# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Jian-Ping Lang'
_publ_contact_author_email       JPLANG@SUDA.EDU.CN

_publ_section_title              
;
Solvothermal assembly of a mixed-valence Cu(I,II)
cyanide coordination polymer [Cu(II)Cu(I)2(?-Br)2(?-CN)2(bdmpp)]n
by C-C bond cleavage of acetonitrile
;
loop_
_publ_author_name
'Jian-Ping Lang'
'Hong-Xi Li'
'Ling-Ling Li'
'Lei-Lei Liu'
'Zhi-Gang Ren'
'Yong Zhang'

# Attachment 'JPLangCIF__revised_.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 714394'

#==============================================================================
# CHEMICAL DATA

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H17 Br2 Cu3 N7'
_chemical_formula_sum            'C17 H17 Br2 Cu3 N7'
_chemical_formula_weight         669.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   8.9718(18)
_cell_length_b                   11.025(2)
_cell_length_c                   11.152(2)
_cell_angle_alpha                93.22(3)
_cell_angle_beta                 102.11(3)
_cell_angle_gamma                96.21(3)
_cell_volume                     1068.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3486
_cell_measurement_theta_min      3.1680
_cell_measurement_theta_max      25.3491

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             650
_exptl_absorpt_coefficient_mu    6.715
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.1793
_exptl_absorpt_correction_T_max  0.2153
_exptl_absorpt_process_details   
'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(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  'Rigaku MercuryCCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            10373
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         25.34
_reflns_number_total             3878
_reflns_number_gt                2733
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0934P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3878
_refine_ls_number_parameters     266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0629
_refine_ls_wR_factor_ref         0.1749
_refine_ls_wR_factor_gt          0.1524
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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
Cu1 Cu 0.20850(10) 0.72589(9) 0.64183(8) 0.0365(3) Uani 1 1 d . . .
Cu2 Cu -0.32258(13) 0.52735(12) 0.58062(15) 0.0717(5) Uani 1 1 d . . .
Cu3 Cu 0.22322(12) 0.98038(11) 0.90614(10) 0.0548(4) Uani 1 1 d . . .
Br1 Br 0.14587(10) 0.95766(8) 0.68173(8) 0.0478(3) Uani 1 1 d . . .
Br2 Br -0.53838(10) 0.45369(9) 0.65244(8) 0.0517(3) Uani 1 1 d . . .
N1 N 0.4263(7) 0.7707(6) 0.6450(5) 0.0335(14) Uani 1 1 d . . .
N2 N 0.4631(8) 0.7224(7) 0.8411(6) 0.0471(18) Uani 1 1 d . . .
N3 N 0.3039(8) 0.7024(6) 0.8183(6) 0.0412(16) Uani 1 1 d . . .
N4 N 0.3424(8) 0.7979(6) 0.4437(6) 0.0401(16) Uani 1 1 d . . .
N5 N 0.2014(7) 0.7513(6) 0.4625(6) 0.0415(16) Uani 1 1 d . . .
N6 N 0.0084(8) 0.6320(7) 0.6286(6) 0.0460(18) Uani 1 1 d . . .
C1 C 0.4675(9) 0.8083(7) 0.5447(8) 0.0405(19) Uani 1 1 d . . .
C2 C 0.6179(10) 0.8520(8) 0.5470(9) 0.055(3) Uani 1 1 d . . .
H2 H 0.6479 0.8775 0.4766 0.066 Uiso 1 1 calc R . .
C3 C 0.7212(11) 0.8565(9) 0.6565(11) 0.064(3) Uani 1 1 d . . .
H3 H 0.8228 0.8880 0.6607 0.077 Uiso 1 1 calc R . .
C4 C 0.6803(10) 0.8159(10) 0.7608(10) 0.064(3) Uani 1 1 d . . .
H4 H 0.7513 0.8188 0.8351 0.076 Uiso 1 1 calc R . .
C5 C 0.5288(9) 0.7710(8) 0.7491(8) 0.042(2) Uani 1 1 d . . .
C6 C 0.5231(13) 0.6874(9) 0.9567(9) 0.063(3) Uani 1 1 d . . .
C7 C 0.4012(14) 0.6467(9) 1.0060(9) 0.073(3) Uani 1 1 d . . .
H7 H 0.4060 0.6165 1.0827 0.088 Uiso 1 1 calc R . .
C8 C 0.2687(11) 0.6594(8) 0.9191(8) 0.051(2) Uani 1 1 d . . .
C9 C 0.6900(13) 0.6907(11) 1.0103(11) 0.092(4) Uani 1 1 d . . .
H9A H 0.7356 0.6422 0.9568 0.138 Uiso 1 1 calc R . .
H9B H 0.7039 0.6582 1.0895 0.138 Uiso 1 1 calc R . .
H9C H 0.7384 0.7737 1.0193 0.138 Uiso 1 1 calc R . .
C10 C 0.1053(14) 0.6285(11) 0.9274(10) 0.080(3) Uani 1 1 d . . .
H10A H 0.0413 0.6745 0.8716 0.120 Uiso 1 1 calc R . .
H10B H 0.0951 0.6487 1.0099 0.120 Uiso 1 1 calc R . .
H10C H 0.0745 0.5426 0.9059 0.120 Uiso 1 1 calc R . .
C11 C 0.3250(12) 0.8277(8) 0.3224(8) 0.048(2) Uani 1 1 d . . .
C12 C 0.1756(12) 0.8013(8) 0.2707(8) 0.059(3) Uani 1 1 d . . .
H12 H 0.1299 0.8120 0.1897 0.070 Uiso 1 1 calc R . .
C13 C 0.1006(10) 0.7553(7) 0.3576(7) 0.043(2) Uani 1 1 d . . .
C14 C 0.4587(14) 0.8757(10) 0.2699(9) 0.073(3) Uani 1 1 d . . .
H14A H 0.4235 0.8868 0.1843 0.110 Uiso 1 1 calc R . .
H14B H 0.5327 0.8183 0.2788 0.110 Uiso 1 1 calc R . .
H14C H 0.5054 0.9527 0.3131 0.110 Uiso 1 1 calc R . .
C15 C -0.0681(11) 0.7135(10) 0.3457(9) 0.067(3) Uani 1 1 d . . .
H15A H -0.0802 0.6344 0.3769 0.100 Uiso 1 1 calc R . .
H15B H -0.1199 0.7083 0.2607 0.100 Uiso 1 1 calc R . .
H15C H -0.1114 0.7710 0.3920 0.100 Uiso 1 1 calc R . .
C16 C -0.1151(10) 0.5865(8) 0.6152(8) 0.049(2) Uani 1 1 d . . .
N7' N 0.4353(8) 0.9951(8) 0.9767(7) 0.048(2) Uani 0.50 1 d P . .
C7' C 0.4353(8) 0.9951(8) 0.9767(7) 0.048(2) Uani 0.50 1 d P . .
N8' N 0.0388(8) 0.9957(13) 0.9877(11) 0.052(3) Uani 0.50 1 d P . .
C8' C 0.0388(8) 0.9957(13) 0.9877(11) 0.052(3) Uani 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N6 1.946(7) . ?
Cu1 N1 1.955(6) . ?
Cu1 N3 2.018(6) . ?
Cu1 N5 2.023(6) . ?
Cu1 Br1 2.7076(15) . ?
Cu2 C16 1.857(9) . ?
Cu2 Br2 2.3310(16) . ?
Cu2 Br2 2.667(2) 2_466 ?
Cu3 N7 1.886(8) . ?
Cu3 N8 2.066(9) . ?
Cu3 Br1 2.4434(15) . ?
Br2 Cu2 2.667(2) 2_466 ?
N1 C5 1.321(10) . ?
N1 C1 1.324(10) . ?
N2 C6 1.382(12) . ?
N2 N3 1.388(9) . ?
N2 C5 1.390(11) . ?
N3 C8 1.328(10) . ?
N4 N5 1.375(9) . ?
N4 C11 1.391(10) . ?
N4 C1 1.403(10) . ?
N5 C13 1.327(10) . ?
N6 C16 1.142(10) . ?
C1 C2 1.378(11) . ?
C2 C3 1.364(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.375(14) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(12) . ?
C4 H4 0.9300 . ?
C6 C7 1.368(16) . ?
C6 C9 1.488(14) . ?
C7 C8 1.393(13) . ?
C7 H7 0.9300 . ?
C8 C10 1.491(14) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.336(13) . ?
C11 C14 1.501(13) . ?
C12 C13 1.379(12) . ?
C12 H12 0.9300 . ?
C13 C15 1.510(12) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N7' C7' 1.159(15) 2_677 ?
N7' N7' 1.159(15) 2_677 ?
N8' C8' 0.813(16) 2_577 ?
N8' N8' 0.813(16) 2_577 ?

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
N6 Cu1 N1 162.6(3) . . ?
N6 Cu1 N3 99.3(3) . . ?
N1 Cu1 N3 79.0(3) . . ?
N6 Cu1 N5 100.3(3) . . ?
N1 Cu1 N5 78.9(3) . . ?
N3 Cu1 N5 157.2(3) . . ?
N6 Cu1 Br1 101.7(2) . . ?
N1 Cu1 Br1 95.68(19) . . ?
N3 Cu1 Br1 96.7(2) . . ?
N5 Cu1 Br1 90.6(2) . . ?
C16 Cu2 Br2 148.6(3) . . ?
C16 Cu2 Br2 113.0(3) . 2_466 ?
Br2 Cu2 Br2 98.10(6) . 2_466 ?
N7 Cu3 N8 130.2(4) . . ?
N7 Cu3 Br1 117.4(2) . . ?
N8 Cu3 Br1 112.1(3) . . ?
Cu3 Br1 Cu1 99.14(6) . . ?
Cu2 Br2 Cu2 81.90(6) . 2_466 ?
C5 N1 C1 121.0(7) . . ?
C5 N1 Cu1 119.6(5) . . ?
C1 N1 Cu1 119.3(5) . . ?
C6 N2 N3 109.2(8) . . ?
C6 N2 C5 133.5(8) . . ?
N3 N2 C5 117.3(6) . . ?
C8 N3 N2 106.3(7) . . ?
C8 N3 Cu1 141.5(6) . . ?
N2 N3 Cu1 111.5(5) . . ?
N5 N4 C11 108.7(7) . . ?
N5 N4 C1 117.3(6) . . ?
C11 N4 C1 134.0(7) . . ?
C13 N5 N4 106.8(6) . . ?
C13 N5 Cu1 140.3(6) . . ?
N4 N5 Cu1 111.9(5) . . ?
C16 N6 Cu1 173.1(7) . . ?
N1 C1 C2 120.8(8) . . ?
N1 C1 N4 112.0(6) . . ?
C2 C1 N4 127.2(8) . . ?
C3 C2 C1 117.5(9) . . ?
C3 C2 H2 121.3 . . ?
C1 C2 H2 121.3 . . ?
C2 C3 C4 122.2(8) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C5 C4 C3 116.3(9) . . ?
C5 C4 H4 121.9 . . ?
C3 C4 H4 121.9 . . ?
N1 C5 C4 122.1(9) . . ?
N1 C5 N2 111.8(6) . . ?
C4 C5 N2 126.1(8) . . ?
C7 C6 N2 107.0(9) . . ?
C7 C6 C9 128.6(10) . . ?
N2 C6 C9 124.4(11) . . ?
C6 C7 C8 106.8(8) . . ?
C6 C7 H7 126.6 . . ?
C8 C7 H7 126.6 . . ?
N3 C8 C7 110.7(9) . . ?
N3 C8 C10 120.9(8) . . ?
C7 C8 C10 128.4(9) . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N4 106.4(8) . . ?
C12 C11 C14 131.2(8) . . ?
N4 C11 C14 122.3(9) . . ?
C11 C12 C13 108.6(7) . . ?
C11 C12 H12 125.7 . . ?
C13 C12 H12 125.7 . . ?
N5 C13 C12 109.5(7) . . ?
N5 C13 C15 121.2(8) . . ?
C12 C13 C15 129.3(8) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 Cu2 173.0(8) . . ?
C7' N7' N7' 0.0(11) 2_677 2_677 ?
C7' N7' Cu3 178.1(10) 2_677 . ?
N7' N7' Cu3 178.1(10) 2_677 . ?
C8' N8' N8' 0.0(4) 2_577 2_577 ?
C8' N8' Cu3 173(2) 2_577 . ?
N8' N8' Cu3 173(2) 2_577 . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.34
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.864
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.158

#===END

#==============================================================================

data_2
_database_code_depnum_ccdc_archive 'CCDC 714395'

#==============================================================================

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H17 Cu4 N10'
_chemical_formula_sum            'C20 H17 Cu4 N10'
_chemical_formula_weight         651.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   7.5111(15)
_cell_length_b                   25.426(5)
_cell_length_c                   12.294(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.74(3)
_cell_angle_gamma                90.00
_cell_volume                     2248.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8174
_cell_measurement_theta_min      3.2029
_cell_measurement_theta_max      25.3491

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1292
_exptl_absorpt_coefficient_mu    3.764
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2882
_exptl_absorpt_correction_T_max  0.3525
_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  'Rigaku MercuryCCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            20823
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         25.35
_reflns_number_total             4096
_reflns_number_gt                3815
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0454P)²+2.0367P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0055(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4096
_refine_ls_number_parameters     312
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.0952
_refine_ls_wR_factor_gt          0.0926
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.020
_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
Cu1 Cu 0.36472(6) 0.590523(16) 1.00706(4) 0.03184(15) Uani 1 1 d . . .
Cu2 Cu 0.44861(7) 0.445522(19) 1.28417(4) 0.04085(16) Uani 1 1 d . . .
Cu3 Cu 0.01408(7) 0.313332(19) 1.04139(4) 0.04020(16) Uani 1 1 d . . .
Cu4 Cu -0.21283(7) 0.360049(19) 0.64065(4) 0.04088(16) Uani 1 1 d . . .
N1 N 0.3253(4) 0.64216(11) 0.8872(2) 0.0287(6) Uani 1 1 d . . .
N2 N 0.1387(4) 0.58040(12) 0.7784(2) 0.0328(7) Uani 1 1 d . . .
N3 N 0.1930(4) 0.55070(11) 0.8772(2) 0.0318(6) Uani 1 1 d . . .
N4 N 0.5284(4) 0.69154(11) 1.0208(2) 0.0309(6) Uani 1 1 d . . .
N5 N 0.5425(4) 0.64661(11) 1.0857(2) 0.0322(7) Uani 1 1 d . . .
N6 N 0.4145(5) 0.53799(13) 1.1222(3) 0.0433(8) Uani 1 1 d . . .
N7 N 0.2926(5) 0.38738(14) 1.1976(3) 0.0479(8) Uani 1 1 d . . .
N8 N -0.1330(5) 0.34584(14) 0.8952(3) 0.0486(8) Uani 1 1 d . . .
N9 N -0.1042(5) 0.29871(14) 0.5779(3) 0.0457(8) Uani 1 1 d . . .
N10 N -0.3411(5) 0.40565(14) 0.5190(3) 0.0524(9) Uani 1 1 d . . .
C1 C 0.4180(5) 0.68782(13) 0.9077(3) 0.0291(7) Uani 1 1 d . . .
C2 C 0.4007(5) 0.72473(14) 0.8234(3) 0.0371(8) Uani 1 1 d . . .
H2 H 0.4650 0.7564 0.8376 0.045 Uiso 1 1 calc R . .
C3 C 0.2852(6) 0.71313(15) 0.7176(3) 0.0415(9) Uani 1 1 d . . .
H3 H 0.2698 0.7377 0.6596 0.050 Uiso 1 1 calc R . .
C4 C 0.1909(5) 0.66567(15) 0.6950(3) 0.0393(9) Uani 1 1 d . . .
H4 H 0.1135 0.6578 0.6230 0.047 Uiso 1 1 calc R . .
C5 C 0.2164(5) 0.63076(13) 0.7834(3) 0.0300(7) Uani 1 1 d . . .
C6 C 0.0175(5) 0.55231(15) 0.6939(3) 0.0359(8) Uani 1 1 d . . .
C7 C -0.0023(5) 0.50495(15) 0.7394(3) 0.0411(9) Uani 1 1 d . . .
H7 H -0.0763 0.4774 0.7020 0.049 Uiso 1 1 calc R . .
C8 C 0.1078(5) 0.50476(14) 0.8525(3) 0.0367(8) Uani 1 1 d . . .
C9 C -0.0742(6) 0.57228(18) 0.5762(3) 0.0496(10) Uani 1 1 d . . .
H9A H -0.1461 0.6030 0.5804 0.074 Uiso 1 1 calc R . .
H9B H -0.1544 0.5455 0.5331 0.074 Uiso 1 1 calc R . .
H9C H 0.0191 0.5810 0.5398 0.074 Uiso 1 1 calc R . .
C10 C 0.1331(6) 0.46112(15) 0.9351(4) 0.0472(10) Uani 1 1 d . . .
H10A H 0.2498 0.4440 0.9420 0.071 Uiso 1 1 calc R . .
H10B H 0.0338 0.4362 0.9092 0.071 Uiso 1 1 calc R . .
H10C H 0.1320 0.4748 1.0077 0.071 Uiso 1 1 calc R . .
C11 C 0.6288(5) 0.73188(14) 1.0832(3) 0.0357(8) Uani 1 1 d . . .
C12 C 0.7069(5) 0.71152(16) 1.1891(3) 0.0419(9) Uani 1 1 d . . .
H12 H 0.7835 0.7294 1.2510 0.050 Uiso 1 1 calc R . .
C13 C 0.6515(5) 0.65918(15) 1.1881(3) 0.0369(8) Uani 1 1 d . . .
C14 C 0.6384(6) 0.78641(16) 1.0422(4) 0.0517(11) Uani 1 1 d . . .
H14A H 0.7003 0.7863 0.9839 0.078 Uiso 1 1 calc R . .
H14B H 0.7062 0.8081 1.1042 0.078 Uiso 1 1 calc R . .
H14C H 0.5148 0.8001 1.0119 0.078 Uiso 1 1 calc R . .
C15 C 0.6989(6) 0.62141(17) 1.2852(3) 0.0488(10) Uani 1 1 d . . .
H15A H 0.5967 0.6190 1.3172 0.073 Uiso 1 1 calc R . .
H15B H 0.8074 0.6336 1.3422 0.073 Uiso 1 1 calc R . .
H15C H 0.7231 0.5874 1.2587 0.073 Uiso 1 1 calc R . .
C16 C 0.4369(5) 0.50471(15) 1.1887(3) 0.0394(9) Uani 1 1 d . . .
C17 C 0.1911(5) 0.35850(15) 1.1388(3) 0.0381(9) Uani 1 1 d . . .
C18 C -0.1689(5) 0.35321(14) 0.7988(3) 0.0380(9) Uani 1 1 d . . .
C19 C -0.0576(5) 0.25757(15) 0.5593(3) 0.0364(8) Uani 1 1 d . . .
C20 C -0.4225(5) 0.42521(14) 0.4351(3) 0.0376(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N6 1.903(3) . ?
Cu1 N1 1.932(3) . ?
Cu1 N5 2.002(3) . ?
Cu1 N3 2.013(3) . ?
Cu2 C16 1.895(4) . ?
Cu2 C20 1.901(4) 1_656 ?
Cu2 N7 1.993(4) . ?
Cu3 C17 1.899(4) . ?
Cu3 C19 1.912(4) 4_566 ?
Cu3 N8 1.998(3) . ?
Cu4 C18 1.885(4) . ?
Cu4 N10 1.919(4) . ?
Cu4 N9 2.014(4) . ?
N1 C5 1.334(4) . ?
N1 C1 1.340(4) . ?
N2 C6 1.369(5) . ?
N2 N3 1.389(4) . ?
N2 C5 1.401(5) . ?
N3 C8 1.325(5) . ?
N4 C11 1.370(5) . ?
N4 N5 1.380(4) . ?
N4 C1 1.402(5) . ?
N5 C13 1.328(5) . ?
N6 C16 1.156(5) . ?
N7 C17 1.151(5) . ?
N8 C18 1.152(5) . ?
N9 C19 1.147(5) . ?
N10 C20 1.149(5) . ?
C1 C2 1.376(5) . ?
C2 C3 1.371(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(5) . ?
C4 H4 0.9300 . ?
C6 C7 1.354(6) . ?
C6 C9 1.500(5) . ?
C7 C8 1.398(5) . ?
C7 H7 0.9300 . ?
C8 C10 1.479(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.366(5) . ?
C11 C14 1.484(5) . ?
C12 C13 1.393(6) . ?
C12 H12 0.9300 . ?
C13 C15 1.493(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C19 Cu3 1.912(4) 4_565 ?
C20 Cu2 1.901(4) 1_454 ?

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
N6 Cu1 N1 176.75(14) . . ?
N6 Cu1 N5 100.36(13) . . ?
N1 Cu1 N5 79.56(12) . . ?
N6 Cu1 N3 100.40(13) . . ?
N1 Cu1 N3 79.30(12) . . ?
N5 Cu1 N3 158.02(12) . . ?
C16 Cu2 C20 137.74(16) . 1_656 ?
C16 Cu2 N7 110.07(15) . . ?
C20 Cu2 N7 112.07(15) 1_656 . ?
C17 Cu3 C19 131.82(15) . 4_566 ?
C17 Cu3 N8 115.01(15) . . ?
C19 Cu3 N8 113.12(15) 4_566 . ?
C18 Cu4 N10 139.46(16) . . ?
C18 Cu4 N9 110.73(15) . . ?
N10 Cu4 N9 109.71(15) . . ?
C5 N1 C1 120.7(3) . . ?
C5 N1 Cu1 119.9(2) . . ?
C1 N1 Cu1 119.2(2) . . ?
C6 N2 N3 110.1(3) . . ?
C6 N2 C5 133.5(3) . . ?
N3 N2 C5 116.4(3) . . ?
C8 N3 N2 106.1(3) . . ?
C8 N3 Cu1 141.5(2) . . ?
N2 N3 Cu1 112.3(2) . . ?
C11 N4 N5 110.9(3) . . ?
C11 N4 C1 132.8(3) . . ?
N5 N4 C1 116.3(3) . . ?
C13 N5 N4 105.8(3) . . ?
C13 N5 Cu1 140.6(3) . . ?
N4 N5 Cu1 112.4(2) . . ?
C16 N6 Cu1 176.5(3) . . ?
C17 N7 Cu2 171.7(3) . . ?
C18 N8 Cu3 153.8(3) . . ?
C19 N9 Cu4 164.5(3) . . ?
C20 N10 Cu4 168.2(4) . . ?
N1 C1 C2 121.2(3) . . ?
N1 C1 N4 111.8(3) . . ?
C2 C1 N4 127.0(3) . . ?
C1 C2 C3 117.7(3) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 H2 121.2 . . ?
C2 C3 C4 121.6(3) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C5 C4 C3 117.2(3) . . ?
C5 C4 H4 121.4 . . ?
C3 C4 H4 121.4 . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 N2 111.9(3) . . ?
C4 C5 N2 126.5(3) . . ?
C7 C6 N2 106.2(3) . . ?
C7 C6 C9 128.7(4) . . ?
N2 C6 C9 125.1(3) . . ?
C6 C7 C8 108.1(3) . . ?
C6 C7 H7 126.0 . . ?
C8 C7 H7 126.0 . . ?
N3 C8 C7 109.5(3) . . ?
N3 C8 C10 123.1(3) . . ?
C7 C8 C10 127.4(4) . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 105.4(3) . . ?
N4 C11 C14 125.6(3) . . ?
C12 C11 C14 128.9(4) . . ?
C11 C12 C13 107.9(3) . . ?
C11 C12 H12 126.0 . . ?
C13 C12 H12 126.0 . . ?
N5 C13 C12 109.9(3) . . ?
N5 C13 C15 122.9(4) . . ?
C12 C13 C15 127.2(3) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 Cu2 172.6(3) . . ?
N7 C17 Cu3 177.2(4) . . ?
N8 C18 Cu4 174.7(4) . . ?
N9 C19 Cu3 174.3(4) . 4_565 ?
N10 C20 Cu2 169.4(4) . 1_454 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.082

#===END


