# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

#------------------ AUDIT DETAILS -------------------------------------------#

_audit_creation_date             2003-06-17
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record             ?

_publ_contact_author_name        'Dr Nicolas Mercier'
_publ_contact_author_address     
;
Laboratoire Ingenierie Moleculaire Materiaux Organiques
UMR CNRS 6501, Faculte des Sciences, 2 Bd Lavoisier, F-49045 Angers, France
;
_publ_contact_author_email       nicolas.mercier@univ-angers.fr
_publ_contact_author_fax         (33)2.41.73.54.05
_publ_contact_author_phone       (33)2.41.73.50.83

_publ_section_title              
;
An Organic-Inorganic Hybrid Perovskite Containing
Copper Paddle-Wheel Clusters Linking Perovskite Layers :
[Cu(O2C-(CH2)3-NH3)2]PbBr4
;

_publ_section_references         
;
Allen, F.H., Kennard, O. & Taylor, R. (1983).
Acc. Chem. Res.  16, 146-153.

Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A.
(1993) J. Appl. Cryst. 26, 343-350.

Altomare, A. Burla, M. C., Camalli, M., Cascarano, G. L.,
Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G.
& Spagna, R. (1999) J. Appl. Cryst. 32, 115-119.

Blessing, R. H. (1995) Acta Cryst., A51, 33-38.

Blessing, R. H. (1987) Cryst. Rev. 1, 3-58.

Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397.

Beurskens, P.T., Beurskens, G., de Gelder, R.,
Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M.
(1999) The DIRDIF-99 program system,
Technical Report of the Crystallography Laboratory,
University of Nijmegen, The Netherlands.

Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358.

Enraf-Nonius (1994). CAD4Express Software. Enraf-Nonius, Delft,
The Netherlands.

Farrugia, L. J. (1997) ORTEP-3 for Windows, J. Appl. Cryst. 30, 565.

Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838.

Flack, H.D. (1983). Acta Cryst. A39, 876-881.

Harms, K. & Wocadlo, S. (1995) XCAD-4. Program for Processing CAD-4
Diffractometer Data. University of Marburg, Germany.

Johnson, C.K. (1965). ORTEP. Report ORNL-3794. Oak Ridge National
Laboratory, Tennessee, USA.

Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580

LePage, Y. (1987). J. Appl. Cryst. 20, 264-269.

North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst,
A24, 351-359

Orpen, A. G., Brammer, L., Allen, F. H., Kennard, O., Watson, D. G.,
& Taylor, R. (1992). International Tables for Crystallography,
Volume C.

Sheldrick, G.M. (1993) SHELXL93. Program for crystal structure
refinement. University of Gottingen, Germany.

Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure
refinement. University of Gottingen, Germany.

Sheldrick, G.M. (1985). SHELXS86. In Crystallographic Computing 3,
edited by G. M. Sheldrick, C. Kruger & R. Goddard, pp. 175-189.
Oxford University Press.

Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution.
University of G\"ottingen, Germany.

Spek, A.L. (1990). Acta Cryst. A46, C34

Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr.
34, 824-828

Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr.
35, 281.

Walker, N. &  Stuart, D. (1983). Acta Cryst., A39, 158 - 166.

Wilson, A.J.C. (1992) Ed. International Tables for Crystallography,
Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands.
;
_publ_section_figure_captions    
;
Figure 1. View of (I) (50% probability displacement ellipsoids)
;
_publ_section_acknowledgements   
;
?
;
_publ_section_table_legends      
;
Table 1. Fractional atomic coordinates and equivalent
isotropic displacement parameters (\%A^2^)

Table 2. Selected geometric parameters (\%A ,\% )
;
loop_
_publ_author_name
'Nicolas Mercier'
'Amedee Riou'

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

data_per61
_database_code_depnum_ccdc_archive 'CCDC 215378'

_audit_creation_date             2003-06-17T11:12:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_sum            'C8 H18 Br4 Cu N2 O4 Pb'
_chemical_formula_weight         796.6

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'

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

_cell_length_a                   8.4581(5)
_cell_length_b                   8.3703(4)
_cell_length_c                   26.9075(19)
_cell_angle_alpha                90
_cell_angle_beta                 98.620(10)
_cell_angle_gamma                90
_cell_volume                     1883.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      4.8
_cell_measurement_theta_max      26

#------------------ CRYSTAL INFORMATION -------------------------------------#
_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    2.809
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1452
_exptl_absorpt_coefficient_mu    18.552
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.098
_exptl_absorpt_correction_T_max  0.492

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

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Oscillation Phi Incr 0.9 deg'
_diffrn_detector_area_resol_mean 6.66
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?

_diffrn_reflns_number            14122
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         25.77
_diffrn_reflns_theta_full        25.77
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_reflns_number_total             3572
_reflns_number_gt                2554
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       'EXPOSE, STOE IPDS'
_computing_cell_refinement       'CELL, STOE IPDS'
_computing_data_reduction        'INTEGRATE, STOE IPDS'
_computing_structure_solution    'Direct methods(SIR92,Altomare et al.,1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND 2.1e (Crystal impact GbR 2001)'
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w==1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3572
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0685
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_restrained_S_all      0.892
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         2.367
_refine_diff_density_min         -1.604

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.29 2.46 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.32 1.265 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.394 10.111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
O3 O 0.1919(5) 0.5453(7) 0.06350(19) 0.0403(14) Uani 1 d . . A
O2 O -0.1232(6) 0.6581(7) 0.0459(2) 0.0372(13) Uani 1 d . . A
O1 O 0.2285(5) 0.6363(7) -0.0113(2) 0.0384(13) Uani 1 d . . .
O4 O 0.0810(6) 0.2492(7) 0.0284(2) 0.0413(13) Uani 1 d . . .
C5 C 0.2754(7) 0.6087(9) 0.0335(3) 0.0290(16) Uani 1 d . . .
C4 C -0.1291(7) 0.7655(9) 0.0131(3) 0.0291(16) Uani 1 d . . .
C2 C -0.1804(8) 0.9616(10) 0.0808(3) 0.043(2) Uani 1 d . . .
H2A H -0.2237 1.0672 0.0851 0.051 Uiso 1 calc R . .
H2B H -0.2431 0.8853 0.0967 0.051 Uiso 1 calc R . .
C3 C -0.1965(8) 0.9244(10) 0.0256(3) 0.0343(18) Uani 1 d . . .
H1A H -0.1432 1.0077 0.0093 0.041 Uiso 1 calc R . .
H1B H -0.309 0.9273 0.0115 0.041 Uiso 1 calc R . .
C1 C -0.0109(9) 0.9560(12) 0.1062(3) 0.048(2) Uani 1 d . . .
H3A H 0.0288 0.8477 0.1046 0.057 Uiso 1 calc R . .
H3B H 0.0535 1.0242 0.088 0.057 Uiso 1 calc R . .
N1 N 0.0097(9) 1.0069(10) 0.1590(3) 0.0543(19) Uani 1 d . . .
H1C H 0.1126 1.0009 0.1721 0.081 Uiso 1 calc R . .
H1D H -0.047 0.9434 0.1761 0.081 Uiso 1 calc R . .
H1E H -0.024 1.1071 0.1608 0.081 Uiso 1 calc R . .
C6 C 0.4440(8) 0.6582(11) 0.0548(3) 0.045(2) Uani 1 d . 1 A
H11A H 0.4396 0.7624 0.0703 0.054 Uiso 1 calc R 1 A
H11B H 0.5047 0.6695 0.0272 0.054 Uiso 1 calc R 1 A
C7 C 0.5339(10) 0.546(2) 0.0931(5) 0.106(6) Uani 1 d . 1 A
H7A1 H 0.5221 0.4406 0.078 0.127 Uiso 1 calc R 1 A
H7A2 H 0.6459 0.574 0.0948 0.127 Uiso 1 calc R 1 A
C8 C 0.5109(10) 0.526(2) 0.1411(4) 0.096(5) Uani 1 d . 1 A
H15A H 0.511 0.6309 0.1562 0.115 Uiso 1 calc R 1 A
H15B H 0.6036 0.4695 0.1583 0.115 Uiso 1 calc R 1 A
N2 N 0.3690(7) 0.4418(10) 0.1527(3) 0.0449(18) Uani 1 d . . .
H2C H 0.3705 0.4397 0.1858 0.067 Uiso 1 calc R 1 A
H2D H 0.3687 0.3422 0.1411 0.067 Uiso 1 calc R 1 A
H2E H 0.2815 0.4924 0.1382 0.067 Uiso 1 calc R 1 A
Pb Pb -0.00882(3) 0.49567(4) 0.252250(10) 0.02755(9) Uani 1 d . . .
Br3 Br 0.26416(8) 0.72011(10) 0.23712(3) 0.0413(2) Uani 1 d . . .
Br2 Br 0.07458(10) 0.54325(12) 0.35862(3) 0.0492(2) Uani 1 d . . .
Br1 Br -0.20682(9) 0.79233(12) 0.23597(4) 0.0533(2) Uani 1 d . . .
Cu Cu -0.02255(8) 0.44786(11) 0.04489(3) 0.0251(2) Uani 1 d . . .
Br4 Br -0.04860(8) 0.39437(10) 0.14014(3) 0.03653(19) Uani 1 d . . A

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
O3 0.031(2) 0.059(4) 0.030(3) 0.002(3) -0.001(2) -0.015(2)
O2 0.046(3) 0.030(4) 0.038(3) 0.003(3) 0.012(2) 0.001(2)
O1 0.037(2) 0.042(4) 0.033(3) 0.001(3) -0.004(2) -0.013(2)
O4 0.056(3) 0.034(4) 0.036(3) 0.006(3) 0.013(2) 0.011(2)
C5 0.029(3) 0.025(4) 0.033(4) -0.003(3) 0.004(3) -0.002(3)
C4 0.022(3) 0.026(5) 0.038(4) 0.000(4) 0.001(3) -0.005(3)
C2 0.038(4) 0.033(5) 0.058(6) -0.008(4) 0.009(4) 0.002(3)
C3 0.030(3) 0.028(5) 0.044(5) 0.002(4) 0.003(3) 0.004(3)
C1 0.046(4) 0.041(6) 0.053(5) -0.009(4) -0.001(4) -0.002(3)
N1 0.074(5) 0.045(5) 0.040(4) -0.004(4) -0.002(3) -0.010(4)
C6 0.026(3) 0.052(6) 0.056(6) 0.001(5) 0.003(3) -0.018(3)
C7 0.033(4) 0.180(16) 0.097(10) 0.065(10) -0.018(5) -0.028(6)
C8 0.035(4) 0.178(16) 0.075(8) 0.039(9) 0.012(5) -0.014(6)
N2 0.037(3) 0.063(5) 0.033(4) 0.006(3) 0.004(3) -0.001(3)
Pb 0.02393(11) 0.02514(16) 0.03332(14) -0.00097(13) 0.00346(8) -0.00059(10)
Br3 0.0373(4) 0.0364(5) 0.0503(5) -0.0012(4) 0.0068(3) -0.0131(3)
Br2 0.0566(5) 0.0560(7) 0.0343(5) 0.0011(4) 0.0045(4) -0.0069(4)
Br1 0.0447(4) 0.0469(6) 0.0691(6) 0.0017(5) 0.0107(4) 0.0228(4)
Cu 0.0250(4) 0.0249(5) 0.0245(5) 0.0013(4) 0.0003(3) -0.0025(3)
Br4 0.0402(4) 0.0447(5) 0.0246(4) 0.0037(3) 0.0045(3) 0.0020(3)

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

_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
O3 C5 1.266(8) . ?
O3 Cu 1.983(5) . ?
O2 C4 1.256(9) . ?
O2 Cu 1.957(5) . ?
O1 C5 1.234(9) . ?
O1 Cu 1.969(5) 3_565 ?
O4 C4 1.252(9) 3_565 ?
O4 Cu 1.961(5) . ?
C5 C6 1.512(9) . ?
C4 O4 1.252(9) 3_565 ?
C4 C3 1.504(10) . ?
C2 C1 1.494(10) . ?
C2 C3 1.503(11) . ?
C1 N1 1.468(11) . ?
C6 C7 1.513(14) . ?
C7 C8 1.345(15) . ?
C8 N2 1.464(11) . ?
Pb Br2 2.8711(9) . ?
Pb Br1 2.9904(9) . ?
Pb Br1 3.0018(8) 2_445 ?
Pb Br3 3.0509(7) . ?
Pb Br3 3.0833(8) 2_545 ?
Pb Br4 3.1029(8) . ?
Br3 Pb 3.0833(8) 2 ?
Br1 Pb 3.0018(8) 2_455 ?
Cu O1 1.969(5) 3_565 ?
Cu Br4 2.6431(11) . ?
Cu Cu 2.6496(16) 3_565 ?

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
C5 O3 Cu 126.0(5) . . ?
C4 O2 Cu 127.3(5) . . ?
C5 O1 Cu 121.0(4) . 3_565 ?
C4 O4 Cu 120.1(5) 3_565 . ?
O1 C5 O3 124.9(6) . . ?
O1 C5 C6 117.8(6) . . ?
O3 C5 C6 117.3(7) . . ?
O4 C4 O2 125.0(7) 3_565 . ?
O4 C4 C3 118.1(7) 3_565 . ?
O2 C4 C3 117.0(6) . . ?
C1 C2 C3 112.6(6) . . ?
C2 C3 C4 114.9(7) . . ?
N1 C1 C2 113.6(7) . . ?
C5 C6 C7 115.9(7) . . ?
C8 C7 C6 127.0(13) . . ?
C7 C8 N2 120.4(10) . . ?
Br2 Pb Br1 94.55(3) . . ?
Br2 Pb Br1 93.12(3) . 2_445 ?
Br1 Pb Br1 92.655(10) . 2_445 ?
Br2 Pb Br3 88.27(3) . . ?
Br1 Pb Br3 83.54(3) . . ?
Br1 Pb Br3 176.05(3) 2_445 . ?
Br2 Pb Br3 87.14(3) . 2_545 ?
Br1 Pb Br3 171.15(3) . 2_545 ?
Br1 Pb Br3 95.93(3) 2_445 2_545 ?
Br3 Pb Br3 87.832(8) . 2_545 ?
Br2 Pb Br4 169.03(3) . . ?
Br1 Pb Br4 96.18(3) . . ?
Br1 Pb Br4 88.62(3) 2_445 . ?
Br3 Pb Br4 90.72(2) . . ?
Br3 Pb Br4 81.91(2) 2_545 . ?
Pb Br3 Pb 163.56(3) . 2 ?
Pb Br1 Pb 153.55(4) . 2_455 ?
O2 Cu O4 167.4(2) . . ?
O2 Cu O1 88.4(2) . 3_565 ?
O4 Cu O1 89.3(2) . 3_565 ?
O2 Cu O3 90.6(2) . . ?
O4 Cu O3 89.0(2) . . ?
O1 Cu O3 167.4(2) 3_565 . ?
O2 Cu Br4 92.22(15) . . ?
O4 Cu Br4 100.40(16) . . ?
O1 Cu Br4 100.82(15) 3_565 . ?
O3 Cu Br4 91.77(15) . . ?
O2 Cu Cu 80.75(15) . 3_565 ?
O4 Cu Cu 86.73(16) . 3_565 ?
O1 Cu Cu 86.44(16) 3_565 3_565 ?
O3 Cu Cu 81.00(15) . 3_565 ?
Br4 Cu Cu 169.81(6) . 3_565 ?
Cu Br4 Pb 152.09(4) . . ?

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
N1 H1C Br2 2 0.89 2.91 3.631(8) 139.3
N1 H1D Br1 . 0.89 2.58 3.465(8) 171.4
N1 H1E Br4 1_565 0.89 2.47 3.308(9) 157.3
N2 H2C Br3 . 0.89 2.93 3.461(8) 119.8
N2 H2D Br2 2_545 0.89 2.55 3.390(8) 158.1
N2 H2E O3 . 0.89 2.09 2.771(9) 132.9
N2 H2E Br4 . 0.89 2.92 3.520(6) 126.4

data_per70
_database_code_depnum_ccdc_archive 'CCDC 229739'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H36 Br4 Cu2 N4 O8'
_chemical_formula_sum            'C16 H36 Br4 Cu2 N4 O8'
_chemical_formula_weight         859.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Br Br -0.2900 2.4600 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.577(5)
_cell_length_b                   8.972(6)
_cell_length_c                   10.503(3)
_cell_angle_alpha                100.60(4)
_cell_angle_beta                 105.73(3)
_cell_angle_gamma                111.38(4)
_cell_volume                     687.4(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             422
_exptl_absorpt_coefficient_mu    7.405
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_correction_T_min  0.5602
_exptl_absorpt_correction_T_max  0.8651
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  120
_diffrn_standards_decay_%        1
_diffrn_reflns_number            1790
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         21.98
_reflns_number_total             1664
_reflns_number_gt                1366
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w==1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1664
_refine_ls_number_parameters     156
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0875
_refine_ls_wR_factor_gt          0.0814
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7802(8) 0.2783(7) 0.6224(6) 0.0229(14) Uani 1 1 d . . .
C5 C 0.3804(7) 0.0333(7) 0.6957(6) 0.0210(13) Uani 1 1 d . . .
C2 C 0.9636(7) 0.4268(7) 0.6801(6) 0.0244(14) Uani 1 1 d . . .
H2A H 0.9998 0.4736 0.7800 0.029 Uiso 1 1 calc R . .
H2B H 0.9580 0.5138 0.6387 0.029 Uiso 1 1 calc R . .
C6 C 0.3009(8) 0.0536(7) 0.8061(6) 0.0261(14) Uani 1 1 d . . .
H6A H 0.1913 0.0646 0.7656 0.031 Uiso 1 1 calc R . .
H6B H 0.3850 0.1578 0.8807 0.031 Uiso 1 1 calc R . .
C4 C 1.2852(7) 0.5163(7) 0.6979(7) 0.0262(14) Uani 1 1 d . . .
H4A H 1.2778 0.6022 0.6556 0.031 Uiso 1 1 calc R . .
H4B H 1.3290 0.5664 0.7982 0.031 Uiso 1 1 calc R . .
C3 C 1.1014(8) 0.3732(7) 0.6492(7) 0.0299(15) Uani 1 1 d . . .
H3A H 1.1091 0.2893 0.6939 0.036 Uiso 1 1 calc R . .
H3B H 1.0604 0.3208 0.5494 0.036 Uiso 1 1 calc R . .
C8 C 0.2039(8) -0.0418(7) 0.9905(6) 0.0265(14) Uani 1 1 d . . .
H8A H 0.3085 0.0499 1.0653 0.032 Uiso 1 1 calc R . .
H8B H 0.1137 -0.0011 0.9620 0.032 Uiso 1 1 calc R . .
N2 N 0.1307(7) -0.1845(6) 1.0442(5) 0.0328(13) Uani 1 1 d . . .
H2C H 0.0154 -0.2498 0.9907 0.049 Uiso 1 1 calc R . .
H2D H 0.1399 -0.1440 1.1313 0.049 Uiso 1 1 calc R . .
H2E H 0.1931 -0.2448 1.0427 0.049 Uiso 1 1 calc R . .
N1 N 1.4135(7) 0.4597(6) 0.6614(6) 0.0363(13) Uani 1 1 d . . .
H1A H 1.4384 0.3980 0.7139 0.054 Uiso 1 1 calc R . .
H1B H 1.5145 0.5492 0.6764 0.054 Uiso 1 1 calc R . .
H1C H 1.3648 0.3979 0.5719 0.054 Uiso 1 1 calc R . .
C7 C 0.2571(8) -0.0894(7) 0.8685(6) 0.0219(13) Uani 1 1 d . . .
H7A H 0.1590 -0.1912 0.7984 0.026 Uiso 1 1 calc R . .
H7B H 0.3614 -0.1114 0.8996 0.026 Uiso 1 1 calc R . .
Br1 Br 0.22245(8) 0.21397(7) 0.31505(6) 0.0289(2) Uani 1 1 d . . .
Cu1 Cu 0.42058(8) 0.08360(8) 0.43825(7) 0.0180(2) Uani 1 1 d . . .
Br2 Br -0.27405(9) 0.48004(9) -0.05530(7) 0.0425(3) Uani 1 1 d . . .
O2 O 0.3485(5) 0.0993(5) 0.6024(4) 0.0272(10) Uani 1 1 d . . .
O3 O 0.6478(5) 0.2881(5) 0.5440(4) 0.0263(10) Uani 1 1 d . . .
O4 O 0.5258(5) 0.0477(5) 0.2962(4) 0.0263(10) Uani 1 1 d . . .
O1 O 0.2270(5) -0.1472(5) 0.3458(4) 0.0272(10) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.021(4) 0.021(3) 0.025(3) 0.004(3) 0.013(3) 0.006(3)
C5 0.018(3) 0.018(3) 0.021(3) 0.002(3) 0.008(3) 0.003(3)
C2 0.021(3) 0.021(3) 0.029(3) 0.007(3) 0.011(3) 0.006(3)
C6 0.032(4) 0.029(4) 0.030(4) 0.013(3) 0.022(3) 0.017(3)
C4 0.022(3) 0.023(3) 0.038(4) 0.012(3) 0.018(3) 0.010(3)
C3 0.026(4) 0.021(3) 0.042(4) 0.007(3) 0.016(3) 0.009(3)
C8 0.028(4) 0.025(3) 0.031(4) 0.016(3) 0.017(3) 0.009(3)
N2 0.032(3) 0.041(3) 0.035(3) 0.020(3) 0.022(3) 0.015(3)
N1 0.028(3) 0.023(3) 0.052(4) 0.008(3) 0.018(3) 0.005(2)
C7 0.021(3) 0.023(3) 0.028(3) 0.011(3) 0.014(3) 0.011(3)
Br1 0.0240(4) 0.0289(4) 0.0371(4) 0.0139(3) 0.0097(3) 0.0145(3)
Cu1 0.0157(4) 0.0166(4) 0.0237(4) 0.0083(3) 0.0106(3) 0.0060(3)
Br2 0.0324(4) 0.0484(5) 0.0453(5) 0.0202(4) 0.0132(3) 0.0145(3)
O2 0.029(2) 0.035(2) 0.029(2) 0.017(2) 0.019(2) 0.018(2)
O3 0.016(2) 0.022(2) 0.033(2) 0.009(2) 0.0068(19) 0.0017(18)
O4 0.031(2) 0.032(2) 0.032(2) 0.018(2) 0.023(2) 0.019(2)
O1 0.024(2) 0.017(2) 0.035(2) 0.010(2) 0.0095(19) 0.0032(18)

_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
C1 O3 1.253(7) . ?
C1 O1 1.265(7) 2_656 ?
C1 C2 1.508(8) . ?
C5 O2 1.254(7) . ?
C5 O4 1.262(7) 2_656 ?
C5 C6 1.511(8) . ?
C2 C3 1.516(8) . ?
C6 C7 1.519(8) . ?
C4 N1 1.476(7) . ?
C4 C3 1.497(8) . ?
C8 N2 1.491(7) . ?
C8 C7 1.513(8) . ?
Br1 Cu1 2.5969(15) . ?
Cu1 O3 1.967(4) . ?
Cu1 O1 1.967(4) . ?
Cu1 O4 1.977(4) . ?
Cu1 O2 1.981(4) . ?
Cu1 Cu1 2.6527(18) 2_656 ?
O4 C5 1.262(7) 2_656 ?
O1 C1 1.265(7) 2_656 ?

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 C1 O1 124.1(5) . 2_656 ?
O3 C1 C2 119.7(5) . . ?
O1 C1 C2 116.1(5) 2_656 . ?
O2 C5 O4 124.7(5) . 2_656 ?
O2 C5 C6 117.1(5) . . ?
O4 C5 C6 118.2(5) 2_656 . ?
C1 C2 C3 110.5(5) . . ?
C5 C6 C7 115.3(5) . . ?
N1 C4 C3 111.6(5) . . ?
C4 C3 C2 113.4(5) . . ?
N2 C8 C7 113.3(5) . . ?
C8 C7 C6 109.6(5) . . ?
O3 Cu1 O1 167.01(17) . . ?
O3 Cu1 O4 86.73(17) . . ?
O1 Cu1 O4 89.37(17) . . ?
O3 Cu1 O2 90.78(17) . . ?
O1 Cu1 O2 90.37(17) . . ?
O4 Cu1 O2 167.54(16) . . ?
O3 Cu1 Br1 100.18(14) . . ?
O1 Cu1 Br1 92.62(13) . . ?
O4 Cu1 Br1 97.73(12) . . ?
O2 Cu1 Br1 94.73(12) . . ?
O3 Cu1 Cu1 87.04(14) . 2_656 ?
O1 Cu1 Cu1 80.35(13) . 2_656 ?
O4 Cu1 Cu1 86.40(12) . 2_656 ?
O2 Cu1 Cu1 81.28(12) . 2_656 ?
Br1 Cu1 Cu1 171.84(4) . 2_656 ?
C5 O2 Cu1 126.8(4) . . ?
C1 O3 Cu1 120.0(4) . . ?
C5 O4 Cu1 120.8(4) 2_656 . ?
C1 O1 Cu1 127.3(4) 2_656 . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        21.98
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.142