821) H11B(0.5652) H11C(0.5242) H12(0.6232)
 H15A(0.6926) H15B(0.6353) H15C(0.6831) H13A(0.6942) H13B(0.6448) H13C(0.6901)
 Fixed Z: Cu1(0.5) H1(-0.174) H6(0.3047) H5(0.1712) H3(0.0154) H14(0.5945)
 H31A(-0.0434) H31B(0.0447) H31C(-0.0837) H2(0.1489) H51A(-0.1259) H51B(-
 0.0347) H51C(0.0035) H10(-0.1635) H11A(-0.1196) H11B(0.0013) H11C(-0.1024)
 H12(0.5239) H15A(0.6417) H15B(0.7037) H15C(0.6973) H13A(0.5028) H13B(0.5768)
 H13C(0.6328)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.5000 0.5000 0.0190(2) Uani 1 2 d S T P . .
O2 O 0.44780(8) 0.54079(8) 0.40323(16) 0.0245(4) Uani 1 1 d . . . . .
N1 N 0.22301(10) 0.64478(10) -0.1339(2) 0.0224(5) Uani 1 1 d . . . . .
H1 H 0.1925 0.6441 -0.1740 0.027 Uiso 1 1 calc R . . . .
O1 O 0.44309(9) 0.45846(9) 0.3128(2) 0.0355(5) Uani 1 1 d . . . . .
N2 N 0.26353(10) 0.68570(9) -0.14265(19) 0.0215(5) Uani 1 1 d . . . . .
C6 C 0.38055(13) 0.59547(12) 0.2462(2) 0.0247(6) Uani 1 1 d . . . . .
H6 H 0.3969 0.6164 0.3047 0.030 Uiso 1 1 calc R . . . .
C4' C 0.28826(12) 0.62130(12) -0.0104(2) 0.0216(6) Uani 1 1 d . . . . .
C1 C 0.39024(12) 0.53725(13) 0.2394(2) 0.0236(6) Uani 1 1 d . . . . .
C5 C 0.34672(12) 0.62218(12) 0.1659(2) 0.0250(6) Uani 1 1 d . . . . .
H5 H 0.3405 0.6610 0.1712 0.030 Uiso 1 1 calc R . . . .
C4 C 0.32190(11) 0.59147(12) 0.0773(2) 0.0220(6) Uani 1 1 d . . . . .
C5' C 0.30365(11) 0.67170(12) -0.0675(2) 0.0221(6) Uani 1 1 d . . . . .
C3' C 0.23619(12) 0.60576(12) -0.0558(2) 0.0222(6) Uani 1 1 d . . . . .
C3 C 0.33081(12) 0.53286(12) 0.0727(2) 0.0253(6) Uani 1 1 d . . . . .
H3 H 0.3138 0.5116 0.0154 0.030 Uiso 1 1 calc R . . . .
O14 O 0.38918(18) 0.6358(2) 0.5393(7) 0.0349(18) Uani 0.571(18) 1 d D . . A 2
H14 H 0.3679 0.6346 0.5945 0.052 Uiso 0.571(18) 1 calc GR . . A 2
C7 C 0.42944(11) 0.50933(12) 0.3238(2) 0.0237(6) Uani 1 1 d . . . . .
C31 C 0.19775(13) 0.55692(13) -0.0325(3) 0.0287(6) Uani 1 1 d . . . . .
H31A H 0.1591 0.5685 -0.0434 0.043 Uiso 1 1 calc GR . . . .
H31B H 0.2029 0.5444 0.0447 0.043 Uiso 1 1 calc GR . . . .
H31C H 0.2065 0.5264 -0.0837 0.043 Uiso 1 1 calc GR . . . .
C2 C 0.36469(12) 0.50619(12) 0.1530(2) 0.0260(6) Uani 1 1 d . . . . .
H2 H 0.3704 0.4672 0.1489 0.031 Uiso 1 1 calc R . . . .
C51 C 0.35723(13) 0.70504(13) -0.0551(3) 0.0321(7) Uani 1 1 d . . . . .
H51A H 0.3659 0.7234 -0.1259 0.048 Uiso 1 1 calc GR . . . .
H51B H 0.3877 0.6800 -0.0347 0.048 Uiso 1 1 calc GR . . . .
H51C H 0.3525 0.7331 0.0035 0.048 Uiso 1 1 calc GR . . . .
O10 O 0.51212(18) 0.5887(2) -0.1027(4) 0.0946(13) Uani 1 1 d D . . . .
H10 H 0.5244 0.5768 -0.1635 0.142 Uiso 1 1 calc GR . . . .
C11 C 0.4618(2) 0.5632(3) -0.0791(6) 0.0850(18) Uani 1 1 d D . . . .
H11A H 0.4320 0.5821 -0.1196 0.127 Uiso 1 1 calc GR . . . .
H11B H 0.4546 0.5652 0.0013 0.127 Uiso 1 1 calc GR . . . .
H11C H 0.4634 0.5242 -0.1024 0.127 Uiso 1 1 calc GR . . . .
O16 O 0.4619(8) 0.7331(7) 0.337(2) 0.235(9) Uani 0.5 1 d . U . . .
O12 O 0.4044(14) 0.6422(7) 0.5538(12) 0.196(13) Uani 0.429(18) 1 d D . . A 1
H12 H 0.4294 0.6232 0.5239 0.294 Uiso 0.429(18) 1 calc GR . . A 1
C15 C 0.4246(6) 0.6652(5) 0.6574(17) 0.072(5) Uani 0.429(18) 1 d D . . A 1
H15A H 0.4536 0.6926 0.6417 0.109 Uiso 0.429(18) 1 calc GR . . A 1
H15B H 0.4400 0.6353 0.7037 0.109 Uiso 0.429(18) 1 calc GR . . A 1
H15C H 0.3939 0.6831 0.6973 0.109 Uiso 0.429(18) 1 calc GR . . A 1
C13 C 0.4357(3) 0.6687(6) 0.565(2) 0.103(6) Uani 0.571(18) 1 d D . . A 2
H13A H 0.4432 0.6942 0.5028 0.155 Uiso 0.571(18) 1 calc GR . . A 2
H13B H 0.4681 0.6448 0.5768 0.155 Uiso 0.571(18) 1 calc GR . . A 2
H13C H 0.4283 0.6901 0.6328 0.155 Uiso 0.571(18) 1 calc GR . . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.9320(19) 9_666 ?
Cu1 O2 1.9320(18) . ?
Cu1 N2 1.998(2) 16_655 ?
Cu1 N2 1.998(2) 8_455 ?
O2 C7 1.268(4) . ?
N1 H1 0.8600 . ?
N1 N2 1.363(3) . ?
N1 C3' 1.336(4) . ?
O1 C7 1.249(4) . ?
N2 Cu1 1.998(2) 2_554 ?
N2 C5' 1.335(4) . ?
C6 H6 0.9300 . ?
C6 C1 1.395(4) . ?
C6 C5 1.386(4) . ?
C4' C4 1.478(4) . ?
C4' C5' 1.412(4) . ?
C4' C3' 1.388(4) . ?
C1 C7 1.507(4) . ?
C1 C2 1.389(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.397(4) . ?
C4 C3 1.400(4) . ?
C5' C51 1.496(4) . ?
C3' C31 1.492(4) . ?
C3 H3 0.9300 . ?
C3 C2 1.386(4) . ?
O14 H14 0.8200 . ?
O14 C13 1.379(8) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C2 H2 0.9300 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
O10 H10 0.8200 . ?
O10 C11 1.359(5) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
O12 H12 0.8200 . ?
O12 C15 1.414(10) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.0 9_666 . ?
O2 Cu1 N2 88.07(9) 9_666 16_655 ?
O2 Cu1 N2 91.93(9) . 16_655 ?
O2 Cu1 N2 88.07(9) . 8_455 ?
O2 Cu1 N2 91.93(9) 9_666 8_455 ?
N2 Cu1 N2 180.00(13) 16_655 8_455 ?
C7 O2 Cu1 110.99(17) . . ?
N2 N1 H1 123.9 . . ?
C3' N1 H1 123.9 . . ?
C3' N1 N2 112.1(2) . . ?
N1 N2 Cu1 118.27(17) . 2_554 ?
C5' N2 Cu1 135.87(19) . 2_554 ?
C5' N2 N1 105.8(2) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C1 120.2(3) . . ?
C5' C4' C4 126.4(3) . . ?
C3' C4' C4 128.1(3) . . ?
C3' C4' C5' 105.6(2) . . ?
C6 C1 C7 119.6(3) . . ?
C2 C1 C6 119.3(3) . . ?
C2 C1 C7 121.1(3) . . ?
C6 C5 H5 119.6 . . ?
C6 C5 C4 120.8(3) . . ?
C4 C5 H5 119.6 . . ?
C5 C4 C4' 119.8(2) . . ?
C5 C4 C3 118.5(2) . . ?
C3 C4 C4' 121.6(2) . . ?
N2 C5' C4' 109.8(2) . . ?
N2 C5' C51 122.2(2) . . ?
C4' C5' C51 127.9(2) . . ?
N1 C3' C4' 106.7(2) . . ?
N1 C3' C31 121.1(2) . . ?
C4' C3' C31 132.2(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 C4 120.6(3) . . ?
C2 C3 H3 119.7 . . ?
C13 O14 H14 109.5 . . ?
O2 C7 C1 115.9(2) . . ?
O1 C7 O2 123.4(3) . . ?
O1 C7 C1 120.7(3) . . ?
C3' C31 H31A 109.5 . . ?
C3' C31 H31B 109.5 . . ?
C3' C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1 C2 H2 119.8 . . ?
C3 C2 C1 120.5(3) . . ?
C3 C2 H2 119.8 . . ?
C5' C51 H51A 109.5 . . ?
C5' C51 H51B 109.5 . . ?
C5' C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C11 O10 H10 109.5 . . ?
O10 C11 H11A 109.5 . . ?
O10 C11 H11B 109.5 . . ?
O10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C15 O12 H12 109.5 . . ?
O12 C15 H15A 109.5 . . ?
O12 C15 H15B 109.5 . . ?
O12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O14 C13 H13A 109.5 . . ?
O14 C13 H13B 109.5 . . ?
O14 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?

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
Cu1 O2 C7 O1 1.3(3) . . . . ?
Cu1 O2 C7 C1 -177.38(18) . . . . ?
Cu1 N2 C5' C4' 176.7(2) 2_554 . . . ?
Cu1 N2 C5' C51 -6.2(4) 2_554 . . . ?
N1 N2 C5' C4' 0.0(3) . . . . ?
N1 N2 C5' C51 177.0(3) . . . . ?
N2 N1 C3' C4' -0.2(3) . . . . ?
N2 N1 C3' C31 -179.8(2) . . . . ?
C6 C1 C7 O2 5.8(4) . . . . ?
C6 C1 C7 O1 -173.0(3) . . . . ?
C6 C1 C2 C3 1.3(4) . . . . ?
C6 C5 C4 C4' -177.1(3) . . . . ?
C6 C5 C4 C3 1.5(4) . . . . ?
C4' C4 C3 C2 177.0(3) . . . . ?
C1 C6 C5 C4 -0.1(4) . . . . ?
C5 C6 C1 C7 177.0(3) . . . . ?
C5 C6 C1 C2 -1.4(4) . . . . ?
C5 C4 C3 C2 -1.6(4) . . . . ?
C4 C4' C5' N2 178.7(3) . . . . ?
C4 C4' C5' C51 1.9(5) . . . . ?
C4 C4' C3' N1 -178.6(3) . . . . ?
C4 C4' C3' C31 0.9(5) . . . . ?
C4 C3 C2 C1 0.2(4) . . . . ?
C5' C4' C4 C5 45.9(4) . . . . ?
C5' C4' C4 C3 -132.6(3) . . . . ?
C5' C4' C3' N1 0.2(3) . . . . ?
C5' C4' C3' C31 179.7(3) . . . . ?
C3' N1 N2 Cu1 -177.24(18) . . . 2_554 ?
C3' N1 N2 C5' 0.2(3) . . . . ?
C3' C4' C4 C5 -135.5(3) . . . . ?
C3' C4' C4 C3 46.0(4) . . . . ?
C3' C4' C5' N2 -0.1(3) . . . . ?
C3' C4' C5' C51 -177.0(3) . . . . ?
C7 C1 C2 C3 -177.0(3) . . . . ?
C2 C1 C7 O2 -175.9(2) . . . . ?
C2 C1 C7 O1 5.3(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT430_55crw               
;
PROBLEM: Short Inter D...A Contact  O16    ..  O16     ..       1.97 Ang.  
RESPONSE: O16 is the oxygen of a 50% partially occupied water molecule 
located in a channel system in the lattice. O16 is located close to the 
4-fold rotoinversion axis and the short inter D...A contact is not 
chemically meaningful because of the 50% partial occupancy.
;
####################################################################### 
# 
# 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_i2a
_database_code_depnum_ccdc_archive 'CCDC 1040606'
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_audit_creation_date             2014-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C204 H172 Cu16 N40 O32)'
_chemical_formula_sum            'C51 H43 Cu4 N10 O8'
_chemical_formula_weight         1178.11
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3280 1.2590 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y, -z'
3 'x+1/2, y+1/2, z+1/2'
4 '-x+1, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x-1/2, -y, z'
7 '-x+1/2, -y+1/2, -z+1/2'
8 'x, -y+1/2, z+1/2'

_symmetry_int_tables_number      15
_cell_length_a                   18.658(4)
_cell_length_b                   13.470(3)
_cell_length_c                   18.736(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.11(3)
_cell_angle_gamma                90.00
_cell_volume                     4705.6(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4578
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.18
_exptl_absorpt_coefficient_mu    1.852
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2396
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.1242
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30696
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.18
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71080
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_reflns_number_gt                2471
_reflns_number_total             4578
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XLMP (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         3.722
_refine_diff_density_min         -2.042
_refine_diff_density_rms         0.461
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.520
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4578
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.3323
_refine_ls_R_factor_gt           0.2556
_refine_ls_restrained_S_all      2.543
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5936
_refine_ls_wR_factor_ref         0.6441
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The structure model is based on very poor quality diffraction data which 
 were collected from a single crystal after high temperature desolvation in
 air. As such, significant non-merohedral twinning and substantial loss of
 diffraction intensity hindered the collection of a high quality dataset 
 using synchrotron radiation. The structure model is presented purely to
 establish connectivity. Most likely due to this twinning caused by fracturing
 of the crystals upon desolvation, substantial disorder appears throughout 
 the asymmetric unit, including both copper atoms being split over two positions 
 across symmetry elements. All atoms except for Cu1 and Cu2 were refined 
 isotropically to minimise the number of refined parameters and prevent 
 unreasonable ADPs. Most C-C and C-N distances were restrained with DFIX
 instructions in order to maintain sensible chemical geometries, with 
 standard uncertainties 0.02 Angstroms. All CH3 groups were modelled with
 AFIX 33 instructions to allow the refinement to properly converge. Clearly
 defined disorder was observed on both pyrazole rings within the ASU, and 
 both were modelled split across two orientations with 50% occupancy at each
 site. Similar disorder was modelled on both carboxylate groups. We were 
 unable to sensibly assign any lattice solvent molecules from the Fourier
 residuals, however residual electron density maps suggest the possibility 
 of water molecules present in the axial positions of the metal sites. Despite
 the poor quality of the data, no heavy atom constraints or rigid body 
 treatments proved necessary to form a reasonable structural model.
;
_olex2_refinement_description    
;
1. Others
 Fixed Sof: O1(0.5) O1A(0.5) O1B(0.5) O1C(0.5) N1(0.5) N1A(0.5) N1B(0.5)
 N1C(0.5) O2(0.5) O2A(0.5) O2B(0.5) O2C(0.5) N2B(0.5) N2C(0.5) C3'(0.5)
 C3A'(0.5) C3C'(0.5) C4C'(0.5) C7(0.5) C7A(0.5) C7B(0.5) C7C(0.5) C31(0.5)
 H31A(0.5) H31B(0.5) H31C(0.5) C31A(0.5) H31D(0.5) H31E(0.5) H31F(0.5)
 C31B(0.5) H31G(0.5) H31H(0.5) H31I(0.5) C31C(0.5) H31J(0.5) H31K(0.5)
 H31L(0.5) C51C(0.5) H51G(0.5) H51H(0.5) H51I(0.5)
 Fixed Uiso: H2(0.069) H2B(0.073) H3(0.057) H3B(0.058) H5(0.039) H5B(0.051)
 H6(0.055) H6B(0.068) H31A(0.069) H31B(0.069) H31C(0.069) H31D(0.111)
 H31E(0.111) H31F(0.111) H31G(0.072) H31H(0.072) H31I(0.072) H31J(0.124)
 H31K(0.124) H31L(0.124) H51A(0.163) H51B(0.163) H51C(0.163) H51D(0.16)
 H51E(0.16) H51F(0.16) H51G(0.097) H51H(0.097) H51I(0.097)
 Fixed X: H2(0.4297) H2B(0.7971) H3(0.4831) H3B(0.8309) H5(0.665) H5B(0.9135)
 H6(0.6065) H6B(0.8909) H31A(0.5644) H31B(0.6179) H31C(0.6447) H31D(0.5785)
 H31E(0.6638) H31F(0.623) H31G(1.0368) H31H(1.0514) H31I(1.0243) H31J(1.064)
 H31K(1.045) H31L(1.0178) H51A(0.6555) H51B(0.7232) H51C(0.6464) H51D(0.7357)
 H51E(0.7306) H51F(0.7407) H51G(0.768) H51H(0.7511) H51I(0.7485)
 Fixed Y: H2(0.8336) H2B(1.0113) H3(0.9882) H3B(0.874) H5(0.8829) H5B(0.7592)
 H6(0.7343) H6B(0.9194) H31A(1.0599) H31B(1.1412) H31C(1.0295) H31D(1.0632)
 H31E(1.0616) H31F(0.9661) H31G(0.7337) H31H(0.6172) H31I(0.6807) H31J(0.7003)
 H31K(0.7672) H31L(0.7996) H51A(1.0097) H51B(1.0821) H51C(1.1259) H51D(0.719)
 H51E(0.6071) H51F(0.6965) H51G(0.5795) H51H(0.5732) H51I(0.6781)
 Fixed Z: H2(0.6505) H2B(0.6377) H3(0.6706) H3B(0.5746) H5(0.5857) H5B(0.7619)
 H6(0.5561) H6B(0.813) H31A(0.7664) H31B(0.8008) H31C(0.7901) H31D(0.8127)
 H31E(0.8249) H31F(0.7928) H31G(0.6024) H31H(0.6114) H31I(0.6774) H31J(0.5877)
 H31K(0.655) H31L(0.5764) H51A(0.4996) H51B(0.5085) H51C(0.4843) H51D(0.6105)
 H51E(0.582) H51F(0.527) H51G(0.6779) H51H(0.5937) H51I(0.6337)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Cu1 Cu 0.7504(3) 1.2649(3) 0.7260(2) 0.0805(16) Uani 1 d . . .
O1 O 0.4210(15) 0.6504(19) 0.5690(13) 0.033(5) Uiso 0.50 d A 2 .
O1A O 0.3944(15) 0.698(2) 0.5530(15) 0.045(6) Uiso 0.50 d B 1 .
O1B O 0.8084(17) 1.039(2) 0.8515(17) 0.056(7) Uiso 0.50 d C 1 .
O1C O 0.8076(13) 1.0963(19) 0.8136(13) 0.035(5) Uiso 0.50 d . 2 .
N1 N 0.690(2) 1.177(2) 0.6004(16) 0.071(12) Uiso 0.50 d D 2 D
N1A N 0.6892(18) 1.163(2) 0.6318(13) 0.047(8) Uiso 0.50 d D 1 D
N1B N 0.8586(17) 0.577(2) 0.5490(17) 0.039(7) Uiso 0.50 d E 2 .
N1C N 0.8972(16) 0.562(2) 0.5818(16) 0.029(6) Uiso 0.50 d F 1 D
C1 C 0.5118(11) 0.7683(16) 0.5961(11) 0.047(5) Uiso 1 d . . .
C1B C 0.8414(13) 0.9812(16) 0.7307(12) 0.053(5) Uiso 1 d . . D
Cu2 Cu 0.52261(19) 0.4865(2) 0.5109(2) 0.0721(14) Uani 1 d . . .
O2 O 0.5342(11) 0.5927(14) 0.5770(10) 0.019(4) Uiso 0.50 d . 2 .
O2A O 0.4981(15) 0.615(2) 0.5575(14) 0.036(5) Uiso 0.50 d . 1 .
O2B O 0.8145(15) 1.128(2) 0.7477(16) 0.040(6) Uiso 0.50 d . 1 .
O2C O 0.8143(13) 1.1574(18) 0.7032(14) 0.035(5) Uiso 0.50 d . 2 .
N2 N 0.6734(12) 1.1872(15) 0.6681(13) 0.065(5) Uiso 1 d D 2 D
N2A N 0.6761(11) 1.1633(15) 0.7037(11) 0.061(5) Uiso 1 d . 1 D
N2B N 0.9257(14) 0.5752(16) 0.5530(14) 0.015(5) Uiso 0.50 d . 2 .
N2C N 0.9545(15) 0.5852(18) 0.5757(14) 0.021(5) Uiso 0.50 d . 1 .
C2 C 0.4766(14) 0.8453(18) 0.6344(13) 0.058(6) Uiso 1 d . . .
H2 H 0.4297 0.8336 0.6505 0.069 Uiso 1 calc . . R
C2B C 0.8243(14) 0.962(2) 0.6628(13) 0.061(6) Uiso 1 d . . .
H2B H 0.7971 1.0113 0.6377 0.073 Uiso 1 calc . . R
C3 C 0.5090(12) 0.9363(16) 0.6489(11) 0.048(5) Uiso 1 d . . .
H3 H 0.4831 0.9882 0.6706 0.057 Uiso 1 calc B . R
C3' C 0.639(2) 1.108(2) 0.6975(10) 0.039(9) Uiso 0.50 d D 2 D
C3A' C 0.6330(19) 1.083(2) 0.7109(12) 0.034(8) Uiso 0.50 d D 1 D
C3B C 0.8415(12) 0.8785(16) 0.6245(11) 0.048(5) Uiso 1 d . . .
H3B H 0.8309 0.8740 0.5746 0.058 Uiso 1 calc C . R
C3B' C 0.9456(12) 0.652(2) 0.6027(16) 0.071(7) Uiso 1 d G 2 D
C3C' C 0.9600(12) 0.685(3) 0.617(3) 0.077(18) Uiso 0.50 d G 1 D
C4 C 0.5804(9) 0.9502(13) 0.6309(9) 0.032(4) Uiso 1 d D . .
C4' C 0.6203(10) 1.0477(13) 0.6415(8) 0.043(4) Uiso 1 d . . D
C4B C 0.8756(8) 0.8000(12) 0.6624(8) 0.027(3) Uiso 1 d G . .
C4B' C 0.8886(7) 0.7052(11) 0.6234(8) 0.029(3) Uiso 1 d . . D
C4C' C 0.8450(19) 0.628(2) 0.620(2) 0.044(9) Uiso 0.50 d F 1 D
C5 C 0.6163(10) 0.8743(13) 0.5972(9) 0.033(4) Uiso 1 d . . .
H5 H 0.6650 0.8829 0.5857 0.039 Uiso 1 calc D . R
C5' C 0.6555(17) 1.092(2) 0.5866(10) 0.093(9) Uiso 1 d D . D
C5B C 0.8924(10) 0.8111(15) 0.7340(10) 0.042(4) Uiso 1 d . . .
H5B H 0.9135 0.7592 0.7619 0.051 Uiso 1 calc G . R
C5B' C 0.8323(14) 0.662(3) 0.5841(17) 0.081(8) Uiso 1 d E 2 D
C6 C 0.5810(11) 0.7848(16) 0.5799(11) 0.046(4) Uiso 1 d D . .
H6 H 0.6065 0.7343 0.5561 0.055 Uiso 1 calc . . R
C6B C 0.8758(13) 0.9080(18) 0.7648(13) 0.057(5) Uiso 1 d G . .
H6B H 0.8909 0.9194 0.8130 0.068 Uiso 1 calc . . R
C7 C 0.459(4) 0.674(4) 0.561(3) 0.054(11) Uiso 0.50 d B 1 .
C7A C 0.488(2) 0.661(3) 0.581(2) 0.027(7) Uiso 0.50 d A 2 .
C7B C 0.820(2) 1.054(3) 0.782(2) 0.039(8) Uiso 0.50 d C 1 .
C7C C 0.8211(19) 1.086(2) 0.753(2) 0.032(8) Uiso 0.50 d . 2 D
C31 C 0.614(2) 1.083(3) 0.7699(15) 0.046(9) Uiso 0.50 d D 2 D
H31A H 0.5644 1.0599 0.7664 0.069 Uiso 0.50 calc D 2 R
H31B H 0.6179 1.1412 0.8008 0.069 Uiso 0.50 calc D 2 R
H31C H 0.6447 1.0295 0.7901 0.069 Uiso 0.50 calc D 2 R
C31A C 0.624(3) 1.039(5) 0.794(3) 0.074(15) Uiso 0.50 d D 1 .
H31D H 0.5785 1.0632 0.8127 0.111 Uiso 0.50 calc D 1 R
H31E H 0.6638 1.0616 0.8249 0.111 Uiso 0.50 calc D 1 R
H31F H 0.6230 0.9661 0.7928 0.111 Uiso 0.50 calc D 1 R
C31B C 1.0209(16) 0.673(3) 0.625(2) 0.048(9) Uiso 0.50 d G 2 D
H31G H 1.0368 0.7337 0.6024 0.072 Uiso 0.50 calc G 2 R
H31H H 1.0514 0.6172 0.6114 0.072 Uiso 0.50 calc G 2 R
H31I H 1.0243 0.6807 0.6774 0.072 Uiso 0.50 calc G 2 R
C31C C 1.028(3) 0.743(5) 0.608(3) 0.083(16) Uiso 0.50 d G 1 D
H31J H 1.0640 0.7003 0.5877 0.124 Uiso 0.50 calc G 1 R
H31K H 1.0450 0.7672 0.6550 0.124 Uiso 0.50 calc G 1 R
H31L H 1.0178 0.7996 0.5764 0.124 Uiso 0.50 calc G 1 R
C51 C 0.671(2) 1.076(3) 0.514(2) 0.109(12) Uiso 1 d . . .
H51A H 0.6555 1.0097 0.4996 0.163 Uiso 1 calc D . R
H51B H 0.7232 1.0821 0.5085 0.163 Uiso 1 calc . . R
H51C H 0.6464 1.1259 0.4843 0.163 Uiso 1 calc . . R
C51B C 0.753(2) 0.672(3) 0.575(2) 0.107(11) Uiso 1 d E 2 .
H51D H 0.7357 0.7190 0.6105 0.160 Uiso 1 calc E 2 R
H51E H 0.7306 0.6071 0.5820 0.160 Uiso 1 calc E 2 R
H51F H 0.7407 0.6965 0.5270 0.160 Uiso 1 calc E 2 R
C51C C 0.773(3) 0.614(4) 0.632(3) 0.064(12) Uiso 0.50 d F 1 .
H51G H 0.7680 0.5795 0.6779 0.097 Uiso 0.50 calc F 1 R
H51H H 0.7511 0.5732 0.5937 0.097 Uiso 0.50 calc F 1 R
H51I H 0.7485 0.6781 0.6337 0.097 Uiso 0.50 calc F 1 R


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cu1 0.984(7) 7_676 ?
Cu1 O1C 2.27(3) 7_676 ?
Cu1 N1A 2.48(2) . ?
Cu1 O2B 2.23(3) . ?
Cu1 O2B 1.96(3) 7_676 ?
Cu1 O2C 1.93(2) . ?
Cu1 O2C 2.11(2) 7_676 ?
Cu1 N2 2.05(2) . ?
Cu1 N2A 1.983(19) . ?
Cu1 N2A 2.101(18) 7_676 ?
Cu1 C7C 2.46(3) 7_676 ?
O1 C7A 1.28(5) . ?
O1A C7 1.24(7) . ?
O1B C7B 1.33(6) . ?
O1C Cu1 2.27(3) 7_676 ?
O1C C7C 1.19(5) . ?
N1 N2 1.323(19) . ?
N1 C5' 1.333(19) . ?
N1A N2A 1.378(18) . ?
N1A C5' 1.412(18) . ?
N1B N2B 1.25(4) . ?
N1B C5B' 1.42(4) . ?
N1C N2C 1.12(4) . ?
N1C C4C' 1.52(5) . ?
C1 C2 1.43(3) . ?
C1 C6 1.36(3) . ?
C1 C7 1.72(6) . ?
C1 C7A 1.53(4) . ?
C1B C2B 1.33(3) . ?
C1B C6B 1.33(3) . ?
C1B C7B 1.45(5) . ?
C1B C7C 1.517(19) . ?
Cu2 Cu2 0.993(7) 5_666 ?
Cu2 O2 2.20(2) 5_666 ?
Cu2 O2 1.900(19) . ?
Cu2 O2A 1.90(3) 5_666 ?
Cu2 O2A 2.00(3) . ?
Cu2 N2B 1.97(2) 2_656 ?
Cu2 N2B 2.16(3) 6_565 ?
Cu2 N2C 2.15(3) 2_656 ?
Cu2 N2C 2.03(2) 6_565 ?
O2 Cu2 2.20(2) 5_666 ?
O2 C7A 1.26(5) . ?
O2A Cu2 1.90(3) 5_666 ?
O2A C7 1.09(6) . ?
O2B Cu1 1.96(3) 7_676 ?
O2B C7B 1.19(5) . ?
O2C Cu1 2.11(2) 7_676 ?
O2C C7C 1.34(5) . ?
N2 C3' 1.371(18) . ?
N2A Cu1 2.101(18) 7_676 ?
N2A C3A' 1.358(18) . ?
N2B Cu2 1.97(2) 2_656 ?
N2B Cu2 2.16(3) 6_665 ?
N2B C3B' 1.43(4) . ?
N2C Cu2 2.15(3) 2_656 ?
N2C Cu2 2.03(2) 6_665 ?
N2C C3C' 1.55(5) . ?
C2 C3 1.39(3) . ?
C2B C3B 1.38(3) . ?
C3 C4 1.40(3) . ?
C3' C4' 1.364(17) . ?
C3' C31 1.486(19) . ?
C3A' C4' 1.396(18) . ?
C3A' C31A 1.68(7) . ?
C3B C4B 1.41(3) . ?
C3B' C4B' 1.352(18) . ?
C3B' C31B 1.480(19) . ?
C3C' C4B' 1.37(2) . ?
C3C' C31C 1.50(2) . ?
C4 C4' 1.52(2) . ?
C4 C5 1.39(2) . ?
C4' C5' 1.377(13) . ?
C4B C4B' 1.50(2) . ?
C4B C5B 1.37(3) . ?
C4B' C4C' 1.318(19) . ?
C4B' C5B' 1.387(18) . ?
C4C' C51C 1.39(6) . ?
C5 C6 1.41(3) . ?
C5' C51 1.42(4) . ?
C5B C6B 1.46(3) . ?
C5B' C51B 1.49(5) . ?
C7C Cu1 2.46(3) 7_676 ?

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
Cu1 Cu1 O1C 127.6(9) 7_676 7_676 ?
Cu1 Cu1 N1A 113.7(8) 7_676 . ?
Cu1 Cu1 O2B 92.3(10) 7_676 7_676 ?
Cu1 Cu1 O2B 61.5(9) 7_676 . ?
Cu1 Cu1 O2C 85.9(9) 7_676 . ?
Cu1 Cu1 O2C 66.3(8) 7_676 7_676 ?
Cu1 Cu1 N2 103.9(9) 7_676 . ?
Cu1 Cu1 N2A 82.9(8) 7_676 . ?
Cu1 Cu1 N2A 69.4(8) 7_676 7_676 ?
Cu1 Cu1 C7C 99.1(12) 7_676 7_676 ?
O1C Cu1 N1A 91.2(10) 7_676 . ?
O1C Cu1 C7C 28.8(12) 7_676 7_676 ?
O2B Cu1 O1C 35.2(11) 7_676 7_676 ?
O2B Cu1 O1C 170.9(10) . 7_676 ?
O2B Cu1 N1A 84.4(11) . . ?
O2B Cu1 N1A 108.2(12) 7_676 . ?
O2B Cu1 O2B 153.9(5) 7_676 . ?
O2B Cu1 O2C 26.0(9) 7_676 7_676 ?
O2B Cu1 N2 94.7(10) 7_676 . ?
O2B Cu1 N2A 97.3(10) 7_676 . ?
O2B Cu1 N2A 84.2(10) 7_676 7_676 ?
O2B Cu1 C7C 160.1(15) . 7_676 ?
O2B Cu1 C7C 8.2(14) 7_676 7_676 ?
O2C Cu1 O1C 61.2(10) 7_676 7_676 ?
O2C Cu1 O1C 146.5(10) . 7_676 ?
O2C Cu1 N1A 117.6(11) 7_676 . ?
O2C Cu1 N1A 72.6(11) . . ?
O2C Cu1 O2B 24.4(9) . . ?
O2C Cu1 O2B 178.2(9) . 7_676 ?
O2C Cu1 O2B 127.9(8) 7_676 . ?
O2C Cu1 O2C 152.2(4) . 7_676 ?
O2C Cu1 N2 85.8(10) . . ?
O2C Cu1 N2A 82.5(9) . . ?
O2C Cu1 N2A 95.2(9) . 7_676 ?
O2C Cu1 C7C 33.0(13) 7_676 7_676 ?
O2C Cu1 C7C 173.2(13) . 7_676 ?
N2 Cu1 O1C 86.1(9) . 7_676 ?
N2 Cu1 N1A 17.8(8) . . ?
N2 Cu1 O2B 92.0(10) . . ?
N2 Cu1 O2C 100.4(9) . 7_676 ?
N2 Cu1 N2A 173.1(7) . 7_676 ?
N2 Cu1 C7C 97.5(11) . 7_676 ?
N2A Cu1 O1C 96.7(9) 7_676 7_676 ?
N2A Cu1 O1C 100.3(9) . 7_676 ?
N2A Cu1 N1A 33.7(6) . . ?
N2A Cu1 N1A 166.7(10) 7_676 . ?
N2A Cu1 O2B 80.4(10) . . ?
N2A Cu1 O2B 86.2(10) 7_676 . ?
N2A Cu1 O2C 75.7(9) 7_676 7_676 ?
N2A Cu1 O2C 93.6(9) . 7_676 ?
N2A Cu1 N2 21.1(6) . . ?
N2A Cu1 N2A 152.3(3) . 7_676 ?
N2A Cu1 C7C 102.7(11) . 7_676 ?
N2A Cu1 C7C 82.3(10) 7_676 7_676 ?
C7C Cu1 N1A 109.3(13) 7_676 . ?
C7C O1C Cu1 84(2) . 7_676 ?
N2 N1 C5' 98.5(17) . . ?
N2A N1A Cu1 53.0(11) . . ?
N2A N1A C5' 119.7(18) . . ?
C5' N1A Cu1 170(2) . . ?
N2B N1B C5B' 111(3) . . ?
N2C N1C C4C' 121(2) . . ?
C2 C1 C7 117(3) . . ?
C2 C1 C7A 130(2) . . ?
C6 C1 C2 117(2) . . ?
C6 C1 C7 125(3) . . ?
C6 C1 C7A 112(2) . . ?
C7A C1 C7 23.3(17) . . ?
C2B C1B C6B 114(2) . . ?
C2B C1B C7B 135(3) . . ?
C2B C1B C7C 113(2) . . ?
C6B C1B C7B 109(3) . . ?
C6B C1B C7C 133(3) . . ?
C7B C1B C7C 27.5(17) . . ?
Cu2 Cu2 O2 93.8(8) 5_666 . ?
Cu2 Cu2 O2 59.4(7) 5_666 5_666 ?
Cu2 Cu2 O2A 80.6(10) 5_666 5_666 ?
Cu2 Cu2 O2A 70.0(9) 5_666 . ?
Cu2 Cu2 N2B 65.3(8) 5_666 6_565 ?
Cu2 Cu2 N2B 87.4(9) 5_666 2_656 ?
Cu2 Cu2 N2C 83.0(10) 5_666 6_565 ?
Cu2 Cu2 N2C 69.7(9) 5_666 2_656 ?
O2 Cu2 O2 153.3(3) . 5_666 ?
O2 Cu2 O2A 23.9(7) . . ?
O2 Cu2 O2A 174.4(8) . 5_666 ?
O2 Cu2 N2B 97.3(9) . 6_565 ?
O2 Cu2 N2B 83.9(9) . 2_656 ?
O2 Cu2 N2C 90.3(9) . 2_656 ?
O2 Cu2 N2C 91.5(9) . 6_565 ?
O2A Cu2 O2 129.4(8) . 5_666 ?
O2A Cu2 O2 21.2(8) 5_666 5_666 ?
O2A Cu2 O2A 150.6(5) 5_666 . ?
O2A Cu2 N2B 96.7(10) 5_666 2_656 ?
O2A Cu2 N2B 79.6(10) 5_666 6_565 ?
O2A Cu2 N2B 88.0(10) . 6_565 ?
O2A Cu2 N2C 89.5(10) . 6_565 ?
O2A Cu2 N2C 81.4(10) . 2_656 ?
O2A Cu2 N2C 86.9(10) 5_666 6_565 ?
O2A Cu2 N2C 88.6(10) 5_666 2_656 ?
N2B Cu2 O2 72.6(8) 6_565 5_666 ?
N2B Cu2 O2 94.1(9) 2_656 5_666 ?
N2B Cu2 O2A 82.3(10) 2_656 . ?
N2B Cu2 N2B 152.7(4) 2_656 6_565 ?
N2B Cu2 N2C 18.5(8) 2_656 2_656 ?
N2B Cu2 N2C 169.1(9) 2_656 6_565 ?
N2C Cu2 O2 85.5(9) 6_565 5_666 ?
N2C Cu2 O2 80.7(9) 2_656 5_666 ?
N2C Cu2 N2B 18.4(8) 6_565 6_565 ?
N2C Cu2 N2B 134.7(7) 2_656 6_565 ?
N2C Cu2 N2C 152.7(4) 6_565 2_656 ?
Cu2 O2 Cu2 26.7(3) . 5_666 ?
C7A O2 Cu2 122(2) . . ?
C7A O2 Cu2 95(2) . 5_666 ?
Cu2 O2A Cu2 29.4(5) 5_666 . ?
C7 O2A Cu2 117(4) . 5_666 ?
C7 O2A Cu2 146(4) . . ?
Cu1 O2B Cu1 26.1(5) 7_676 . ?
C7B O2B Cu1 145(3) . . ?
C7B O2B Cu1 121(3) . 7_676 ?
Cu1 O2C Cu1 27.8(4) . 7_676 ?
C7C O2C Cu1 115(2) . . ?
C7C O2C Cu1 88.0(19) . 7_676 ?
N1 N2 Cu1 112.2(19) . . ?
N1 N2 C3' 115.9(17) . . ?
C3' N2 Cu1 121.0(19) . . ?
Cu1 N2A Cu1 27.7(3) . 7_676 ?
N1A N2A Cu1 93.3(14) . . ?
N1A N2A Cu1 118.5(15) . 7_676 ?
C3A' N2A Cu1 160.3(18) . . ?
C3A' N2A Cu1 132.8(17) . 7_676 ?
C3A' N2A N1A 102.9(15) . . ?
N1B N2B Cu2 147(2) . 6_665 ?
N1B N2B Cu2 119(2) . 2_656 ?
N1B N2B C3B' 105(2) . . ?
Cu2 N2B Cu2 27.3(4) 2_656 6_665 ?
C3B' N2B Cu2 135.5(19) . 2_656 ?
C3B' N2B Cu2 108.4(17) . 6_665 ?
N1C N2C Cu2 97(2) . 2_656 ?
N1C N2C Cu2 123(2) . 6_665 ?
N1C N2C C3C' 104(2) . . ?
Cu2 N2C Cu2 27.3(4) 6_665 2_656 ?
C3C' N2C Cu2 154(2) . 2_656 ?
C3C' N2C Cu2 133(2) . 6_665 ?
C3 C2 C1 122(2) . . ?
C1B C2B C3B 127(2) . . ?
C2 C3 C4 119(2) . . ?
N2 C3' C31 136(2) . . ?
C4' C3' N2 105.3(14) . . ?
C4' C3' C31 119(2) . . ?
N2A C3A' C4' 105.0(17) . . ?
N2A C3A' C31A 117(3) . . ?
C4' C3A' C31A 136(3) . . ?
C2B C3B C4B 117.2(19) . . ?
N2B C3B' C31B 123(2) . . ?
C4B' C3B' N2B 113(2) . . ?
C4B' C3B' C31B 124(3) . . ?
C4B' C3C' N2C 100(2) . . ?
C4B' C3C' C31C 137(4) . . ?
C31C C3C' N2C 116(4) . . ?
C3 C4 C4' 123.4(17) . . ?
C5 C4 C3 119.4(17) . . ?
C5 C4 C4' 117.0(15) . . ?
C3' C4' C3A' 18.3(14) . . ?
C3' C4' C4 136.6(16) . . ?
C3' C4' C5' 101.7(13) . . ?
C3A' C4' C4 118.8(16) . . ?
C5' C4' C3A' 118.7(16) . . ?
C5' C4' C4 121.4(14) . . ?
C3B C4B C4B' 118.1(15) . . ?
C5B C4B C3B 119.4(16) . . ?
C5B C4B C4B' 122.4(15) . . ?
C3B' C4B' C3C' 24(2) . . ?
C3B' C4B' C4B 137.5(18) . . ?
C3B' C4B' C5B' 102(2) . . ?
C3C' C4B' C4B 113(2) . . ?
C3C' C4B' C5B' 126(3) . . ?
C4C' C4B' C3B' 93(2) . . ?
C4C' C4B' C3C' 116(3) . . ?
C4C' C4B' C4B 126(2) . . ?
C4C' C4B' C5B' 35.9(18) . . ?
C5B' C4B' C4B 118.9(18) . . ?
C4B' C4C' N1C 95(2) . . ?
C4B' C4C' C51C 135(4) . . ?
C51C C4C' N1C 130(3) . . ?
C4 C5 C6 120.5(17) . . ?
N1 C5' N1A 25.8(15) . . ?
N1 C5' C4' 117.8(15) . . ?
N1 C5' C51 101(2) . . ?
N1A C5' C51 125(3) . . ?
C4' C5' N1A 93.5(15) . . ?
C4' C5' C51 141(2) . . ?
C4B C5B C6B 115.9(18) . . ?
N1B C5B' C51B 112(3) . . ?
C4B' C5B' N1B 108(2) . . ?
C4B' C5B' C51B 139(3) . . ?
C1 C6 C5 122.0(19) . . ?
C1B C6B C5B 125(2) . . ?
O1A C7 C1 114(4) . . ?
O2A C7 O1A 146(6) . . ?
O2A C7 C1 101(5) . . ?
O1 C7A C1 114(3) . . ?
O2 C7A O1 125(3) . . ?
O2 C7A C1 121(3) . . ?
O1B C7B C1B 128(4) . . ?
O2B C7B O1B 130(4) . . ?
O2B C7B C1B 102(4) . . ?
O1C C7C Cu1 66.9(17) . 7_676 ?
O1C C7C C1B 116(4) . . ?
O1C C7C O2C 124(3) . . ?
C1B C7C Cu1 161(2) . 7_676 ?
O2C C7C Cu1 58.9(15) . 7_676 ?
O2C C7C C1B 120(3) . . ?

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
Cu1 Cu1 N1A N2A 26(2) 7_676 . . . ?
Cu1 Cu1 N1A C5' -18(15) 7_676 . . . ?
Cu1 Cu1 O2B C7B 28(4) 7_676 . . . ?
Cu1 Cu1 O2C C7C 9(2) 7_676 . . . ?
Cu1 Cu1 N2 N1 -147(2) 7_676 . . . ?
Cu1 Cu1 N2 C3' -5(2) 7_676 . . . ?
Cu1 Cu1 N2A N1A -156.5(19) 7_676 . . . ?
Cu1 Cu1 N2A C3A' -11(6) 7_676 . . . ?
Cu1 O1C C7C C1B -159(3) 7_676 . . . ?
Cu1 O1C C7C O2C 16(3) 7_676 . . . ?
Cu1 N1A N2A Cu1 -12.1(9) . . . 7_676 ?
Cu1 N1A N2A C3A' -169(3) . . . . ?
Cu1 N1A C5' N1 -160(19) . . . . ?
Cu1 N1A C5' C4' 39(15) . . . . ?
Cu1 N1A C5' C51 -132(13) . . . . ?
Cu1 O2B C7B O1B -41(7) . . . . ?
Cu1 O2B C7B O1B -27(5) 7_676 . . . ?
Cu1 O2B C7B C1B 153(2) 7_676 . . . ?
Cu1 O2B C7B C1B 139(4) . . . . ?
Cu1 O2C C7C Cu1 -4.4(10) . . . 7_676 ?
Cu1 O2C C7C O1C -17(4) 7_676 . . . ?
Cu1 O2C C7C O1C -21(4) . . . . ?
Cu1 O2C C7C C1B 158(3) 7_676 . . . ?
Cu1 O2C C7C C1B 154(2) . . . . ?
Cu1 N2 C3' C4' -151(2) . . . . ?
Cu1 N2 C3' C31 34(6) . . . . ?
Cu1 N2A C3A' C4' -156.2(17) 7_676 . . . ?
Cu1 N2A C3A' C4' -150(5) . . . . ?
Cu1 N2A C3A' C31A 12(5) 7_676 . . . ?
Cu1 N2A C3A' C31A 18(8) . . . . ?
O1C Cu1 N1A N2A -106.9(18) 7_676 . . . ?
O1C Cu1 N1A C5' -150(15) 7_676 . . . ?
O1C Cu1 O2B Cu1 178(6) 7_676 . . 7_676 ?
O1C Cu1 O2B C7B -154(6) 7_676 . . . ?
O1C Cu1 O2C Cu1 179.4(18) 7_676 . . 7_676 ?
O1C Cu1 O2C C7C -171(2) 7_676 . . . ?
O1C Cu1 N2 N1 85(2) 7_676 . . . ?
O1C Cu1 N2 C3' -132(2) 7_676 . . . ?
O1C Cu1 N2A Cu1 -127.0(9) 7_676 . . 7_676 ?
O1C Cu1 N2A N1A 76(2) 7_676 . . . ?
O1C Cu1 N2A C3A' -138(6) 7_676 . . . ?
N1 N2 C3' C4' -10(5) . . . . ?
N1 N2 C3' C31 175(5) . . . . ?
N1A Cu1 O2B Cu1 -120.9(10) . . . 7_676 ?
N1A Cu1 O2B C7B -93(5) . . . . ?
N1A Cu1 O2C Cu1 -116.4(9) . . . 7_676 ?
N1A Cu1 O2C C7C -107(2) . . . . ?
N1A Cu1 N2 N1 -21(4) . . . . ?
N1A Cu1 N2 C3' 121(4) . . . . ?
N1A Cu1 N2A Cu1 156.5(19) . . . 7_676 ?
N1A Cu1 N2A C3A' 146(7) . . . . ?
N1A N2A C3A' C4' -4(3) . . . . ?
N1A N2A C3A' C31A 163(4) . . . . ?
N1B N2B C3B' C4B' -5(3) . . . . ?
N1B N2B C3B' C31B 178(3) . . . . ?
N1C N2C C3C' C4B' -15(4) . . . . ?
N1C N2C C3C' C31C -170(5) . . . . ?
C1 C2 C3 C4 -6(3) . . . . ?
C1B C2B C3B C4B 6(4) . . . . ?
Cu2 Cu2 O2 C7A 3(2) 5_666 . . . ?
Cu2 Cu2 O2A C7 5(6) 5_666 . . . ?
Cu2 O2 C7A O1 33(4) 5_666 . . . ?
Cu2 O2 C7A O1 32(5) . . . . ?
Cu2 O2 C7A C1 -142(3) 5_666 . . . ?
Cu2 O2 C7A C1 -143(2) . . . . ?
Cu2 O2A C7 O1A 25(14) . . . . ?
Cu2 O2A C7 O1A 28(11) 5_666 . . . ?
Cu2 O2A C7 C1 -158(4) . . . . ?
Cu2 O2A C7 C1 -155.6(19) 5_666 . . . ?
Cu2 N2B C3B' C4B' 170.2(19) 6_665 . . . ?
Cu2 N2B C3B' C4B' 167.4(19) 2_656 . . . ?
Cu2 N2B C3B' C31B -10(5) 2_656 . . . ?
Cu2 N2B C3B' C31B -7(4) 6_665 . . . ?
Cu2 N2C C3C' C4B' 156(2) 6_665 . . . ?
Cu2 N2C C3C' C4B' 127(4) 2_656 . . . ?
Cu2 N2C C3C' C31C 0(7) 6_665 . . . ?
Cu2 N2C C3C' C31C -29(9) 2_656 . . . ?
O2 Cu2 O2 Cu2 -0.001(2) 5_666 . . 5_666 ?
O2 Cu2 O2 C7A 3(2) 5_666 . . . ?
O2 Cu2 O2A Cu2 1.0(12) 5_666 . . 5_666 ?
O2 Cu2 O2A Cu2 -178(3) . . . 5_666 ?
O2 Cu2 O2A C7 6(7) 5_666 . . . ?
O2 Cu2 O2A C7 -173(7) . . . . ?
O2A Cu2 O2 Cu2 -9(10) 5_666 . . 5_666 ?
O2A Cu2 O2 Cu2 2(2) . . . 5_666 ?
O2A Cu2 O2 C7A -6(12) 5_666 . . . ?
O2A Cu2 O2 C7A 5(3) . . . . ?
O2A Cu2 O2A Cu2 0.004(3) 5_666 . . 5_666 ?
O2A Cu2 O2A C7 5(6) 5_666 . . . ?
O2B Cu1 N1A N2A 81.1(19) . . . . ?
O2B Cu1 N1A N2A -75(2) 7_676 . . . ?
O2B Cu1 N1A C5' -119(15) 7_676 . . . ?
O2B Cu1 N1A C5' 38(15) . . . . ?
O2B Cu1 O2B Cu1 0.002(3) 7_676 . . 7_676 ?
O2B Cu1 O2B C7B 28(4) 7_676 . . . ?
O2B Cu1 O2C Cu1 0(2) . . . 7_676 ?
O2B Cu1 O2C Cu1 0(37) 7_676 . . 7_676 ?
O2B Cu1 O2C C7C 10(38) 7_676 . . . ?
O2B Cu1 O2C C7C 9(3) . . . . ?
O2B Cu1 N2 N1 119(3) 7_676 . . . ?
O2B Cu1 N2 N1 -86(3) . . . . ?
O2B Cu1 N2 C3' -98(3) 7_676 . . . ?
O2B Cu1 N2 C3' 57(2) . . . . ?
O2B Cu1 N2A Cu1 62.2(9) . . . 7_676 ?
O2B Cu1 N2A Cu1 -91.4(10) 7_676 . . 7_676 ?
O2B Cu1 N2A N1A 112(2) 7_676 . . . ?
O2B Cu1 N2A N1A -94(2) . . . . ?
O2B Cu1 N2A C3A' -102(6) 7_676 . . . ?
O2B Cu1 N2A C3A' 52(6) . . . . ?
O2C Cu1 N1A N2A -49(2) 7_676 . . . ?
O2C Cu1 N1A N2A 103(2) . . . . ?
O2C Cu1 N1A C5' -93(15) 7_676 . . . ?
O2C Cu1 N1A C5' 59(15) . . . . ?
O2C Cu1 O2B Cu1 0.0(13) 7_676 . . 7_676 ?
O2C Cu1 O2B Cu1 180(3) . . . 7_676 ?
O2C Cu1 O2B C7B 28(5) 7_676 . . . ?
O2C Cu1 O2B C7B -152(6) . . . . ?
O2C Cu1 O2C Cu1 0.004(2) 7_676 . . 7_676 ?
O2C Cu1 O2C C7C 9(2) 7_676 . . . ?
O2C Cu1 N2 N1 -62(2) . . . . ?
O2C Cu1 N2 N1 145(2) 7_676 . . . ?
O2C Cu1 N2 C3' -73(2) 7_676 . . . ?
O2C Cu1 N2 C3' 80(2) . . . . ?
O2C Cu1 N2A Cu1 86.8(9) . . . 7_676 ?
O2C Cu1 N2A Cu1 -65.6(8) 7_676 . . 7_676 ?
O2C Cu1 N2A N1A -70(2) . . . . ?
O2C Cu1 N2A N1A 138(2) 7_676 . . . ?
O2C Cu1 N2A C3A' -76(6) 7_676 . . . ?
O2C Cu1 N2A C3A' 76(6) . . . . ?
N2 Cu1 N1A N2A -34(3) . . . . ?
N2 Cu1 N1A C5' -77(13) . . . . ?
N2 Cu1 O2B Cu1 -104.8(10) . . . 7_676 ?
N2 Cu1 O2B C7B -77(5) . . . . ?
N2 Cu1 O2C Cu1 -104.3(9) . . . 7_676 ?
N2 Cu1 O2C C7C -95(2) . . . . ?
N2 Cu1 N2A Cu1 -175(2) . . . 7_676 ?
N2 Cu1 N2A N1A 28(2) . . . . ?
N2 Cu1 N2A C3A' 174(8) . . . . ?
N2 N1 C5' N1A -22(4) . . . . ?
N2 N1 C5' C4' -1(5) . . . . ?
N2 N1 C5' C51 -180(3) . . . . ?
N2 C3' C4' C3A' 167(11) . . . . ?
N2 C3' C4' C4 -178(2) . . . . ?
N2 C3' C4' C5' 8(4) . . . . ?
N2A Cu1 N1A N2A 126(2) 7_676 . . . ?
N2A Cu1 N1A C5' 83(14) 7_676 . . . ?
N2A Cu1 N1A C5' -44(14) . . . . ?
N2A Cu1 O2B Cu1 -87.1(9) . . . 7_676 ?
N2A Cu1 O2B Cu1 68.6(9) 7_676 . . 7_676 ?
N2A Cu1 O2B C7B -60(5) . . . . ?
N2A Cu1 O2B C7B 96(5) 7_676 . . . ?
N2A Cu1 O2C Cu1 -83.4(8) . . . 7_676 ?
N2A Cu1 O2C Cu1 68.9(8) 7_676 . . 7_676 ?
N2A Cu1 O2C C7C 78(2) 7_676 . . . ?
N2A Cu1 O2C C7C -74(2) . . . . ?
N2A Cu1 N2 N1 -161(7) 7_676 . . . ?
N2A Cu1 N2 N1 -142(4) . . . . ?
N2A Cu1 N2 C3' 0(3) . . . . ?
N2A Cu1 N2 C3' -18(9) 7_676 . . . ?
N2A Cu1 N2A Cu1 0.002(2) 7_676 . . 7_676 ?
N2A Cu1 N2A N1A -156.5(19) 7_676 . . . ?
N2A Cu1 N2A C3A' -10(6) 7_676 . . . ?
N2A N1A C5' N1 161(8) . . . . ?
N2A N1A C5' C4' -1(4) . . . . ?
N2A N1A C5' C51 -172(4) . . . . ?
N2A C3A' C4' C3' -19(7) . . . . ?
N2A C3A' C4' C4 173(2) . . . . ?
N2A C3A' C4' C5' 5(4) . . . . ?
N2B N1B C5B' C4B' -11(4) . . . . ?
N2B N1B C5B' C51B 175(3) . . . . ?
N2B Cu2 O2 Cu2 87.0(9) 2_656 . . 5_666 ?
N2B Cu2 O2 Cu2 -65.6(8) 6_565 . . 5_666 ?
N2B Cu2 O2 C7A -63(2) 6_565 . . . ?
N2B Cu2 O2 C7A 90(2) 2_656 . . . ?
N2B Cu2 O2A Cu2 -64.4(9) 6_565 . . 5_666 ?
N2B Cu2 O2A Cu2 90.1(10) 2_656 . . 5_666 ?
N2B Cu2 O2A C7 -59(6) 6_565 . . . ?
N2B Cu2 O2A C7 95(6) 2_656 . . . ?
N2B C3B' C4B' C3C' -167(10) . . . . ?
N2B C3B' C4B' C4B -168(2) . . . . ?
N2B C3B' C4B' C4C' 34(3) . . . . ?
N2B C3B' C4B' C5B' -1(3) . . . . ?
N2C N1C C4C' C4B' 10(4) . . . . ?
N2C N1C C4C' C51C 179(5) . . . . ?
N2C Cu2 O2 Cu2 69.7(9) 2_656 . . 5_666 ?
N2C Cu2 O2 Cu2 -83.1(10) 6_565 . . 5_666 ?
N2C Cu2 O2 C7A -80(2) 6_565 . . . ?
N2C Cu2 O2 C7A 73(2) 2_656 . . . ?
N2C Cu2 O2A Cu2 71.4(9) 2_656 . . 5_666 ?
N2C Cu2 O2A Cu2 -82.8(10) 6_565 . . 5_666 ?
N2C Cu2 O2A C7 -78(6) 6_565 . . . ?
N2C Cu2 O2A C7 77(6) 2_656 . . . ?
N2C C3C' C4B' C3B' 0(6) . . . . ?
N2C C3C' C4B' C4B 180(2) . . . . ?
N2C C3C' C4B' C4C' 23(5) . . . . ?
N2C C3C' C4B' C5B' -17(5) . . . . ?
C2 C1 C6 C5 -2(3) . . . . ?
C2 C1 C7 O1A 22(5) . . . . ?
C2 C1 C7 O2A -156(3) . . . . ?
C2 C1 C7A O1 37(4) . . . . ?
C2 C1 C7A O2 -147(3) . . . . ?
C2 C3 C4 C4' 177.6(19) . . . . ?
C2 C3 C4 C5 2(3) . . . . ?
C2B C1B C6B C5B -3(4) . . . . ?
C2B C1B C7B O1B 140(4) . . . . ?
C2B C1B C7B O2B -40(5) . . . . ?
C2B C1B C7C Cu1 57(10) . . . 7_676 ?
C2B C1B C7C O1C 151(3) . . . . ?
C2B C1B C7C O2C -24(4) . . . . ?
C2B C3B C4B C4B' 174.4(19) . . . . ?
C2B C3B C4B C5B -3(3) . . . . ?
C3 C4 C4' C3' 59(4) . . . . ?
C3 C4 C4' C3A' 65(3) . . . . ?
C3 C4 C4' C5' -128(3) . . . . ?
C3 C4 C5 C6 1(3) . . . . ?
C3' C4' C5' N1 -4(5) . . . . ?
C3' C4' C5' N1A 5(3) . . . . ?
C3' C4' C5' C51 173(5) . . . . ?
C3A' C4' C5' N1 -12(5) . . . . ?
C3A' C4' C5' N1A -3(4) . . . . ?
C3A' C4' C5' C51 166(5) . . . . ?
C3B C4B C4B' C3B' 115(3) . . . . ?
C3B C4B C4B' C3C' 115(3) . . . . ?
C3B C4B C4B' C4C' -92(3) . . . . ?
C3B C4B C4B' C5B' -50(3) . . . . ?
C3B C4B C5B C6B -3(3) . . . . ?
C3B' C4B' C4C' N1C -11(3) . . . . ?
C3B' C4B' C4C' C51C -180(5) . . . . ?
C3B' C4B' C5B' N1B 7(3) . . . . ?
C3B' C4B' C5B' C51B 178(5) . . . . ?
C3C' C4B' C4C' N1C -20(4) . . . . ?
C3C' C4B' C4C' C51C 171(6) . . . . ?
C3C' C4B' C5B' N1B 14(5) . . . . ?
C3C' C4B' C5B' C51B -175(5) . . . . ?
C4 C4' C5' N1 -180(3) . . . . ?
C4 C4' C5' N1A -171(2) . . . . ?
C4 C4' C5' C51 -2(6) . . . . ?
C4 C5 C6 C1 -1(3) . . . . ?
C4' C4 C5 C6 -174.6(16) . . . . ?
C4B C4B' C4C' N1C -173.3(18) . . . . ?
C4B C4B' C4C' C51C 18(7) . . . . ?
C4B C4B' C5B' N1B 177(2) . . . . ?
C4B C4B' C5B' C51B -12(6) . . . . ?
C4B C5B C6B C1B 6(3) . . . . ?
C4B' C4B C5B C6B -179.4(17) . . . . ?
C4C' N1C N2C Cu2 -161(3) . . . 2_656 ?
C4C' N1C N2C Cu2 -169(2) . . . 6_665 ?
C4C' N1C N2C C3C' 3(5) . . . . ?
C4C' C4B' C5B' N1B -71(4) . . . . ?
C4C' C4B' C5B' C51B 100(6) . . . . ?
C5 C4 C4' C3' -125(3) . . . . ?
C5 C4 C4' C3A' -120(3) . . . . ?
C5 C4 C4' C5' 48(3) . . . . ?
C5' N1 N2 Cu1 152(3) . . . . ?
C5' N1 N2 C3' 7(5) . . . . ?
C5' N1A N2A Cu1 160(3) . . . 7_676 ?
C5' N1A N2A Cu1 172(3) . . . . ?
C5' N1A N2A C3A' 3(4) . . . . ?
C5B C4B C4B' C3B' -68(3) . . . . ?
C5B C4B C4B' C3C' -68(4) . . . . ?
C5B C4B C4B' C4C' 85(3) . . . . ?
C5B C4B C4B' C5B' 127(2) . . . . ?
C5B' N1B N2B Cu2 -164(2) . . . 2_656 ?
C5B' N1B N2B Cu2 -163(3) . . . 6_665 ?
C5B' N1B N2B C3B' 10(4) . . . . ?
C5B' C4B' C4C' N1C 96(4) . . . . ?
C5B' C4B' C4C' C51C -73(6) . . . . ?
C6 C1 C2 C3 6(3) . . . . ?
C6 C1 C7 O1A -146(3) . . . . ?
C6 C1 C7 O2A 36(5) . . . . ?
C6 C1 C7A O1 -154(3) . . . . ?
C6 C1 C7A O2 21(4) . . . . ?
C6B C1B C2B C3B -4(4) . . . . ?
C6B C1B C7B O1B -24(5) . . . . ?
C6B C1B C7B O2B 155(3) . . . . ?
C6B C1B C7C Cu1 -127(8) . . . 7_676 ?
C6B C1B C7C O1C -33(5) . . . . ?
C6B C1B C7C O2C 152(3) . . . . ?
C7 C1 C2 C3 -163(3) . . . . ?
C7 C1 C6 C5 165(3) . . . . ?
C7 C1 C7A O1 -26(5) . . . . ?
C7 C1 C7A O2 149(8) . . . . ?
C7A C1 C2 C3 173(3) . . . . ?
C7A C1 C6 C5 -172(2) . . . . ?
C7A C1 C7 O1A 151(9) . . . . ?
C7A C1 C7 O2A -27(4) . . . . ?
C7B C1B C2B C3B -168(3) . . . . ?
C7B C1B C6B C5B 166(3) . . . . ?
C7B C1B C7C Cu1 -93(10) . . . 7_676 ?
C7B C1B C7C O1C 1(4) . . . . ?
C7B C1B C7C O2C -174(7) . . . . ?
C7C Cu1 N1A N2A -84(2) 7_676 . . . ?
C7C Cu1 N1A C5' -128(15) 7_676 . . . ?
C7C Cu1 O2B Cu1 14(4) 7_676 . . 7_676 ?
C7C Cu1 O2B C7B 41(7) 7_676 . . . ?
C7C Cu1 O2C Cu1 137(10) 7_676 . . 7_676 ?
C7C Cu1 O2C C7C 146(9) 7_676 . . . ?
C7C Cu1 N2 N1 112(3) 7_676 . . . ?
C7C Cu1 N2 C3' -106(3) 7_676 . . . ?
C7C Cu1 N2A Cu1 -97.7(12) 7_676 . . 7_676 ?
C7C Cu1 N2A N1A 106(2) 7_676 . . . ?
C7C Cu1 N2A C3A' -108(6) 7_676 . . . ?
C7C C1B C2B C3B 173(3) . . . . ?
C7C C1B C6B C5B -178(3) . . . . ?
C7C C1B C7B O1B -179(7) . . . . ?
C7C C1B C7B O2B 1(4) . . . . ?
C31 C3' C4' C3A' -17(7) . . . . ?
C31 C3' C4' C4 -2(6) . . . . ?
C31 C3' C4' C5' -176(4) . . . . ?
C31A C3A' C4' C3' 177(13) . . . . ?
C31A C3A' C4' C4 9(6) . . . . ?
C31A C3A' C4' C5' -159(5) . . . . ?
C31B C3B' C4B' C3C' 10(7) . . . . ?
C31B C3B' C4B' C4B 9(5) . . . . ?
C31B C3B' C4B' C4C' -149(4) . . . . ?
C31B C3B' C4B' C5B' 175(3) . . . . ?
C31C C3C' C4B' C3B' 148(15) . . . . ?
C31C C3C' C4B' C4B -33(8) . . . . ?
C31C C3C' C4B' C4C' 171(7) . . . . ?
C31C C3C' C4B' C5B' 130(7) . . . . ?

_olex2_computing_structure_refinement_long 'SHELXL-97 (Sheldrick, 1997)'
_olex2_computing_structure_solution_long 'SHELXS-97 (Sheldrick, 1997)'
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_DIFF020_i2a                 
;
PROBLEM: _diffrn_standards_interval_count and
RESPONSE: ...
;
_vrf_DIFF022_i2a                 
;
PROBLEM: _diffrn_standards_decay_% is missing
RESPONSE: ...
;
_vrf_PLAT082_i2a                 
;
PROBLEM: High R1 Value ..................................       0.26 Report
RESPONSE: See vrf_RFACG01_i2a for a report.
;
_vrf_PLAT084_i2a                 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.64 Report
RESPONSE: See vrf_RFACR01_i2a for a report.
;
_vrf_PLAT201_i2a                 
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         21 Report
RESPONSE: The structure model that could be generated from the data on 
desolvated crystals required fixing SOFs and Sigmas for a stable refinement
and so there are isotropic non-H atoms. This refinement strategy is made 
clear in the cif under olex2_refinement_description. The structure is 
extremely disordered and there are multiple positions for atoms around the 
metal centres. We acknowledge this limitation and are making no claims to the
precision of the structure. The topology and overall connectivity of the 
coordination network has been found.  
;
_vrf_PLAT412_i2a                 
;
PROBLEM: Short Intra XH3 .. XHn     H51B   ..  H51B    ..       1.06 Ang.  
RESPONSE: While alternative positions can be found for the hydrogen atoms
on C51 (H51A, H51B, H51C) that negate this short contact this will not 
change anything at the level of resolution for this structure. As noted 
before this structure determination is useful only for revealing the 
topology and overall connectivity of the coordination network.
;
_vrf_RFACG01_i2a                 
;
PROBLEM: The value of the R factor is > 0.20
RESPONSE: This was a challenging sample and in order to get data
synchrotron radiation was required. The data quality from the 
diffraction experiments was not high and contributes to the high
R factor. The model developed is severely aflicted by disorder and
many atoms are not refined anisotropically. With the quality of 
the data being what it is, we are pleased that a reasonable structural 
model could be developed. This has served the purpose of ascertaining
the topology of the coordination network, which is the goal of the 
diffraction experiments.
;
_vrf_RFACR01_i2a                 
;
PROBLEM: The value of the weighted R factor is > 0.45
RESPONSE: As noted for the response to the large R factor there are 
considerable shortcomings on the data quality. A high WR is a reflection 
(no pun intended) of that.
;
