# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Jonathan Dilworth'
_publ_contact_author_email       JON.DILWORTH@CHEM.OX.AC.UK

_publ_section_title              
;
Synthesis, X-ray crystallography and catalytic
studies on nitrite reduction by copper complexes
;
loop_
_publ_author_name
'J Dilworth'
'Jason Holland'
'Michael W. Jones'
'John Woollard-Shore'

# Attachment 'Combined_CIF_File.cif'

data_complex11
_database_code_depnum_ccdc_archive 'CCDC 737901'
#=============================================================
# Diffractometer details
#=============================================================
_diffrn_measurement_device_type  
;
Nonius KappaCCD
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction        
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_cell_refinement       
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
#=============================================================
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'

_chemical_name_systematic        # IUPAC name, in full
;
?
;
_chemical_melting_point          'not measured'
_exptl_crystal_thermal_history   
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled at 120K per hour to 150K for single-crystal X-ray diffraction
analysis.
;
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_special_details          
;
Coordinates and anisotropic thermal parameters of all non-hydrogen atoms
were refined. Examination of the resulting model showed one of the nitrite
ligands to be disordered and this was modelled as being due to approximately
half of this fragment being coordinated through N and half through O. All
six disordered N and O sites were clearly resolved and their coordinates,
anisotropic thermal parameters and site occupancies were refined. No
geometric restraints were applied but similarity restraints were applied
to the thermal parameters of directly-bonded pairs of atoms. The N- and
O-bonded ligands are approximately coplanar (interplanar angle 11.9 degrees).
The NH hydrogen atoms were located in a difference Fourier map and their
coordinates and isotropic thermal parameters subsequently refined. Other
hydrogen atoms were positioned geometrically after each cycle of refinement.
The asymmetric unit contains two molecules each of the anion and cation.

There was no evidence of any disorder in the other NO2 group.

In addition to the disorder of the NO2 group described above, the fluorine
atoms of the anions exhibit large thermal parameters, suggesting that there
may also be unresolved disorder of these molecules. Attempts to model this
did not lead to an improvement in the agreement with the X-ray data and were
abandoned.

There are a number of relatively short contacts between the coordinated
amine N atoms and O or F atoms, but in view of the disorder it is difficult
to identify clearly any hydrogen bonds.

Determination of the unit-cell parameters over the range 290-110K show that
they vary smoothly, with no discontinuities indicative of an order-disorder
phase change.
;
#=============================================================

_cell_length_a                   17.2657(2)
_cell_angle_alpha                90
_cell_length_b                   7.5928(2)
_cell_angle_beta                 91.5155(4)
_cell_length_c                   21.4050(2)
_cell_angle_gamma                90
_cell_volume                     2805.11(8)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'Cu ' 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 International_Tables_Vol_IV_Table_2.2B
'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 International_Tables_Vol_IV_Table_2.2B

_cell_formula_units_Z            8
_chemical_formula_sum            ' C6 H18 Cu F6 N5 O2 P '
_chemical_formula_moiety         ' C6 H18 Cu N5 O2, P F6 '
_chemical_compound_source        
;
synthesis as described
;
_chemical_formula_weight         400.75

_cell_measurement_reflns_used    31156
_cell_measurement_theta_min      5
_cell_measurement_theta_max      28
_cell_measurement_temperature    150

_exptl_crystal_description       ' block '
_exptl_crystal_colour            ' dark green '
_exptl_crystal_size_min          0.12
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_max          0.24

_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_meas      'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1624
_exptl_absorpt_coefficient_mu    1.752

_diffrn_measurement_method       \w

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_T_max  0.81

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0.00

_diffrn_ambient_temperature      150
_diffrn_reflns_number            31156
_reflns_number_total             6372
#6845 unique reflections including absences
_diffrn_reflns_av_R_equivalents  0.032

_diffrn_reflns_theta_min         5.135
_diffrn_reflns_theta_max         27.477
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        27.477
_diffrn_measured_fraction_theta_full 0.997

_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_reflns_limit_h_min              -22
_reflns_limit_h_max              22
_reflns_limit_k_min              0
_reflns_limit_k_max              9
_reflns_limit_l_min              0
_reflns_limit_l_max              27

_refine_diff_density_min         -0.41
_refine_diff_density_max         0.50

_refine_ls_number_reflns         5270
_refine_ls_number_restraints     4
_refine_ls_number_parameters     455

#_refine_ls_R_factor_ref 0.0291
_refine_ls_wR_factor_ref         0.0371
_refine_ls_goodness_of_fit_ref   1.0553

#_reflns_number_all 6372
_refine_ls_R_factor_all          0.0372
_refine_ls_wR_factor_all         0.0424

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                5270
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_gt          0.0371

_refine_ls_shift/su_max          0.036435
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.904 0.457 0.613
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_disorder_assembly
_atom_site_refinement_disorder_group
Cu1 Cu 0.396152(12) 0.17994(3) 0.177327(10) 0.0183 1.0000 Uani . . . . .
N1 N 0.37293(9) -0.0433(2) 0.12611(7) 0.0220 1.0000 Uani . . . . .
C1 C 0.31748(12) 0.0065(3) 0.07466(9) 0.0256 1.0000 Uani . . . . .
C2 C 0.25815(12) 0.1349(3) 0.09928(10) 0.0299 1.0000 Uani . . . . .
N2 N 0.29968(11) 0.2858(2) 0.12836(9) 0.0273 1.0000 Uani . . . . .
C3 C 0.33759(12) -0.1756(3) 0.16851(10) 0.0279 1.0000 Uani . . . . .
C4 C 0.37051(14) -0.1522(3) 0.23412(10) 0.0302 1.0000 Uani . . . . .
N3 N 0.36194(14) 0.0333(2) 0.25223(9) 0.0307 1.0000 Uani . . . . .
C5 C 0.44802(12) -0.1070(3) 0.10160(10) 0.0268 1.0000 Uani . . . . .
C6 C 0.49770(12) 0.0483(3) 0.08337(9) 0.0283 1.0000 Uani . . . . .
N4 N 0.50261(10) 0.1700(2) 0.13735(8) 0.0244 1.0000 Uani . . . . .
N5 N 0.42176(9) 0.3944(2) 0.22772(8) 0.0232 1.0000 Uani . . . . .
O1 O 0.46869(9) 0.5037(2) 0.20836(9) 0.0373 1.0000 Uani . . . . .
O2 O 0.39246(9) 0.4207(2) 0.27949(7) 0.0344 1.0000 Uani . . . . .
Cu2 Cu 0.136144(13) 0.36700(3) 0.338533(10) 0.0203 1.0000 Uani . . . . .
N6 N 0.11928(9) 0.5637(2) 0.40293(7) 0.0204 1.0000 Uani . . . . .
C7 C 0.03927(11) 0.6322(3) 0.39349(10) 0.0258 1.0000 Uani . . . . .
C8 C 0.01789(12) 0.6391(3) 0.32408(10) 0.0282 1.0000 Uani . . . . .
N7 N 0.03061(10) 0.4632(2) 0.29698(8) 0.0242 1.0000 Uani . . . . .
C9 C 0.17815(12) 0.7042(3) 0.39327(10) 0.0260 1.0000 Uani . . . . .
C10 C 0.25097(12) 0.6252(3) 0.36759(10) 0.0299 1.0000 Uani . . . . .
N8 N 0.22764(12) 0.5178(3) 0.31239(9) 0.0336 1.0000 Uani . . . . .
C11 C 0.13128(12) 0.4808(3) 0.46509(9) 0.0260 1.0000 Uani . . . . .
C12 C 0.09286(12) 0.3013(3) 0.46669(9) 0.0284 1.0000 Uani . . . . .
N9 N 0.11867(11) 0.1999(2) 0.41226(9) 0.0265 1.0000 Uani . . . . .
N10 N 0.1565(6) 0.1656(13) 0.2822(5) 0.0242 0.587(5) Uani . U P 1 1
O3 O 0.20530(19) 0.1805(4) 0.24112(15) 0.0369 0.587(5) Uani . U P 1 1
O4 O 0.1209(3) 0.0258(10) 0.2872(4) 0.0350 0.587(5) Uani . U P 1 1
O13 O 0.1718(8) 0.1942(16) 0.2754(6) 0.0354 0.413(5) Uani . U P 1 2
N20 N 0.1464(5) 0.0341(17) 0.2868(7) 0.0291 0.413(5) Uani . U P 1 2
O14 O 0.1744(3) -0.0751(5) 0.25264(19) 0.0379 0.413(5) Uani . U P 1 2
P1 P 0.34749(3) 0.07112(7) 0.44634(3) 0.0288 1.0000 Uani . . . . .
F1 F 0.34607(14) 0.2763(2) 0.43369(10) 0.0714 1.0000 Uani . . . . .
F2 F 0.34771(14) -0.1346(2) 0.46031(10) 0.0710 1.0000 Uani . . . . .
F3 F 0.27180(10) 0.0931(3) 0.48656(8) 0.0661 1.0000 Uani . . . . .
F4 F 0.42129(11) 0.0488(4) 0.40513(10) 0.0751 1.0000 Uani . . . . .
F5 F 0.39986(10) 0.1047(3) 0.50733(9) 0.0588 1.0000 Uani . . . . .
F6 F 0.29229(9) 0.0398(2) 0.38580(6) 0.0420 1.0000 Uani . . . . .
P2 P 0.11582(3) 0.60437(7) 0.11604(3) 0.0257 1.0000 Uani . . . . .
F7 F 0.10453(11) 0.81377(19) 0.11736(8) 0.0484 1.0000 Uani . . . . .
F8 F 0.12474(9) 0.39524(18) 0.11477(8) 0.0442 1.0000 Uani . . . . .
F9 F 0.19485(10) 0.6272(2) 0.08137(9) 0.0563 1.0000 Uani . . . . .
F10 F 0.03650(9) 0.5838(2) 0.15292(8) 0.0517 1.0000 Uani . . . . .
F11 F 0.06908(11) 0.5972(2) 0.05123(8) 0.0571 1.0000 Uani . . . . .
F12 F 0.16212(11) 0.6104(3) 0.18120(8) 0.0584 1.0000 Uani . . . . .
H1 H 0.3135(19) 0.366(4) 0.1006(16) 0.045(8) 1.0000 Uiso . . . . .
H2 H 0.2710(19) 0.327(4) 0.1510(15) 0.040(8) 1.0000 Uiso . . . . .
H3 H 0.3202(18) 0.061(4) 0.2601(13) 0.033(7) 1.0000 Uiso . . . . .
H4 H 0.3897(18) 0.058(4) 0.2849(15) 0.045(8) 1.0000 Uiso . . . . .
H5 H 0.5343(17) 0.129(4) 0.1632(14) 0.037(7) 1.0000 Uiso . . . . .
H6 H 0.5175(16) 0.268(4) 0.1277(13) 0.032(7) 1.0000 Uiso . . . . .
H7 H -0.0076(18) 0.398(4) 0.3029(13) 0.035(7) 1.0000 Uiso . . . . .
H8 H 0.0332(17) 0.471(4) 0.2564(15) 0.042(8) 1.0000 Uiso . . . . .
H9 H 0.215(2) 0.582(5) 0.2778(18) 0.067(11) 1.0000 Uiso . . . . .
H10 H 0.264(2) 0.451(5) 0.3008(16) 0.054(9) 1.0000 Uiso . . . . .
H11 H 0.1611(18) 0.152(4) 0.4196(13) 0.036(7) 1.0000 Uiso . . . . .
H12 H 0.0868(19) 0.125(4) 0.3996(14) 0.043(8) 1.0000 Uiso . . . . .
H13 H 0.3463 0.0634 0.0401 0.0305 1.0000 Uiso . . . . .
H14 H 0.2905 -0.1013 0.0584 0.0305 1.0000 Uiso . . . . .
H21 H 0.2260 0.0750 0.1311 0.0357 1.0000 Uiso . . . . .
H22 H 0.2239 0.1775 0.0640 0.0357 1.0000 Uiso . . . . .
H31 H 0.3495 -0.2970 0.1534 0.0333 1.0000 Uiso . . . . .
H32 H 0.2802 -0.1583 0.1685 0.0333 1.0000 Uiso . . . . .
H41 H 0.4266 -0.1852 0.2354 0.0362 1.0000 Uiso . . . . .
H42 H 0.3418 -0.2289 0.2636 0.0362 1.0000 Uiso . . . . .
H51 H 0.4760 -0.1773 0.1347 0.0322 1.0000 Uiso . . . . .
H52 H 0.4377 -0.1829 0.0641 0.0322 1.0000 Uiso . . . . .
H61 H 0.5507 0.0067 0.0728 0.0340 1.0000 Uiso . . . . .
H62 H 0.4736 0.1098 0.0464 0.0340 1.0000 Uiso . . . . .
H71 H 0.0361 0.7534 0.4115 0.0310 1.0000 Uiso . . . . .
H72 H 0.0022 0.5529 0.4151 0.0310 1.0000 Uiso . . . . .
H81 H -0.0378 0.6729 0.3183 0.0337 1.0000 Uiso . . . . .
H82 H 0.0512 0.7275 0.3029 0.0337 1.0000 Uiso . . . . .
H91 H 0.1908 0.7628 0.4341 0.0312 1.0000 Uiso . . . . .
H92 H 0.1567 0.7932 0.3630 0.0312 1.0000 Uiso . . . . .
H101 H 0.2771 0.5492 0.3999 0.0360 1.0000 Uiso . . . . .
H102 H 0.2871 0.7209 0.3549 0.0360 1.0000 Uiso . . . . .
H111 H 0.1083 0.5579 0.4977 0.0311 1.0000 Uiso . . . . .
H112 H 0.1881 0.4670 0.4740 0.0311 1.0000 Uiso . . . . .
H121 H 0.1084 0.2386 0.5062 0.0340 1.0000 Uiso . . . . .
H122 H 0.0353 0.3151 0.4645 0.0340 1.0000 Uiso . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.01930(11) 0.01813(12) 0.01734(11) -0.00076(7) -0.00015(8) 0.00095(8)
N1 0.0257(8) 0.0213(7) 0.0188(7) -0.0008(6) -0.0028(6) 0.0014(6)
C1 0.0299(10) 0.0246(9) 0.0217(9) -0.0032(7) -0.0100(7) 0.0049(8)
C2 0.0289(10) 0.0320(10) 0.0283(10) -0.0041(8) -0.0109(8) 0.0065(8)
N2 0.0302(9) 0.0238(8) 0.0274(8) -0.0040(7) -0.0071(7) 0.0072(7)
C3 0.0313(10) 0.0224(9) 0.0295(10) 0.0032(7) -0.0049(8) -0.0036(8)
C4 0.0413(12) 0.0217(9) 0.0275(10) 0.0067(8) -0.0025(8) -0.0027(8)
N3 0.0450(12) 0.0262(9) 0.0212(8) 0.0025(7) 0.0050(8) -0.0007(8)
C5 0.0296(10) 0.0243(9) 0.0266(9) -0.0043(7) 0.0006(7) 0.0079(8)
C6 0.0301(10) 0.0323(10) 0.0227(9) -0.0038(8) 0.0067(7) 0.0070(8)
N4 0.0257(8) 0.0245(8) 0.0233(8) 0.0016(7) 0.0031(6) 0.0007(7)
N5 0.0197(7) 0.0218(8) 0.0279(8) -0.0022(6) -0.0011(6) 0.0023(6)
O1 0.0343(8) 0.0243(7) 0.0539(10) -0.0034(7) 0.0122(7) -0.0047(6)
O2 0.0373(8) 0.0358(8) 0.0303(8) -0.0122(7) 0.0053(6) -0.0031(7)
Cu2 0.02436(12) 0.01739(12) 0.01890(12) -0.00298(8) -0.00153(8) 0.00112(8)
N6 0.0227(8) 0.0182(7) 0.0202(7) -0.0028(6) -0.0001(6) -0.0017(6)
C7 0.0234(9) 0.0266(9) 0.0274(10) -0.0055(7) 0.0005(7) 0.0052(7)
C8 0.0286(10) 0.0251(9) 0.0306(10) -0.0005(8) -0.0046(8) 0.0061(8)
N7 0.0269(8) 0.0249(8) 0.0206(8) -0.0012(6) -0.0054(6) 0.0001(7)
C9 0.0290(10) 0.0196(9) 0.0294(9) -0.0027(7) 0.0005(7) -0.0045(7)
C10 0.0290(10) 0.0299(10) 0.0310(10) -0.0062(8) 0.0036(8) -0.0083(8)
N8 0.0298(9) 0.0399(11) 0.0317(10) -0.0114(8) 0.0092(7) -0.0091(8)
C11 0.0319(10) 0.0301(10) 0.0158(8) -0.0015(7) -0.0030(7) -0.0057(8)
C12 0.0309(10) 0.0319(10) 0.0223(9) 0.0062(8) -0.0009(7) -0.0082(8)
N9 0.0267(9) 0.0198(8) 0.0328(9) 0.0023(7) -0.0037(7) -0.0010(7)
N10 0.030(3) 0.025(3) 0.018(2) -0.001(2) -0.0011(16) 0.0039(19)
O3 0.0420(17) 0.0384(16) 0.0311(16) -0.0082(12) 0.0150(14) 0.0002(12)
O4 0.036(3) 0.0295(17) 0.0399(19) -0.0079(13) 0.001(3) -0.004(2)
O13 0.049(6) 0.024(4) 0.033(4) -0.002(3) 0.004(3) 0.001(3)
N20 0.028(5) 0.024(3) 0.035(3) -0.004(2) -0.001(4) 0.005(3)
O14 0.048(2) 0.028(2) 0.038(2) -0.0110(16) 0.0068(17) -0.0009(16)
P1 0.0277(3) 0.0269(3) 0.0320(3) -0.0077(2) 0.0043(2) -0.0043(2)
F1 0.1049(17) 0.0275(8) 0.0816(13) -0.0024(8) -0.0017(12) -0.0108(9)
F2 0.1069(17) 0.0326(8) 0.0714(13) 0.0059(8) -0.0383(12) -0.0070(9)
F3 0.0373(8) 0.1231(18) 0.0384(8) -0.0054(10) 0.0108(6) -0.0019(10)
F4 0.0418(9) 0.1133(18) 0.0713(12) -0.0294(12) 0.0223(9) 0.0004(10)
F5 0.0450(9) 0.0673(11) 0.0629(11) -0.0326(9) -0.0206(8) 0.0066(8)
F6 0.0512(8) 0.0443(8) 0.0303(7) -0.0022(6) -0.0051(6) -0.0020(6)
P2 0.0229(2) 0.0262(3) 0.0281(2) 0.00178(19) 0.00127(18) 0.00424(19)
F7 0.0696(11) 0.0276(7) 0.0485(9) 0.0014(6) 0.0097(8) 0.0073(7)
F8 0.0392(8) 0.0275(7) 0.0658(10) 0.0005(6) 0.0021(7) 0.0072(6)
F9 0.0396(8) 0.0575(10) 0.0733(12) 0.0107(8) 0.0257(8) 0.0023(7)
F10 0.0344(7) 0.0543(9) 0.0675(10) 0.0101(8) 0.0214(7) 0.0099(7)
F11 0.0668(11) 0.0608(11) 0.0426(8) -0.0083(8) -0.0217(8) 0.0171(9)
F12 0.0644(11) 0.0659(11) 0.0436(9) 0.0049(8) -0.0241(8) -0.0038(9)
_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 . N1 . 2.0523(16) yes
Cu1 . N2 . 2.1040(17) yes
Cu1 . N3 . 2.0515(18) yes
Cu1 . N4 . 2.0493(17) yes
Cu1 . N5 . 1.9961(17) yes
N1 . C1 . 1.489(2) yes
N1 . C3 . 1.495(3) yes
N1 . C5 . 1.492(2) yes
C1 . C2 . 1.518(3) yes
C1 . H13 . 1.000 no
C1 . H14 . 1.000 no
C2 . N2 . 1.481(3) yes
C2 . H21 . 1.000 no
C2 . H22 . 1.000 no
N2 . H1 . 0.89(3) no
N2 . H2 . 0.77(3) no
C3 . C4 . 1.511(3) yes
C3 . H31 . 1.000 no
C3 . H32 . 1.000 no
C4 . N3 . 1.470(3) yes
C4 . H41 . 1.000 no
C4 . H42 . 1.000 no
N3 . H3 . 0.77(3) no
N3 . H4 . 0.86(3) no
C5 . C6 . 1.516(3) yes
C5 . H51 . 1.000 no
C5 . H52 . 1.000 no
C6 . N4 . 1.480(3) yes
C6 . H61 . 1.000 no
C6 . H62 . 1.000 no
N4 . H5 . 0.83(3) no
N4 . H6 . 0.82(3) no
N5 . O1 . 1.239(2) yes
N5 . O2 . 1.246(2) yes
Cu2 . N6 . 2.0584(15) yes
Cu2 . N7 . 2.1352(17) yes
Cu2 . N8 . 2.0410(19) yes
Cu2 . N9 . 2.0533(18) yes
Cu2 . N10 . 1.984(10) yes
Cu2 . O13 . 1.992(13) yes
N6 . C7 . 1.485(2) yes
N6 . C9 . 1.492(2) yes
N6 . C11 . 1.481(2) yes
C7 . C8 . 1.522(3) yes
C7 . H71 . 1.000 no
C7 . H72 . 1.000 no
C8 . N7 . 1.475(3) yes
C8 . H81 . 1.000 no
C8 . H82 . 1.000 no
N7 . H7 . 0.84(3) no
N7 . H8 . 0.87(3) no
C9 . C10 . 1.510(3) yes
C9 . H91 . 1.000 no
C9 . H92 . 1.000 no
C10 . N8 . 1.483(3) yes
C10 . H101 . 1.000 no
C10 . H102 . 1.000 no
N8 . H9 . 0.91(4) no
N8 . H10 . 0.84(4) no
C11 . C12 . 1.517(3) yes
C11 . H111 . 1.000 no
C11 . H112 . 1.000 no
C12 . N9 . 1.475(3) yes
C12 . H121 . 1.000 no
C12 . H122 . 1.000 no
N9 . H11 . 0.83(3) no
N9 . H12 . 0.83(3) no
N10 . O3 . 1.240(9) yes
N10 . O4 . 1.232(7) yes
O13 . N20 . 1.317(10) yes
N20 . O14 . 1.214(13) yes
P1 . F1 . 1.5817(18) yes
P1 . F2 . 1.5899(18) yes
P1 . F3 . 1.5927(17) yes
P1 . F4 . 1.5780(18) yes
P1 . F5 . 1.5889(16) yes
P1 . F6 . 1.6060(15) yes
P2 . F7 . 1.6022(15) yes
P2 . F8 . 1.5956(15) yes
P2 . F9 . 1.5799(16) yes
P2 . F10 . 1.6064(15) yes
P2 . F11 . 1.5871(16) yes
P2 . F12 . 1.5898(16) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Cu1 . N2 . 84.75(7) yes
N1 . Cu1 . N3 . 85.02(7) yes
N2 . Cu1 . N3 . 110.86(9) yes
N1 . Cu1 . N4 . 84.90(7) yes
N2 . Cu1 . N4 . 120.87(8) yes
N3 . Cu1 . N4 . 125.89(8) yes
N1 . Cu1 . N5 . 178.36(6) yes
N2 . Cu1 . N5 . 96.81(7) yes
N3 . Cu1 . N5 . 94.85(7) yes
N4 . Cu1 . N5 . 93.87(7) yes
Cu1 . N1 . C1 . 107.34(11) yes
Cu1 . N1 . C3 . 107.92(12) yes
C1 . N1 . C3 . 110.79(15) yes
Cu1 . N1 . C5 . 107.24(12) yes
C1 . N1 . C5 . 111.72(15) yes
C3 . N1 . C5 . 111.59(15) yes
N1 . C1 . C2 . 109.44(15) yes
N1 . C1 . H13 . 109.479 no
C2 . C1 . H13 . 109.479 no
N1 . C1 . H14 . 109.479 no
C2 . C1 . H14 . 109.479 no
H13 . C1 . H14 . 109.467 no
C1 . C2 . N2 . 108.61(17) yes
C1 . C2 . H21 . 109.688 no
N2 . C2 . H21 . 109.688 no
C1 . C2 . H22 . 109.687 no
N2 . C2 . H22 . 109.688 no
H21 . C2 . H22 . 109.467 no
Cu1 . N2 . C2 . 106.37(12) yes
Cu1 . N2 . H1 . 112(2) no
C2 . N2 . H1 . 113(2) no
Cu1 . N2 . H2 . 111(2) no
C2 . N2 . H2 . 106(2) no
H1 . N2 . H2 . 109(3) no
N1 . C3 . C4 . 109.61(16) yes
N1 . C3 . H31 . 109.438 no
C4 . C3 . H31 . 109.438 no
N1 . C3 . H32 . 109.438 no
C4 . C3 . H32 . 109.438 no
H31 . C3 . H32 . 109.467 no
C3 . C4 . N3 . 108.64(17) yes
C3 . C4 . H41 . 109.679 no
N3 . C4 . H41 . 109.679 no
C3 . C4 . H42 . 109.679 no
N3 . C4 . H42 . 109.679 no
H41 . C4 . H42 . 109.467 no
Cu1 . N3 . C4 . 106.31(13) yes
Cu1 . N3 . H3 . 108(2) no
C4 . N3 . H3 . 115(2) no
Cu1 . N3 . H4 . 111(2) no
C4 . N3 . H4 . 112(2) no
H3 . N3 . H4 . 105(3) no
N1 . C5 . C6 . 109.93(16) yes
N1 . C5 . H51 . 109.356 no
C6 . C5 . H51 . 109.356 no
N1 . C5 . H52 . 109.357 no
C6 . C5 . H52 . 109.356 no
H51 . C5 . H52 . 109.467 no
C5 . C6 . N4 . 107.81(16) yes
C5 . C6 . H61 . 109.886 no
N4 . C6 . H61 . 109.886 no
C5 . C6 . H62 . 109.886 no
N4 . C6 . H62 . 109.886 no
H61 . C6 . H62 . 109.467 no
Cu1 . N4 . C6 . 108.40(13) yes
Cu1 . N4 . H5 . 108.5(20) no
C6 . N4 . H5 . 108(2) no
Cu1 . N4 . H6 . 111.4(19) no
C6 . N4 . H6 . 112.6(19) no
H5 . N4 . H6 . 108(3) no
Cu1 . N5 . O1 . 120.22(14) yes
Cu1 . N5 . O2 . 121.47(13) yes
O1 . N5 . O2 . 118.30(17) yes
N6 . Cu2 . N7 . 84.06(6) yes
N6 . Cu2 . N8 . 84.31(7) yes
N7 . Cu2 . N8 . 110.61(9) yes
N6 . Cu2 . N9 . 84.69(7) yes
N7 . Cu2 . N9 . 112.98(7) yes
N8 . Cu2 . N9 . 133.45(8) yes
N6 . Cu2 . N10 . 175.2(3) yes
N7 . Cu2 . N10 . 100.0(3) yes
N8 . Cu2 . N10 . 96.6(2) yes
N9 . Cu2 . N10 . 91.3(3) yes
N6 . Cu2 . O13 . 169.6(3) yes
N7 . Cu2 . O13 . 102.6(5) yes
N8 . Cu2 . O13 . 85.9(2) yes
N9 . Cu2 . O13 . 99.7(3) yes
Cu2 . N6 . C7 . 108.09(11) yes
Cu2 . N6 . C9 . 108.48(11) yes
C7 . N6 . C9 . 111.45(15) yes
Cu2 . N6 . C11 . 105.93(12) yes
C7 . N6 . C11 . 112.24(15) yes
C9 . N6 . C11 . 110.40(15) yes
N6 . C7 . C8 . 110.22(16) yes
N6 . C7 . H71 . 109.286 no
C8 . C7 . H71 . 109.286 no
N6 . C7 . H72 . 109.286 no
C8 . C7 . H72 . 109.286 no
H71 . C7 . H72 . 109.467 no
C7 . C8 . N7 . 108.55(16) yes
C7 . C8 . H81 . 109.702 no
N7 . C8 . H81 . 109.702 no
C7 . C8 . H82 . 109.702 no
N7 . C8 . H82 . 109.703 no
H81 . C8 . H82 . 109.467 no
Cu2 . N7 . C8 . 106.28(12) yes
Cu2 . N7 . H7 . 113.7(19) no
C8 . N7 . H7 . 110.4(19) no
Cu2 . N7 . H8 . 111.9(19) no
C8 . N7 . H8 . 110(2) no
H7 . N7 . H8 . 105(3) no
N6 . C9 . C10 . 110.11(16) yes
N6 . C9 . H91 . 109.313 no
C10 . C9 . H91 . 109.313 no
N6 . C9 . H92 . 109.313 no
C10 . C9 . H92 . 109.313 no
H91 . C9 . H92 . 109.467 no
C9 . C10 . N8 . 107.29(17) yes
C9 . C10 . H101 . 110.014 no
N8 . C10 . H101 . 110.014 no
C9 . C10 . H102 . 110.014 no
N8 . C10 . H102 . 110.014 no
H101 . C10 . H102 . 109.467 no
Cu2 . N8 . C10 . 106.63(13) yes
Cu2 . N8 . H9 . 111(2) no
C10 . N8 . H9 . 114(2) no
Cu2 . N8 . H10 . 109(2) no
C10 . N8 . H10 . 112(2) no
H9 . N8 . H10 . 104(3) no
N6 . C11 . C12 . 110.55(15) yes
N6 . C11 . H111 . 109.201 no
C12 . C11 . H111 . 109.201 no
N6 . C11 . H112 . 109.201 no
C12 . C11 . H112 . 109.201 no
H111 . C11 . H112 . 109.467 no
C11 . C12 . N9 . 108.05(16) yes
C11 . C12 . H121 . 109.827 no
N9 . C12 . H121 . 109.827 no
C11 . C12 . H122 . 109.827 no
N9 . C12 . H122 . 109.827 no
H121 . C12 . H122 . 109.467 no
Cu2 . N9 . C12 . 109.77(12) yes
Cu2 . N9 . H11 . 106(2) no
C12 . N9 . H11 . 111(2) no
Cu2 . N9 . H12 . 106(2) no
C12 . N9 . H12 . 114(2) no
H11 . N9 . H12 . 110(3) no
Cu2 . N10 . O3 . 119.7(6) yes
Cu2 . N10 . O4 . 121.0(7) yes
O3 . N10 . O4 . 119.3(9) yes
Cu2 . O13 . N20 . 111.9(9) yes
O13 . N20 . O14 . 112.3(12) yes
F1 . P1 . F2 . 178.76(13) yes
F1 . P1 . F3 . 88.85(13) yes
F2 . P1 . F3 . 89.97(13) yes
F1 . P1 . F4 . 91.10(13) yes
F2 . P1 . F4 . 90.08(14) yes
F3 . P1 . F4 . 178.71(11) yes
F1 . P1 . F5 . 89.34(11) yes
F2 . P1 . F5 . 90.27(10) yes
F3 . P1 . F5 . 89.79(10) yes
F4 . P1 . F5 . 91.50(11) yes
F1 . P1 . F6 . 90.08(10) yes
F2 . P1 . F6 . 90.28(9) yes
F3 . P1 . F6 . 88.50(9) yes
F4 . P1 . F6 . 90.21(10) yes
F5 . P1 . F6 . 178.21(9) yes
F7 . P2 . F8 . 178.54(9) yes
F7 . P2 . F9 . 90.37(10) yes
F8 . P2 . F9 . 90.94(9) yes
F7 . P2 . F10 . 88.97(9) yes
F8 . P2 . F10 . 89.74(9) yes
F9 . P2 . F10 . 178.44(11) yes
F7 . P2 . F11 . 89.44(10) yes
F8 . P2 . F11 . 89.89(9) yes
F9 . P2 . F11 . 91.08(11) yes
F10 . P2 . F11 . 90.33(10) yes
F7 . P2 . F12 . 90.84(10) yes
F8 . P2 . F12 . 89.83(9) yes
F9 . P2 . F12 . 89.33(11) yes
F10 . P2 . F12 . 89.26(10) yes
F11 . P2 . F12 . 179.50(11) yes

#===END

#############################################################
# ***dilworth group***
#
# this structure was solved by Michael Jones on 22/12/2008
#############################################################
data_complex12
_database_code_depnum_ccdc_archive 'CCDC 737902'
_audit_creation_date             08-12-22
_audit_creation_method           CRYSTALS_ver_12.85

_oxford_structure_analysis_title 001mwj08
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_refine_special_details          
;
The following features were observed during the refinement, which should
be noted
when considering this structure.
There appeared to be a minor component of disorder in the ligand (<20%).
However, when added, the resultant model was unstable despite copious
restraints.
The presence of this disorder is thought to account for the unusual atomic
displacement parameters and the presence of the short contacts. In addition,
the structure appears to exhibit pseudo-symmetry. The structure
solved in Pnma (with a cell transformation of 001,100,010) but the
model for this was decidedly inferior to P212121, so the P212121 model
was retained instead.
The structure was also found to be twinned by inversion. Refinement of the
scale factor gave the minor component as 44(4)%.
Multiple restraints were necessary to maintain a chemically sensible
model. Although there may be considerable deficiencies in the model,
this should not affect the connectivity and the gross structure is believed to
be correct.
;
_cell_length_a                   10.5877(2)
_cell_length_b                   12.3918(2)
_cell_length_c                   16.0937(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2111.50(7)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21 '
_symmetry_space_group_name_Hall  'p 2ac 2ab '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,-y+1/2,-z
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_formula_units_Z            4

# Given Formula = C12 H30 Cu1 F3 N5 O5 S1
# Dc = 1.50 Fooo = 1020.00 Mu = 11.90 M = 477.01
# Found Formula = C13 H30 Cu1 F3 N5 O5 S1
# Dc = 1.54 FOOO = 1020.00 Mu = 11.93 M = 489.02

_chemical_formula_sum            'C13 H30 Cu1 F3 N5 O5 S1'
_chemical_formula_moiety         'C13 H30 Cu1 F3 N5 O5 S1'
_chemical_compound_source        .
_chemical_formula_weight         489.02

_cell_measurement_reflns_used    2627
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_min          0.05
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_max          0.15

_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1020
_exptl_absorpt_coefficient_mu    1.193

# Sheldrick geometric approximatio 0.93 0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_T_max  0.94
# For a Kappa CCD, set Tmin to 1.0 and
# Tmax to the ratio of max:min frame scales in scale_all.log
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       \w

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            17955
_reflns_number_total             4780
_diffrn_reflns_av_R_equivalents  0.045
# Number of reflections with Friedels Law is 2706
# Number of reflections without Friedels Law is 4780
# Theoretical number of reflections is about 2419

_diffrn_reflns_theta_min         5.222
_diffrn_reflns_theta_max         27.484
_diffrn_measured_fraction_theta_max 0.990

_diffrn_reflns_theta_full        27.484
_diffrn_measured_fraction_theta_full 0.990

_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              20

_oxford_diffrn_Wilson_B_factor   2.68
_oxford_diffrn_Wilson_scale      9.06

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.50
_refine_diff_density_max         0.62

# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold

# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_refine_ls_number_reflns         3530
_refine_ls_number_restraints     317
_refine_ls_number_parameters     264
_oxford_refine_ls_R_factor_ref   0.0506
_refine_ls_wR_factor_ref         0.0524
_refine_ls_goodness_of_fit_ref   1.0076
_refine_ls_shift/su_max          0.007501

# The values computed from all data
_oxford_reflns_number_all        4780
_refine_ls_R_factor_all          0.0823
_refine_ls_wR_factor_all         0.0771

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                3530
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_gt          0.0524

# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration unk

_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.669 0.211 0.300
;
# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands.

Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.

Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.

Watkin D.J. (1994).
Acta Cryst, A50, 411-437.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Cu1 Cu 0.24989(15) 0.59828(3) 0.70472(2) 0.0344 1.0000 Uani . U . . . . .
S2 S 0.2499(3) 1.00501(6) 0.94332(4) 0.0292 1.0000 Uani . U . . . . .
O1 O 0.2462(10) 0.9510(2) 0.86413(15) 0.0399 1.0000 Uani . U . . . . .
C4 C 0.2459(15) 0.8948(3) 1.0168(2) 0.0512 1.0000 Uani . U . . . . .
O6 O 0.3638(7) 1.0610(6) 0.9627(4) 0.0490 1.0000 Uani . U . . . . .
N7 N 0.2481(11) 0.7272(2) 0.62776(17) 0.0354 1.0000 Uani . U . . . . .
F8 F 0.3551(10) 0.8318(6) 1.0063(5) 0.0904 1.0000 Uani . U . . . . .
O9 O 0.1354(7) 1.0629(5) 0.9643(4) 0.0414 1.0000 Uani . U . . . . .
C11 C 0.1503(7) 0.4535(6) 0.5717(4) 0.0551 1.0000 Uani . U . . . . .
N13 N 0.2687(7) 0.5027(3) 0.5938(2) 0.0445 1.0000 Uani . U . . . . .
N14 N 0.4251(7) 0.6609(7) 0.7478(5) 0.0453 1.0000 Uani . U . . . . .
C15 C 0.3689(7) 0.4164(5) 0.5984(4) 0.0480 1.0000 Uani . U . . . . .
F16 F 0.1521(9) 0.8310(6) 1.0063(5) 0.0880 1.0000 Uani . U . . . . .
C17 C 0.3796(10) 0.7834(8) 0.6423(7) 0.0632 1.0000 Uani . U . . . . .
C18 C 0.2479(12) 0.6875(3) 0.5400(2) 0.0367 1.0000 Uani . U . . . . .
C19 C 0.4264(5) 0.7799(4) 0.7277(3) 0.0459 1.0000 Uani . U . . . . .
N21 N 0.0789(8) 0.6653(6) 0.7551(5) 0.0452 1.0000 Uani . U . . . . .
C22 C 0.0783(9) 0.6717(6) 0.8512(4) 0.0574 1.0000 Uani . U . . . . .
C23 C 0.1477(10) 0.7984(7) 0.6473(7) 0.0604 1.0000 Uani . U . . . . .
C24 C 0.0425(6) 0.7379(5) 0.6768(4) 0.0514 1.0000 Uani . U . . . . .
C25 C 0.4152(8) 0.7090(6) 0.8259(4) 0.0568 1.0000 Uani . U . . . . .
C26 C -0.0327(10) 0.5996(10) 0.7360(6) 0.0615 1.0000 Uani . U . . . . .
C27 C 0.3154(5) 0.5822(4) 0.5292(3) 0.0427 1.0000 Uani . U . . . . .
C28 C 0.5315(11) 0.5839(12) 0.7420(8) 0.0849 1.0000 Uani . U . . . . .
F3 F 0.2463(12) 0.9285(2) 1.09496(14) 0.0731 1.0000 Uani . U . . . . .
H111 H 0.0874 0.5078 0.5603 0.0828 1.0000 Uiso R . . . . . .
H113 H 0.1232 0.4092 0.6168 0.0824 1.0000 Uiso R . . . . . .
H112 H 0.1603 0.4082 0.5241 0.0832 1.0000 Uiso R . . . . . .
H151 H 0.4485 0.4498 0.6119 0.0721 1.0000 Uiso R . . . . . .
H153 H 0.3468 0.3637 0.6402 0.0719 1.0000 Uiso R . . . . . .
H152 H 0.3745 0.3812 0.5448 0.0717 1.0000 Uiso R . . . . . .
H181 H 0.2855 0.7405 0.5040 0.0442 1.0000 Uiso R . . . . . .
H182 H 0.1607 0.6759 0.5235 0.0439 1.0000 Uiso R . . . . . .
H192 H 0.5110 0.8072 0.7323 0.0559 1.0000 Uiso R . . . . . .
H221 H 0.0896 0.5995 0.8717 0.0872 1.0000 Uiso R . . . . . .
H223 H 0.1484 0.7174 0.8674 0.0868 1.0000 Uiso R . . . . . .
H222 H -0.0003 0.7014 0.8702 0.0867 1.0000 Uiso R . . . . . .
H232 H 0.1249 0.8413 0.5992 0.0717 1.0000 Uiso R . . . . . .
H241 H 0.0135 0.6907 0.6317 0.0622 1.0000 Uiso R . . . . . .
H251 H 0.3911 0.6553 0.8647 0.0847 1.0000 Uiso R . . . . . .
H253 H 0.4963 0.7369 0.8424 0.0851 1.0000 Uiso R . . . . . .
H252 H 0.3535 0.7669 0.8263 0.0849 1.0000 Uiso R . . . . . .
H261 H -0.0438 0.5982 0.6766 0.0928 1.0000 Uiso R . . . . . .
H262 H -0.1063 0.6301 0.7612 0.0926 1.0000 Uiso R . . . . . .
H263 H -0.0204 0.5284 0.7563 0.0926 1.0000 Uiso R . . . . . .
H271 H 0.4071 0.5930 0.5365 0.0521 1.0000 Uiso R . . . . . .
H272 H 0.2989 0.5537 0.4737 0.0522 1.0000 Uiso R . . . . . .
H283 H 0.5254 0.5320 0.7860 0.1250 1.0000 Uiso R . . . . . .
H282 H 0.6100 0.6223 0.7468 0.1248 1.0000 Uiso R . . . . . .
H281 H 0.5280 0.5461 0.6899 0.1249 1.0000 Uiso R . . . . . .
H242 H -0.0247 0.7866 0.6930 0.0621 1.0000 Uiso R . . . . . .
H191 H 0.3716 0.8223 0.7640 0.0556 1.0000 Uiso R . . . . . .
H231 H 0.1786 0.8450 0.6918 0.0721 1.0000 Uiso R . . . . . .
O100 O 0.2054(9) 0.4798(6) 0.7806(5) 0.0498 0.655(11) Uani D U P . 2 . .
N200 N 0.2262(8) 0.3998(5) 0.7801(4) 0.0522 0.655(11) Uani D U P . 2 . .
O120 O 0.2408(14) 0.3315(6) 0.8315(5) 0.0514 0.655(11) Uani D U P . 2 . .
O101 O 0.2817(17) 0.4882(11) 0.7897(10) 0.0498 0.345(11) Uani D U P . 1 . .
N201 N 0.3055(16) 0.4120(10) 0.7965(9) 0.0522 0.345(11) Uani D U P . 1 . .
O121 O 0.2830(19) 0.3429(13) 0.8456(12) 0.0514 0.345(11) Uani D U P . 1 . .
H171 H 0.3722 0.8573 0.6241 0.0761 1.0000 Uiso R . . . . . .
H172 H 0.4403 0.7458 0.6083 0.0767 1.0000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0557(3) 0.02092(18) 0.02675(19) 0.00231(14) -0.0002(7) 0.0015(6)
S2 0.0353(4) 0.0252(4) 0.0270(4) -0.0041(3) -0.0019(12) 0.0011(12)
O1 0.0575(19) 0.0360(13) 0.0263(11) -0.0089(9) 0.000(3) 0.009(4)
C4 0.090(2) 0.0331(16) 0.0303(14) -0.0005(11) -0.002(6) 0.003(3)
O6 0.040(2) 0.049(4) 0.058(5) -0.008(3) 0.000(3) -0.013(2)
N7 0.0552(17) 0.0228(12) 0.0281(12) 0.0025(8) -0.001(3) -0.004(3)
F8 0.143(3) 0.055(4) 0.073(5) -0.002(3) -0.008(4) 0.054(4)
O9 0.039(2) 0.043(4) 0.042(4) -0.015(3) 0.005(3) 0.006(2)
C11 0.062(3) 0.061(4) 0.042(4) -0.021(3) -0.004(3) 0.004(3)
N13 0.073(3) 0.0253(13) 0.0356(14) -0.0052(10) -0.005(2) 0.0046(19)
N14 0.0401(19) 0.046(3) 0.050(3) -0.006(2) -0.001(2) 0.0141(19)
C15 0.057(3) 0.043(3) 0.043(3) -0.005(2) 0.006(3) 0.009(2)
F16 0.145(3) 0.063(4) 0.057(4) 0.017(3) 0.016(4) -0.050(4)
C17 0.088(4) 0.038(4) 0.064(4) 0.009(3) -0.025(4) -0.033(4)
C18 0.049(2) 0.0322(16) 0.0286(14) 0.0026(11) -0.007(4) 0.001(3)
C19 0.043(3) 0.043(2) 0.051(2) -0.018(2) 0.001(2) -0.007(2)
N21 0.046(2) 0.045(3) 0.044(2) 0.006(2) 0.009(2) -0.0081(19)
C22 0.063(4) 0.068(4) 0.041(2) -0.023(3) 0.002(3) 0.002(4)
C23 0.100(4) 0.030(3) 0.050(3) 0.019(3) 0.022(4) 0.025(3)
C24 0.058(3) 0.051(3) 0.046(3) -0.009(2) -0.005(2) 0.019(2)
C25 0.057(4) 0.064(4) 0.049(2) -0.017(2) -0.011(3) 0.001(3)
C26 0.050(3) 0.090(5) 0.045(4) -0.023(4) 0.005(3) -0.018(4)
C27 0.060(3) 0.039(2) 0.0295(19) -0.0061(16) -0.0011(19) 0.0066(19)
C28 0.060(4) 0.112(7) 0.082(7) -0.042(6) -0.035(5) 0.056(5)
F3 0.136(3) 0.0573(15) 0.0263(10) 0.0021(10) 0.010(4) 0.010(5)
O100 0.055(3) 0.0403(16) 0.054(2) 0.0178(16) -0.015(3) 0.000(2)
N200 0.058(4) 0.0392(15) 0.059(3) 0.0227(16) -0.009(3) -0.002(2)
O120 0.058(5) 0.0416(19) 0.055(3) 0.021(2) -0.006(3) -0.001(3)
O101 0.055(3) 0.0403(16) 0.054(2) 0.0178(16) -0.015(3) 0.000(2)
N201 0.058(4) 0.0392(15) 0.059(3) 0.0227(16) -0.009(3) -0.002(2)
O121 0.058(5) 0.0416(19) 0.055(3) 0.021(2) -0.006(3) -0.001(3)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.3422(6)

loop_
_oxford_twin_element_scale_factors
0.61(4)
0.39(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 . N7 . 2.022(3) yes
Cu1 . N13 . 2.152(4) yes
Cu1 . N14 . 2.127(8) yes
Cu1 . N21 . 2.151(8) yes
Cu1 . O101 . 1.961(12) yes
S2 . O1 . 1.440(2) yes
S2 . C4 . 1.807(4) yes
S2 . O6 . 1.426(8) yes
S2 . O9 . 1.448(7) yes
C4 . F8 . 1.405(16) yes
C4 . F16 . 1.280(15) yes
C4 . F3 . 1.326(4) yes
N7 . C17 . 1.574(15) yes
N7 . C18 . 1.495(4) yes
N7 . C23 . 1.416(14) yes
C11 . N13 . 1.439(9) yes
C11 . H111 . 0.964 no
C11 . H113 . 0.953 no
C11 . H112 . 0.956 no
N13 . C15 . 1.508(8) yes
N13 . C27 . 1.515(6) yes
N14 . C19 . 1.510(10) yes
N14 . C25 . 1.396(9) yes
N14 . C28 . 1.479(12) yes
C15 . H151 . 0.964 no
C15 . H153 . 0.966 no
C15 . H152 . 0.970 no
C17 . C19 . 1.461(12) yes
C17 . H171 . 0.965 no
C17 . H172 . 0.965 no
C18 . C27 . 1.498(8) yes
C18 . H181 . 0.962 no
C18 . H182 . 0.972 no
C19 . H192 . 0.961 no
C19 . H191 . 0.976 no
N21 . C22 . 1.549(9) yes
N21 . C24 . 1.595(10) yes
N21 . C26 . 1.466(12) yes
C22 . H221 . 0.962 no
C22 . H223 . 0.970 no
C22 . H222 . 0.960 no
C23 . C24 . 1.425(12) yes
C23 . H232 . 0.969 no
C23 . H231 . 0.977 no
C24 . H241 . 0.981 no
C24 . H242 . 0.969 no
C25 . H251 . 0.948 no
C25 . H253 . 0.963 no
C25 . H252 . 0.970 no
C26 . H261 . 0.963 no
C26 . H262 . 0.957 no
C26 . H263 . 0.950 no
C27 . H271 . 0.987 no
C27 . H272 . 0.977 no
C28 . H283 . 0.960 no
C28 . H282 . 0.961 no
C28 . H281 . 0.960 no
O100 . N200 . 1.016(6) yes
N200 . O120 . 1.193(6) yes
O101 . N201 . 0.984(9) yes
N201 . O121 . 1.189(9) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N7 . Cu1 . N13 . 85.84(13) yes
N7 . Cu1 . N14 . 85.4(4) yes
N13 . Cu1 . N14 . 113.0(3) yes
N7 . Cu1 . N21 . 85.3(4) yes
N13 . Cu1 . N21 . 127.1(3) yes
N14 . Cu1 . N21 . 118.10(14) yes
N7 . Cu1 . O101 . 168.2(6) yes
N13 . Cu1 . O101 . 100.4(5) yes
N14 . Cu1 . O101 . 82.9(6) yes
N21 . Cu1 . O101 . 98.7(5) yes
O1 . S2 . C4 . 103.12(17) yes
O1 . S2 . O6 . 116.3(5) yes
C4 . S2 . O6 . 104.2(6) yes
O1 . S2 . O9 . 114.4(5) yes
C4 . S2 . O9 . 101.7(5) yes
O6 . S2 . O9 . 114.57(17) yes
S2 . C4 . F8 . 108.8(8) yes
S2 . C4 . F16 . 113.5(8) yes
F8 . C4 . F16 . 106.2(4) yes
S2 . C4 . F3 . 112.5(3) yes
F8 . C4 . F3 . 106.7(9) yes
F16 . C4 . F3 . 108.8(9) yes
Cu1 . N7 . C17 . 104.5(5) yes
Cu1 . N7 . C18 . 108.57(19) yes
C17 . N7 . C18 . 106.7(9) yes
Cu1 . N7 . C23 . 111.3(5) yes
C17 . N7 . C23 . 110.8(5) yes
C18 . N7 . C23 . 114.4(8) yes
N13 . C11 . H111 . 110.6 no
N13 . C11 . H113 . 108.6 no
H111 . C11 . H113 . 109.8 no
N13 . C11 . H112 . 110.5 no
H111 . C11 . H112 . 109.5 no
H113 . C11 . H112 . 107.8 no
C11 . N13 . Cu1 . 110.9(4) yes
C11 . N13 . C15 . 108.9(4) yes
Cu1 . N13 . C15 . 114.5(4) yes
C11 . N13 . C27 . 113.0(5) yes
Cu1 . N13 . C27 . 104.0(2) yes
C15 . N13 . C27 . 105.4(5) yes
Cu1 . N14 . C19 . 107.1(5) yes
Cu1 . N14 . C25 . 112.6(6) yes
C19 . N14 . C25 . 77.1(5) yes
Cu1 . N14 . C28 . 114.1(8) yes
C19 . N14 . C28 . 127.6(9) yes
C25 . N14 . C28 . 112.9(8) yes
N13 . C15 . H151 . 108.8 no
N13 . C15 . H153 . 110.1 no
H151 . C15 . H153 . 110.2 no
N13 . C15 . H152 . 108.6 no
H151 . C15 . H152 . 109.9 no
H153 . C15 . H152 . 109.3 no
N7 . C17 . C19 . 115.3(8) yes
N7 . C17 . H171 . 107.7 no
C19 . C17 . H171 . 109.9 no
N7 . C17 . H172 . 107.0 no
C19 . C17 . H172 . 107.1 no
H171 . C17 . H172 . 109.9 no
N7 . C18 . C27 . 113.4(5) yes
N7 . C18 . H181 . 110.2 no
C27 . C18 . H181 . 109.1 no
N7 . C18 . H182 . 107.9 no
C27 . C18 . H182 . 107.0 no
H181 . C18 . H182 . 109.2 no
N14 . C19 . C17 . 103.1(6) yes
N14 . C19 . H192 . 109.6 no
C17 . C19 . H192 . 112.3 no
N14 . C19 . H191 . 113.0 no
C17 . C19 . H191 . 110.2 no
H192 . C19 . H191 . 108.6 no
Cu1 . N21 . C22 . 113.6(6) yes
Cu1 . N21 . C24 . 97.1(4) yes
C22 . N21 . C24 . 139.3(7) yes
Cu1 . N21 . C26 . 112.6(7) yes
C22 . N21 . C26 . 103.6(7) yes
C24 . N21 . C26 . 87.3(7) yes
N21 . C22 . H221 . 107.2 no
N21 . C22 . H223 . 107.3 no
H221 . C22 . H223 . 110.8 no
N21 . C22 . H222 . 110.0 no
H221 . C22 . H222 . 110.8 no
H223 . C22 . H222 . 110.7 no
N7 . C23 . C24 . 109.5(7) yes
N7 . C23 . H232 . 110.6 no
C24 . C23 . H232 . 111.1 no
N7 . C23 . H231 . 106.2 no
C24 . C23 . H231 . 109.1 no
H232 . C23 . H231 . 110.1 no
N21 . C24 . C23 . 111.8(6) yes
N21 . C24 . H241 . 108.8 no
C23 . C24 . H241 . 108.1 no
N21 . C24 . H242 . 108.5 no
C23 . C24 . H242 . 109.6 no
H241 . C24 . H242 . 110.0 no
N14 . C25 . H251 . 108.3 no
N14 . C25 . H253 . 109.6 no
H251 . C25 . H253 . 108.1 no
N14 . C25 . H252 . 111.9 no
H251 . C25 . H252 . 109.5 no
H253 . C25 . H252 . 109.5 no
N21 . C26 . H261 . 108.5 no
N21 . C26 . H262 . 110.4 no
H261 . C26 . H262 . 109.2 no
N21 . C26 . H263 . 109.5 no
H261 . C26 . H263 . 109.9 no
H262 . C26 . H263 . 109.4 no
N13 . C27 . C18 . 109.3(5) yes
N13 . C27 . H271 . 109.1 no
C18 . C27 . H271 . 109.7 no
N13 . C27 . H272 . 109.5 no
C18 . C27 . H272 . 109.7 no
H271 . C27 . H272 . 109.6 no
N14 . C28 . H283 . 109.6 no
N14 . C28 . H282 . 109.6 no
H283 . C28 . H282 . 109.2 no
N14 . C28 . H281 . 109.9 no
H283 . C28 . H281 . 108.3 no
H282 . C28 . H281 . 110.2 no
Cu1 . O100 . N200 . 132.1(7) yes
O100 . N200 . O120 . 135.54(10) yes
Cu1 . O101 . N201 . 142.1(13) yes
O101 . N201 . O121 . 135.54(10) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C11 . H111 . O9 3_546 151 0.96 2.49 3.365(11) yes
C19 . H192 . N201 3_656 160 0.96 2.38 3.299(11) yes
C19 . H192 . O121 3_656 145 0.96 2.55 3.386(11) yes
C23 . H232 . O6 4_574 162 0.97 2.51 3.445(11) yes
C26 . H261 . O9 3_546 162 0.96 2.50 3.432(11) yes
C27 . H271 . O6 3_646 162 0.99 2.46 3.409(11) yes
C27 . H272 . O121 4_564 128 0.98 2.58 3.268(11) yes
C24 . H242 . N200 3_556 171 0.97 2.59 3.549(11) yes
C24 . H242 . O120 3_556 144 0.97 2.39 3.218(11) yes

# start Validation Reply Form
_vrf_PLAT412_complex12           
;
PROBLEM: Short Intra XH3 .. XHn H191 .. H252 ..
1.23 Ang.
RESPONSE: This was believed to occur as a result of disorder within
the ligand spreading to the whole structure. See refine_special_details
for full details.
;
_vrf_PLAT111_complex12           
;
PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry .....
88 PerFi
RESPONSE: The alternative pseudo symmetry was modelled, See
refine_special_details for full details.
;
_chemical_name_common            .
# end Validation Reply Form

#===END

#############################################################
# ***dilworth group***
#
# this structure was solved by Michael Jones on 22/12/2008
#############################################################
data_complex17
_database_code_depnum_ccdc_archive 'CCDC 737903'
_audit_creation_date             08-12-22
_audit_creation_method           CRYSTALS_ver_12.85

_oxford_structure_analysis_title 003mwj08
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_refine_special_details          
;
;

_cell_length_a                   8.44540(10)
_cell_length_b                   14.2019(2)
_cell_length_c                   14.0713(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.4736(8)
_cell_angle_gamma                90
_cell_volume                     1680.03(4)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-p 2yn '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_formula_units_Z            4

# Given Formula = C15 H12 Cu1 N4 O2 P1
# Dc = 1.48 Fooo = 852.00 Mu = 14.08 M = 374.81
# Found Formula = C15 H12 Cu1 N5 O4 P1
# Dc = 1.66 FOOO = 852.00 Mu = 14.28 M = 420.81

_chemical_formula_sum            'C15 H12 Cu1 N5 O4 P1'
_chemical_formula_moiety         'C15 H12 Cu1 N5 O4 P1'
_chemical_compound_source        .
_chemical_formula_weight         420.81

_cell_measurement_reflns_used    3949
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       prism
_exptl_crystal_colour            clear_intense_green
_exptl_crystal_size_min          0.08
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             852
_exptl_absorpt_coefficient_mu    1.428

# Sheldrick geometric approximatio 0.83 0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.89
# For a Kappa CCD, set Tmin to 1.0 and
# Tmax to the ratio of max:min frame scales in scale_all.log
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       \w

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            27014
_reflns_number_total             3818
_diffrn_reflns_av_R_equivalents  0.039
# Number of reflections with Friedels Law is 3818
# Number of reflections without Friedels Law is 36210
# Theoretical number of reflections is about 3850

_diffrn_reflns_theta_min         5.134
_diffrn_reflns_theta_max         27.476
_diffrn_measured_fraction_theta_max 0.993

_diffrn_reflns_theta_full        27.476
_diffrn_measured_fraction_theta_full 0.993

_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -10
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   1.58
_oxford_diffrn_Wilson_scale      9.87

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.48
_refine_diff_density_max         0.56

# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold

# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         3034
_refine_ls_number_restraints     0
_refine_ls_number_parameters     235
_oxford_refine_ls_R_factor_ref   0.0330
_refine_ls_wR_factor_ref         0.0757
_refine_ls_goodness_of_fit_ref   1.0123
_refine_ls_shift/su_max          0.001289

# The values computed from all data
_oxford_reflns_number_all        3818
_refine_ls_R_factor_all          0.0436
_refine_ls_wR_factor_all         0.0806

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                3192
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_gt          0.0773

# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 2.25P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands.

Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Cu1 Cu 0.53458(3) 0.852178(19) 0.740729(19) 0.0190 1.0000 Uani . . . . . . .
O2 O 0.5012(2) 0.74605(12) 0.82674(12) 0.0308 1.0000 Uani . . . . . . .
N3 N 0.4110(3) 0.76314(17) 0.89373(17) 0.0407 1.0000 Uani . . . . . . .
O4 O 0.3902(3) 0.69578(16) 0.94504(16) 0.0573 1.0000 Uani . . . . . . .
O5 O 0.4839(2) 0.75982(12) 0.63260(13) 0.0292 1.0000 Uani . . . . . . .
N6 N 0.6006(3) 0.70271(15) 0.63010(16) 0.0310 1.0000 Uani . . . . . . .
O7 O 0.7186(2) 0.72419(14) 0.68510(14) 0.0350 1.0000 Uani . . . . . . .
N8 N 0.6272(2) 0.93123(13) 0.85264(13) 0.0200 1.0000 Uani . . . . . . .
C9 C 0.7302(3) 0.89230(18) 0.92054(17) 0.0254 1.0000 Uani . . . . . . .
C10 C 0.7941(3) 0.94173(19) 0.99974(17) 0.0273 1.0000 Uani . . . . . . .
C11 C 0.7473(3) 1.03392(18) 1.01114(16) 0.0270 1.0000 Uani . . . . . . .
C12 C 0.6404(3) 1.07454(17) 0.94235(16) 0.0213 1.0000 Uani . . . . . . .
C13 C 0.5837(3) 1.02186(16) 0.86279(16) 0.0184 1.0000 Uani . . . . . . .
P14 P 0.45871(7) 1.08274(4) 0.76688(4) 0.0187 1.0000 Uani . . . . . . .
C15 C 0.2826(3) 1.00518(16) 0.74961(15) 0.0187 1.0000 Uani . . . . . . .
N16 N 0.2985(2) 0.91212(14) 0.73528(14) 0.0213 1.0000 Uani . . . . . . .
C17 C 0.1671(3) 0.85863(17) 0.72537(17) 0.0252 1.0000 Uani . . . . . . .
C18 C 0.0160(3) 0.8953(2) 0.72945(19) 0.0308 1.0000 Uani . . . . . . .
C19 C -0.0009(3) 0.9909(2) 0.74303(18) 0.0300 1.0000 Uani . . . . . . .
C20 C 0.1338(3) 1.04727(18) 0.75269(16) 0.0230 1.0000 Uani . . . . . . .
C21 C 0.5691(3) 1.04623(16) 0.66599(15) 0.0189 1.0000 Uani . . . . . . .
N22 N 0.6023(2) 0.95419(13) 0.65090(13) 0.0191 1.0000 Uani . . . . . . .
C23 C 0.6862(3) 0.93301(18) 0.57694(16) 0.0230 1.0000 Uani . . . . . . .
C24 C 0.7416(3) 1.00064(19) 0.51761(17) 0.0279 1.0000 Uani . . . . . . .
C25 C 0.7078(3) 1.09421(19) 0.53292(18) 0.0306 1.0000 Uani . . . . . . .
C26 C 0.6194(3) 1.11692(18) 0.60813(17) 0.0255 1.0000 Uani . . . . . . .
H91 H 0.7573 0.8279 0.9121 0.0304 1.0000 Uiso R . . . . . .
H101 H 0.8702 0.9136 1.0451 0.0339 1.0000 Uiso R . . . . . .
H111 H 0.7869 1.0686 1.0662 0.0321 1.0000 Uiso R . . . . . .
H121 H 0.6056 1.1378 0.9490 0.0265 1.0000 Uiso R . . . . . .
H171 H 0.1804 0.7931 0.7152 0.0302 1.0000 Uiso R . . . . . .
H181 H -0.0752 0.8559 0.7221 0.0367 1.0000 Uiso R . . . . . .
H191 H -0.1041 1.0192 0.7462 0.0363 1.0000 Uiso R . . . . . .
H201 H 0.1264 1.1131 0.7610 0.0279 1.0000 Uiso R . . . . . .
H231 H 0.7062 0.8686 0.5665 0.0267 1.0000 Uiso R . . . . . .
H241 H 0.8023 0.9823 0.4673 0.0334 1.0000 Uiso R . . . . . .
H251 H 0.7444 1.1424 0.4938 0.0372 1.0000 Uiso R . . . . . .
H261 H 0.5939 1.1807 0.6203 0.0300 1.0000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.02111(16) 0.01461(15) 0.02168(15) -0.00151(11) 0.00447(11) -0.00009(11)
O2 0.0452(11) 0.0199(9) 0.0296(9) -0.0019(7) 0.0148(8) -0.0019(8)
N3 0.0610(17) 0.0312(13) 0.0331(12) 0.0005(10) 0.0214(12) -0.0041(12)
O4 0.0944(19) 0.0367(12) 0.0467(12) 0.0080(10) 0.0376(13) -0.0088(12)
O5 0.0298(10) 0.0246(9) 0.0338(9) -0.0017(7) 0.0052(7) 0.0002(8)
N6 0.0320(13) 0.0254(11) 0.0370(12) -0.0068(9) 0.0100(10) 0.0003(10)
O7 0.0287(10) 0.0373(11) 0.0393(10) -0.0044(9) 0.0043(8) -0.0009(8)
N8 0.0215(10) 0.0189(9) 0.0200(9) 0.0004(8) 0.0042(7) 0.0016(8)
C9 0.0260(13) 0.0240(12) 0.0265(12) 0.0022(10) 0.0041(10) 0.0033(10)
C10 0.0247(13) 0.0343(14) 0.0224(11) 0.0028(10) -0.0002(9) 0.0005(11)
C11 0.0288(13) 0.0339(14) 0.0184(11) -0.0014(10) 0.0017(9) -0.0086(11)
C12 0.0237(12) 0.0197(11) 0.0213(11) -0.0007(9) 0.0065(9) -0.0053(9)
C13 0.0178(11) 0.0175(11) 0.0206(10) -0.0004(9) 0.0046(8) -0.0022(9)
P14 0.0196(3) 0.0141(3) 0.0224(3) -0.0004(2) 0.0022(2) 0.0003(2)
C15 0.0199(11) 0.0186(11) 0.0179(10) 0.0012(8) 0.0040(9) 0.0008(9)
N16 0.0197(10) 0.0192(10) 0.0252(10) -0.0016(8) 0.0026(8) 0.0003(8)
C17 0.0222(12) 0.0216(12) 0.0319(13) -0.0025(10) 0.0023(10) -0.0033(10)
C18 0.0212(13) 0.0347(14) 0.0358(14) -0.0017(11) -0.0006(11) -0.0057(11)
C19 0.0202(13) 0.0359(14) 0.0334(13) 0.0004(11) 0.0000(10) 0.0051(11)
C20 0.0223(12) 0.0243(12) 0.0221(11) -0.0001(9) 0.0013(9) 0.0028(10)
C21 0.0178(11) 0.0183(11) 0.0199(10) 0.0003(9) -0.0014(8) -0.0031(9)
N22 0.0172(10) 0.0196(9) 0.0204(9) -0.0012(7) 0.0015(7) -0.0011(8)
C23 0.0213(12) 0.0267(12) 0.0209(11) -0.0038(9) 0.0018(9) -0.0007(10)
C24 0.0273(13) 0.0370(14) 0.0199(11) -0.0007(10) 0.0055(10) -0.0027(11)
C25 0.0356(15) 0.0331(14) 0.0234(12) 0.0064(10) 0.0041(11) -0.0077(12)
C26 0.0296(14) 0.0216(12) 0.0251(11) 0.0020(10) 0.0019(10) -0.0029(10)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.3063(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 . O2 . 1.9701(17) yes
Cu1 . O5 . 2.0235(18) yes
Cu1 . O7 . 2.5620(19) yes
Cu1 . N8 . 2.0292(19) yes
Cu1 . N16 . 2.162(2) yes
Cu1 . N22 . 2.0401(19) yes
O2 . N3 . 1.290(3) yes
N3 . O4 . 1.221(3) yes
O5 . N6 . 1.280(3) yes
N6 . O7 . 1.240(3) yes
N8 . C9 . 1.347(3) yes
N8 . C13 . 1.350(3) yes
C9 . C10 . 1.383(4) yes
C9 . H91 . 0.953 no
C10 . C11 . 1.382(4) yes
C10 . H101 . 0.949 no
C11 . C12 . 1.385(4) yes
C11 . H111 . 0.951 no
C12 . C13 . 1.393(3) yes
C12 . H121 . 0.952 no
C13 . P14 . 1.847(2) yes
P14 . C15 . 1.848(2) yes
P14 . C21 . 1.846(2) yes
C15 . N16 . 1.346(3) yes
C15 . C20 . 1.396(3) yes
N16 . C17 . 1.341(3) yes
C17 . C18 . 1.384(4) yes
C17 . H171 . 0.950 no
C18 . C19 . 1.381(4) yes
C18 . H181 . 0.950 no
C19 . C20 . 1.387(4) yes
C19 . H191 . 0.965 no
C20 . H201 . 0.946 no
C21 . N22 . 1.358(3) yes
C21 . C26 . 1.385(3) yes
N22 . C23 . 1.348(3) yes
C23 . C24 . 1.383(3) yes
C23 . H231 . 0.944 no
C24 . C25 . 1.380(4) yes
C24 . H241 . 0.949 no
C25 . C26 . 1.390(4) yes
C25 . H251 . 0.948 no
C26 . H261 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 . Cu1 . O5 . 86.19(7) yes
O2 . Cu1 . O7 . 76.79(7) yes
O5 . Cu1 . O7 . 53.23(7) yes
O2 . Cu1 . N8 . 90.79(7) yes
O5 . Cu1 . N8 . 168.66(8) yes
O7 . Cu1 . N8 . 115.43(7) yes
O2 . Cu1 . N16 . 97.90(8) yes
O5 . Cu1 . N16 . 95.75(7) yes
O7 . Cu1 . N16 . 148.49(7) yes
N8 . Cu1 . N16 . 95.50(7) yes
O2 . Cu1 . N22 . 171.50(8) yes
O5 . Cu1 . N22 . 92.65(7) yes
O7 . Cu1 . N22 . 95.77(7) yes
N8 . Cu1 . N22 . 88.72(7) yes
N16 . Cu1 . N22 . 90.60(7) yes
Cu1 . O2 . N3 . 115.73(15) yes
O2 . N3 . O4 . 114.4(2) yes
Cu1 . O5 . N6 . 108.85(15) yes
O5 . N6 . O7 . 113.7(2) yes
Cu1 . O7 . N6 . 83.71(14) yes
Cu1 . N8 . C9 . 119.88(16) yes
Cu1 . N8 . C13 . 121.38(15) yes
C9 . N8 . C13 . 118.7(2) yes
N8 . C9 . C10 . 122.6(2) yes
N8 . C9 . H91 . 116.9 no
C10 . C9 . H91 . 120.5 no
C9 . C10 . C11 . 118.7(2) yes
C9 . C10 . H101 . 121.0 no
C11 . C10 . H101 . 120.3 no
C10 . C11 . C12 . 119.2(2) yes
C10 . C11 . H111 . 120.2 no
C12 . C11 . H111 . 120.6 no
C11 . C12 . C13 . 119.3(2) yes
C11 . C12 . H121 . 120.7 no
C13 . C12 . H121 . 120.0 no
C12 . C13 . N8 . 121.4(2) yes
C12 . C13 . P14 . 117.68(17) yes
N8 . C13 . P14 . 120.77(16) yes
C13 . P14 . C15 . 102.33(10) yes
C13 . P14 . C21 . 97.77(10) yes
C15 . P14 . C21 . 101.00(10) yes
P14 . C15 . N16 . 120.93(17) yes
P14 . C15 . C20 . 117.15(18) yes
N16 . C15 . C20 . 121.9(2) yes
C15 . N16 . Cu1 . 119.12(15) yes
C15 . N16 . C17 . 118.6(2) yes
Cu1 . N16 . C17 . 122.12(16) yes
N16 . C17 . C18 . 122.7(2) yes
N16 . C17 . H171 . 117.5 no
C18 . C17 . H171 . 119.8 no
C17 . C18 . C19 . 118.9(2) yes
C17 . C18 . H181 . 121.0 no
C19 . C18 . H181 . 120.0 no
C18 . C19 . C20 . 119.1(2) yes
C18 . C19 . H191 . 121.4 no
C20 . C19 . H191 . 119.5 no
C15 . C20 . C19 . 118.8(2) yes
C15 . C20 . H201 . 119.8 no
C19 . C20 . H201 . 121.3 no
P14 . C21 . N22 . 121.18(16) yes
P14 . C21 . C26 . 117.02(18) yes
N22 . C21 . C26 . 121.8(2) yes
C21 . N22 . Cu1 . 120.84(15) yes
C21 . N22 . C23 . 117.9(2) yes
Cu1 . N22 . C23 . 121.27(16) yes
N22 . C23 . C24 . 123.0(2) yes
N22 . C23 . H231 . 116.8 no
C24 . C23 . H231 . 120.2 no
C23 . C24 . C25 . 119.2(2) yes
C23 . C24 . H241 . 119.9 no
C25 . C24 . H241 . 121.0 no
C24 . C25 . C26 . 118.4(2) yes
C24 . C25 . H251 . 121.4 no
C26 . C25 . H251 . 120.2 no
C25 . C26 . C21 . 119.8(2) yes
C25 . C26 . H261 . 120.3 no
C21 . C26 . H261 . 119.9 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C18 . H181 . O7 1_455 167 0.95 2.57 3.508(3) yes
C20 . H201 . O2 3_556 137 0.95 2.45 3.206(3) yes
C23 . H231 . O4 4_564 125 0.94 2.58 3.220(3) yes

# start Validation Reply Form
_vrf_PLAT232_complex17           
;
PROBLEM: Hirshfeld Test Diff (M-X) Cu1 -- O5 .. 12.16 su
RESPONSE: ... The components of the anisotropic displacement
parameters along chemical bonds are assumed to be equal in magnitude,
however, in the case of the copper-oxygen bond in this complex, this is
not the case. This is due to the ionic nature of the bond between the
two components.
;
_chemical_name_common            .
# end Validation Reply Form

#===END

data_complex19
_database_code_depnum_ccdc_archive 'CCDC 737904'
#=============================================================
# Diffractometer details
#=============================================================
_diffrn_measurement_device_type  
;
Nonius KappaCCD
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction        
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_cell_refinement       
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
#=============================================================
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'

_chemical_name_systematic        # IUPAC name, in full
;
?
;
_chemical_melting_point          'not measured'
_exptl_crystal_thermal_history   
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis.
;
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_special_details          
;
It was clear that the coordinated NO~2~ ligand was disordered and examination
of the Fourier difference map suggested that this was due to the majority
of these groups being coordinated in the NO~2~ binding mode but a smaller
proportion were in the ONO binding mode. The coordinates, anisotropic
thermal parameters and site occupancies of the N and O atoms were refined.
The N-O distances of the nitro ligand were restrained to their common mean
su 0.02 \%A). Similarity restraints were applied to the displacement
parameters of directly-bonded pairs of atoms within the disordered NO~2~
groups.

The NH hydrogen atoms were located in a difference Fourier map and their
coordinates and isotropic displacement parameters subsequently refined.
All other hydrogen atoms were positioned geometrically.
;

#=============================================================
_cell_length_a                   9.2603(2)
_cell_angle_alpha                71.7144(10)
_cell_length_b                   10.5430(2)
_cell_angle_beta                 89.4148(9)
_cell_length_c                   16.2011(4)
_cell_angle_gamma                79.4600(11)
_cell_volume                     1474.64(6)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'Cu ' 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B

_cell_formula_units_Z            2
_chemical_formula_sum            ' C28 H27 Cu N11 O4 '
_chemical_formula_moiety         ' C24 H21 Cu N8 O2, 2( C2 H3 N ), N O2 '
_chemical_compound_source        
;
synthesis as described
;
_chemical_formula_weight         645.14

_cell_measurement_reflns_used    17156
_cell_measurement_theta_min      5
_cell_measurement_theta_max      28
_cell_measurement_temperature    150

_exptl_crystal_description       ' plate '
_exptl_crystal_colour            ' brown-green '
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_max          0.38

_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_meas      'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             666
_exptl_absorpt_coefficient_mu    0.795

_diffrn_measurement_method       \w

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.92

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0.00

_diffrn_ambient_temperature      150
_diffrn_reflns_number            17156
_reflns_number_total             6624
_diffrn_reflns_av_R_equivalents  0.041

_diffrn_reflns_theta_min         5.094
_diffrn_reflns_theta_max         27.407
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        27.407
_diffrn_measured_fraction_theta_full 0.998

_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              -12
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              20

_refine_diff_density_min         -0.49
_refine_diff_density_max         0.62

_refine_ls_number_reflns         3808
_refine_ls_number_restraints     8
_refine_ls_number_parameters     437

#_refine_ls_R_factor_ref 0.0416
_refine_ls_wR_factor_ref         0.0478
_refine_ls_goodness_of_fit_ref   1.1222

#_reflns_number_all 6624
_refine_ls_R_factor_all          0.0819
_refine_ls_wR_factor_all         0.0781

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                3808
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_gt          0.0478

_refine_ls_shift/su_max          0.015964
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.604 0.268 0.317
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_disorder_assembly
_atom_site_refinement_disorder_group
Cu1 Cu 0.24571(5) 0.62283(4) 0.23548(3) 0.0407 1.0000 Uani . U . . .
N1 N 0.4444(3) 0.5790(2) 0.17129(16) 0.0342 1.0000 Uani . . . . .
C1 C 0.4395(3) 0.7000(3) 0.0925(2) 0.0364 1.0000 Uani . . . . .
C2 C 0.2828(3) 0.7465(3) 0.05888(19) 0.0307 1.0000 Uani . . . . .
N2 N 0.1731(3) 0.7198(2) 0.11036(16) 0.0326 1.0000 Uani . . . . .
C3 C 0.0450(3) 0.7815(3) 0.05720(19) 0.0306 1.0000 Uani . . . . .
C4 C -0.1034(4) 0.7897(3) 0.0746(2) 0.0373 1.0000 Uani . . . . .
C5 C -0.2042(3) 0.8600(3) 0.0053(2) 0.0398 1.0000 Uani . . . . .
C6 C -0.1611(4) 0.9207(3) -0.0782(2) 0.0403 1.0000 Uani . . . . .
C7 C -0.0144(4) 0.9150(3) -0.09644(19) 0.0359 1.0000 Uani . . . . .
C8 C 0.0866(3) 0.8441(3) -0.02730(19) 0.0307 1.0000 Uani . . . . .
N3 N 0.2393(3) 0.8194(2) -0.02316(17) 0.0307 1.0000 Uani . . . . .
C9 C 0.4388(3) 0.4548(3) 0.14667(18) 0.0305 1.0000 Uani . . . . .
C10 C 0.3608(3) 0.3631(3) 0.21363(18) 0.0307 1.0000 Uani . . . . .
N4 N 0.2637(3) 0.4088(2) 0.26306(15) 0.0330 1.0000 Uani . . . . .
C11 C 0.2095(3) 0.2951(3) 0.31312(19) 0.0361 1.0000 Uani . . . . .
C12 C 0.1040(4) 0.2828(4) 0.3758(2) 0.0451 1.0000 Uani . . . . .
C13 C 0.0707(4) 0.1540(4) 0.4127(3) 0.0581 1.0000 Uani . . . . .
C14 C 0.1377(5) 0.0418(4) 0.3884(3) 0.0627 1.0000 Uani . . . . .
C15 C 0.2427(4) 0.0523(3) 0.3265(2) 0.0515 1.0000 Uani . . . . .
C16 C 0.2776(3) 0.1797(3) 0.2903(2) 0.0378 1.0000 Uani . . . . .
N5 N 0.3745(3) 0.2282(3) 0.22742(17) 0.0357 1.0000 Uani . . . . .
C17 C 0.5764(4) 0.5595(3) 0.2286(2) 0.0440 1.0000 Uani . . . . .
C18 C 0.5295(4) 0.6116(3) 0.3020(2) 0.0444 1.0000 Uani . . . . .
N6 N 0.3918(4) 0.6298(2) 0.32450(17) 0.0441 1.0000 Uani . . . . .
C19 C 0.3971(5) 0.6632(3) 0.4018(2) 0.0485 1.0000 Uani . . . . .
C20 C 0.2858(5) 0.6843(3) 0.4572(2) 0.0583 1.0000 Uani . . . . .
C21 C 0.3291(6) 0.7107(4) 0.5317(2) 0.0690 1.0000 Uani . . . . .
C22 C 0.4727(6) 0.7169(4) 0.5493(3) 0.0763 1.0000 Uani . . . . .
C23 C 0.5833(6) 0.6948(4) 0.4950(3) 0.0652 1.0000 Uani . . . . .
C24 C 0.5421(5) 0.6666(3) 0.4215(2) 0.0531 1.0000 Uani . . . . .
N7 N 0.6246(5) 0.6332(3) 0.3564(2) 0.0512 1.0000 Uani . . . . .
N8 N 0.0516(11) 0.6727(7) 0.2856(5) 0.0478 0.651(8) Uani D U P 1 1
O1 O -0.0546(9) 0.6021(9) 0.2958(7) 0.0624 0.651(8) Uani D U P 1 1
O2 O 0.0146(6) 0.7802(5) 0.3001(3) 0.0824 0.651(8) Uani D U P 1 1
O11 O 0.1029(11) 0.7042(17) 0.2920(8) 0.0798 0.349(8) Uani . U P 1 2
N18 N -0.016(2) 0.643(2) 0.2999(13) 0.0538 0.349(8) Uani . U P 1 2
O12 O -0.1093(9) 0.6702(12) 0.3480(7) 0.0821 0.349(8) Uani . U P 1 2
N9 N 0.5591(3) -0.0333(3) 0.14818(19) 0.0450 1.0000 Uani . . . . .
O3 O 0.5652(3) 0.0895(2) 0.14034(15) 0.0428 1.0000 Uani . . . . .
O4 O 0.4834(3) -0.0869(2) 0.20547(17) 0.0521 1.0000 Uani . . . . .
N10 N 0.7511(4) 0.2270(4) 0.2609(2) 0.0635 1.0000 Uani . . . . .
C25 C 0.7393(4) 0.1207(4) 0.3004(2) 0.0510 1.0000 Uani . . . . .
C26 C 0.7194(6) -0.0140(5) 0.3528(3) 0.0759 1.0000 Uani . . . . .
N11 N 0.7506(3) 0.5001(3) 0.0377(2) 0.0503 1.0000 Uani . . . . .
C27 C 0.8562(4) 0.4586(3) 0.0802(2) 0.0395 1.0000 Uani . . . . .
C28 C 0.9896(4) 0.4071(4) 0.1361(3) 0.0516 1.0000 Uani . . . . .
H1 H 0.297(4) 0.852(4) -0.063(3) 0.055(11) 1.0000 Uiso . . . . .
H2 H 0.441(4) 0.178(4) 0.206(2) 0.045(10) 1.0000 Uiso . . . . .
H3 H 0.710(5) 0.630(4) 0.354(3) 0.058(15) 1.0000 Uiso . . . . .
H11 H 0.4753 0.7738 0.1081 0.0439 1.0000 Uiso . . . . .
H12 H 0.5024 0.6747 0.0474 0.0439 1.0000 Uiso . . . . .
H41 H -0.1359 0.7468 0.1343 0.0461 1.0000 Uiso . . . . .
H51 H -0.3116 0.8672 0.0157 0.0495 1.0000 Uiso . . . . .
H61 H -0.2380 0.9696 -0.1261 0.0481 1.0000 Uiso . . . . .
H71 H 0.0173 0.9595 -0.1561 0.0426 1.0000 Uiso . . . . .
H91 H 0.5412 0.4065 0.1433 0.0373 1.0000 Uiso . . . . .
H92 H 0.3850 0.4816 0.0888 0.0373 1.0000 Uiso . . . . .
H121 H 0.0548 0.3624 0.3932 0.0494 1.0000 Uiso . . . . .
H131 H -0.0038 0.1412 0.4583 0.0626 1.0000 Uiso . . . . .
H141 H 0.1089 -0.0483 0.4165 0.0668 1.0000 Uiso . . . . .
H151 H 0.2906 -0.0277 0.3089 0.0571 1.0000 Uiso . . . . .
H171 H 0.6500 0.6110 0.1949 0.0545 1.0000 Uiso . . . . .
H172 H 0.6213 0.4606 0.2518 0.0545 1.0000 Uiso . . . . .
H201 H 0.1814 0.6809 0.4445 0.0666 1.0000 Uiso . . . . .
H211 H 0.2532 0.7256 0.5738 0.0780 1.0000 Uiso . . . . .
H221 H 0.4971 0.7381 0.6030 0.0880 1.0000 Uiso . . . . .
H231 H 0.6874 0.6988 0.5079 0.0759 1.0000 Uiso . . . . .
H261 H 0.7364 -0.0254 0.4158 0.0867 1.0000 Uiso . . . . .
H262 H 0.7911 -0.0842 0.3365 0.0867 1.0000 Uiso . . . . .
H263 H 0.6169 -0.0251 0.3423 0.0867 1.0000 Uiso . . . . .
H281 H 1.0751 0.4360 0.1020 0.0616 1.0000 Uiso . . . . .
H282 H 0.9794 0.4443 0.1859 0.0616 1.0000 Uiso . . . . .
H283 H 1.0059 0.3055 0.1588 0.0616 1.0000 Uiso . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0522(3) 0.0387(2) 0.0324(2) -0.01713(17) 0.00041(16) -0.00165(18)
N1 0.0400(14) 0.0283(12) 0.0351(13) -0.0124(10) -0.0055(11) -0.0041(11)
C1 0.0370(17) 0.0261(14) 0.0467(18) -0.0106(13) 0.0005(14) -0.0094(12)
C2 0.0355(16) 0.0216(13) 0.0362(15) -0.0095(12) 0.0033(12) -0.0081(11)
N2 0.0378(14) 0.0277(12) 0.0345(13) -0.0117(10) 0.0040(11) -0.0085(10)
C3 0.0354(16) 0.0230(13) 0.0350(15) -0.0109(12) 0.0036(12) -0.0066(12)
C4 0.0415(18) 0.0327(16) 0.0409(17) -0.0129(13) 0.0095(14) -0.0132(13)
C5 0.0328(17) 0.0378(17) 0.0532(19) -0.0206(15) 0.0031(14) -0.0064(13)
C6 0.0410(18) 0.0334(16) 0.0458(18) -0.0144(14) -0.0041(14) -0.0018(14)
C7 0.0447(18) 0.0283(15) 0.0336(15) -0.0094(12) 0.0030(13) -0.0050(13)
C8 0.0364(16) 0.0239(14) 0.0335(15) -0.0109(12) 0.0038(12) -0.0068(12)
N3 0.0340(14) 0.0246(12) 0.0333(13) -0.0076(10) 0.0058(11) -0.0078(10)
C9 0.0358(16) 0.0282(14) 0.0293(14) -0.0110(12) 0.0002(12) -0.0073(12)
C10 0.0319(15) 0.0306(14) 0.0296(14) -0.0107(12) -0.0026(12) -0.0041(12)
N4 0.0342(13) 0.0365(14) 0.0289(12) -0.0115(11) 0.0011(10) -0.0062(11)
C11 0.0327(16) 0.0383(16) 0.0314(15) -0.0053(13) -0.0016(12) -0.0016(13)
C12 0.0384(18) 0.053(2) 0.0322(16) -0.0028(15) 0.0025(13) 0.0015(15)
C13 0.044(2) 0.063(2) 0.049(2) 0.0029(18) 0.0145(17) -0.0027(18)
C14 0.055(2) 0.043(2) 0.069(3) 0.0073(19) 0.017(2) -0.0018(18)
C15 0.050(2) 0.0363(18) 0.057(2) -0.0020(16) 0.0118(17) -0.0020(16)
C16 0.0335(16) 0.0369(16) 0.0343(15) -0.0011(13) 0.0043(13) -0.0032(13)
N5 0.0375(14) 0.0286(13) 0.0384(14) -0.0085(11) 0.0069(12) -0.0039(11)
C17 0.0472(19) 0.0404(18) 0.0486(19) -0.0215(15) -0.0141(15) -0.0050(15)
C18 0.065(2) 0.0259(15) 0.0412(18) -0.0127(13) -0.0177(16) -0.0018(15)
N6 0.073(2) 0.0253(13) 0.0337(14) -0.0102(11) -0.0088(13) -0.0058(13)
C19 0.086(3) 0.0243(15) 0.0310(16) -0.0101(13) -0.0169(17) 0.0025(16)
C20 0.096(3) 0.0333(18) 0.0375(18) -0.0118(15) -0.0191(19) 0.0107(18)
C21 0.114(4) 0.043(2) 0.0380(19) -0.0157(16) -0.023(2) 0.022(2)
C22 0.127(4) 0.050(2) 0.043(2) -0.0218(18) -0.044(3) 0.021(2)
C23 0.108(3) 0.0372(19) 0.044(2) -0.0133(16) -0.036(2) 0.004(2)
C24 0.091(3) 0.0249(15) 0.0369(18) -0.0071(13) -0.0262(19) 0.0023(17)
N7 0.074(3) 0.0316(15) 0.0463(17) -0.0121(12) -0.0258(17) -0.0040(15)
N8 0.052(4) 0.051(3) 0.034(3) -0.012(3) 0.000(4) 0.002(3)
O1 0.047(4) 0.062(5) 0.070(4) -0.014(3) 0.010(3) 0.000(3)
O2 0.085(4) 0.083(3) 0.082(4) -0.051(3) -0.014(3) 0.024(3)
O11 0.024(5) 0.176(14) 0.074(7) -0.085(8) 0.013(5) -0.025(5)
N18 0.041(10) 0.080(16) 0.040(7) -0.022(10) 0.004(7) -0.007(6)
O12 0.046(5) 0.130(9) 0.092(7) -0.065(7) 0.025(4) -0.020(5)
N9 0.0475(17) 0.0401(16) 0.0501(17) -0.0159(13) 0.0090(14) -0.0124(13)
O3 0.0501(14) 0.0298(11) 0.0514(13) -0.0153(10) 0.0197(11) -0.0121(10)
O4 0.0568(15) 0.0401(13) 0.0568(15) -0.0089(11) 0.0104(12) -0.0148(12)
N10 0.060(2) 0.058(2) 0.068(2) -0.0179(19) -0.0106(17) -0.0040(17)
C25 0.056(2) 0.048(2) 0.0456(19) -0.0172(17) -0.0120(17) 0.0044(17)
C26 0.100(4) 0.055(2) 0.062(3) -0.008(2) -0.012(2) -0.005(2)
N11 0.0490(18) 0.0540(18) 0.0501(17) -0.0199(14) -0.0062(15) -0.0088(14)
C27 0.0411(18) 0.0399(17) 0.0420(17) -0.0164(14) 0.0006(15) -0.0123(14)
C28 0.044(2) 0.053(2) 0.057(2) -0.0131(17) -0.0095(17) -0.0143(16)
_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 . N1 . 2.152(3) yes
Cu1 . N2 . 2.020(2) yes
Cu1 . N4 . 2.133(2) yes
Cu1 . N6 . 2.014(3) yes
Cu1 . N8 . 2.015(9) yes
Cu1 . O11 . 1.837(10) yes
N1 . C1 . 1.488(4) yes
N1 . C9 . 1.493(3) yes
N1 . C17 . 1.486(4) yes
C1 . C2 . 1.494(4) yes
C1 . H11 . 1.000 no
C1 . H12 . 1.000 no
C2 . N2 . 1.321(4) yes
C2 . N3 . 1.333(4) yes
N2 . C3 . 1.400(4) yes
C3 . C4 . 1.392(4) yes
C3 . C8 . 1.405(4) yes
C4 . C5 . 1.389(5) yes
C4 . H41 . 1.000 no
C5 . C6 . 1.392(5) yes
C5 . H51 . 1.000 no
C6 . C7 . 1.382(5) yes
C6 . H61 . 1.000 no
C7 . C8 . 1.389(4) yes
C7 . H71 . 1.000 no
C8 . N3 . 1.388(4) yes
N3 . H1 . 0.86(4) no
C9 . C10 . 1.488(4) yes
C9 . H91 . 1.000 no
C9 . H92 . 1.000 no
C10 . N4 . 1.324(4) yes
C10 . N5 . 1.351(4) yes
N4 . C11 . 1.395(4) yes
C11 . C12 . 1.394(5) yes
C11 . C16 . 1.419(4) yes
C12 . C13 . 1.391(6) yes
C12 . H121 . 1.000 no
C13 . C14 . 1.400(6) yes
C13 . H131 . 1.000 no
C14 . C15 . 1.383(5) yes
C14 . H141 . 1.000 no
C15 . C16 . 1.383(5) yes
C15 . H151 . 1.000 no
C16 . N5 . 1.388(4) yes
N5 . H2 . 0.88(4) no
C17 . C18 . 1.488(5) yes
C17 . H171 . 1.000 no
C17 . H172 . 1.000 no
C18 . N6 . 1.320(5) yes
C18 . N7 . 1.349(4) yes
N6 . C19 . 1.407(4) yes
C19 . C20 . 1.393(6) yes
C19 . C24 . 1.392(6) yes
C20 . C21 . 1.399(5) yes
C20 . H201 . 1.000 no
C21 . C22 . 1.380(7) yes
C21 . H211 . 1.000 no
C22 . C23 . 1.379(7) yes
C22 . H221 . 1.000 no
C23 . C24 . 1.388(5) yes
C23 . H231 . 1.000 no
C24 . N7 . 1.391(5) yes
N7 . H3 . 0.79(4) no
N8 . O1 . 1.318(9) yes
N8 . O2 . 1.217(8) yes
O11 . N18 . 1.361(17) yes
N18 . O12 . 1.21(2) yes
N9 . O3 . 1.272(3) yes
N9 . O4 . 1.214(4) yes
N10 . C25 . 1.128(5) yes
C25 . C26 . 1.451(6) yes
C26 . H261 . 1.000 no
C26 . H262 . 1.000 no
C26 . H263 . 1.000 no
N11 . C27 . 1.135(4) yes
C27 . C28 . 1.453(5) yes
C28 . H281 . 1.000 no
C28 . H282 . 1.000 no
C28 . H283 . 1.000 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Cu1 . N2 . 80.35(10) yes
N1 . Cu1 . N4 . 80.12(9) yes
N2 . Cu1 . N4 . 109.57(9) yes
N1 . Cu1 . N6 . 81.43(11) yes
N2 . Cu1 . N6 . 140.40(11) yes
N4 . Cu1 . N6 . 101.46(10) yes
N1 . Cu1 . N8 . 175.2(2) yes
N2 . Cu1 . N8 . 94.8(2) yes
N4 . Cu1 . N8 . 101.7(2) yes
N6 . Cu1 . N8 . 102.5(3) yes
N1 . Cu1 . O11 . 162.1(4) yes
N2 . Cu1 . O11 . 100.5(5) yes
N4 . Cu1 . O11 . 115.8(5) yes
N6 . Cu1 . O11 . 87.0(3) yes
Cu1 . N1 . C1 . 105.08(18) yes
Cu1 . N1 . C9 . 107.50(18) yes
C1 . N1 . C9 . 110.9(2) yes
Cu1 . N1 . C17 . 110.9(2) yes
C1 . N1 . C17 . 110.6(2) yes
C9 . N1 . C17 . 111.6(2) yes
N1 . C1 . C2 . 107.0(2) yes
N1 . C1 . H11 . 110.098 no
C2 . C1 . H11 . 110.098 no
N1 . C1 . H12 . 110.098 no
C2 . C1 . H12 . 110.098 no
H11 . C1 . H12 . 109.467 no
C1 . C2 . N2 . 121.6(3) yes
C1 . C2 . N3 . 124.7(3) yes
N2 . C2 . N3 . 113.7(3) yes
Cu1 . N2 . C2 . 111.7(2) yes
Cu1 . N2 . C3 . 142.6(2) yes
C2 . N2 . C3 . 105.3(2) yes
N2 . C3 . C4 . 132.0(3) yes
N2 . C3 . C8 . 108.0(3) yes
C4 . C3 . C8 . 120.0(3) yes
C3 . C4 . C5 . 117.0(3) yes
C3 . C4 . H41 . 121.513 no
C5 . C4 . H41 . 121.513 no
C4 . C5 . C6 . 122.3(3) yes
C4 . C5 . H51 . 118.843 no
C6 . C5 . H51 . 118.843 no
C5 . C6 . C7 . 121.5(3) yes
C5 . C6 . H61 . 119.253 no
C7 . C6 . H61 . 119.253 no
C6 . C7 . C8 . 116.3(3) yes
C6 . C7 . H71 . 121.871 no
C8 . C7 . H71 . 121.871 no
C3 . C8 . C7 . 123.0(3) yes
C3 . C8 . N3 . 106.1(3) yes
C7 . C8 . N3 . 130.9(3) yes
C2 . N3 . C8 . 106.8(3) yes
C2 . N3 . H1 . 125(3) no
C8 . N3 . H1 . 128(3) no
N1 . C9 . C10 . 109.2(2) yes
N1 . C9 . H91 . 109.543 no
C10 . C9 . H91 . 109.543 no
N1 . C9 . H92 . 109.543 no
C10 . C9 . H92 . 109.543 no
H91 . C9 . H92 . 109.467 no
C9 . C10 . N4 . 122.3(2) yes
C9 . C10 . N5 . 124.5(3) yes
N4 . C10 . N5 . 113.1(3) yes
Cu1 . N4 . C10 . 110.64(19) yes
Cu1 . N4 . C11 . 144.1(2) yes
C10 . N4 . C11 . 105.3(2) yes
N4 . C11 . C12 . 130.7(3) yes
N4 . C11 . C16 . 109.2(3) yes
C12 . C11 . C16 . 120.1(3) yes
C11 . C12 . C13 . 116.7(3) yes
C11 . C12 . H121 . 121.666 no
C13 . C12 . H121 . 121.666 no
C12 . C13 . C14 . 122.3(3) yes
C12 . C13 . H131 . 118.844 no
C14 . C13 . H131 . 118.844 no
C13 . C14 . C15 . 121.8(4) yes
C13 . C14 . H141 . 119.112 no
C15 . C14 . H141 . 119.112 no
C14 . C15 . C16 . 116.2(3) yes
C14 . C15 . H151 . 121.921 no
C16 . C15 . H151 . 121.921 no
C11 . C16 . C15 . 123.0(3) yes
C11 . C16 . N5 . 104.7(3) yes
C15 . C16 . N5 . 132.3(3) yes
C10 . N5 . C16 . 107.7(3) yes
C10 . N5 . H2 . 126(2) no
C16 . N5 . H2 . 126(2) no
N1 . C17 . C18 . 108.3(3) yes
N1 . C17 . H171 . 109.767 no
C18 . C17 . H171 . 109.767 no
N1 . C17 . H172 . 109.767 no
C18 . C17 . H172 . 109.767 no
H171 . C17 . H172 . 109.467 no
C17 . C18 . N6 . 122.9(3) yes
C17 . C18 . N7 . 123.5(4) yes
N6 . C18 . N7 . 113.4(3) yes
Cu1 . N6 . C18 . 113.8(2) yes
Cu1 . N6 . C19 . 140.7(3) yes
C18 . N6 . C19 . 105.0(3) yes
N6 . C19 . C20 . 130.1(4) yes
N6 . C19 . C24 . 108.8(3) yes
C20 . C19 . C24 . 121.0(3) yes
C19 . C20 . C21 . 115.9(4) yes
C19 . C20 . H201 . 122.051 no
C21 . C20 . H201 . 122.051 no
C20 . C21 . C22 . 122.4(4) yes
C20 . C21 . H211 . 118.786 no
C22 . C21 . H211 . 118.786 no
C21 . C22 . C23 . 121.8(3) yes
C21 . C22 . H221 . 119.102 no
C23 . C22 . H221 . 119.103 no
C22 . C23 . C24 . 116.3(4) yes
C22 . C23 . H231 . 121.848 no
C24 . C23 . H231 . 121.848 no
C19 . C24 . C23 . 122.5(4) yes
C19 . C24 . N7 . 106.1(3) yes
C23 . C24 . N7 . 131.4(4) yes
C18 . N7 . C24 . 106.7(4) yes
C18 . N7 . H3 . 129(3) no
C24 . N7 . H3 . 124(3) no
Cu1 . N8 . O1 . 124.1(6) yes
Cu1 . N8 . O2 . 122.5(8) yes
O1 . N8 . O2 . 112.9(9) yes
Cu1 . O11 . N18 . 109.5(11) yes
O11 . N18 . O12 . 117.1(15) yes
O3 . N9 . O4 . 115.3(3) yes
N10 . C25 . C26 . 177.9(5) yes
C25 . C26 . H261 . 109.467 no
C25 . C26 . H262 . 109.467 no
H261 . C26 . H262 . 109.476 no
C25 . C26 . H263 . 109.466 no
H261 . C26 . H263 . 109.476 no
H262 . C26 . H263 . 109.476 no
N11 . C27 . C28 . 178.5(4) yes
C27 . C28 . H281 . 109.467 no
C27 . C28 . H282 . 109.467 no
H281 . C28 . H282 . 109.476 no
C27 . C28 . H283 . 109.467 no
H281 . C28 . H283 . 109.476 no
H282 . C28 . H283 . 109.476 no

loop_
_geom_hbond_atom_site_label_d
_geom_hbond_atom_site_label_h
_geom_hbond_atom_site_label_a
_geom_hbond_site_symmetry_a
_geom_hbond_distance_dh
_geom_hbond_distance_ha
_geom_hbond_distance_da
_geom_hbond_angle_dha
_geom_hbond_publ_flag
N3 H1 O3 2_665 0.86(4) 1.83(4) 2.688(3) 174(4) yes
N5 H2 O3 . 0.88(4) 1.88(4) 2.747(3) 170(3) yes
N7 H3 O1 1_655 0.79(4) 2.37(4) 3.112(9) 158(4) yes
N7 H3 O12 1_655 0.79(4) 1.79(5) 2.561(9) 164(5) yes

#===END