# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012
data_publication_text
_journal_name_full 'New J.Chem.'
_journal_coden_cambridge 0440
#TrackingRef '- All-crystaldata-revised.CIF'
_publ_contact_author_name 'Christoph Janiak'
_publ_contact_author_address
;
Departament of Chemistry
Faculty of Sciences
Zanjan University 45195-313
Zanjan
Iran
;
_publ_contact_author_email janiak@uni-duesseldorf.de
_publ_contact_author_phone +49-211-8112286
loop_
_publ_author_name
_publ_author_address
J.K.Maclaren
;
Institut f\u"r Anorganische Chemie und Strukturchemie
Universit\"at D\"usseldorf
Universit\"atsstr. 1
D-40225 D\"usseldorf
Germany
;
P.Gili
;
Departamento de Qu\'imica Inorg\'anica
Universidad de La Laguna
38206 La Laguna, Tenerife
Spain
;
J.Sanchiz
;
Departamento de Qu\'imica Inorg\'anica
Universidad de La Laguna
38206 La Laguna, Tenerife
Spain
;
C.Janiak
;
Institut f\u"r Anorganische Chemie und Strukturchemie
Universit\"at D\"usseldorf
Universit\"atsstr. 1
D-40225 D\"usseldorf
Germany
;
_publ_section_title
;
Hydrophobic-exterior layer structures and magnetic properties of trinuclear
copper complexes with chiral amino alcoholate ligands
;
#==============================================================================
data_p21c
_database_code_depnum_ccdc_archive 'CCDC 864924'
#TrackingRef '- All-crystaldata.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Tetrakis(\m-amino-ethanolato-\kN,O:O)-dibromido-tricopper(II)
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C8 H24 Br2 Cu3 N4 O4'
_chemical_formula_sum 'C8 H24 Br2 Cu3 N4 O4'
_chemical_formula_weight 590.75
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 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 8.7424(2)
_cell_length_b 8.9246(2)
_cell_length_c 11.6251(3)
_cell_angle_alpha 90.00
_cell_angle_beta 108.5920(10)
_cell_angle_gamma 90.00
_cell_volume 859.68(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 4472
_cell_measurement_theta_min 2.457
_cell_measurement_theta_max 28.079
_exptl_crystal_description 'square plate'
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.01
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.282
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 578
_exptl_absorpt_coefficient_mu 8.342
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.2862
_exptl_absorpt_correction_T_max 0.9212
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(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 'Bruker APEX2 CCD area detector'
_diffrn_measurement_method '\w scans and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 10595
_diffrn_reflns_av_R_equivalents 0.0402
_diffrn_reflns_av_sigmaI/netI 0.0334
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 2.46
_diffrn_reflns_theta_max 26.36
_reflns_number_total 1737
_reflns_number_gt 1423
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material 'publCIF (Westrip, 2009)'
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH and CH~2~were positioned
geometrically
(C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~) and refined
using a riding model (AFIX 13 for aliphatic CH, AFIX 23 for CH~2~),
with U~iso~(H) = 1.2U~eq~(CH).
H atoms on the amin nitrogen atoms were positioned geometrically
(C---H = 0.91 \%A for aliphatic NH~2~) and refined using a riding model
(AFIX 23 for NH~2~), with U~iso~(H) = 1.2U~eq~(CH).with U~iso~(H) = 1.2U~eq~(N).
The largest residual Fourier peak ( 2.90 e \%A^-3^) is
found within 1.17 \%A of the Br atom. The deepest hole (-0.97) is 0.57
\%A from the Cu2 atom.
minimum Crystal Dimension can actually not be determined as crystals are
very thin
platelets which split into even thinner plates when touched from the side.
(Explainable with layer structure) This leads to unsatisfactory absorbtion
correction.
Resulting in large residual peak in proxmity to heavy atoms, more precise in
between
Cu and Br atoms and other large calculated non-metal positve residual
densities.
;
_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^)+(0.0673P)^2^+0.0652P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1737
_refine_ls_number_parameters 97
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0473
_refine_ls_R_factor_gt 0.0366
_refine_ls_wR_factor_ref 0.0991
_refine_ls_wR_factor_gt 0.0924
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_restrained_S_all 1.042
_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 0.50114(6) 0.27630(6) 0.17114(5) 0.01081(17) Uani 1 1 d . . .
Br Br 0.50230(6) 0.31504(5) 0.40869(4) 0.01406(16) Uani 1 1 d . . .
Cu2 Cu 0.5000 0.5000 0.0000 0.0110(2) Uani 1 2 d S . .
O1 O 0.6557(3) 0.4288(3) 0.1544(2) 0.0112(6) Uani 1 1 d . . .
O2 O 0.3457(3) 0.4268(3) 0.0795(2) 0.0112(6) Uani 1 1 d . . .
N1 N 0.6886(4) 0.1375(4) 0.2295(3) 0.0137(8) Uani 1 1 d . . .
H1A H 0.6844 0.0855 0.2968 0.016 Uiso 1 1 calc R . .
H1B H 0.6891 0.0699 0.1699 0.016 Uiso 1 1 calc R . .
N2 N 0.3154(4) 0.1360(4) 0.1405(3) 0.0129(8) Uani 1 1 d . . .
H2A H 0.3159 0.0676 0.0814 0.015 Uiso 1 1 calc R . .
H2B H 0.3195 0.0850 0.2102 0.015 Uiso 1 1 calc R . .
C1 C 0.8049(5) 0.3575(5) 0.1644(4) 0.0135(9) Uani 1 1 d . . .
H1C H 0.8939 0.4313 0.1887 0.016 Uiso 1 1 calc R . .
H1D H 0.8012 0.3141 0.0852 0.016 Uiso 1 1 calc R . .
C2 C 0.8333(5) 0.2336(5) 0.2600(4) 0.0146(10) Uani 1 1 d . . .
H2C H 0.9288 0.1733 0.2610 0.018 Uiso 1 1 calc R . .
H2D H 0.8536 0.2783 0.3415 0.018 Uiso 1 1 calc R . .
C3 C 0.1986(5) 0.3530(5) 0.0177(4) 0.0128(9) Uani 1 1 d . . .
H3A H 0.2045 0.3083 -0.0588 0.015 Uiso 1 1 calc R . .
H3B H 0.1082 0.4255 -0.0027 0.015 Uiso 1 1 calc R . .
C4 C 0.1705(5) 0.2307(5) 0.1003(4) 0.0134(9) Uani 1 1 d . . .
H4A H 0.1494 0.2762 0.1714 0.016 Uiso 1 1 calc R . .
H4B H 0.0757 0.1694 0.0558 0.016 Uiso 1 1 calc 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 0.0146(3) 0.0082(3) 0.0105(3) 0.0010(2) 0.0052(2) 0.0005(2)
Br 0.0263(3) 0.0090(3) 0.0093(2) -0.00005(15) 0.00907(19) -0.00039(17)
Cu2 0.0160(4) 0.0099(4) 0.0084(4) 0.0026(3) 0.0056(3) 0.0004(3)
O1 0.0130(16) 0.0088(17) 0.0128(16) -0.0001(12) 0.0055(12) 0.0007(12)
O2 0.0132(16) 0.0102(17) 0.0113(15) 0.0002(12) 0.0054(12) -0.0016(13)
N1 0.022(2) 0.010(2) 0.0109(18) 0.0017(15) 0.0087(16) 0.0015(16)
N2 0.020(2) 0.010(2) 0.0102(18) -0.0005(14) 0.0067(15) -0.0004(16)
C1 0.018(2) 0.012(2) 0.011(2) 0.0006(17) 0.0063(18) 0.0007(19)
C2 0.015(2) 0.015(2) 0.013(2) 0.0026(18) 0.0031(18) 0.0005(19)
C3 0.016(2) 0.011(2) 0.013(2) 0.0024(17) 0.0049(18) -0.0003(18)
C4 0.013(2) 0.015(2) 0.015(2) 0.0016(18) 0.0084(19) 0.0010(19)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.965(3) . ?
Cu1 O1 1.971(3) . ?
Cu1 N2 1.991(4) . ?
Cu1 N1 1.993(4) . ?
Cu1 Br 2.7799(7) . ?
Cu1 Cu2 2.8163(5) . ?
Cu2 O2 1.973(3) . ?
Cu2 O2 1.973(3) 3_665 ?
Cu2 O1 1.980(3) 3_665 ?
Cu2 O1 1.981(3) . ?
Cu2 Cu1 2.8163(5) 3_665 ?
O1 C1 1.422(5) . ?
O2 C3 1.420(5) . ?
N1 C2 1.475(6) . ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
N2 C4 1.469(5) . ?
N2 H2A 0.9200 . ?
N2 H2B 0.9200 . ?
C1 C2 1.531(6) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C3 C4 1.525(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O1 81.48(12) . . ?
O2 Cu1 N2 87.10(14) . . ?
O1 Cu1 N2 164.30(13) . . ?
O2 Cu1 N1 163.90(13) . . ?
O1 Cu1 N1 86.99(13) . . ?
N2 Cu1 N1 101.85(16) . . ?
O2 Cu1 Br 103.68(8) . . ?
O1 Cu1 Br 103.10(8) . . ?
N2 Cu1 Br 90.01(10) . . ?
N1 Cu1 Br 89.82(10) . . ?
O2 Cu1 Cu2 44.47(8) . . ?
O1 Cu1 Cu2 44.68(8) . . ?
N2 Cu1 Cu2 120.04(10) . . ?
N1 Cu1 Cu2 119.91(10) . . ?
Br Cu1 Cu2 127.71(2) . . ?
O2 Cu2 O2 180.0 . 3_665 ?
O2 Cu2 O1 98.96(12) . 3_665 ?
O2 Cu2 O1 81.04(12) 3_665 3_665 ?
O2 Cu2 O1 81.04(12) . . ?
O2 Cu2 O1 98.96(12) 3_665 . ?
O1 Cu2 O1 180.0 3_665 . ?
O2 Cu2 Cu1 44.24(8) . . ?
O2 Cu2 Cu1 135.76(8) 3_665 . ?
O1 Cu2 Cu1 135.60(8) 3_665 . ?
O1 Cu2 Cu1 44.40(8) . . ?
O2 Cu2 Cu1 135.76(8) . 3_665 ?
O2 Cu2 Cu1 44.24(8) 3_665 3_665 ?
O1 Cu2 Cu1 44.40(8) 3_665 3_665 ?
O1 Cu2 Cu1 135.60(8) . 3_665 ?
Cu1 Cu2 Cu1 180.0 . 3_665 ?
C1 O1 Cu1 108.8(2) . . ?
C1 O1 Cu2 124.4(2) . . ?
Cu1 O1 Cu2 90.92(12) . . ?
C3 O2 Cu1 108.4(2) . . ?
C3 O2 Cu2 124.1(2) . . ?
Cu1 O2 Cu2 91.29(12) . . ?
C2 N1 Cu1 105.6(3) . . ?
C2 N1 H1A 110.6 . . ?
Cu1 N1 H1A 110.6 . . ?
C2 N1 H1B 110.6 . . ?
Cu1 N1 H1B 110.6 . . ?
H1A N1 H1B 108.7 . . ?
C4 N2 Cu1 105.5(3) . . ?
C4 N2 H2A 110.6 . . ?
Cu1 N2 H2A 110.6 . . ?
C4 N2 H2B 110.6 . . ?
Cu1 N2 H2B 110.6 . . ?
H2A N2 H2B 108.8 . . ?
O1 C1 C2 108.3(3) . . ?
O1 C1 H1C 110.0 . . ?
C2 C1 H1C 110.0 . . ?
O1 C1 H1D 110.0 . . ?
C2 C1 H1D 110.0 . . ?
H1C C1 H1D 108.4 . . ?
N1 C2 C1 108.5(4) . . ?
N1 C2 H2C 110.0 . . ?
C1 C2 H2C 110.0 . . ?
N1 C2 H2D 110.0 . . ?
C1 C2 H2D 110.0 . . ?
H2C C2 H2D 108.4 . . ?
O2 C3 C4 108.4(3) . . ?
O2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
O2 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
N2 C4 C3 108.5(3) . . ?
N2 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
N2 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2B O1 0.92 2.06 2.963(4) 166.4 2_645
N2 H2A Br 0.92 2.74 3.414(4) 130.9 2_645
N1 H1B Br 0.92 2.80 3.455(4) 129.2 2_645
N1 H1A O2 0.92 2.09 2.997(4) 166.6 2_645
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full 26.36
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max 2.902
_refine_diff_density_min -0.967
_refine_diff_density_rms 0.188
#===END
data_jv27
_database_code_depnum_ccdc_archive 'CCDC 864925'
#TrackingRef '- All-crystaldata.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Tetrakis(\m-(R)-2-amino-butan-1-olato-\kN,O:O)-dibromido-tricopper(II)
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C32 H80 Br4 Cu6 N8 O8'
_chemical_formula_sum 'C32 H80 Br4 Cu6 N8 O8'
_chemical_formula_weight 1405.92
_chemical_absolute_configuration rmad
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_cell_length_a 9.0782(18)
_cell_length_b 11.603(2)
_cell_length_c 12.489(3)
_cell_angle_alpha 102.76(3)
_cell_angle_beta 100.94(3)
_cell_angle_gamma 90.00(3)
_cell_volume 1258.4(4)
_cell_formula_units_Z 1
_cell_measurement_temperature 118(2)
_cell_measurement_reflns_used 2094
_cell_measurement_theta_min 2.461
_cell_measurement_theta_max 23.454
_exptl_crystal_description 'square plate'
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.01
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.855
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 706
_exptl_absorpt_coefficient_mu 5.715
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.4811
_exptl_absorpt_correction_T_max 0.9451
_exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 118(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 RAXIS conversion'
_diffrn_measurement_method '\w scans and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 8784
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.1529
_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 -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 3.11
_diffrn_reflns_theta_max 25.00
_reflns_number_total 8784
_reflns_number_gt 5751
_reflns_threshold_expression >2sigma(I)
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material 'publCIF (Westrip, 2009)'
_publ_section_references
;
Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Rigaku (2009). Spider and CrystalClear.
Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
H atoms on crystal water oxygen / on nitrogen atoms have been found and
refined with U~iso~(H) = 1.5U~eq~(O)
;
_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^)+(0.1627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.0068(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.00(3)
_refine_ls_number_reflns 8784
_refine_ls_number_parameters 529
_refine_ls_number_restraints 549
_refine_ls_R_factor_all 0.1358
_refine_ls_R_factor_gt 0.0994
_refine_ls_wR_factor_ref 0.2730
_refine_ls_wR_factor_gt 0.2423
_refine_ls_goodness_of_fit_ref 0.994
_refine_ls_restrained_S_all 0.968
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.2803(3) 0.1721(3) 0.5002(2) 0.0202(7) Uani 1 1 d . . .
Cu2 Cu 0.4999(4) -0.0001(3) 0.5000(2) 0.0194(5) Uani 1 1 d . . .
Cu3 Cu 0.7199(3) -0.1718(3) 0.5014(2) 0.0203(7) Uani 1 1 d . . .
Cu4 Cu -0.2225(3) 0.3263(3) 0.4907(2) 0.0198(7) Uani 1 1 d . . .
Cu5 Cu -0.0032(4) 0.4977(3) 0.4909(2) 0.0182(5) Uani 1 1 d . . .
Cu6 Cu 0.2167(3) 0.6685(3) 0.4896(2) 0.0214(7) Uani 1 1 d . . .
Br2 Br 0.6832(2) -0.4066(2) 0.5075(2) 0.0238(6) Uani 1 1 d . . .
Br1 Br 0.3197(2) 0.4099(2) 0.5067(2) 0.0238(6) Uani 1 1 d . . .
Br4 Br 0.1760(2) 0.9046(2) 0.4819(2) 0.0251(6) Uani 1 1 d . . .
Br3 Br -0.1867(2) 0.0873(2) 0.48324(19) 0.0230(6) Uani 1 1 d . . .
O1 O 0.4070(17) 0.0939(14) 0.3947(11) 0.019(3) Uani 1 1 d DU . .
O2 O 0.4479(19) 0.1388(15) 0.6107(13) 0.025(3) Uani 1 1 d DU . .
O3 O 0.5369(17) -0.1437(14) 0.3969(11) 0.019(3) Uani 1 1 d DU . .
O4 O 0.6082(18) -0.0855(15) 0.6096(14) 0.031(4) Uani 1 1 d DU . .
O5 O -0.0460(18) 0.4015(14) 0.5934(12) 0.022(3) Uani 1 1 d DU . .
O6 O -0.113(2) 0.3594(14) 0.3797(13) 0.029(4) Uani 1 1 d DU . .
O7 O 0.0928(17) 0.6440(14) 0.5957(11) 0.020(3) Uani 1 1 d DU . .
O8 O 0.0452(19) 0.5829(15) 0.3790(13) 0.027(4) Uani 1 1 d DU . .
N1 N 0.116(3) 0.157(2) 0.3665(18) 0.034(5) Uani 1 1 d DU . .
H1A H 0.0536 0.0921 0.3588 0.041 Uiso 1 1 calc R . .
H1B H 0.0597 0.2235 0.3726 0.041 Uiso 1 1 calc R . .
N2 N 0.168(2) 0.2009(18) 0.6227(13) 0.017(4) Uani 1 1 d DU . .
H2A H 0.1183 0.2701 0.6236 0.021 Uiso 1 1 calc R . .
H2B H 0.0974 0.1402 0.6112 0.021 Uiso 1 1 calc R . .
N3 N 0.813(2) -0.2228(18) 0.3682(15) 0.021(4) Uani 1 1 d DU . .
H3A H 0.8716 -0.1623 0.3594 0.026 Uiso 1 1 calc R . .
H3B H 0.8709 -0.2868 0.3743 0.026 Uiso 1 1 calc R . .
N4 N 0.897(2) -0.144(2) 0.6204(14) 0.029(5) Uani 1 1 d DU . .
H4A H 0.9449 -0.2137 0.6215 0.034 Uiso 1 1 calc R . .
H4B H 0.9618 -0.0904 0.6077 0.034 Uiso 1 1 calc R . .
N5 N -0.3154(19) 0.3371(17) 0.6248(13) 0.013(3) Uani 1 1 d DU . .
H5A H -0.3782 0.3994 0.6321 0.016 Uiso 1 1 calc R . .
H5B H -0.3696 0.2685 0.6197 0.016 Uiso 1 1 calc R . .
N6 N -0.405(3) 0.293(2) 0.3667(15) 0.033(5) Uani 1 1 d DU . .
H6A H -0.4512 0.2220 0.3647 0.040 Uiso 1 1 calc R . .
H6B H -0.4721 0.3517 0.3782 0.040 Uiso 1 1 calc R . .
N7 N 0.382(2) 0.719(2) 0.6226(15) 0.024(4) Uani 1 1 d DU . .
H7A H 0.4456 0.6583 0.6295 0.029 Uiso 1 1 calc R . .
H7B H 0.4358 0.7831 0.6160 0.029 Uiso 1 1 calc R . .
N8 N 0.330(2) 0.6415(18) 0.3667(15) 0.024(4) Uani 1 1 d DU . .
H8A H 0.3762 0.7114 0.3645 0.029 Uiso 1 1 calc R . .
H8B H 0.4036 0.5884 0.3786 0.029 Uiso 1 1 calc R . .
C1 C 0.312(2) 0.054(2) 0.2888(16) 0.034(6) Uiso 1 1 d DU . .
H1C H 0.2629 -0.0237 0.2854 0.041 Uiso 1 1 calc R . .
H1D H 0.3719 0.0429 0.2292 0.041 Uiso 1 1 calc R . .
C2 C 0.191(2) 0.1440(19) 0.2695(15) 0.029(4) Uani 1 1 d DU . .
H2 H 0.2433 0.2214 0.2739 0.035 Uiso 1 1 calc R . .
C3 C 0.085(2) 0.110(2) 0.1575(17) 0.033(5) Uani 1 1 d DU . .
H3C H -0.0041 0.1589 0.1593 0.039 Uiso 1 1 calc R . .
H3D H 0.0503 0.0261 0.1444 0.039 Uiso 1 1 calc R . .
C4 C 0.157(5) 0.126(4) 0.061(3) 0.076(12) Uani 1 1 d DU . .
H4C H 0.0891 0.0930 -0.0098 0.115 Uiso 1 1 calc R . .
H4D H 0.2515 0.0842 0.0641 0.115 Uiso 1 1 calc R . .
H4E H 0.1781 0.2101 0.0680 0.115 Uiso 1 1 calc R . .
C5 C 0.398(3) 0.124(2) 0.7075(17) 0.030(5) Uani 1 1 d DU . .
H5C H 0.4832 0.1400 0.7722 0.036 Uiso 1 1 calc R . .
H5D H 0.3607 0.0412 0.6964 0.036 Uiso 1 1 calc R . .
C6 C 0.271(2) 0.2093(17) 0.7322(15) 0.028(4) Uani 1 1 d DU . .
H6 H 0.2150 0.1795 0.7832 0.033 Uiso 1 1 calc R . .
C7 C 0.324(2) 0.3356(18) 0.7853(17) 0.034(5) Uani 1 1 d DU . .
H7C H 0.2398 0.3878 0.7710 0.040 Uiso 1 1 calc R . .
H7D H 0.4048 0.3573 0.7491 0.040 Uiso 1 1 calc R . .
C8 C 0.383(4) 0.358(3) 0.9111(18) 0.043(8) Uani 1 1 d DU . .
H8C H 0.4310 0.4371 0.9381 0.065 Uiso 1 1 calc R . .
H8D H 0.4565 0.2988 0.9268 0.065 Uiso 1 1 calc R . .
H8E H 0.2993 0.3514 0.9491 0.065 Uiso 1 1 calc R . .
C9 C 0.578(3) -0.152(2) 0.2910(16) 0.033(5) Uani 1 1 d DU . .
H9A H 0.6290 -0.0770 0.2896 0.040 Uiso 1 1 calc R . .
H9B H 0.4869 -0.1664 0.2309 0.040 Uiso 1 1 calc R . .
C10 C 0.683(2) -0.2549(17) 0.2729(13) 0.024(4) Uani 1 1 d DU . .
H10 H 0.6312 -0.3282 0.2794 0.029 Uiso 1 1 calc R . .
C11 C 0.729(2) -0.278(2) 0.1604(16) 0.031(5) Uani 1 1 d DU . .
H11A H 0.7393 -0.2017 0.1380 0.037 Uiso 1 1 calc R . .
H11B H 0.8284 -0.3141 0.1657 0.037 Uiso 1 1 calc R . .
C12 C 0.615(3) -0.359(3) 0.073(2) 0.046(8) Uani 1 1 d DU . .
H12A H 0.6210 -0.4388 0.0865 0.069 Uiso 1 1 calc R . .
H12B H 0.6348 -0.3594 -0.0013 0.069 Uiso 1 1 calc R . .
H12C H 0.5141 -0.3301 0.0781 0.069 Uiso 1 1 calc R . .
C13 C 0.713(2) -0.0246(18) 0.7047(16) 0.024(4) Uani 1 1 d DU . .
H13A H 0.6632 -0.0072 0.7704 0.029 Uiso 1 1 calc R . .
H13B H 0.7450 0.0517 0.6914 0.029 Uiso 1 1 calc R . .
C14 C 0.852(2) -0.0981(16) 0.7301(14) 0.022(4) Uani 1 1 d DU . .
H14 H 0.9347 -0.0437 0.7798 0.026 Uiso 1 1 calc R . .
C15 C 0.821(3) -0.1930(19) 0.7887(17) 0.033(5) Uani 1 1 d DU . .
H15A H 0.8962 -0.2539 0.7772 0.040 Uiso 1 1 calc R . .
H15B H 0.7213 -0.2312 0.7512 0.040 Uiso 1 1 calc R . .
C16 C 0.822(3) -0.157(3) 0.9133(17) 0.037(7) Uani 1 1 d DU . .
H16A H 0.9176 -0.1153 0.9521 0.056 Uiso 1 1 calc R . .
H16B H 0.8093 -0.2275 0.9421 0.056 Uiso 1 1 calc R . .
H16C H 0.7393 -0.1044 0.9262 0.056 Uiso 1 1 calc R . .
C17 C -0.079(3) 0.4471(19) 0.7005(16) 0.031(4) Uani 1 1 d DU . .
H17A H -0.1274 0.5239 0.7027 0.037 Uiso 1 1 calc R . .
H17B H 0.0137 0.4591 0.7584 0.037 Uiso 1 1 calc R . .
C18 C -0.1866(19) 0.3561(19) 0.7214(13) 0.022(4) Uani 1 1 d DU . .
H18 H -0.1337 0.2800 0.7171 0.026 Uiso 1 1 calc R . .
C19 C -0.234(2) 0.387(2) 0.8339(14) 0.030(5) Uani 1 1 d DU . .
H19A H -0.2544 0.4718 0.8524 0.036 Uiso 1 1 calc R . .
H19B H -0.3276 0.3410 0.8300 0.036 Uiso 1 1 calc R . .
C20 C -0.113(3) 0.359(3) 0.925(2) 0.043(8) Uani 1 1 d DU . .
H20A H -0.0574 0.2919 0.8928 0.065 Uiso 1 1 calc R . .
H20B H -0.1591 0.3392 0.9835 0.065 Uiso 1 1 calc R . .
H20C H -0.0438 0.4282 0.9567 0.065 Uiso 1 1 calc R . .
C21 C -0.215(2) 0.374(2) 0.2853(18) 0.028(4) Uani 1 1 d DU . .
H21A H -0.1652 0.3603 0.2200 0.034 Uiso 1 1 calc R . .
H21B H -0.2476 0.4570 0.2981 0.034 Uiso 1 1 calc R . .
C22 C -0.354(2) 0.2892(16) 0.2598(16) 0.029(5) Uani 1 1 d DU . .
H22 H -0.4357 0.3176 0.2073 0.035 Uiso 1 1 calc R . .
C23 C -0.321(3) 0.1643(18) 0.2070(17) 0.031(5) Uani 1 1 d DU . .
H23A H -0.3941 0.1086 0.2206 0.037 Uiso 1 1 calc R . .
H23B H -0.2193 0.1459 0.2428 0.037 Uiso 1 1 calc R . .
C24 C -0.329(4) 0.147(4) 0.0819(17) 0.053(9) Uani 1 1 d DU . .
H24A H -0.2630 0.2065 0.0678 0.079 Uiso 1 1 calc R . .
H24B H -0.4324 0.1551 0.0450 0.079 Uiso 1 1 calc R . .
H24C H -0.2963 0.0677 0.0520 0.079 Uiso 1 1 calc R . .
C25 C 0.188(2) 0.6496(17) 0.7001(15) 0.020(4) Uani 1 1 d DU . .
H25A H 0.2377 0.5735 0.7001 0.024 Uiso 1 1 calc R . .
H25B H 0.1292 0.6643 0.7603 0.024 Uiso 1 1 calc R . .
C26 C 0.308(2) 0.750(2) 0.7213(14) 0.026(4) Uani 1 1 d DU . .
H26 H 0.2543 0.8250 0.7172 0.031 Uiso 1 1 calc R . .
C27 C 0.412(2) 0.770(3) 0.8348(15) 0.037(6) Uani 1 1 d DU . .
H27A H 0.4408 0.6923 0.8507 0.044 Uiso 1 1 calc R . .
H27B H 0.5054 0.8128 0.8316 0.044 Uiso 1 1 calc R . .
C28 C 0.345(3) 0.840(4) 0.930(2) 0.060(11) Uani 1 1 d DU . .
H28A H 0.4241 0.8640 0.9969 0.089 Uiso 1 1 calc R . .
H28B H 0.2684 0.7899 0.9460 0.089 Uiso 1 1 calc R . .
H28C H 0.2991 0.9098 0.9089 0.089 Uiso 1 1 calc R . .
C29 C 0.096(3) 0.5223(18) 0.2821(17) 0.029(5) Uani 1 1 d DU . .
H29A H 0.0112 0.5090 0.2171 0.035 Uiso 1 1 calc R . .
H29B H 0.1313 0.4442 0.2927 0.035 Uiso 1 1 calc R . .
C30 C 0.225(2) 0.5940(19) 0.2585(16) 0.032(5) Uani 1 1 d DU . .
H30 H 0.2801 0.5389 0.2080 0.038 Uiso 1 1 calc R . .
C31 C 0.169(3) 0.6920(19) 0.2023(16) 0.032(5) Uani 1 1 d DU . .
H31A H 0.2529 0.7507 0.2126 0.039 Uiso 1 1 calc R . .
H31B H 0.0893 0.7324 0.2381 0.039 Uiso 1 1 calc R . .
C32 C 0.109(4) 0.646(3) 0.0784(18) 0.046(8) Uani 1 1 d DU . .
H32A H 0.1868 0.6041 0.0431 0.069 Uiso 1 1 calc R . .
H32B H 0.0781 0.7127 0.0440 0.069 Uiso 1 1 calc R . .
H32C H 0.0217 0.5919 0.0681 0.069 Uiso 1 1 calc 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 0.0081(16) 0.0227(17) 0.0303(15) 0.0058(13) 0.0050(12) 0.0028(14)
Cu2 0.0129(10) 0.0196(11) 0.0260(13) 0.0063(10) 0.0034(9) 0.0043(8)
Cu3 0.0136(17) 0.0191(16) 0.0304(15) 0.0104(12) 0.0043(12) 0.0074(14)
Cu4 0.0117(17) 0.0243(17) 0.0270(14) 0.0118(12) 0.0058(12) 0.0024(14)
Cu5 0.0115(10) 0.0208(11) 0.0233(13) 0.0055(10) 0.0050(9) -0.0029(8)
Cu6 0.0108(17) 0.0240(18) 0.0274(15) 0.0008(12) 0.0046(12) -0.0009(14)
Br2 0.0119(12) 0.0201(14) 0.0395(15) 0.0087(11) 0.0031(10) 0.0011(10)
Br1 0.0134(12) 0.0210(14) 0.0392(15) 0.0086(11) 0.0087(10) 0.0036(10)
Br4 0.0151(13) 0.0195(14) 0.0443(16) 0.0109(12) 0.0105(10) 0.0031(10)
Br3 0.0113(12) 0.0175(13) 0.0420(15) 0.0123(11) 0.0030(10) 0.0040(10)
O1 0.016(5) 0.020(5) 0.024(5) 0.007(4) 0.009(4) -0.004(4)
O2 0.014(8) 0.023(8) 0.042(9) 0.010(7) 0.008(6) 0.006(7)
O3 0.012(5) 0.019(5) 0.024(5) 0.005(4) 0.001(4) 0.003(4)
O4 0.006(7) 0.029(9) 0.053(10) 0.006(7) 0.001(6) 0.009(7)
O5 0.017(5) 0.020(5) 0.028(5) 0.008(4) 0.003(4) -0.001(4)
O6 0.034(9) 0.016(8) 0.031(8) 0.002(7) -0.001(6) -0.008(7)
O7 0.017(5) 0.020(5) 0.023(5) 0.004(4) 0.009(4) 0.004(4)
O8 0.015(8) 0.030(9) 0.042(9) 0.011(7) 0.015(7) 0.009(7)
N1 0.036(12) 0.016(10) 0.061(11) 0.013(9) 0.034(10) 0.019(9)
N2 0.013(5) 0.016(5) 0.022(5) 0.002(4) 0.003(4) 0.008(4)
N3 0.015(8) 0.016(9) 0.033(9) 0.003(7) 0.005(7) 0.001(7)
N4 0.012(9) 0.041(13) 0.037(9) 0.015(9) 0.007(7) 0.017(9)
N5 0.012(5) 0.012(5) 0.015(5) 0.005(4) 0.000(4) 0.010(4)
N6 0.029(11) 0.040(12) 0.036(10) 0.010(9) 0.017(8) 0.000(9)
N7 0.022(6) 0.022(6) 0.027(5) 0.003(4) 0.008(4) 0.007(4)
N8 0.007(8) 0.024(11) 0.040(10) 0.013(8) -0.006(7) -0.009(7)
C2 0.031(11) 0.021(10) 0.040(9) 0.012(9) 0.012(7) 0.005(9)
C3 0.025(12) 0.027(12) 0.051(10) 0.014(11) 0.011(8) 0.010(10)
C4 0.06(2) 0.12(3) 0.040(12) 0.00(2) 0.022(15) 0.00(2)
C5 0.018(10) 0.046(12) 0.030(11) 0.013(9) 0.007(8) 0.020(9)
C6 0.025(11) 0.040(10) 0.018(8) 0.007(8) 0.005(6) 0.013(8)
C7 0.006(9) 0.048(11) 0.037(10) -0.002(10) -0.006(8) 0.012(8)
C8 0.08(2) 0.013(13) 0.034(11) 0.007(10) -0.008(13) -0.004(13)
C9 0.030(12) 0.043(13) 0.030(10) 0.007(10) 0.013(9) 0.018(10)
C10 0.033(10) 0.015(10) 0.019(8) -0.005(8) 0.003(6) -0.005(8)
C11 0.034(12) 0.023(11) 0.032(9) -0.009(9) 0.015(8) 0.004(9)
C12 0.027(14) 0.08(2) 0.018(10) -0.001(11) -0.007(10) 0.006(14)
C13 0.022(5) 0.022(6) 0.027(6) 0.004(4) 0.004(4) 0.004(4)
C14 0.019(5) 0.021(5) 0.022(5) -0.002(4) 0.003(4) 0.002(4)
C15 0.033(13) 0.034(12) 0.038(11) 0.008(9) 0.022(10) 0.010(10)
C16 0.032(14) 0.048(19) 0.037(11) 0.019(12) 0.010(11) 0.027(13)
C17 0.028(6) 0.032(6) 0.032(6) 0.007(4) 0.004(4) -0.001(4)
C18 0.013(9) 0.039(11) 0.015(7) 0.010(8) -0.002(6) 0.003(8)
C19 0.016(10) 0.050(15) 0.023(8) 0.003(10) 0.005(7) 0.011(10)
C20 0.055(18) 0.06(2) 0.019(10) 0.028(13) 0.006(11) 0.008(16)
C21 0.025(6) 0.028(6) 0.032(6) 0.009(4) 0.003(4) -0.004(4)
C22 0.036(10) 0.026(9) 0.022(9) -0.002(8) 0.006(8) -0.016(8)
C23 0.025(12) 0.029(9) 0.040(11) 0.003(9) 0.017(10) 0.003(9)
C24 0.042(17) 0.07(2) 0.027(11) -0.019(12) -0.003(12) 0.017(17)
C25 0.016(9) 0.012(10) 0.030(9) -0.002(8) 0.006(6) 0.007(7)
C26 0.012(9) 0.042(12) 0.022(8) 0.004(9) 0.000(6) 0.000(8)
C27 0.023(11) 0.065(16) 0.019(8) 0.011(10) -0.005(7) 0.007(10)
C28 0.031(16) 0.09(3) 0.039(12) -0.027(16) 0.002(11) -0.001(17)
C29 0.039(12) 0.021(11) 0.028(11) 0.002(8) 0.010(8) -0.020(9)
C30 0.019(10) 0.050(12) 0.031(9) 0.026(9) -0.004(7) -0.017(9)
C31 0.016(10) 0.053(14) 0.036(10) 0.028(10) 0.005(9) -0.010(10)
C32 0.049(18) 0.05(2) 0.033(11) 0.021(12) -0.012(12) -0.007(16)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.951(17) . ?
Cu1 N2 1.965(18) . ?
Cu1 O1 1.983(16) . ?
Cu1 N1 1.99(3) . ?
Cu1 Br1 2.764(4) . ?
Cu1 Cu2 2.823(5) . ?
Cu2 O3 1.940(15) . ?
Cu2 O1 1.961(15) . ?
Cu2 O4 1.977(17) . ?
Cu2 O2 1.999(16) . ?
Cu2 Cu3 2.821(5) . ?
Cu3 N4 1.94(2) . ?
Cu3 O4 1.944(18) . ?
Cu3 N3 1.98(2) . ?
Cu3 O3 1.983(15) . ?
Cu3 Br2 2.764(4) . ?
Cu4 O5 1.924(16) . ?
Cu4 O6 1.952(19) . ?
Cu4 N5 1.994(19) . ?
Cu4 N6 2.01(2) . ?
Cu4 Br3 2.775(4) . ?
Cu4 Cu5 2.814(5) . ?
Cu5 O5 1.964(15) . ?
Cu5 O7 1.984(15) . ?
Cu5 O8 1.992(17) . ?
Cu5 O6 1.998(16) . ?
Cu5 Cu6 2.817(5) . ?
Cu6 O7 1.957(15) . ?
Cu6 O8 1.974(18) . ?
Cu6 N8 1.98(2) . ?
Cu6 N7 1.99(2) . ?
Cu6 Br4 2.785(4) . ?
O1 C1 1.417(14) . ?
O2 C5 1.412(14) . ?
O3 C9 1.423(14) . ?
O4 C13 1.417(14) . ?
O5 C17 1.414(14) . ?
O6 C21 1.398(14) . ?
O7 C25 1.411(14) . ?
O8 C29 1.415(14) . ?
N1 C2 1.481(15) . ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
N2 C6 1.486(14) . ?
N2 H2A 0.9200 . ?
N2 H2B 0.9200 . ?
N3 C10 1.486(14) . ?
N3 H3A 0.9200 . ?
N3 H3B 0.9200 . ?
N4 C14 1.488(14) . ?
N4 H4A 0.9200 . ?
N4 H4B 0.9200 . ?
N5 C18 1.490(14) . ?
N5 H5A 0.9200 . ?
N5 H5B 0.9200 . ?
N6 C22 1.485(14) . ?
N6 H6A 0.9200 . ?
N6 H6B 0.9200 . ?
N7 C26 1.489(14) . ?
N7 H7A 0.9200 . ?
N7 H7B 0.9200 . ?
N8 C30 1.493(14) . ?
N8 H8A 0.9200 . ?
N8 H8B 0.9200 . ?
C1 C2 1.537(15) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 C3 1.513(15) . ?
C2 H2 1.0000 . ?
C3 C4 1.517(16) . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C4 H4C 0.9800 . ?
C4 H4D 0.9800 . ?
C4 H4E 0.9800 . ?
C5 C6 1.554(14) . ?
C5 H5C 0.9900 . ?
C5 H5D 0.9900 . ?
C6 C7 1.507(15) . ?
C6 H6 1.0000 . ?
C7 C8 1.524(15) . ?
C7 H7C 0.9900 . ?
C7 H7D 0.9900 . ?
C8 H8C 0.9800 . ?
C8 H8D 0.9800 . ?
C8 H8E 0.9800 . ?
C9 C10 1.539(15) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.510(15) . ?
C10 H10 1.0000 . ?
C11 C12 1.506(16) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.547(14) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.504(15) . ?
C14 H14 1.0000 . ?
C15 C16 1.518(15) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.533(15) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.514(15) . ?
C18 H18 1.0000 . ?
C19 C20 1.510(15) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.541(15) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.509(15) . ?
C22 H22 1.0000 . ?
C23 C24 1.519(16) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.538(15) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.520(15) . ?
C26 H26 1.0000 . ?
C27 C28 1.513(16) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.546(14) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.502(15) . ?
C30 H30 1.0000 . ?
C31 C32 1.514(15) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 N2 85.7(6) . . ?
O2 Cu1 O1 82.2(6) . . ?
N2 Cu1 O1 160.8(7) . . ?
O2 Cu1 N1 163.3(8) . . ?
N2 Cu1 N1 101.8(7) . . ?
O1 Cu1 N1 86.4(7) . . ?
O2 Cu1 Br1 104.6(5) . . ?
N2 Cu1 Br1 93.7(6) . . ?
O1 Cu1 Br1 103.8(5) . . ?
N1 Cu1 Br1 89.9(7) . . ?
O2 Cu1 Cu2 45.1(5) . . ?
N2 Cu1 Cu2 118.1(5) . . ?
O1 Cu1 Cu2 44.0(4) . . ?
N1 Cu1 Cu2 119.0(6) . . ?
Br1 Cu1 Cu2 127.91(13) . . ?
O3 Cu2 O1 100.7(6) . . ?
O3 Cu2 O4 81.1(6) . . ?
O1 Cu2 O4 175.2(8) . . ?
O3 Cu2 O2 174.6(8) . . ?
O1 Cu2 O2 81.5(6) . . ?
O4 Cu2 O2 97.1(7) . . ?
O3 Cu2 Cu3 44.6(4) . . ?
O1 Cu2 Cu3 135.8(5) . . ?
O4 Cu2 Cu3 43.5(5) . . ?
O2 Cu2 Cu3 135.9(5) . . ?
O3 Cu2 Cu1 135.7(5) . . ?
O1 Cu2 Cu1 44.6(5) . . ?
O4 Cu2 Cu1 136.1(5) . . ?
O2 Cu2 Cu1 43.7(5) . . ?
Cu3 Cu2 Cu1 179.61(15) . . ?
N4 Cu3 O4 87.7(7) . . ?
N4 Cu3 N3 100.9(7) . . ?
O4 Cu3 N3 163.2(8) . . ?
N4 Cu3 O3 161.4(8) . . ?
O4 Cu3 O3 80.8(6) . . ?
N3 Cu3 O3 86.9(6) . . ?
N4 Cu3 Br2 93.6(7) . . ?
O4 Cu3 Br2 105.0(6) . . ?
N3 Cu3 Br2 89.0(6) . . ?
O3 Cu3 Br2 103.5(5) . . ?
N4 Cu3 Cu2 119.2(6) . . ?
O4 Cu3 Cu2 44.5(5) . . ?
N3 Cu3 Cu2 119.2(6) . . ?
O3 Cu3 Cu2 43.4(4) . . ?
Br2 Cu3 Cu2 127.80(14) . . ?
O5 Cu4 O6 82.6(6) . . ?
O5 Cu4 N5 86.3(6) . . ?
O6 Cu4 N5 164.5(7) . . ?
O5 Cu4 N6 162.6(8) . . ?
O6 Cu4 N6 86.7(7) . . ?
N5 Cu4 N6 101.3(7) . . ?
O5 Cu4 Br3 103.7(5) . . ?
O6 Cu4 Br3 104.4(5) . . ?
N5 Cu4 Br3 88.6(6) . . ?
N6 Cu4 Br3 92.2(7) . . ?
O5 Cu4 Cu5 44.2(5) . . ?
O6 Cu4 Cu5 45.2(5) . . ?
N5 Cu4 Cu5 119.8(6) . . ?
N6 Cu4 Cu5 119.6(6) . . ?
Br3 Cu4 Cu5 127.84(13) . . ?
O5 Cu5 O7 102.3(6) . . ?
O5 Cu5 O8 175.2(7) . . ?
O7 Cu5 O8 81.4(6) . . ?
O5 Cu5 O6 80.4(6) . . ?
O7 Cu5 O6 175.0(8) . . ?
O8 Cu5 O6 96.1(7) . . ?
O5 Cu5 Cu4 43.1(5) . . ?
O7 Cu5 Cu4 136.4(5) . . ?
O8 Cu5 Cu4 135.2(5) . . ?
O6 Cu5 Cu4 43.9(5) . . ?
O5 Cu5 Cu6 137.2(5) . . ?
O7 Cu5 Cu6 44.0(4) . . ?
O8 Cu5 Cu6 44.5(5) . . ?
O6 Cu5 Cu6 135.7(5) . . ?
Cu4 Cu5 Cu6 179.58(15) . . ?
O7 Cu6 O8 82.5(6) . . ?
O7 Cu6 N8 162.8(8) . . ?
O8 Cu6 N8 86.9(6) . . ?
O7 Cu6 N7 86.2(7) . . ?
O8 Cu6 N7 164.0(8) . . ?
N8 Cu6 N7 101.2(7) . . ?
O7 Cu6 Br4 103.0(5) . . ?
O8 Cu6 Br4 104.0(5) . . ?
N8 Cu6 Br4 92.7(6) . . ?
N7 Cu6 Br4 89.6(7) . . ?
O7 Cu6 Cu5 44.8(5) . . ?
O8 Cu6 Cu5 45.0(5) . . ?
N8 Cu6 Cu5 119.2(5) . . ?
N7 Cu6 Cu5 119.6(6) . . ?
Br4 Cu6 Cu5 127.56(14) . . ?
C1 O1 Cu2 128.1(13) . . ?
C1 O1 Cu1 107.5(13) . . ?
Cu2 O1 Cu1 91.4(6) . . ?
C5 O2 Cu1 110.7(13) . . ?
C5 O2 Cu2 121.0(14) . . ?
Cu1 O2 Cu2 91.2(7) . . ?
C9 O3 Cu2 126.6(14) . . ?
C9 O3 Cu3 107.0(13) . . ?
Cu2 O3 Cu3 91.9(6) . . ?
C13 O4 Cu3 108.3(13) . . ?
C13 O4 Cu2 120.8(14) . . ?
Cu3 O4 Cu2 92.0(8) . . ?
C17 O5 Cu4 110.5(14) . . ?
C17 O5 Cu5 124.9(13) . . ?
Cu4 O5 Cu5 92.7(6) . . ?
C21 O6 Cu4 109.5(15) . . ?
C21 O6 Cu5 121.2(14) . . ?
Cu4 O6 Cu5 90.8(7) . . ?
C25 O7 Cu6 108.1(13) . . ?
C25 O7 Cu5 125.7(12) . . ?
Cu6 O7 Cu5 91.2(6) . . ?
C29 O8 Cu6 109.6(13) . . ?
C29 O8 Cu5 121.4(13) . . ?
Cu6 O8 Cu5 90.5(7) . . ?
C2 N1 Cu1 105.7(15) . . ?
C2 N1 H1A 110.6 . . ?
Cu1 N1 H1A 110.6 . . ?
C2 N1 H1B 110.6 . . ?
Cu1 N1 H1B 110.6 . . ?
H1A N1 H1B 108.7 . . ?
C6 N2 Cu1 110.7(13) . . ?
C6 N2 H2A 109.5 . . ?
Cu1 N2 H2A 109.5 . . ?
C6 N2 H2B 109.5 . . ?
Cu1 N2 H2B 109.5 . . ?
H2A N2 H2B 108.1 . . ?
C10 N3 Cu3 104.5(12) . . ?
C10 N3 H3A 110.9 . . ?
Cu3 N3 H3A 110.9 . . ?
C10 N3 H3B 110.9 . . ?
Cu3 N3 H3B 110.9 . . ?
H3A N3 H3B 108.9 . . ?
C14 N4 Cu3 109.8(13) . . ?
C14 N4 H4A 109.7 . . ?
Cu3 N4 H4A 109.7 . . ?
C14 N4 H4B 109.7 . . ?
Cu3 N4 H4B 109.7 . . ?
H4A N4 H4B 108.2 . . ?
C18 N5 Cu4 105.0(12) . . ?
C18 N5 H5A 110.7 . . ?
Cu4 N5 H5A 110.7 . . ?
C18 N5 H5B 110.7 . . ?
Cu4 N5 H5B 110.7 . . ?
H5A N5 H5B 108.8 . . ?
C22 N6 Cu4 107.7(15) . . ?
C22 N6 H6A 110.2 . . ?
Cu4 N6 H6A 110.2 . . ?
C22 N6 H6B 110.2 . . ?
Cu4 N6 H6B 110.2 . . ?
H6A N6 H6B 108.5 . . ?
C26 N7 Cu6 106.1(13) . . ?
C26 N7 H7A 110.5 . . ?
Cu6 N7 H7A 110.5 . . ?
C26 N7 H7B 110.5 . . ?
Cu6 N7 H7B 110.5 . . ?
H7A N7 H7B 108.7 . . ?
C30 N8 Cu6 109.0(13) . . ?
C30 N8 H8A 109.9 . . ?
Cu6 N8 H8A 109.9 . . ?
C30 N8 H8B 109.9 . . ?
Cu6 N8 H8B 109.9 . . ?
H8A N8 H8B 108.3 . . ?
O1 C1 C2 109.9(16) . . ?
O1 C1 H1C 109.7 . . ?
C2 C1 H1C 109.7 . . ?
O1 C1 H1D 109.7 . . ?
C2 C1 H1D 109.7 . . ?
H1C C1 H1D 108.2 . . ?
N1 C2 C3 113.7(19) . . ?
N1 C2 C1 104.4(17) . . ?
C3 C2 C1 114.0(16) . . ?
N1 C2 H2 108.2 . . ?
C3 C2 H2 108.2 . . ?
C1 C2 H2 108.2 . . ?
C2 C3 C4 112(2) . . ?
C2 C3 H3C 109.1 . . ?
C4 C3 H3C 109.1 . . ?
C2 C3 H3D 109.1 . . ?
C4 C3 H3D 109.1 . . ?
H3C C3 H3D 107.8 . . ?
C3 C4 H4C 109.5 . . ?
C3 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
C3 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
O2 C5 C6 110.3(17) . . ?
O2 C5 H5C 109.6 . . ?
C6 C5 H5C 109.6 . . ?
O2 C5 H5D 109.6 . . ?
C6 C5 H5D 109.6 . . ?
H5C C5 H5D 108.1 . . ?
N2 C6 C7 111.0(16) . . ?
N2 C6 C5 105.6(16) . . ?
C7 C6 C5 114.5(19) . . ?
N2 C6 H6 108.5 . . ?
C7 C6 H6 108.5 . . ?
C5 C6 H6 108.5 . . ?
C6 C7 C8 113.6(19) . . ?
C6 C7 H7C 108.9 . . ?
C8 C7 H7C 108.9 . . ?
C6 C7 H7D 108.9 . . ?
C8 C7 H7D 108.9 . . ?
H7C C7 H7D 107.7 . . ?
C7 C8 H8C 109.5 . . ?
C7 C8 H8D 109.5 . . ?
H8C C8 H8D 109.5 . . ?
C7 C8 H8E 109.5 . . ?
H8C C8 H8E 109.5 . . ?
H8D C8 H8E 109.5 . . ?
O3 C9 C10 107.8(15) . . ?
O3 C9 H9A 110.1 . . ?
C10 C9 H9A 110.1 . . ?
O3 C9 H9B 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.5 . . ?
N3 C10 C11 113.0(16) . . ?
N3 C10 C9 104.7(16) . . ?
C11 C10 C9 113.4(16) . . ?
N3 C10 H10 108.5 . . ?
C11 C10 H10 108.5 . . ?
C9 C10 H10 108.5 . . ?
C12 C11 C10 110.5(18) . . ?
C12 C11 H11A 109.6 . . ?
C10 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
C10 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O4 C13 C14 111.5(16) . . ?
O4 C13 H13A 109.3 . . ?
C14 C13 H13A 109.3 . . ?
O4 C13 H13B 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
N4 C14 C15 113.9(16) . . ?
N4 C14 C13 105.6(16) . . ?
C15 C14 C13 112.1(18) . . ?
N4 C14 H14 108.4 . . ?
C15 C14 H14 108.4 . . ?
C13 C14 H14 108.4 . . ?
C14 C15 C16 118(2) . . ?
C14 C15 H15A 107.8 . . ?
C16 C15 H15A 107.8 . . ?
C14 C15 H15B 107.8 . . ?
C16 C15 H15B 107.8 . . ?
H15A C15 H15B 107.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C17 C18 106.9(15) . . ?
O5 C17 H17A 110.3 . . ?
C18 C17 H17A 110.3 . . ?
O5 C17 H17B 110.3 . . ?
C18 C17 H17B 110.3 . . ?
H17A C17 H17B 108.6 . . ?
N5 C18 C19 113.4(15) . . ?
N5 C18 C17 105.8(16) . . ?
C19 C18 C17 115.5(17) . . ?
N5 C18 H18 107.3 . . ?
C19 C18 H18 107.3 . . ?
C17 C18 H18 107.3 . . ?
C20 C19 C18 110.9(17) . . ?
C20 C19 H19A 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 108.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O6 C21 C22 111.4(18) . . ?
O6 C21 H21A 109.4 . . ?
C22 C21 H21A 109.4 . . ?
O6 C21 H21B 109.4 . . ?
C22 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
N6 C22 C23 110.5(17) . . ?
N6 C22 C21 107.7(18) . . ?
C23 C22 C21 112.3(19) . . ?
N6 C22 H22 108.8 . . ?
C23 C22 H22 108.8 . . ?
C21 C22 H22 108.8 . . ?
C22 C23 C24 112(2) . . ?
C22 C23 H23A 109.3 . . ?
C24 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
C24 C23 H23B 109.3 . . ?
H23A C23 H23B 107.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O7 C25 C26 109.1(15) . . ?
O7 C25 H25A 109.9 . . ?
C26 C25 H25A 109.9 . . ?
O7 C25 H25B 109.9 . . ?
C26 C25 H25B 109.9 . . ?
H25A C25 H25B 108.3 . . ?
N7 C26 C27 115.6(16) . . ?
N7 C26 C25 103.5(16) . . ?
C27 C26 C25 114.1(18) . . ?
N7 C26 H26 107.8 . . ?
C27 C26 H26 107.8 . . ?
C25 C26 H26 107.8 . . ?
C28 C27 C26 113.8(19) . . ?
C28 C27 H27A 108.8 . . ?
C26 C27 H27A 108.8 . . ?
C28 C27 H27B 108.8 . . ?
C26 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O8 C29 C30 110.9(17) . . ?
O8 C29 H29A 109.5 . . ?
C30 C29 H29A 109.5 . . ?
O8 C29 H29B 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 108.0 . . ?
N8 C30 C31 110.9(17) . . ?
N8 C30 C29 108.2(17) . . ?
C31 C30 C29 112.7(18) . . ?
N8 C30 H30 108.3 . . ?
C31 C30 H30 108.3 . . ?
C29 C30 H30 108.3 . . ?
C30 C31 C32 112(2) . . ?
C30 C31 H31A 109.3 . . ?
C32 C31 H31A 109.3 . . ?
C30 C31 H31B 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Br3 0.92 2.92 3.52(2) 124.3 .
N1 H1A Br4 0.92 3.03 3.54(2) 117.0 1_545
N1 H1B O6 0.92 2.22 3.13(3) 169.1 .
N2 H2A O5 0.92 2.17 3.07(2) 164.3 .
N2 H2B Br4 0.92 3.01 3.51(2) 115.3 1_545
N2 H2B Br3 0.92 2.75 3.463(18) 134.7 .
N3 H3A Br4 0.92 2.91 3.517(17) 125.1 1_645
N3 H3A Br3 0.92 3.07 3.57(2) 116.1 1_655
N3 H3B O8 0.92 2.19 3.10(2) 167.8 1_645
N4 H4A O7 0.92 2.14 3.03(3) 163.9 1_645
N4 H4B Br4 0.92 2.71 3.44(2) 136.6 1_645
N4 H4B Br3 0.92 3.02 3.50(2) 114.6 1_655
N5 H5A Br1 0.92 2.91 3.544(16) 127.7 1_455
N5 H5A Br2 0.92 3.11 3.593(19) 114.6 1_465
N5 H5B O2 0.92 2.21 3.10(3) 163.6 1_455
N6 H6A O1 0.92 2.11 3.00(3) 162.1 1_455
N6 H6B Br1 0.92 2.70 3.43(2) 137.2 1_455
N6 H6B Br2 0.92 3.10 3.55(2) 112.6 1_465
N7 H7A Br2 0.92 2.88 3.500(18) 126.1 1_565
N7 H7A Br1 0.92 3.06 3.56(2) 116.0 .
N7 H7B O4 0.92 2.21 3.11(3) 167.6 1_565
N8 H8B Br2 0.92 2.73 3.458(17) 136.9 1_565
N8 H8B Br1 0.92 3.06 3.52(2) 113.3 .
N8 H8A O3 0.92 2.14 3.03(2) 161.8 1_565
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 3.798
_refine_diff_density_min -2.724
_refine_diff_density_rms 0.378
#===END
data_jkvamith
_database_code_depnum_ccdc_archive 'CCDC 864926'
#TrackingRef '- All-crystaldata-revised.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Bis[bis(\m-(R)-2-amino-butan-1-olato-\kN,O:O)-dibromido-dicopper(II)]-
[bis((R)-2-amino-butan-1-ol-\kN,O)-dibromido-copper(II)]-
[((R)-2-amino-butan-1-ol-\kN,O)-dibromido-methanol-copper(II)]
;
_chemical_name_common
;
Bis(bis(mu-(R)-2-amino-butan-1-olato-kappaN,O:O)-dibromido-
dicopper(ii))-(bis((R)-2-amino-butan-1-ol-kappaN,O)-dibromido-
copper(ii))-(((R)-2-amino-butan-1-ol-kappaN,O)-dibromido-methanol-
copper(ii))
;
_chemical_melting_point ?
_chemical_formula_moiety 'C29 H77 Br8 Cu6 N7 O8'
_chemical_formula_sum 'C29 H77 Br8 Cu6 N7 O8'
_chemical_formula_weight 1672.50
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 monoclinic
_symmetry_space_group_name_H-M 'P 21'
_symmetry_space_group_name_Hall 'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 10.2700(17)
_cell_length_b 12.8186(16)
_cell_length_c 20.588(3)
_cell_angle_alpha 90.00
_cell_angle_beta 93.281(8)
_cell_angle_gamma 90.00
_cell_volume 2706.0(7)
_cell_formula_units_Z 2
_cell_measurement_temperature 103(2)
_cell_measurement_reflns_used 776
_cell_measurement_theta_min 2.721
_cell_measurement_theta_max 18.404
_exptl_crystal_description needle
_exptl_crystal_colour green
_exptl_crystal_size_max 0.05
_exptl_crystal_size_mid 0.01
_exptl_crystal_size_min 0.01
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.053
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1636
_exptl_absorpt_coefficient_mu 8.268
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6826
_exptl_absorpt_correction_T_max 0.9219
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 103(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 'Bruker APEX2 CCD area detector'
_diffrn_measurement_method '\w scans and \f scans '
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 9898
_diffrn_reflns_av_R_equivalents 0.0861
_diffrn_reflns_av_sigmaI/netI 0.1326
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 1.87
_diffrn_reflns_theta_max 18.85
_reflns_number_total 4223
_reflns_number_gt 2829
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material 'publCIF (Westrip, 2009)'
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH and CH~2~
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~)
and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~),
with U~iso~(H) = 1.2U~eq~(CH).
H atoms on the amin nitrogen atoms were found and
refined with U~iso~(H) = 1.2U~eq~(N).
;
_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.
44 Uiso/Uij restrained atom sites, 48 distance or angle restraints and
428 least-squares restraints were used in the refinement.
The DFIX restraint was applied to the O-H Bonds with a distance of 0.87 Ang.
for O-H bonds of compounds measured at the according temperature.
(O5-H5, O8-H8 and O7-H7)
The SADI restraint was used for the chemically equivalent alcoholate
ligands in the dimeric
units and for the chemically similar alcohol ligands of the monomeric units.
The soft restraint DANG was used to fix problems with the tetrahedral
angle of
C3, C26 and C27 as well as avoiding the movement of the lightweight
proton towards
the Cu-atom
The restraints SIMU (similar Uij values for adjoining atoms) and DELU
(rigid-bond) were
applied to the Uij values of all N, C and O atoms with the defult esd.
(SIMU $N $C $O, DELU $N $O $C).
However, some atoms went to non-positive-definite and were further
restrained with a soft restraint to be approximately isotropic with the
ISOR restraint
with default esd.
(ISOR C9 O8 N6 N2 C29)
;
_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^)+(0.0557P)^2^+11.2618P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.04(4)
_refine_ls_number_reflns 4223
_refine_ls_number_parameters 538
_refine_ls_number_restraints 429
_refine_ls_R_factor_all 0.1149
_refine_ls_R_factor_gt 0.0649
_refine_ls_wR_factor_ref 0.1502
_refine_ls_wR_factor_gt 0.1260
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_restrained_S_all 1.010
_refine_ls_shift/su_max 0.002
_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 0.5086(4) 0.3148(4) 0.65443(19) 0.0495(13) Uani 1 1 d . . .
Cu2 Cu 0.4870(4) 0.4657(3) 0.7561(2) 0.0553(14) Uani 1 1 d . . .
Cu3 Cu 0.5048(3) 0.8156(3) 0.84187(17) 0.0301(11) Uani 1 1 d . . .
Cu4 Cu 0.4885(4) 0.9620(3) 0.7370(2) 0.0393(12) Uani 1 1 d . . .
Cu5 Cu 0.5345(4) 0.1760(3) 0.90672(19) 0.0358(12) Uani 1 1 d . . .
Cu6 Cu 0.4902(5) 0.6699(3) 0.5902(2) 0.0696(16) Uani 1 1 d D . .
Br1 Br 0.6708(3) 0.2231(3) 0.60096(16) 0.0452(10) Uani 1 1 d . . .
Br2 Br 0.3226(4) 0.4824(3) 0.83204(18) 0.0579(12) Uani 1 1 d . . .
Br3 Br 0.6626(3) 0.7195(2) 0.90805(15) 0.0340(9) Uani 1 1 d . . .
Br4 Br 0.3190(4) 0.9818(3) 0.65320(17) 0.0527(11) Uani 1 1 d . . .
Br5 Br 0.5145(3) 0.1908(2) 0.77201(15) 0.0355(10) Uani 1 1 d . . .
Br6 Br 0.6714(3) 0.3191(3) 0.95072(16) 0.0468(10) Uani 1 1 d . . .
Br7 Br 0.4837(3) 0.6945(3) 0.72152(16) 0.0373(10) Uani 1 1 d . . .
Br8 Br 0.6366(4) 0.7975(3) 0.55086(17) 0.0602(12) Uani 1 1 d . . .
O1 O 0.375(2) 0.4181(17) 0.6780(11) 0.061(7) Uani 1 1 d DU . .
C1 C 0.243(3) 0.371(3) 0.686(2) 0.085(10) Uani 1 1 d DU . .
H1A H 0.2225 0.3693 0.7323 0.102 Uiso 1 1 calc R . .
H1B H 0.1745 0.4103 0.6609 0.102 Uiso 1 1 calc R . .
C2 C 0.254(3) 0.264(3) 0.6602(18) 0.107(10) Uani 1 1 d DU . .
H2 H 0.2506 0.2109 0.6955 0.129 Uiso 1 1 calc R . .
C3 C 0.137(4) 0.255(4) 0.6110(19) 0.175(16) Uani 1 1 d DU . .
H3C H 0.1336 0.1852 0.5899 0.210 Uiso 1 1 calc R . .
H3D H 0.1378 0.3096 0.5773 0.210 Uiso 1 1 calc R . .
C4 C 0.024(3) 0.270(5) 0.656(3) 0.28(3) Uani 1 1 d DU . .
H4C H 0.0367 0.3354 0.6801 0.416 Uiso 1 1 calc R . .
H4D H 0.0233 0.2116 0.6870 0.416 Uiso 1 1 calc R . .
H4E H -0.0584 0.2719 0.6301 0.416 Uiso 1 1 calc R . .
N1 N 0.363(2) 0.242(2) 0.6170(12) 0.053(8) Uani 1 1 d DU . .
H1C H 0.3421 0.2652 0.5754 0.064 Uiso 1 1 calc R . .
H1D H 0.3793 0.1714 0.6155 0.064 Uiso 1 1 calc R . .
O2 O 0.620(2) 0.4229(16) 0.6921(11) 0.061(7) Uani 1 1 d DU . .
C5 C 0.742(3) 0.396(3) 0.7333(16) 0.087(9) Uani 1 1 d DU . .
H5C H 0.7313 0.3251 0.7518 0.105 Uiso 1 1 calc R . .
H5D H 0.8163 0.3934 0.7049 0.105 Uiso 1 1 calc R . .
C6 C 0.773(3) 0.471(2) 0.7880(14) 0.065(7) Uani 1 1 d DU . .
H6 H 0.8379 0.4400 0.8206 0.078 Uiso 1 1 calc R . .
C7 C 0.825(3) 0.576(2) 0.7616(16) 0.075(10) Uani 1 1 d DU . .
H7C H 0.7563 0.6059 0.7313 0.089 Uiso 1 1 calc R . .
H7D H 0.8383 0.6247 0.7985 0.089 Uiso 1 1 calc R . .
C8 C 0.953(3) 0.569(4) 0.726(2) 0.18(2) Uani 1 1 d DU . .
H8A H 1.0145 0.5227 0.7499 0.264 Uiso 1 1 calc R . .
H8B H 0.9913 0.6386 0.7229 0.264 Uiso 1 1 calc R . .
H8C H 0.9345 0.5411 0.6819 0.264 Uiso 1 1 calc R . .
N2 N 0.643(2) 0.489(2) 0.8184(12) 0.042(7) Uani 1 1 d DU . .
H2A H 0.6406 0.5564 0.8338 0.051 Uiso 1 1 calc R . .
H2B H 0.6373 0.4450 0.8534 0.051 Uiso 1 1 calc R . .
O3 O 0.3805(17) 0.9263(13) 0.8070(9) 0.026(5) Uani 1 1 d DU . .
C9 C 0.248(2) 0.877(2) 0.8022(12) 0.032(7) Uani 1 1 d DU . .
H9A H 0.2398 0.8312 0.7635 0.038 Uiso 1 1 calc R . .
H9B H 0.1802 0.9317 0.7977 0.038 Uiso 1 1 calc R . .
C10 C 0.232(2) 0.815(2) 0.8625(13) 0.043(7) Uani 1 1 d DU . .
H10 H 0.2298 0.8636 0.9004 0.052 Uiso 1 1 calc R . .
C11 C 0.099(3) 0.757(3) 0.8544(15) 0.064(9) Uani 1 1 d DU . .
H11A H 0.0285 0.8095 0.8481 0.077 Uiso 1 1 calc R . .
H11B H 0.0982 0.7134 0.8147 0.077 Uiso 1 1 calc R . .
C12 C 0.071(3) 0.688(3) 0.9128(16) 0.095(14) Uani 1 1 d DU . .
H12A H 0.1398 0.6351 0.9187 0.142 Uiso 1 1 calc R . .
H12B H -0.0134 0.6540 0.9051 0.142 Uiso 1 1 calc R . .
H12C H 0.0703 0.7313 0.9521 0.142 Uiso 1 1 calc R . .
N3 N 0.350(2) 0.7438(18) 0.8726(13) 0.049(7) Uani 1 1 d DU . .
H3A H 0.3360 0.6827 0.8498 0.059 Uiso 1 1 calc R . .
H3B H 0.3633 0.7277 0.9160 0.059 Uiso 1 1 calc R . .
O4 O 0.6170(19) 0.9167(14) 0.8053(9) 0.034(5) Uani 1 1 d DU . .
C13 C 0.739(2) 0.888(2) 0.7725(13) 0.042(7) Uani 1 1 d DU . .
H13A H 0.8139 0.8845 0.8050 0.050 Uiso 1 1 calc R . .
H13B H 0.7287 0.8192 0.7512 0.050 Uiso 1 1 calc R . .
C14 C 0.763(2) 0.970(2) 0.7227(13) 0.048(7) Uani 1 1 d DU . .
H14 H 0.7838 1.0379 0.7455 0.058 Uiso 1 1 calc R . .
C15 C 0.885(3) 0.933(3) 0.6887(17) 0.091(11) Uani 1 1 d DU . .
H15A H 0.9614 0.9305 0.7204 0.109 Uiso 1 1 calc R . .
H15B H 0.8702 0.8619 0.6710 0.109 Uiso 1 1 calc R . .
C16 C 0.912(4) 1.009(4) 0.633(2) 0.18(2) Uani 1 1 d DU . .
H16A H 0.8908 1.0801 0.6467 0.263 Uiso 1 1 calc R . .
H16B H 0.8574 0.9901 0.5945 0.263 Uiso 1 1 calc R . .
H16C H 1.0040 1.0050 0.6238 0.263 Uiso 1 1 calc R . .
N4 N 0.634(2) 0.981(2) 0.6832(10) 0.037(6) Uani 1 1 d DU . .
H4A H 0.6305 0.9321 0.6504 0.045 Uiso 1 1 calc R . .
H4B H 0.6295 1.0460 0.6643 0.045 Uiso 1 1 calc R . .
O5 O 0.4062(18) 0.0516(15) 0.9041(11) 0.042(6) Uani 1 1 d DU . .
H5 H 0.397(5) 0.003(17) 0.874(11) 0.064 Uiso 1 1 d D . .
C17 C 0.273(3) 0.091(2) 0.9182(16) 0.054(8) Uani 1 1 d DU . .
H17A H 0.2051 0.0472 0.8954 0.065 Uiso 1 1 calc R . .
H17B H 0.2606 0.0871 0.9655 0.065 Uiso 1 1 calc R . .
C18 C 0.259(2) 0.202(2) 0.8956(14) 0.048(7) Uani 1 1 d DU . .
H18 H 0.2581 0.2021 0.8471 0.057 Uiso 1 1 calc R . .
C19 C 0.130(3) 0.252(3) 0.9158(16) 0.074(10) Uani 1 1 d DU . .
H19A H 0.1159 0.2342 0.9617 0.089 Uiso 1 1 calc R . .
H19B H 0.1361 0.3286 0.9122 0.089 Uiso 1 1 calc R . .
C20 C 0.014(3) 0.213(4) 0.872(2) 0.152(19) Uani 1 1 d DU . .
H20A H 0.0176 0.2435 0.8289 0.228 Uiso 1 1 calc R . .
H20B H -0.0675 0.2329 0.8913 0.228 Uiso 1 1 calc R . .
H20C H 0.0182 0.1365 0.8689 0.228 Uiso 1 1 calc R . .
N5 N 0.384(2) 0.2524(18) 0.9219(12) 0.051(7) Uani 1 1 d DU . .
H5A H 0.3793 0.2618 0.9660 0.061 Uiso 1 1 calc R . .
H5B H 0.3903 0.3172 0.9032 0.061 Uiso 1 1 calc R . .
O6 O 0.575(2) 0.084(2) 1.0154(10) 0.094(8) Uani 1 1 d DU . .
H6A H 0.5102 0.0929 0.9856 0.140 Uiso 1 1 d D . .
C21 C 0.673(3) 0.001(3) 0.9978(19) 0.101(12) Uani 1 1 d DU . .
H21A H 0.7204 -0.0241 1.0378 0.121 Uiso 1 1 calc R . .
H21B H 0.6263 -0.0585 0.9767 0.121 Uiso 1 1 calc R . .
C22 C 0.767(3) 0.046(3) 0.9527(14) 0.080(9) Uani 1 1 d DU . .
H22 H 0.8045 0.1104 0.9738 0.096 Uiso 1 1 calc R . .
C23 C 0.882(3) -0.026(3) 0.9378(16) 0.093(11) Uani 1 1 d DU . .
H23A H 0.9238 0.0008 0.8990 0.112 Uiso 1 1 calc R . .
H23B H 0.8483 -0.0967 0.9274 0.112 Uiso 1 1 calc R . .
C24 C 0.986(4) -0.033(4) 0.995(2) 0.124(16) Uani 1 1 d DU . .
H24A H 1.0509 0.0222 0.9914 0.186 Uiso 1 1 calc R . .
H24B H 1.0299 -0.1014 0.9941 0.186 Uiso 1 1 calc R . .
H24C H 0.9441 -0.0259 1.0365 0.186 Uiso 1 1 calc R . .
N6 N 0.682(2) 0.0805(18) 0.8943(11) 0.050(7) Uani 1 1 d DU . .
H6B H 0.6481 0.0215 0.8742 0.060 Uiso 1 1 calc R . .
H6C H 0.7348 0.1119 0.8656 0.060 Uiso 1 1 calc R . .
O7 O 0.339(3) 0.5578(18) 0.5885(16) 0.146(12) Uani 1 1 d DU . .
H7 H 0.350(5) 0.507(4) 0.616(3) 0.218 Uiso 1 1 d D . .
C25 C 0.225(4) 0.620(3) 0.613(2) 0.150(13) Uani 1 1 d DU . .
H25A H 0.1463 0.5759 0.6162 0.180 Uiso 1 1 calc R . .
H25B H 0.2474 0.6531 0.6554 0.180 Uiso 1 1 calc R . .
C26 C 0.207(3) 0.699(2) 0.5597(18) 0.124(11) Uani 1 1 d DU . .
H26 H 0.1914 0.6666 0.5158 0.149 Uiso 1 1 calc R . .
C27 C 0.096(3) 0.770(3) 0.577(2) 0.164(16) Uani 1 1 d DU . .
H27A H 0.1224 0.8124 0.6159 0.197 Uiso 1 1 calc R . .
H27B H 0.0190 0.7278 0.5876 0.197 Uiso 1 1 calc R . .
C28 C 0.060(5) 0.842(4) 0.520(3) 0.23(3) Uani 1 1 d DU . .
H28A H -0.0223 0.8182 0.4978 0.342 Uiso 1 1 calc R . .
H28B H 0.1291 0.8402 0.4890 0.342 Uiso 1 1 calc R . .
H28C H 0.0489 0.9134 0.5355 0.342 Uiso 1 1 calc R . .
N7 N 0.334(3) 0.758(2) 0.5663(14) 0.089(10) Uani 1 1 d DU . .
H7A H 0.3274 0.8092 0.5975 0.106 Uiso 1 1 calc R . .
H7B H 0.3471 0.7914 0.5275 0.106 Uiso 1 1 calc R . .
O8 O 0.616(3) 0.561(2) 0.6001(13) 0.104(10) Uani 1 1 d DU . .
H8 H 0.667(11) 0.555(11) 0.635(2) 0.155 Uiso 1 1 d D . .
C29 C 0.688(4) 0.524(3) 0.547(2) 0.129(17) Uani 1 1 d DU . .
H29A H 0.6329 0.5281 0.5064 0.194 Uiso 1 1 calc R . .
H29B H 0.7145 0.4514 0.5546 0.194 Uiso 1 1 calc R . .
H29C H 0.7658 0.5673 0.5428 0.194 Uiso 1 1 calc 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 0.071(3) 0.035(3) 0.044(3) -0.001(3) 0.012(2) 0.003(3)
Cu2 0.078(4) 0.036(3) 0.053(3) -0.004(3) 0.010(3) 0.007(3)
Cu3 0.039(3) 0.017(2) 0.034(3) 0.008(2) 0.006(2) -0.001(2)
Cu4 0.052(3) 0.030(3) 0.036(3) -0.001(2) 0.003(2) -0.003(3)
Cu5 0.050(3) 0.020(2) 0.039(3) 0.000(2) 0.016(2) -0.004(2)
Cu6 0.135(5) 0.035(3) 0.042(3) -0.005(2) 0.028(3) -0.008(3)
Br1 0.063(3) 0.036(2) 0.036(2) 0.005(2) 0.0042(19) 0.008(2)
Br2 0.091(3) 0.025(2) 0.060(3) 0.007(2) 0.031(2) 0.007(2)
Br3 0.038(2) 0.026(2) 0.039(2) 0.0038(19) 0.0056(17) 0.0038(19)
Br4 0.082(3) 0.026(2) 0.048(3) 0.005(2) -0.013(2) -0.007(2)
Br5 0.054(2) 0.024(2) 0.029(2) -0.0002(18) 0.0010(18) -0.0014(19)
Br6 0.066(3) 0.037(2) 0.037(2) -0.007(2) -0.003(2) -0.001(2)
Br7 0.048(2) 0.032(2) 0.032(2) -0.0007(19) 0.0056(18) 0.0004(19)
Br8 0.093(3) 0.051(3) 0.037(2) -0.007(2) 0.014(2) -0.001(2)
O1 0.071(16) 0.054(15) 0.062(17) -0.002(13) 0.022(14) 0.018(12)
C1 0.070(19) 0.08(2) 0.11(2) -0.012(18) 0.029(18) 0.010(16)
C2 0.074(18) 0.104(18) 0.15(3) -0.06(2) 0.033(15) -0.007(17)
C3 0.071(18) 0.22(3) 0.24(4) -0.15(3) 0.00(2) 0.05(3)
C4 0.08(2) 0.31(6) 0.45(7) -0.22(6) 0.09(3) 0.00(4)
N1 0.056(16) 0.059(19) 0.043(18) 0.006(15) -0.013(13) 0.012(15)
O2 0.087(18) 0.035(14) 0.064(18) -0.012(12) 0.019(12) -0.006(13)
C5 0.09(2) 0.09(2) 0.08(2) -0.029(16) 0.007(15) 0.005(18)
C6 0.082(16) 0.056(17) 0.058(19) -0.007(14) 0.017(13) 0.017(16)
C7 0.08(2) 0.10(2) 0.05(2) -0.011(17) 0.039(17) -0.028(19)
C8 0.07(3) 0.31(5) 0.16(4) -0.11(4) 0.06(3) -0.11(3)
N2 0.060(13) 0.028(13) 0.039(13) 0.024(11) 0.005(11) -0.004(12)
O3 0.028(11) 0.026(12) 0.023(13) -0.008(9) 0.004(10) 0.019(8)
C9 0.032(12) 0.028(13) 0.035(13) -0.027(10) 0.002(12) 0.002(10)
C10 0.049(14) 0.036(16) 0.046(15) -0.018(13) 0.019(15) 0.002(10)
C11 0.050(14) 0.08(2) 0.06(2) 0.012(16) 0.010(18) -0.006(14)
C12 0.04(2) 0.12(3) 0.12(3) 0.09(3) -0.01(2) 0.00(2)
N3 0.049(14) 0.036(17) 0.062(19) -0.001(13) -0.001(15) -0.012(11)
O4 0.055(14) 0.025(12) 0.022(13) 0.008(10) -0.006(10) 0.002(11)
C13 0.031(17) 0.061(19) 0.032(18) 0.020(13) -0.002(11) -0.012(15)
C14 0.063(15) 0.036(16) 0.048(18) 0.027(14) 0.012(10) 0.033(16)
C15 0.077(18) 0.11(3) 0.09(3) 0.045(19) 0.058(16) 0.02(2)
C16 0.17(4) 0.20(5) 0.17(5) 0.11(3) 0.10(3) 0.00(4)
N4 0.062(15) 0.028(15) 0.023(15) -0.002(13) 0.012(12) -0.003(15)
O5 0.050(13) 0.036(14) 0.042(16) -0.002(12) 0.006(12) -0.020(10)
C17 0.068(17) 0.048(14) 0.05(2) 0.007(16) 0.025(18) 0.006(13)
C18 0.064(15) 0.052(15) 0.030(17) -0.002(15) 0.028(14) 0.008(12)
C19 0.089(17) 0.07(2) 0.07(2) -0.013(19) 0.049(18) 0.024(16)
C20 0.052(18) 0.20(5) 0.21(5) -0.05(4) 0.03(3) 0.01(3)
N5 0.089(17) 0.036(16) 0.027(16) 0.008(13) -0.004(15) 0.014(12)
O6 0.12(2) 0.071(18) 0.09(2) -0.014(16) -0.024(15) 0.031(15)
C21 0.15(3) 0.06(2) 0.10(2) 0.04(2) 0.009(19) 0.050(18)
C22 0.13(2) 0.046(19) 0.065(19) 0.010(17) -0.016(13) 0.040(15)
C23 0.12(2) 0.05(2) 0.11(3) 0.00(2) -0.017(16) 0.036(18)
C24 0.11(3) 0.12(3) 0.14(4) 0.04(3) -0.02(2) 0.03(3)
N6 0.078(15) 0.033(13) 0.038(13) -0.021(11) -0.007(11) 0.019(12)
O7 0.23(3) 0.040(19) 0.17(3) 0.005(19) 0.03(2) -0.051(16)
C25 0.16(3) 0.10(3) 0.18(3) 0.02(2) 0.01(3) -0.057(19)
C26 0.15(3) 0.08(2) 0.14(3) -0.01(2) 0.04(2) -0.034(15)
C27 0.16(3) 0.14(3) 0.20(4) -0.01(3) 0.05(3) 0.00(2)
C28 0.20(5) 0.20(6) 0.29(6) 0.07(4) 0.07(5) 0.04(4)
N7 0.14(2) 0.040(19) 0.08(2) -0.010(16) 0.00(2) -0.013(16)
O8 0.156(18) 0.082(16) 0.076(16) 0.005(14) 0.031(14) 0.028(15)
C29 0.20(4) 0.08(3) 0.11(4) 0.01(3) 0.09(3) 0.01(3)
_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 N1 1.89(2) . ?
Cu1 O2 1.93(2) . ?
Cu1 O1 1.99(2) . ?
Cu1 Br1 2.362(5) . ?
Cu1 Cu2 2.869(6) . ?
Cu1 Br5 2.894(5) . ?
Cu2 N2 2.01(2) . ?
Cu2 O1 2.02(2) . ?
Cu2 O2 2.02(2) . ?
Cu2 Br2 2.375(6) . ?
Cu3 O4 1.92(2) . ?
Cu3 N3 1.97(2) . ?
Cu3 O3 2.012(17) . ?
Cu3 Br3 2.398(4) . ?
Cu3 Cu4 2.857(5) . ?
Cu4 O3 1.923(19) . ?
Cu4 N4 1.93(2) . ?
Cu4 O4 1.960(18) . ?
Cu4 Br4 2.394(5) . ?
Cu5 N5 1.87(2) . ?
Cu5 N6 1.97(2) . ?
Cu5 O5 2.067(18) . ?
Cu5 Br6 2.454(5) . ?
Cu5 Br5 2.776(5) . ?
Cu5 H6A 1.9688 . ?
Cu6 O8 1.91(3) . ?
Cu6 N7 2.00(3) . ?
Cu6 O7 2.11(3) . ?
Cu6 Br8 2.394(6) . ?
Cu6 Br7 2.727(5) . ?
O1 C1 1.503(19) . ?
C1 C2 1.47(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N1 1.492(19) . ?
C2 C3 1.532(15) . ?
C2 H2 1.0000 . ?
C3 C4 1.537(16) . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C4 H4C 0.9800 . ?
C4 H4D 0.9800 . ?
C4 H4E 0.9800 . ?
N1 H1C 0.9200 . ?
N1 H1D 0.9200 . ?
O2 C5 1.514(19) . ?
C5 C6 1.51(2) . ?
C5 H5C 0.9900 . ?
C5 H5D 0.9900 . ?
C6 N2 1.525(18) . ?
C6 C7 1.55(2) . ?
C6 H6 1.0000 . ?
C7 C8 1.55(2) . ?
C7 H7C 0.9900 . ?
C7 H7D 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N2 H2A 0.9200 . ?
N2 H2B 0.9200 . ?
O3 C9 1.495(18) . ?
C9 C10 1.49(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N3 1.520(18) . ?
C10 C11 1.553(19) . ?
C10 H10 1.0000 . ?
C11 C12 1.53(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N3 H3A 0.9200 . ?
N3 H3B 0.9200 . ?
O4 C13 1.503(19) . ?
C13 C14 1.50(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 N4 1.520(18) . ?
C14 C15 1.55(2) . ?
C14 H14 1.0000 . ?
C15 C16 1.53(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N4 H4A 0.9200 . ?
N4 H4B 0.9200 . ?
O5 C17 1.505(19) . ?
O5 H5 0.871(10) . ?
C17 C18 1.50(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 N5 1.512(18) . ?
C18 C19 1.547(19) . ?
C18 H18 1.0000 . ?
C19 C20 1.53(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
N5 H5A 0.9200 . ?
N5 H5B 0.9200 . ?
O6 C21 1.519(19) . ?
O6 H6A 0.8834 . ?
C21 C22 1.49(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N6 1.512(18) . ?
C22 C23 1.55(2) . ?
C22 H22 1.0000 . ?
C23 C24 1.55(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N6 H6B 0.9200 . ?
N6 H6C 0.9200 . ?
O7 C25 1.53(2) . ?
O7 H7 0.869(10) . ?
C25 C26 1.50(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 N7 1.512(19) . ?
C26 C27 1.519(16) . ?
C26 H26 1.0000 . ?
C27 C28 1.526(16) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
N7 H7A 0.9200 . ?
N7 H7B 0.9200 . ?
O8 C29 1.44(4) . ?
O8 H8 0.872(10) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 O2 162.7(10) . . ?
N1 Cu1 O1 83.5(10) . . ?
O2 Cu1 O1 79.8(10) . . ?
N1 Cu1 Br1 97.3(8) . . ?
O2 Cu1 Br1 97.4(7) . . ?
O1 Cu1 Br1 163.9(7) . . ?
N1 Cu1 Cu2 122.5(8) . . ?
O2 Cu1 Cu2 44.8(7) . . ?
O1 Cu1 Cu2 44.6(7) . . ?
Br1 Cu1 Cu2 139.6(2) . . ?
N1 Cu1 Br5 92.7(8) . . ?
O2 Cu1 Br5 94.3(7) . . ?
O1 Cu1 Br5 98.2(7) . . ?
Br1 Cu1 Br5 97.75(18) . . ?
Cu2 Cu1 Br5 76.03(14) . . ?
N2 Cu2 O1 161.4(10) . . ?
N2 Cu2 O2 85.1(10) . . ?
O1 Cu2 O2 76.8(9) . . ?
N2 Cu2 Br2 97.9(7) . . ?
O1 Cu2 Br2 99.1(7) . . ?
O2 Cu2 Br2 169.4(6) . . ?
N2 Cu2 Cu1 118.2(7) . . ?
O1 Cu2 Cu1 43.8(6) . . ?
O2 Cu2 Cu1 42.2(6) . . ?
Br2 Cu2 Cu1 128.9(2) . . ?
O4 Cu3 N3 162.8(9) . . ?
O4 Cu3 O3 76.5(8) . . ?
N3 Cu3 O3 86.4(8) . . ?
O4 Cu3 Br3 99.7(6) . . ?
N3 Cu3 Br3 96.3(7) . . ?
O3 Cu3 Br3 163.5(5) . . ?
O4 Cu3 Cu4 43.1(6) . . ?
N3 Cu3 Cu4 122.4(7) . . ?
O3 Cu3 Cu4 42.2(5) . . ?
Br3 Cu3 Cu4 140.80(18) . . ?
O3 Cu4 N4 163.8(9) . . ?
O3 Cu4 O4 77.6(8) . . ?
N4 Cu4 O4 86.3(9) . . ?
O3 Cu4 Br4 98.0(5) . . ?
N4 Cu4 Br4 97.4(6) . . ?
O4 Cu4 Br4 168.7(6) . . ?
O3 Cu4 Cu3 44.7(5) . . ?
N4 Cu4 Cu3 120.2(7) . . ?
O4 Cu4 Cu3 42.0(6) . . ?
Br4 Cu4 Cu3 128.5(2) . . ?
N5 Cu5 N6 173.0(11) . . ?
N5 Cu5 O5 82.9(9) . . ?
N6 Cu5 O5 90.6(9) . . ?
N5 Cu5 Br6 90.5(7) . . ?
N6 Cu5 Br6 94.9(7) . . ?
O5 Cu5 Br6 159.6(6) . . ?
N5 Cu5 Br5 96.7(7) . . ?
N6 Cu5 Br5 85.8(7) . . ?
O5 Cu5 Br5 90.9(6) . . ?
Br6 Cu5 Br5 109.02(17) . . ?
N5 Cu5 H6A 90.0 . . ?
N6 Cu5 H6A 84.6 . . ?
O5 Cu5 H6A 59.6 . . ?
Br6 Cu5 H6A 101.4 . . ?
Br5 Cu5 H6A 148.8 . . ?
O8 Cu6 N7 166.0(12) . . ?
O8 Cu6 O7 89.8(12) . . ?
N7 Cu6 O7 78.8(11) . . ?
O8 Cu6 Br8 95.8(9) . . ?
N7 Cu6 Br8 92.2(8) . . ?
O7 Cu6 Br8 159.0(9) . . ?
O8 Cu6 Br7 92.0(8) . . ?
N7 Cu6 Br7 96.5(9) . . ?
O7 Cu6 Br7 92.0(9) . . ?
Br8 Cu6 Br7 107.9(2) . . ?
Cu5 Br5 Cu1 150.47(16) . . ?
C1 O1 Cu1 113.3(18) . . ?
C1 O1 Cu2 121(2) . . ?
Cu1 O1 Cu2 91.6(10) . . ?
C2 C1 O1 104(3) . . ?
C2 C1 H1A 110.9 . . ?
O1 C1 H1A 110.9 . . ?
C2 C1 H1B 110.9 . . ?
O1 C1 H1B 110.9 . . ?
H1A C1 H1B 108.9 . . ?
C1 C2 N1 118(3) . . ?
C1 C2 C3 104(3) . . ?
N1 C2 C3 100(3) . . ?
C1 C2 H2 111.4 . . ?
N1 C2 H2 111.4 . . ?
C3 C2 H2 111.4 . . ?
C2 C3 C4 100(2) . . ?
C2 C3 H3C 111.7 . . ?
C4 C3 H3C 111.7 . . ?
C2 C3 H3D 111.7 . . ?
C4 C3 H3D 111.7 . . ?
H3C C3 H3D 109.5 . . ?
C3 C4 H4C 109.5 . . ?
C3 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
C3 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
C2 N1 Cu1 105.2(19) . . ?
C2 N1 H1C 110.7 . . ?
Cu1 N1 H1C 110.7 . . ?
C2 N1 H1D 110.7 . . ?
Cu1 N1 H1D 110.7 . . ?
H1C N1 H1D 108.8 . . ?
C5 O2 Cu1 120.7(19) . . ?
C5 O2 Cu2 105(2) . . ?
Cu1 O2 Cu2 93.0(10) . . ?
C6 C5 O2 114(3) . . ?
C6 C5 H5C 108.8 . . ?
O2 C5 H5C 108.8 . . ?
C6 C5 H5D 108.8 . . ?
O2 C5 H5D 108.8 . . ?
H5C C5 H5D 107.7 . . ?
C5 C6 N2 104(3) . . ?
C5 C6 C7 111(3) . . ?
N2 C6 C7 110(2) . . ?
C5 C6 H6 110.6 . . ?
N2 C6 H6 110.6 . . ?
C7 C6 H6 110.6 . . ?
C8 C7 C6 116(3) . . ?
C8 C7 H7C 108.3 . . ?
C6 C7 H7C 108.3 . . ?
C8 C7 H7D 108.3 . . ?
C6 C7 H7D 108.3 . . ?
H7C C7 H7D 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 N2 Cu2 113.6(19) . . ?
C6 N2 H2A 108.9 . . ?
Cu2 N2 H2A 108.9 . . ?
C6 N2 H2B 108.9 . . ?
Cu2 N2 H2B 108.9 . . ?
H2A N2 H2B 107.7 . . ?
C9 O3 Cu4 127.6(15) . . ?
C9 O3 Cu3 106.3(14) . . ?
Cu4 O3 Cu3 93.1(7) . . ?
O3 C9 C10 108(2) . . ?
O3 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
O3 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
C9 C10 N3 108(2) . . ?
C9 C10 C11 108(2) . . ?
N3 C10 C11 115(2) . . ?
C9 C10 H10 108.8 . . ?
N3 C10 H10 108.8 . . ?
C11 C10 H10 108.8 . . ?
C12 C11 C10 113(2) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 N3 Cu3 109.1(16) . . ?
C10 N3 H3A 109.9 . . ?
Cu3 N3 H3A 109.9 . . ?
C10 N3 H3B 109.9 . . ?
Cu3 N3 H3B 109.9 . . ?
H3A N3 H3B 108.3 . . ?
C13 O4 Cu3 123.2(15) . . ?
C13 O4 Cu4 107.2(15) . . ?
Cu3 O4 Cu4 94.9(9) . . ?
C14 C13 O4 108(2) . . ?
C14 C13 H13A 110.1 . . ?
O4 C13 H13A 110.1 . . ?
C14 C13 H13B 110.1 . . ?
O4 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
C13 C14 N4 105(2) . . ?
C13 C14 C15 105(2) . . ?
N4 C14 C15 119(3) . . ?
C13 C14 H14 109.1 . . ?
N4 C14 H14 109.1 . . ?
C15 C14 H14 109.1 . . ?
C16 C15 C14 109(3) . . ?
C16 C15 H15A 109.9 . . ?
C14 C15 H15A 109.9 . . ?
C16 C15 H15B 109.9 . . ?
C14 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 N4 Cu4 111.2(16) . . ?
C14 N4 H4A 109.4 . . ?
Cu4 N4 H4A 109.4 . . ?
C14 N4 H4B 109.4 . . ?
Cu4 N4 H4B 109.4 . . ?
H4A N4 H4B 108.0 . . ?
C17 O5 Cu5 108.8(16) . . ?
C17 O5 H5 108(3) . . ?
Cu5 O5 H5 127(10) . . ?
C18 C17 O5 109(2) . . ?
C18 C17 H17A 109.8 . . ?
O5 C17 H17A 109.8 . . ?
C18 C17 H17B 109.8 . . ?
O5 C17 H17B 109.8 . . ?
H17A C17 H17B 108.2 . . ?
C17 C18 N5 103(2) . . ?
C17 C18 C19 112(2) . . ?
N5 C18 C19 117(2) . . ?
C17 C18 H18 108.1 . . ?
N5 C18 H18 108.1 . . ?
C19 C18 H18 108.1 . . ?
C20 C19 C18 111(3) . . ?
C20 C19 H19A 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 N5 Cu5 114.2(16) . . ?
C18 N5 H5A 108.7 . . ?
Cu5 N5 H5A 108.7 . . ?
C18 N5 H5B 108.7 . . ?
Cu5 N5 H5B 108.7 . . ?
H5A N5 H5B 107.6 . . ?
C21 O6 H6A 113.8 . . ?
C22 C21 O6 110(3) . . ?
C22 C21 H21A 109.7 . . ?
O6 C21 H21A 109.7 . . ?
C22 C21 H21B 109.7 . . ?
O6 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
C21 C22 N6 104(3) . . ?
C21 C22 C23 115(3) . . ?
N6 C22 C23 116(2) . . ?
C21 C22 H22 107.2 . . ?
N6 C22 H22 107.2 . . ?
C23 C22 H22 107.2 . . ?
C22 C23 C24 113(3) . . ?
C22 C23 H23A 109.0 . . ?
C24 C23 H23A 109.0 . . ?
C22 C23 H23B 109.0 . . ?
C24 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 N6 Cu5 119.4(17) . . ?
C22 N6 H6B 107.5 . . ?
Cu5 N6 H6B 107.5 . . ?
C22 N6 H6C 107.5 . . ?
Cu5 N6 H6C 107.5 . . ?
H6B N6 H6C 107.0 . . ?
C25 O7 Cu6 103(2) . . ?
C25 O7 H7 104(2) . . ?
Cu6 O7 H7 115(5) . . ?
C26 C25 O7 100(2) . . ?
C26 C25 H25A 111.7 . . ?
O7 C25 H25A 111.7 . . ?
C26 C25 H25B 111.7 . . ?
O7 C25 H25B 111.7 . . ?
H25A C25 H25B 109.5 . . ?
C25 C26 N7 102(2) . . ?
C25 C26 C27 107(2) . . ?
N7 C26 C27 110(2) . . ?
C25 C26 H26 112.5 . . ?
N7 C26 H26 112.5 . . ?
C27 C26 H26 112.5 . . ?
C26 C27 C28 109(3) . . ?
C26 C27 H27A 109.8 . . ?
C28 C27 H27A 109.8 . . ?
C26 C27 H27B 109.8 . . ?
C28 C27 H27B 109.8 . . ?
H27A C27 H27B 108.3 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 N7 Cu6 114.4(17) . . ?
C26 N7 H7A 108.6 . . ?
Cu6 N7 H7A 108.6 . . ?
C26 N7 H7B 108.6 . . ?
Cu6 N7 H7B 108.6 . . ?
H7A N7 H7B 107.6 . . ?
C29 O8 Cu6 122(3) . . ?
C29 O8 H8 108(4) . . ?
Cu6 O8 H8 121(5) . . ?
O8 C29 H29A 109.5 . . ?
O8 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O8 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1C Br8 0.92 2.65 3.53(2) 159.2 2_646
N1 H1D Br4 0.92 2.64 3.45(3) 148.0 1_545
N2 H2A Br3 0.92 2.59 3.48(3) 163.0 .
N2 H2B Br6 0.92 2.58 3.49(2) 168.6 .
N3 H3A Br2 0.92 2.60 3.46(2) 156.8 .
N3 H3B Br6 0.92 3.02 3.78(3) 140.9 2_657
N4 H4A Br8 0.92 2.68 3.60(2) 175.1 .
N4 H4B Br1 0.92 2.66 3.56(3) 166.6 1_565
N5 H5A Br3 0.92 2.71 3.59(3) 159.8 2_647
N5 H5B Br2 0.92 2.65 3.52(2) 158.6 .
N7 H7A Br4 0.92 2.50 3.38(3) 162.5 .
N7 H7B Br1 0.92 2.78 3.47(3) 132.5 2_656
N3 H3B O6 0.92 2.39 3.15(3) 140.2 2_657
O5 H5 O3 0.871(10) 1.70(6) 2.57(3) 170(32) 1_545
O8 H8 O2 0.872(10) 2.13(16) 2.59(4) 112(15) .
O7 H7 O1 0.869(10) 1.72(4) 2.58(3) 174(8) .
O8 H8 O2 0.872(10) 2.13(16) 2.59(4) 112(15) .
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 18.85
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 1.187
_refine_diff_density_min -0.639
_refine_diff_density_rms 0.165
#===END
data_f1
_database_code_depnum_ccdc_archive 'CCDC 864927'
#TrackingRef '- All-crystaldata.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Bis[bis(\m-(R)-2-amino-butan-1-olato-\kN,O:O)-dibromido-dicopper(II)]-
bis[((R)-2-amino-butan-1-ol-\kN,O)-dibromido-ethanol-copper(II)]
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C28 H74 Cl8 Cu6 N6 O8'
_chemical_formula_sum 'C28 H74 Cl8 Cu6 N6 O8'
_chemical_formula_weight 1287.77
_chemical_absolute_configuration rmad
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
_symmetry_space_group_name_Hall 'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 10.3649(3)
_cell_length_b 12.7064(3)
_cell_length_c 19.3781(5)
_cell_angle_alpha 90.00
_cell_angle_beta 92.255(2)
_cell_angle_gamma 90.00
_cell_volume 2550.13(12)
_cell_formula_units_Z 2
_cell_measurement_temperature 103(2)
_cell_measurement_reflns_used 3213
_cell_measurement_theta_min 2.64
_cell_measurement_theta_max 18.636
_exptl_crystal_description nedle
_exptl_crystal_colour green
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.01
_exptl_crystal_size_min 0.01
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.677
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1316
_exptl_absorpt_coefficient_mu 2.921
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7588
_exptl_absorpt_correction_T_max 0.9714
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 103(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'micro-focus sealed tube'
_diffrn_radiation_monochromator 'multilayer mirror optics'
_diffrn_measurement_device_type 'Bruker APEX2 CCD area detector'
_diffrn_measurement_method '\w scans and/or \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 45441
_diffrn_reflns_av_R_equivalents 0.1089
_diffrn_reflns_av_sigmaI/netI 0.0753
_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
_diffrn_reflns_theta_min 1.05
_diffrn_reflns_theta_max 22.21
_reflns_number_total 6422
_reflns_number_gt 4315
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material 'publCIF (Westrip, 2009)'
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH and CH~2~
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~)
and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~),
with U~iso~(H) = 1.2U~eq~(CH).
H atoms on the amin nitrogen atoms were found and
refined with U~iso~(H) = 1.2U~eq~(N).
The largest residual Fourier peak (1.06 e \%A^-3^) is
found within 0.6 \%A of the Cd atom. The deepest hole (-0.92) is 0.03
\%A from the Cd atom.
Note on disorder or other problems etc. during refinement
;
_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^)+(0.0315P)^2^+7.7871P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.00(2)
_refine_ls_number_reflns 6422
_refine_ls_number_parameters 610
_refine_ls_number_restraints 811
_refine_ls_R_factor_all 0.0960
_refine_ls_R_factor_gt 0.0494
_refine_ls_wR_factor_ref 0.1095
_refine_ls_wR_factor_gt 0.0912
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_restrained_S_all 1.020
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.49573(15) 0.37449(11) 0.65582(6) 0.0368(4) Uani 1 1 d D . .
Cu2 Cu 0.51641(14) 0.52717(11) 0.76682(6) 0.0395(4) Uani 1 1 d D . .
Cl1 Cl 0.3457(3) 0.2890(2) 0.59023(14) 0.0418(8) Uani 1 1 d . . .
Cl2 Cl 0.6752(4) 0.5427(3) 0.84833(16) 0.0603(10) Uani 1 1 d . . .
O1 O 0.6230(7) 0.4795(5) 0.6917(3) 0.038(2) Uani 1 1 d DU . .
N1 N 0.6462(9) 0.3036(7) 0.6189(4) 0.039(2) Uani 1 1 d DU . .
H1A H 0.6547 0.2379 0.6384 0.047 Uiso 1 1 calc R . .
H1B H 0.6337 0.2952 0.5719 0.047 Uiso 1 1 calc R . .
C1 C 0.7485(9) 0.4313(8) 0.6977(5) 0.042(3) Uani 1 1 d DU . .
H1C H 0.7544 0.3858 0.7391 0.050 Uiso 1 1 calc R . .
H1D H 0.8159 0.4863 0.7026 0.050 Uiso 1 1 calc R . .
C2 C 0.7695(9) 0.3663(8) 0.6337(5) 0.040(3) Uani 1 1 d DU A .
H2 H 0.7773 0.4171 0.5946 0.048 Uiso 1 1 calc R . .
C3 C 0.8934(12) 0.3029(9) 0.6377(6) 0.062(4) Uani 1 1 d DU . .
H3A H 0.9641 0.3507 0.6534 0.075 Uiso 0.763(15) 1 calc PR A 1
H3B H 0.8847 0.2488 0.6740 0.075 Uiso 0.763(15) 1 calc PR A 1
H3C H 0.9082 0.2800 0.6862 0.075 Uiso 0.237(15) 1 d PR A 2
H3D H 0.8817 0.2389 0.6089 0.075 Uiso 0.237(15) 1 d PR A 2
C4 C 0.9328(15) 0.2510(13) 0.5766(7) 0.060(5) Uani 0.763(15) 1 d PDU A 1
H4A H 0.8785 0.1889 0.5679 0.090 Uiso 0.763(15) 1 calc PR A 1
H4B H 1.0232 0.2293 0.5827 0.090 Uiso 0.763(15) 1 calc PR A 1
H4C H 0.9236 0.2993 0.5373 0.090 Uiso 0.763(15) 1 calc PR A 1
C4A C 1.004(2) 0.360(3) 0.616(2) 0.060(5) Uani 0.237(15) 1 d PDU A 2
H4D H 1.0252 0.3371 0.5692 0.090 Uiso 0.237(15) 1 calc PR A 2
H4E H 1.0779 0.3453 0.6478 0.090 Uiso 0.237(15) 1 calc PR A 2
H4F H 0.9857 0.4353 0.6156 0.090 Uiso 0.237(15) 1 calc PR A 2
O2 O 0.3843(7) 0.4781(5) 0.6978(3) 0.0351(19) Uani 1 1 d DU . .
N2 N 0.3696(9) 0.5465(8) 0.8269(4) 0.048(3) Uani 1 1 d DU . .
H2A H 0.3729 0.4965 0.8613 0.057 Uiso 1 1 calc R . .
H2B H 0.3746 0.6118 0.8473 0.057 Uiso 1 1 calc R . .
C5 C 0.2665(9) 0.4547(8) 0.7307(5) 0.040(3) Uani 1 1 d DU . .
H5C H 0.2717 0.3839 0.7520 0.048 Uiso 1 1 calc R . .
H5D H 0.1935 0.4551 0.6961 0.048 Uiso 1 1 calc R . .
C6 C 0.2445(10) 0.5368(10) 0.7856(5) 0.049(3) Uani 1 1 d DU B .
H6C H 0.2299 0.6054 0.7612 0.059 Uiso 1 1 calc R . .
C7 C 0.1262(14) 0.5157(11) 0.8263(6) 0.082(4) Uani 1 1 d DU . .
H7A H 0.1309 0.4429 0.8444 0.099 Uiso 0.288(18) 1 calc PR B 1
H7B H 0.1264 0.5641 0.8663 0.099 Uiso 0.288(18) 1 calc PR B 1
H7C H 0.0506 0.5356 0.7962 0.099 Uiso 0.712(18) 1 d PR B 2
H7D H 0.1199 0.4393 0.8356 0.099 Uiso 0.712(18) 1 d PR B 2
C8 C 0.0064(17) 0.528(5) 0.787(2) 0.119(8) Uani 0.288(18) 1 d PDU B 1
H8A H -0.0641 0.4967 0.8121 0.178 Uiso 0.288(18) 1 calc PR B 1
H8B H 0.0127 0.4932 0.7420 0.178 Uiso 0.288(18) 1 calc PR B 1
H8C H -0.0110 0.6033 0.7796 0.178 Uiso 0.288(18) 1 calc PR B 1
C8A C 0.090(2) 0.5946(18) 0.8750(12) 0.119(8) Uani 0.712(18) 1 d PDU B 2
H8D H 0.1502 0.5933 0.9151 0.178 Uiso 0.712(18) 1 calc PR B 2
H8E H 0.0022 0.5803 0.8899 0.178 Uiso 0.712(18) 1 calc PR B 2
H8F H 0.0920 0.6641 0.8531 0.178 Uiso 0.712(18) 1 calc PR B 2
Cu3 Cu 0.49524(13) 0.87258(11) 0.83959(6) 0.0291(3) Uani 1 1 d D C .
Cu4 Cu 0.51792(14) 1.03064(11) 0.73203(7) 0.0364(4) Uani 1 1 d D C .
Cl3 Cl 0.3415(3) 0.7901(2) 0.89669(13) 0.0331(7) Uani 1 1 d . . .
Cl4 Cl 0.6778(3) 1.0510(2) 0.65817(15) 0.0454(9) Uani 1 1 d . . .
O3 O 0.6262(7) 0.9746(5) 0.8091(3) 0.0331(19) Uani 1 1 d DU . .
N3 N 0.6457(7) 0.7985(7) 0.8802(4) 0.030(2) Uani 1 1 d DU . .
H3E H 0.6657 0.8232 0.9240 0.036 Uiso 0.549(9) 1 calc PR C 2
H3F H 0.6300 0.7274 0.8827 0.036 Uiso 0.549(9) 1 calc PR C 2
H3G H 0.6386 0.7976 0.9274 0.036 Uiso 0.451(9) 1 d PR C 1
H3H H 0.6440 0.7298 0.8652 0.036 Uiso 0.451(9) 1 d PR C 1
C9 C 0.7498(11) 0.9270(15) 0.8033(12) 0.050(6) Uani 0.549(9) 1 d PDU C 2
H9A H 0.8161 0.9712 0.8274 0.060 Uiso 0.549(9) 1 calc PR C 2
H9B H 0.7710 0.9229 0.7540 0.060 Uiso 0.549(9) 1 calc PR C 2
C10 C 0.7527(12) 0.8202(11) 0.8334(9) 0.036(3) Uani 0.549(9) 1 d PDU C 2
H10 H 0.7385 0.7712 0.7935 0.043 Uiso 0.549(9) 1 calc PR C 2
C11 C 0.8777(14) 0.7865(15) 0.8680(10) 0.042(4) Uani 0.549(9) 1 d PDU C 2
H11A H 0.8872 0.8222 0.9133 0.051 Uiso 0.549(9) 1 calc PR C 2
H11B H 0.8740 0.7098 0.8767 0.051 Uiso 0.549(9) 1 calc PR C 2
C12 C 0.9900(15) 0.809(2) 0.8291(13) 0.079(6) Uani 0.549(9) 1 d PDU C 2
H12A H 0.9807 0.7753 0.7836 0.118 Uiso 0.549(9) 1 calc PR C 2
H12B H 1.0671 0.7810 0.8538 0.118 Uiso 0.549(9) 1 calc PR C 2
H12C H 0.9988 0.8850 0.8234 0.118 Uiso 0.549(9) 1 calc PR C 2
C9A C 0.7513(13) 0.927(2) 0.8076(16) 0.050(6) Uani 0.451(9) 1 d PDU C 1
H9C H 0.8178 0.9829 0.8121 0.060 Uiso 0.451(9) 1 calc PR C 1
H9D H 0.7606 0.8925 0.7623 0.060 Uiso 0.451(9) 1 calc PR C 1
C10A C 0.7753(13) 0.8484(14) 0.8630(9) 0.036(3) Uani 0.451(9) 1 d PDU C 1
H10A H 0.8293 0.7914 0.8432 0.043 Uiso 0.451(9) 1 calc PR C 1
C11A C 0.854(2) 0.8977(16) 0.9210(10) 0.042(4) Uani 0.451(9) 1 d PDU C 1
H11C H 0.9238 0.9401 0.9010 0.051 Uiso 0.451(9) 1 calc PR C 1
H11D H 0.7985 0.9465 0.9462 0.051 Uiso 0.451(9) 1 calc PR C 1
C12A C 0.913(2) 0.824(2) 0.9703(12) 0.079(6) Uani 0.451(9) 1 d PDU C 1
H12D H 0.9451 0.8624 1.0114 0.118 Uiso 0.451(9) 1 calc PR C 1
H12E H 0.9847 0.7876 0.9492 0.118 Uiso 0.451(9) 1 calc PR C 1
H12R H 0.8482 0.7724 0.9837 0.118 Uiso 0.451(9) 1 calc PR C 1
N4 N 0.3714(8) 1.0474(8) 0.6655(4) 0.044(3) Uani 1 1 d DU . .
H4G H 0.3710 1.1151 0.6486 0.053 Uiso 1 1 calc R C .
H4H H 0.3819 1.0024 0.6289 0.053 Uiso 1 1 calc R . .
O4 O 0.3847(7) 0.9808(6) 0.7939(3) 0.038(2) Uani 1 1 d DU . .
C13 C 0.2701(9) 0.9496(9) 0.7535(6) 0.063(4) Uani 1 1 d DU C .
H13A H 0.1953 0.9465 0.7837 0.076 Uiso 1 1 calc R . .
H13B H 0.2831 0.8785 0.7340 0.076 Uiso 1 1 calc R . .
C14 C 0.2433(11) 1.0252(10) 0.6970(5) 0.062(3) Uani 1 1 d DU C .
H14 H 0.1827 0.9928 0.6616 0.075 Uiso 1 1 calc R . .
C15 C 0.1855(13) 1.1285(10) 0.7235(7) 0.077(4) Uani 1 1 d DU . .
H15A H 0.1753 1.1787 0.6846 0.092 Uiso 0.86(3) 1 calc PR C 1
H15B H 0.2463 1.1599 0.7584 0.092 Uiso 0.86(3) 1 calc PR C 1
H15C H 0.2482 1.1863 0.7177 0.092 Uiso 0.14(3) 1 d PR C 2
H15D H 0.1647 1.1231 0.7728 0.092 Uiso 0.14(3) 1 d PR C 2
C16 C 0.0534(14) 1.1123(15) 0.7560(12) 0.115(9) Uani 0.86(3) 1 d PDU C 1
H16A H -0.0097 1.0880 0.7205 0.173 Uiso 0.86(3) 1 calc PR C 1
H16B H 0.0242 1.1790 0.7754 0.173 Uiso 0.86(3) 1 calc PR C 1
H16C H 0.0618 1.0595 0.7928 0.173 Uiso 0.86(3) 1 calc PR C 1
C16A C 0.043(5) 1.141(6) 0.696(6) 0.14(2) Uani 0.14(3) 1 d PDU C 2
H16D H 0.0071 1.2065 0.7136 0.204 Uiso 0.14(3) 1 calc PR C 2
H16E H -0.0082 1.0813 0.7110 0.204 Uiso 0.14(3) 1 calc PR C 2
H16F H 0.0408 1.1434 0.6452 0.204 Uiso 0.14(3) 1 calc PR C 2
Cu5 Cu 0.49803(19) 0.22888(12) 0.90106(7) 0.0564(5) Uani 1 1 d D . .
Cl5 Cl 0.5113(3) 0.2472(2) 0.77258(14) 0.0395(8) Uani 1 1 d . D .
Cl6 Cl 0.3653(3) 0.3502(3) 0.94672(14) 0.0551(10) Uani 1 1 d . D .
O5 O 0.5915(13) 0.0894(9) 0.9215(7) 0.041(3) Uani 0.517(8) 1 d PDU D 1
H5 H 0.592(6) 0.056(3) 0.880(2) 0.061 Uiso 0.517(8) 1 d PD D 1
O5A O 0.6565(13) 0.1255(10) 0.8958(8) 0.041(3) Uani 0.483(8) 1 d PDU D 2
H5E H 0.620(4) 0.068(3) 0.875(5) 0.061 Uiso 0.483(8) 1 d PD D 2
N5 N 0.6527(9) 0.3083(8) 0.9320(5) 0.050(3) Uani 1 1 d DU D .
H5A H 0.6719 0.3602 0.9010 0.060 Uiso 1 1 calc R E 1
H5B H 0.6425 0.3380 0.9747 0.060 Uiso 1 1 calc R E 1
C17 C 0.7089(14) 0.1193(12) 0.9603(9) 0.046(5) Uani 0.517(8) 1 d PDU D 1
H17A H 0.7762 0.0652 0.9543 0.055 Uiso 0.517(8) 1 calc PR D 1
H17B H 0.6915 0.1242 1.0100 0.055 Uiso 0.517(8) 1 calc PR D 1
C18 C 0.7556(15) 0.2235(10) 0.9349(10) 0.040(3) Uani 0.517(8) 1 d PDU D 1
H18 H 0.8238 0.2478 0.9692 0.048 Uiso 0.517(8) 1 calc PR D 1
C19 C 0.820(3) 0.2152(19) 0.8660(10) 0.055(6) Uani 0.517(8) 1 d PDU D 1
H19A H 0.7521 0.2099 0.8287 0.067 Uiso 0.517(8) 1 calc PR D 1
H19B H 0.8717 0.1498 0.8655 0.067 Uiso 0.517(8) 1 calc PR D 1
C20 C 0.908(3) 0.310(3) 0.8514(16) 0.150(15) Uani 0.517(8) 1 d PDU D 1
H20A H 0.9619 0.2934 0.8123 0.226 Uiso 0.517(8) 1 calc PR D 1
H20B H 0.9637 0.3247 0.8923 0.226 Uiso 0.517(8) 1 calc PR D 1
H20C H 0.8549 0.3719 0.8402 0.226 Uiso 0.517(8) 1 calc PR D 1
C17A C 0.7682(13) 0.1858(16) 0.8830(12) 0.051(6) Uani 0.483(8) 1 d PDU D 2
H17C H 0.7576 0.2199 0.8372 0.061 Uiso 0.483(8) 1 calc PR D 2
H17D H 0.8441 0.1385 0.8820 0.061 Uiso 0.483(8) 1 calc PR D 2
C18A C 0.7915(13) 0.2674(13) 0.9366(11) 0.040(3) Uani 0.483(8) 1 d PDU D 2
H18A H 0.8012 0.2291 0.9816 0.048 Uiso 0.483(8) 1 calc PR D 2
C19A C 0.917(2) 0.3291(17) 0.9289(11) 0.060(7) Uani 0.483(8) 1 d PDU D 2
H19C H 0.9172 0.3608 0.8822 0.072 Uiso 0.483(8) 1 calc PR D 2
H19D H 0.9912 0.2802 0.9335 0.072 Uiso 0.483(8) 1 calc PR D 2
C20A C 0.933(3) 0.417(2) 0.9838(16) 0.091(11) Uani 0.483(8) 1 d PDU D 2
H20D H 1.0244 0.4231 0.9987 0.136 Uiso 0.483(8) 1 calc PR D 2
H20E H 0.8818 0.4002 1.0237 0.136 Uiso 0.483(8) 1 calc PR D 2
H20F H 0.9037 0.4843 0.9638 0.136 Uiso 0.483(8) 1 calc PR D 2
O6 O 0.3558(12) 0.1238(7) 0.8906(4) 0.092(4) Uani 1 1 d DU D .
H6 H 0.358(8) 0.094(6) 0.8477(17) 0.139 Uiso 1 1 d D . .
C21 C 0.3116(14) 0.0805(11) 0.9541(6) 0.073(4) Uani 1 1 d DU . .
H21A H 0.3797 0.0883 0.9911 0.087 Uiso 0.19(2) 1 calc PR D 1
H21B H 0.2931 0.0045 0.9481 0.087 Uiso 0.19(2) 1 calc PR D 1
H21C H 0.3194 0.1348 0.9907 0.087 Uiso 0.81(2) 1 calc PR D 2
H21D H 0.3681 0.0208 0.9683 0.087 Uiso 0.81(2) 1 calc PR D 2
C22 C 0.188(6) 0.138(6) 0.975(3) 0.153(10) Uani 0.19(2) 1 d PDU D 1
H22A H 0.1558 0.1821 0.9363 0.230 Uiso 0.19(2) 1 calc PR D 1
H22B H 0.2081 0.1833 1.0151 0.230 Uiso 0.19(2) 1 calc PR D 1
H22C H 0.1222 0.0868 0.9865 0.230 Uiso 0.19(2) 1 calc PR D 1
C22A C 0.1723(17) 0.042(2) 0.9485(12) 0.153(10) Uani 0.81(2) 1 d PDU D 2
H22D H 0.1178 0.0972 0.9271 0.230 Uiso 0.81(2) 1 calc PR D 2
H22E H 0.1423 0.0266 0.9947 0.230 Uiso 0.81(2) 1 calc PR D 2
H22F H 0.1673 -0.0214 0.9200 0.230 Uiso 0.81(2) 1 calc PR D 2
Cu6 Cu 0.48895(17) 0.73239(11) 0.59900(7) 0.0475(5) Uani 1 1 d D . .
Cl7 Cl 0.5000(3) 0.7379(2) 0.72720(13) 0.0354(8) Uani 1 1 d . . .
Cl8 Cl 0.3556(4) 0.8558(2) 0.54894(13) 0.0560(10) Uani 1 1 d . . .
O7 O 0.6187(8) 0.6089(5) 0.5884(4) 0.055(2) Uani 1 1 d DU . .
H7 H 0.588(4) 0.559(3) 0.617(4) 0.082 Uiso 1 1 d D . .
N6 N 0.6448(10) 0.8163(7) 0.5851(4) 0.055(3) Uani 1 1 d DU . .
H6A H 0.6516 0.8310 0.5389 0.066 Uiso 1 1 calc R . .
H6B H 0.6396 0.8790 0.6086 0.066 Uiso 1 1 calc R . .
C23 C 0.7440(10) 0.6510(8) 0.5784(6) 0.062(4) Uani 1 1 d DU . .
H23A H 0.7577 0.6570 0.5283 0.074 Uiso 1 1 calc R . .
H23B H 0.8097 0.6020 0.5983 0.074 Uiso 1 1 calc R . .
C24 C 0.7619(10) 0.7562(8) 0.6111(6) 0.054(3) Uani 1 1 d DU F .
H24 H 0.7545 0.7468 0.6620 0.065 Uiso 1 1 calc R . .
C25 C 0.8901(13) 0.8105(10) 0.5997(7) 0.084(4) Uani 1 1 d DU . .
H25A H 0.8826 0.8856 0.6125 0.101 Uiso 0.88(3) 1 calc PR F 1
H25B H 0.9083 0.8072 0.5500 0.101 Uiso 0.88(3) 1 calc PR F 1
H25C H 0.9144 0.8531 0.6410 0.101 Uiso 0.12(3) 1 calc PR F 2
H25D H 0.8797 0.8590 0.5599 0.101 Uiso 0.12(3) 1 calc PR F 2
C26 C 1.0052(13) 0.7612(15) 0.6419(13) 0.109(9) Uani 0.88(3) 1 d PDU F 1
H26A H 1.0106 0.6859 0.6314 0.163 Uiso 0.88(3) 1 calc PR F 1
H26B H 0.9922 0.7706 0.6913 0.163 Uiso 0.88(3) 1 calc PR F 1
H26C H 1.0856 0.7959 0.6296 0.163 Uiso 0.88(3) 1 calc PR F 1
C26A C 1.000(5) 0.732(3) 0.586(10) 0.10(2) Uani 0.12(3) 1 d PDU F 2
H26D H 1.0327 0.7015 0.6298 0.154 Uiso 0.12(3) 1 calc PR F 2
H26E H 1.0704 0.7682 0.5635 0.154 Uiso 0.12(3) 1 calc PR F 2
H26F H 0.9669 0.6750 0.5557 0.154 Uiso 0.12(3) 1 calc PR F 2
O8 O 0.3490(9) 0.6268(6) 0.6016(4) 0.056(3) Uani 1 1 d DU H .
H8 H 0.350(7) 0.596(5) 0.6443(11) 0.084 Uiso 1 1 d D . .
C27 C 0.3159(15) 0.5761(10) 0.5351(6) 0.070(4) Uani 1 1 d DU . .
H27A H 0.3757 0.5169 0.5274 0.084 Uiso 1 1 calc R G 1
H27B H 0.3245 0.6274 0.4971 0.084 Uiso 1 1 calc R G 1
C28 C 0.1772(15) 0.5355(13) 0.5358(7) 0.095(5) Uani 1 1 d DU H 1
H28A H 0.1662 0.4927 0.5772 0.143 Uiso 1 1 calc R H 1
H28B H 0.1589 0.4925 0.4946 0.143 Uiso 1 1 calc R H 1
H28C H 0.1175 0.5953 0.5360 0.143 Uiso 1 1 calc R H 1
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 0.0677(10) 0.0221(8) 0.0207(8) -0.0019(7) 0.0036(7) 0.0041(8)
Cu2 0.0708(11) 0.0284(8) 0.0193(7) 0.0000(7) 0.0005(7) 0.0035(10)
Cl1 0.074(2) 0.0252(16) 0.0262(17) -0.0019(14) 0.0002(16) 0.0036(17)
Cl2 0.108(3) 0.033(2) 0.0376(18) -0.0027(16) -0.0273(18) 0.010(2)
O1 0.067(5) 0.024(4) 0.024(4) 0.004(4) 0.001(4) 0.001(4)
N1 0.079(6) 0.023(6) 0.016(5) 0.007(4) 0.000(5) 0.011(5)
C1 0.060(8) 0.036(7) 0.028(6) 0.010(5) 0.003(6) 0.004(5)
C2 0.068(6) 0.026(7) 0.028(6) 0.016(5) 0.018(5) 0.004(5)
C3 0.084(7) 0.033(8) 0.072(9) 0.015(6) 0.031(8) 0.023(6)
C4 0.064(9) 0.067(12) 0.050(10) -0.007(8) 0.011(8) 0.005(8)
C4A 0.064(9) 0.067(12) 0.050(10) -0.007(8) 0.011(8) 0.005(8)
O2 0.058(5) 0.019(4) 0.028(4) -0.003(3) 0.006(4) 0.002(4)
N2 0.100(7) 0.021(6) 0.023(5) 0.000(4) 0.017(5) -0.003(6)
C5 0.050(8) 0.028(7) 0.044(7) -0.003(5) 0.011(5) 0.006(6)
C6 0.092(7) 0.035(7) 0.023(6) -0.011(6) 0.019(5) -0.009(8)
C7 0.123(9) 0.059(9) 0.071(9) -0.003(8) 0.074(7) -0.008(10)
C8 0.103(10) 0.130(19) 0.129(17) -0.087(14) 0.069(9) -0.055(13)
C8A 0.103(10) 0.130(19) 0.129(17) -0.087(14) 0.069(9) -0.055(13)
Cu3 0.0411(8) 0.0231(8) 0.0229(7) 0.0018(7) 0.0003(6) -0.0011(7)
Cu4 0.0578(10) 0.0273(8) 0.0238(8) 0.0000(7) -0.0019(7) -0.0067(9)
Cl3 0.0453(19) 0.0307(17) 0.0237(15) 0.0010(13) 0.0044(14) -0.0030(15)
Cl4 0.075(2) 0.0249(19) 0.0372(18) -0.0016(14) 0.0163(17) 0.0001(17)
O3 0.049(5) 0.024(4) 0.027(4) -0.003(3) -0.005(4) 0.001(4)
N3 0.033(5) 0.032(5) 0.025(5) -0.007(4) -0.006(4) -0.005(4)
C9 0.035(10) 0.052(11) 0.061(13) 0.016(10) -0.013(10) -0.007(9)
C10 0.035(6) 0.034(8) 0.040(9) -0.008(6) 0.014(5) 0.011(5)
C11 0.036(7) 0.031(9) 0.059(9) 0.009(7) -0.011(6) -0.014(7)
C12 0.040(8) 0.098(17) 0.097(14) 0.046(12) -0.015(8) -0.008(11)
C9A 0.033(11) 0.055(14) 0.062(13) 0.014(11) -0.008(11) -0.012(10)
C10A 0.035(6) 0.034(8) 0.040(9) -0.008(6) 0.014(5) 0.011(5)
C11A 0.036(7) 0.031(9) 0.059(9) 0.009(7) -0.011(6) -0.014(7)
C12A 0.040(8) 0.098(17) 0.097(14) 0.046(12) -0.015(8) -0.008(11)
N4 0.078(7) 0.024(6) 0.030(5) 0.004(5) -0.011(5) -0.008(5)
O4 0.045(5) 0.038(5) 0.031(4) 0.006(4) 0.004(4) -0.007(4)
C13 0.043(8) 0.088(9) 0.058(8) 0.031(7) -0.017(6) -0.007(7)
C14 0.089(8) 0.068(8) 0.029(7) 0.015(6) -0.005(5) -0.027(7)
C15 0.071(9) 0.082(9) 0.078(10) 0.032(8) 0.004(7) 0.003(8)
C16 0.056(11) 0.119(17) 0.17(2) 0.103(15) 0.009(11) 0.026(11)
C16A 0.09(3) 0.15(5) 0.17(5) 0.12(4) -0.03(3) 0.00(3)
Cu5 0.1156(16) 0.0308(10) 0.0227(8) 0.0001(7) 0.0033(9) 0.0093(10)
Cl5 0.063(2) 0.0323(18) 0.0221(16) -0.0009(13) -0.0065(16) 0.0032(16)
Cl6 0.086(3) 0.048(2) 0.0313(17) 0.0088(16) 0.0018(17) 0.0051(19)
O5 0.072(10) 0.023(7) 0.028(7) 0.001(5) 0.001(6) -0.010(5)
O5A 0.072(10) 0.023(7) 0.028(7) 0.001(5) 0.001(6) -0.010(5)
N5 0.084(7) 0.041(7) 0.026(5) -0.006(5) 0.011(5) 0.029(5)
C17 0.054(13) 0.034(9) 0.049(13) 0.007(10) -0.005(9) 0.007(9)
C18 0.056(8) 0.023(8) 0.042(7) -0.013(7) 0.008(7) 0.003(5)
C19 0.031(14) 0.078(15) 0.058(12) -0.020(11) 0.021(10) -0.009(10)
C20 0.15(3) 0.19(3) 0.11(3) 0.00(3) 0.03(2) -0.12(2)
C17A 0.050(14) 0.055(14) 0.049(14) -0.028(10) 0.020(11) -0.002(8)
C18A 0.056(8) 0.023(8) 0.042(7) -0.013(7) 0.008(7) 0.003(5)
C19A 0.096(11) 0.052(15) 0.033(13) 0.002(10) 0.020(14) -0.040(12)
C20A 0.06(2) 0.06(2) 0.15(3) -0.052(17) 0.02(2) -0.013(14)
O6 0.192(11) 0.053(7) 0.032(5) -0.009(5) 0.001(6) -0.035(7)
C21 0.120(11) 0.042(9) 0.058(9) -0.011(7) 0.030(9) -0.017(8)
C22 0.114(13) 0.16(2) 0.19(2) -0.107(17) 0.037(13) -0.028(12)
C22A 0.114(13) 0.16(2) 0.19(2) -0.107(17) 0.037(13) -0.028(12)
Cu6 0.0978(14) 0.0237(9) 0.0207(8) 0.0011(7) -0.0008(8) 0.0023(9)
Cl7 0.061(2) 0.0305(17) 0.0151(15) 0.0008(13) 0.0024(15) -0.0012(16)
Cl8 0.119(3) 0.0261(19) 0.0221(15) -0.0026(14) -0.0125(17) 0.0080(19)
O7 0.112(8) 0.027(5) 0.026(5) 0.014(4) 0.005(5) 0.009(5)
N6 0.130(8) 0.020(6) 0.016(5) 0.003(4) 0.024(6) 0.014(5)
C23 0.123(10) 0.031(6) 0.035(7) 0.012(5) 0.037(8) 0.017(6)
C24 0.092(8) 0.037(7) 0.037(7) 0.008(5) 0.034(7) 0.003(5)
C25 0.119(9) 0.044(9) 0.095(11) 0.002(8) 0.078(9) -0.003(7)
C26 0.067(9) 0.074(15) 0.19(2) -0.023(14) 0.073(11) -0.001(10)
C26A 0.10(2) 0.09(4) 0.12(5) 0.02(4) 0.07(4) 0.01(3)
O8 0.118(8) 0.027(5) 0.022(4) -0.002(4) -0.004(5) -0.004(5)
C27 0.154(12) 0.031(8) 0.023(7) 0.001(5) -0.024(9) -0.008(8)
C28 0.162(13) 0.064(11) 0.055(9) 0.001(9) -0.047(9) -0.020(11)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.949(7) . ?
Cu1 N1 1.961(9) . ?
Cu1 O1 1.983(7) . ?
Cu1 Cl1 2.249(3) . ?
Cu1 Cu2 2.8982(18) . ?
Cu2 O1 1.958(7) . ?
Cu2 N2 1.967(9) . ?
Cu2 O2 1.978(7) . ?
Cu2 Cl2 2.245(3) . ?
O1 C1 1.438(9) . ?
N1 C2 1.524(11) . ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
C1 C2 1.513(10) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 C3 1.515(11) . ?
C2 H2 1.0000 . ?
C3 C4 1.429(13) . ?
C3 C4A 1.435(18) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C4 H3D 0.8504 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4A H4D 0.9800 . ?
C4A H4E 0.9800 . ?
C4A H4F 0.9800 . ?
O2 C5 1.431(9) . ?
N2 C6 1.502(11) . ?
N2 H2A 0.9200 . ?
N2 H2B 0.9200 . ?
C5 C6 1.514(11) . ?
C5 H5C 0.9900 . ?
C5 H5D 0.9900 . ?
C6 C7 1.507(12) . ?
C6 H6C 1.0000 . ?
C7 C8A 1.438(14) . ?
C7 C8 1.441(18) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 H7C 0.9900 . ?
C7 H7D 0.9899 . ?
C8 H7C 0.4956 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8A H8D 0.9800 . ?
C8A H8E 0.9800 . ?
C8A H8F 0.9800 . ?
Cu3 N3 1.960(8) . ?
Cu3 O4 1.977(7) . ?
Cu3 O3 1.984(7) . ?
Cu3 Cl3 2.236(3) . ?
Cu3 Cu4 2.9108(18) . ?
Cu4 N4 1.965(9) . ?
Cu4 O3 1.966(7) . ?
Cu4 O4 1.969(7) . ?
Cu4 Cl4 2.247(3) . ?
O3 C9 1.425(12) . ?
O3 C9A 1.431(13) . ?
N3 C10 1.485(12) . ?
N3 C10A 1.534(14) . ?
N3 H3E 0.9200 . ?
N3 H3F 0.9200 . ?
N3 H3G 0.9200 . ?
N3 H3H 0.9201 . ?
C9 C10 1.477(13) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.498(14) . ?
C10 H10 1.0000 . ?
C11 C12 1.441(16) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C9A C10A 1.480(14) . ?
C9A H9C 0.9900 . ?
C9A H9D 0.9900 . ?
C10A C11A 1.503(15) . ?
C10A H10A 1.0000 . ?
C11A C12A 1.452(17) . ?
C11A H11C 0.9900 . ?
C11A H11D 0.9900 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12R 0.9800 . ?
N4 C14 1.510(11) . ?
N4 H4G 0.9200 . ?
N4 H4H 0.9200 . ?
O4 C13 1.452(10) . ?
C13 C14 1.474(11) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.540(12) . ?
C14 H14 1.0000 . ?
C15 C16 1.544(15) . ?
C15 C16A 1.56(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 H15C 0.9900 . ?
C15 H15D 0.9897 . ?
C16 H15D 1.1943 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16A H16D 0.9800 . ?
C16A H16E 0.9800 . ?
C16A H16F 0.9800 . ?
Cu5 N5 1.967(10) . ?
Cu5 O6 1.993(10) . ?
Cu5 O5 2.051(12) . ?
Cu5 O5A 2.109(12) . ?
Cu5 Cl6 2.269(4) . ?
Cu5 Cl5 2.510(3) . ?
O5 C17 1.455(13) . ?
O5 H5 0.90(2) . ?
O5 H5E 1.00(7) . ?
O5A C17A 1.419(13) . ?
O5A H5 1.14(6) . ?
O5A H5E 0.91(2) . ?
N5 C18 1.515(13) . ?
N5 C18A 1.529(14) . ?
N5 H5A 0.9200 . ?
N5 H5B 0.9200 . ?
C17 C18 1.499(13) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.519(15) . ?
C18 H18 1.0000 . ?
C19 C20 1.547(18) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C17A C18A 1.482(14) . ?
C17A H17C 0.9900 . ?
C17A H17D 0.9900 . ?
C18A C19A 1.531(14) . ?
C18A H18A 1.0000 . ?
C19A C20A 1.550(17) . ?
C19A H19C 0.9900 . ?
C19A H19D 0.9900 . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
O6 C21 1.441(12) . ?
O6 H6 0.911(18) . ?
C21 C22A 1.522(17) . ?
C21 C22 1.54(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 H21C 0.9900 . ?
C21 H21D 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
Cu6 N6 1.963(11) . ?
Cu6 O8 1.978(8) . ?
Cu6 O7 2.082(8) . ?
Cu6 Cl8 2.281(4) . ?
Cu6 Cl7 2.483(3) . ?
O7 C23 1.425(10) . ?
O7 H7 0.899(18) . ?
N6 C24 1.503(11) . ?
N6 H6A 0.9200 . ?
N6 H6B 0.9200 . ?
C23 C24 1.487(11) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.521(11) . ?
C24 H24 1.0000 . ?
C25 C26A 1.55(2) . ?
C25 C26 1.553(16) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 H25C 0.9900 . ?
C25 H25D 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C26A H26D 0.9800 . ?
C26A H26E 0.9800 . ?
C26A H26F 0.9800 . ?
O8 C27 1.468(11) . ?
O8 H8 0.916(18) . ?
C27 C28 1.528(16) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 N1 162.8(4) . . ?
O2 Cu1 O1 78.2(3) . . ?
N1 Cu1 O1 84.8(3) . . ?
O2 Cu1 Cl1 98.9(2) . . ?
N1 Cu1 Cl1 96.5(3) . . ?
O1 Cu1 Cl1 163.5(2) . . ?
O2 Cu1 Cu2 42.8(2) . . ?
N1 Cu1 Cu2 122.8(3) . . ?
O1 Cu1 Cu2 42.3(2) . . ?
Cl1 Cu1 Cu2 140.54(10) . . ?
O1 Cu2 N2 162.0(4) . . ?
O1 Cu2 O2 78.2(3) . . ?
N2 Cu2 O2 84.8(3) . . ?
O1 Cu2 Cl2 97.5(2) . . ?
N2 Cu2 Cl2 97.8(3) . . ?
O2 Cu2 Cl2 166.7(2) . . ?
O1 Cu2 Cu1 43.0(2) . . ?
N2 Cu2 Cu1 119.1(3) . . ?
O2 Cu2 Cu1 42.1(2) . . ?
Cl2 Cu2 Cu1 127.73(11) . . ?
C1 O1 Cu2 127.4(6) . . ?
C1 O1 Cu1 109.2(5) . . ?
Cu2 O1 Cu1 94.7(3) . . ?
C2 N1 Cu1 111.4(6) . . ?
C2 N1 H1A 109.4 . . ?
Cu1 N1 H1A 109.4 . . ?
C2 N1 H1B 109.4 . . ?
Cu1 N1 H1B 109.4 . . ?
H1A N1 H1B 108.0 . . ?
O1 C1 C2 109.0(7) . . ?
O1 C1 H1C 109.9 . . ?
C2 C1 H1C 109.9 . . ?
O1 C1 H1D 109.9 . . ?
C2 C1 H1D 109.9 . . ?
H1C C1 H1D 108.3 . . ?
C1 C2 C3 113.4(8) . . ?
C1 C2 N1 107.0(7) . . ?
C3 C2 N1 115.7(9) . . ?
C1 C2 H2 106.7 . . ?
C3 C2 H2 106.7 . . ?
N1 C2 H2 106.7 . . ?
C4 C3 C4A 74(2) . . ?
C4 C3 C2 118.2(11) . . ?
C4A C3 C2 113.9(14) . . ?
C4 C3 H3A 107.8 . . ?
C4A C3 H3A 36.0 . . ?
C2 C3 H3A 107.8 . . ?
C4 C3 H3B 107.8 . . ?
C4A C3 H3B 130.9 . . ?
C2 C3 H3B 107.8 . . ?
H3A C3 H3B 107.1 . . ?
C4 C3 H3C 127.8 . . ?
C4A C3 H3C 109.3 . . ?
C2 C3 H3C 107.7 . . ?
H3A C3 H3C 78.7 . . ?
H3B C3 H3C 30.3 . . ?
C4 C3 H3D 35.7 . . ?
C4A C3 H3D 109.2 . . ?
C2 C3 H3D 108.9 . . ?
H3A C3 H3D 138.5 . . ?
H3B C3 H3D 79.4 . . ?
H3C C3 H3D 107.7 . . ?
C3 C4 H3D 42.8 . . ?
C3 C4 H4A 109.5 . . ?
H3D C4 H4A 67.1 . . ?
C3 C4 H4B 109.5 . . ?
H3D C4 H4B 118.7 . . ?
C3 C4 H4C 109.5 . . ?
H3D C4 H4C 130.0 . . ?
C3 C4A H4D 109.5 . . ?
C3 C4A H4E 109.5 . . ?
H4D C4A H4E 109.5 . . ?
C3 C4A H4F 109.5 . . ?
H4D C4A H4F 109.5 . . ?
H4E C4A H4F 109.5 . . ?
C5 O2 Cu1 125.2(6) . . ?
C5 O2 Cu2 110.1(5) . . ?
Cu1 O2 Cu2 95.1(3) . . ?
C6 N2 Cu2 110.3(6) . . ?
C6 N2 H2A 109.6 . . ?
Cu2 N2 H2A 109.6 . . ?
C6 N2 H2B 109.6 . . ?
Cu2 N2 H2B 109.6 . . ?
H2A N2 H2B 108.1 . . ?
O2 C5 C6 109.0(7) . . ?
O2 C5 H5C 109.9 . . ?
C6 C5 H5C 109.9 . . ?
O2 C5 H5D 109.9 . . ?
C6 C5 H5D 109.9 . . ?
H5C C5 H5D 108.3 . . ?
N2 C6 C7 116.1(9) . . ?
N2 C6 C5 106.3(8) . . ?
C7 C6 C5 113.1(9) . . ?
N2 C6 H6C 106.9 . . ?
C7 C6 H6C 106.9 . . ?
C5 C6 H6C 106.9 . . ?
C8A C7 C8 92(3) . . ?
C8A C7 C6 117.3(12) . . ?
C8 C7 C6 113.9(15) . . ?
C8A C7 H7A 115.4 . . ?
C8 C7 H7A 108.8 . . ?
C6 C7 H7A 108.8 . . ?
C8A C7 H7B 17.2 . . ?
C8 C7 H7B 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C8A C7 H7C 89.2 . . ?
C8 C7 H7C 9.9 . . ?
C6 C7 H7C 106.8 . . ?
H7A C7 H7C 118.3 . . ?
H7B C7 H7C 106.2 . . ?
C8A C7 H7D 123.0 . . ?
C8 C7 H7D 98.3 . . ?
C6 C7 H7D 109.3 . . ?
H7A C7 H7D 12.0 . . ?
H7B C7 H7D 117.7 . . ?
H7C C7 H7D 107.6 . . ?
C7 C8 H7C 20.0 . . ?
C7 C8 H8A 109.5 . . ?
H7C C8 H8A 126.2 . . ?
C7 C8 H8B 109.5 . . ?
H7C C8 H8B 108.5 . . ?
C7 C8 H8C 109.5 . . ?
H7C C8 H8C 91.8 . . ?
C7 C8A H8D 109.5 . . ?
C7 C8A H8E 109.5 . . ?
H8D C8A H8E 109.5 . . ?
C7 C8A H8F 109.5 . . ?
H8D C8A H8F 109.5 . . ?
H8E C8A H8F 109.5 . . ?
N3 Cu3 O4 162.2(3) . . ?
N3 Cu3 O3 83.7(3) . . ?
O4 Cu3 O3 78.7(3) . . ?
N3 Cu3 Cl3 98.5(3) . . ?
O4 Cu3 Cl3 97.8(2) . . ?
O3 Cu3 Cl3 164.4(2) . . ?
N3 Cu3 Cu4 122.2(2) . . ?
O4 Cu3 Cu4 42.4(2) . . ?
O3 Cu3 Cu4 42.30(19) . . ?
Cl3 Cu3 Cu4 139.19(10) . . ?
N4 Cu4 O3 160.3(3) . . ?
N4 Cu4 O4 83.8(3) . . ?
O3 Cu4 O4 79.3(3) . . ?
N4 Cu4 Cl4 98.0(3) . . ?
O3 Cu4 Cl4 96.4(2) . . ?
O4 Cu4 Cl4 167.9(2) . . ?
N4 Cu4 Cu3 117.6(3) . . ?
O3 Cu4 Cu3 42.8(2) . . ?
O4 Cu4 Cu3 42.6(2) . . ?
Cl4 Cu4 Cu3 128.18(10) . . ?
C9 O3 C9A 3(2) . . ?
C9 O3 Cu4 125.6(9) . . ?
C9A O3 Cu4 128.9(12) . . ?
C9 O3 Cu3 112.0(7) . . ?
C9A O3 Cu3 111.2(9) . . ?
Cu4 O3 Cu3 94.9(3) . . ?
C10 N3 C10A 27.0(9) . . ?
C10 N3 Cu3 105.5(7) . . ?
C10A N3 Cu3 113.8(7) . . ?
C10 N3 H3E 110.7 . . ?
C10A N3 H3E 83.8 . . ?
Cu3 N3 H3E 110.7 . . ?
C10 N3 H3F 110.7 . . ?
C10A N3 H3F 125.2 . . ?
Cu3 N3 H3F 110.7 . . ?
H3E N3 H3F 108.8 . . ?
C10 N3 H3G 134.4 . . ?
C10A N3 H3G 109.1 . . ?
Cu3 N3 H3G 108.2 . . ?
H3E N3 H3G 27.5 . . ?
H3F N3 H3G 85.1 . . ?
C10 N3 H3H 89.4 . . ?
C10A N3 H3H 109.3 . . ?
Cu3 N3 H3H 108.9 . . ?
H3E N3 H3H 128.0 . . ?
H3F N3 H3H 23.5 . . ?
H3G N3 H3H 107.5 . . ?
O3 C9 C10 111.2(9) . . ?
O3 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
O3 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C9 C10 N3 114.1(10) . . ?
C9 C10 C11 116.3(12) . . ?
N3 C10 C11 109.1(12) . . ?
C9 C10 H10 105.4 . . ?
N3 C10 H10 105.4 . . ?
C11 C10 H10 105.4 . . ?
C12 C11 C10 114.4(12) . . ?
C12 C11 H11A 108.7 . . ?
C10 C11 H11A 108.7 . . ?
C12 C11 H11B 108.7 . . ?
C10 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O3 C9A C10A 113.4(13) . . ?
O3 C9A H9C 108.9 . . ?
C10A C9A H9C 108.9 . . ?
O3 C9A H9D 108.9 . . ?
C10A C9A H9D 108.9 . . ?
H9C C9A H9D 107.7 . . ?
C9A C10A C11A 109(2) . . ?
C9A C10A N3 108.3(11) . . ?
C11A C10A N3 117.8(16) . . ?
C9A C10A H10A 107.0 . . ?
C11A C10A H10A 107.0 . . ?
N3 C10A H10A 107.0 . . ?
C12A C11A C10A 115.1(15) . . ?
C12A C11A H11C 108.5 . . ?
C10A C11A H11C 108.5 . . ?
C12A C11A H11D 108.5 . . ?
C10A C11A H11D 108.5 . . ?
H11C C11A H11D 107.5 . . ?
C11A C12A H12D 109.5 . . ?
C11A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
C11A C12A H12R 109.5 . . ?
H12D C12A H12R 109.5 . . ?
H12E C12A H12R 109.5 . . ?
C14 N4 Cu4 112.5(6) . . ?
C14 N4 H4G 109.1 . . ?
Cu4 N4 H4G 109.1 . . ?
C14 N4 H4H 109.1 . . ?
Cu4 N4 H4H 109.1 . . ?
H4G N4 H4H 107.8 . . ?
C13 O4 Cu4 109.7(6) . . ?
C13 O4 Cu3 119.9(6) . . ?
Cu4 O4 Cu3 95.1(3) . . ?
O4 C13 C14 110.4(8) . . ?
O4 C13 H13A 109.6 . . ?
C14 C13 H13A 109.6 . . ?
O4 C13 H13B 109.6 . . ?
C14 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C13 C14 N4 106.2(9) . . ?
C13 C14 C15 111.8(9) . . ?
N4 C14 C15 109.6(10) . . ?
C13 C14 H14 109.7 . . ?
N4 C14 H14 109.7 . . ?
C15 C14 H14 109.7 . . ?
C14 C15 C16 112.7(11) . . ?
C14 C15 C16A 110.3(16) . . ?
C16 C15 C16A 46(5) . . ?
C14 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
C16A C15 H15A 66.4 . . ?
C14 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
C16A C15 H15B 139.7 . . ?
H15A C15 H15B 107.8 . . ?
C14 C15 H15C 109.2 . . ?
C16 C15 H15C 137.9 . . ?
C16A C15 H15C 120.1 . . ?
H15A C15 H15C 59.1 . . ?
H15B C15 H15C 51.3 . . ?
C14 C15 H15D 111.4 . . ?
C16 C15 H15D 50.7 . . ?
C16A C15 H15D 95.8 . . ?
H15A C15 H15D 139.3 . . ?
H15B C15 H15D 61.7 . . ?
H15C C15 H15D 109.3 . . ?
C15 C16 H15D 39.9 . . ?
C15 C16 H16A 109.5 . . ?
H15D C16 H16A 146.9 . . ?
C15 C16 H16B 109.5 . . ?
H15D C16 H16B 96.1 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H15D C16 H16C 79.8 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C16A H16D 109.5 . . ?
C15 C16A H16E 109.5 . . ?
H16D C16A H16E 109.5 . . ?
C15 C16A H16F 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
N5 Cu5 O6 164.8(4) . . ?
N5 Cu5 O5 90.6(5) . . ?
O6 Cu5 O5 77.5(5) . . ?
N5 Cu5 O5A 73.0(4) . . ?
O6 Cu5 O5A 98.7(5) . . ?
O5 Cu5 O5A 26.9(4) . . ?
N5 Cu5 Cl6 91.8(3) . . ?
O6 Cu5 Cl6 92.2(3) . . ?
O5 Cu5 Cl6 143.2(4) . . ?
O5A Cu5 Cl6 158.1(4) . . ?
N5 Cu5 Cl5 100.3(3) . . ?
O6 Cu5 Cl5 91.7(3) . . ?
O5 Cu5 Cl5 103.2(4) . . ?
O5A Cu5 Cl5 86.4(4) . . ?
Cl6 Cu5 Cl5 112.44(11) . . ?
C17 O5 Cu5 104.7(8) . . ?
C17 O5 H5 123(4) . . ?
Cu5 O5 H5 105(2) . . ?
C17 O5 H5E 106(3) . . ?
Cu5 O5 H5E 102(4) . . ?
H5 O5 H5E 20(5) . . ?
C17A O5A Cu5 108.3(10) . . ?
C17A O5A H5 148(3) . . ?
Cu5 O5A H5 92.7(19) . . ?
C17A O5A H5E 133(4) . . ?
Cu5 O5A H5E 102(3) . . ?
H5 O5A H5E 15(5) . . ?
C18 N5 C18A 25.5(7) . . ?
C18 N5 Cu5 102.2(8) . . ?
C18A N5 Cu5 126.7(8) . . ?
C18 N5 H5A 111.3 . . ?
C18A N5 H5A 93.1 . . ?
Cu5 N5 H5A 111.3 . . ?
C18 N5 H5B 111.3 . . ?
C18A N5 H5B 103.2 . . ?
Cu5 N5 H5B 111.3 . . ?
H5A N5 H5B 109.2 . . ?
O5 C17 C18 109.6(10) . . ?
O5 C17 H17A 109.7 . . ?
C18 C17 H17A 109.7 . . ?
O5 C17 H17B 109.7 . . ?
C18 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
C17 C18 N5 113.8(11) . . ?
C17 C18 C19 112.6(12) . . ?
N5 C18 C19 110.4(16) . . ?
C17 C18 H18 106.5 . . ?
N5 C18 H18 106.5 . . ?
C19 C18 H18 106.5 . . ?
C18 C19 C20 113.0(15) . . ?
C18 C19 H19A 109.0 . . ?
C20 C19 H19A 109.0 . . ?
C18 C19 H19B 109.0 . . ?
C20 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O5A C17A C18A 111.6(12) . . ?
O5A C17A H17C 109.3 . . ?
C18A C17A H17C 109.3 . . ?
O5A C17A H17D 109.3 . . ?
C18A C17A H17D 109.3 . . ?
H17C C17A H17D 108.0 . . ?
C17A C18A N5 94.0(11) . . ?
C17A C18A C19A 113.9(12) . . ?
N5 C18A C19A 128.5(18) . . ?
C17A C18A H18A 106.1 . . ?
N5 C18A H18A 106.1 . . ?
C19A C18A H18A 106.1 . . ?
C18A C19A C20A 111.9(14) . . ?
C18A C19A H19C 109.2 . . ?
C20A C19A H19C 109.2 . . ?
C18A C19A H19D 109.2 . . ?
C20A C19A H19D 109.2 . . ?
H19C C19A H19D 107.9 . . ?
C19A C20A H20D 109.5 . . ?
C19A C20A H20E 109.5 . . ?
H20D C20A H20E 109.5 . . ?
C19A C20A H20F 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C21 O6 Cu5 115.3(8) . . ?
C21 O6 H6 130(3) . . ?
Cu5 O6 H6 109(2) . . ?
O6 C21 C22A 113.1(13) . . ?
O6 C21 C22 109.6(17) . . ?
C22A C21 C22 52(4) . . ?
O6 C21 H21A 109.7 . . ?
C22A C21 H21A 137.0 . . ?
C22 C21 H21A 109.7 . . ?
O6 C21 H21B 109.7 . . ?
C22A C21 H21B 60.2 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
O6 C21 H21C 109.0 . . ?
C22A C21 H21C 109.0 . . ?
C22 C21 H21C 61.7 . . ?
H21A C21 H21C 51.4 . . ?
H21B C21 H21C 140.8 . . ?
O6 C21 H21D 109.0 . . ?
C22A C21 H21D 109.0 . . ?
C22 C21 H21D 141.3 . . ?
H21A C21 H21D 58.7 . . ?
H21B C21 H21D 52.8 . . ?
H21C C21 H21D 107.8 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C22A H22D 109.5 . . ?
C21 C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C21 C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
N6 Cu6 O8 168.6(4) . . ?
N6 Cu6 O7 81.8(4) . . ?
O8 Cu6 O7 88.2(3) . . ?
N6 Cu6 Cl8 93.2(3) . . ?
O8 Cu6 Cl8 92.5(3) . . ?
O7 Cu6 Cl8 149.2(2) . . ?
N6 Cu6 Cl7 96.6(3) . . ?
O8 Cu6 Cl7 89.9(2) . . ?
O7 Cu6 Cl7 96.6(2) . . ?
Cl8 Cu6 Cl7 114.17(11) . . ?
C23 O7 Cu6 109.0(6) . . ?
C23 O7 H7 134(3) . . ?
Cu6 O7 H7 102.8(19) . . ?
C24 N6 Cu6 109.7(6) . . ?
C24 N6 H6A 109.7 . . ?
Cu6 N6 H6A 109.7 . . ?
C24 N6 H6B 109.7 . . ?
Cu6 N6 H6B 109.7 . . ?
H6A N6 H6B 108.2 . . ?
O7 C23 C24 112.3(8) . . ?
O7 C23 H23A 109.1 . . ?
C24 C23 H23A 109.1 . . ?
O7 C23 H23B 109.1 . . ?
C24 C23 H23B 109.1 . . ?
H23A C23 H23B 107.9 . . ?
C23 C24 N6 103.2(8) . . ?
C23 C24 C25 116.2(9) . . ?
N6 C24 C25 114.8(10) . . ?
C23 C24 H24 107.4 . . ?
N6 C24 H24 107.4 . . ?
C25 C24 H24 107.4 . . ?
C24 C25 C26A 112.6(16) . . ?
C24 C25 C26 113.5(10) . . ?
C26A C25 C26 43(6) . . ?
C24 C25 H25A 108.9 . . ?
C26A C25 H25A 137.1 . . ?
C26 C25 H25A 108.9 . . ?
C24 C25 H25B 108.9 . . ?
C26A C25 H25B 68.6 . . ?
C26 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
C24 C25 H25C 109.1 . . ?
C26A C25 H25C 109.1 . . ?
C26 C25 H25C 68.2 . . ?
H25A C25 H25C 44.8 . . ?
H25B C25 H25C 139.2 . . ?
C24 C25 H25D 109.1 . . ?
C26A C25 H25D 109.1 . . ?
C26 C25 H25D 136.0 . . ?
H25A C25 H25D 65.7 . . ?
H25B C25 H25D 44.5 . . ?
H25C C25 H25D 107.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C26A H26D 109.5 . . ?
C25 C26A H26E 109.5 . . ?
H26D C26A H26E 109.5 . . ?
C25 C26A H26F 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?
C27 O8 Cu6 114.9(7) . . ?
C27 O8 H8 127(3) . . ?
Cu6 O8 H8 110(2) . . ?
O8 C27 C28 109.1(10) . . ?
O8 C27 H27A 109.9 . . ?
C28 C27 H27A 109.9 . . ?
O8 C27 H27B 109.9 . . ?
C28 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl4 0.92 2.42 3.312(10) 164.8 1_545
N1 H1B Cl8 0.92 2.47 3.318(9) 152.9 2_646
N2 H2B Cl3 0.92 2.49 3.395(10) 168.7 .
N2 H2A Cl6 0.92 2.49 3.408(10) 174.0 .
N3 H3G Cl6 0.92 2.53 3.424(9) 163.6 2_657
N3 H3H Cl2 0.92 2.42 3.325(10) 166.5 .
N4 H4G Cl1 0.92 2.49 3.404(10) 171.6 1_565
N4 H4H Cl8 0.92 2.43 3.320(10) 162.4 .
N5 H5A Cl2 0.92 2.53 3.404(10) 157.9 .
N5 H5B Cl3 0.92 2.56 3.326(9) 140.5 2_647
N6 H6A Cl1 0.92 2.56 3.421(9) 156.0 2_656
N6 H6B Cl4 0.92 2.41 3.313(9) 165.7 .
O5 H5 O3 0.90(2) 1.77(3) 2.659(15) 166(3) 1_545
O5A H5E O3 0.91(2) 1.75(5) 2.560(14) 148(5) 1_545
O6 H6 O4 0.911(18) 1.81(6) 2.635(11) 150(9) 1_545
O7 H7 O1 0.899(18) 1.80(5) 2.590(9) 145(5) .
O8 H8 O2 0.916(18) 1.85(5) 2.669(10) 148(7) .
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 22.21
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.571
_refine_diff_density_min -0.588
_refine_diff_density_rms 0.099
#===END
data_p21212
_database_code_depnum_ccdc_archive 'CCDC 864928'
#TrackingRef '- All-crystaldata.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Bis[rac-(2-amino-butan-1-olato-\kN,O)-rac-(2-amino-butan-1-ol-\kN,O)-aqua-
copper(II)] di-perchlorate
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C16 H46 Cl2 Cu2 N4 O14'
_chemical_formula_sum 'C16 H46 Cl2 Cu2 N4 O14'
_chemical_formula_weight 716.55
_chemical_absolute_configuration ad
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 orthorhombic
_symmetry_space_group_name_H-M 'P 21 21 2'
_symmetry_space_group_name_Hall 'P 2 2ab '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
_cell_length_a 16.2260(3)
_cell_length_b 16.2256(3)
_cell_length_c 5.60100(10)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 1474.61(5)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9914
_cell_measurement_theta_min 2.507
_cell_measurement_theta_max 23.2315
_exptl_crystal_description plate
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.03
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.614
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 748
_exptl_absorpt_coefficient_mu 1.690
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8492
_exptl_absorpt_correction_T_max 0.9510
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'micro-focus sealed tube'
_diffrn_radiation_monochromator 'multilayer mirror optics'
_diffrn_measurement_device_type 'Bruker APEX2 CCD area detector'
_diffrn_measurement_method '\w scans and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 30712
_diffrn_reflns_av_R_equivalents 0.0381
_diffrn_reflns_av_sigmaI/netI 0.0175
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -6
_diffrn_reflns_limit_l_max 6
_diffrn_reflns_theta_min 1.25
_diffrn_reflns_theta_max 23.49
_reflns_number_total 2177
_reflns_number_gt 2031
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material 'publCIF (Westrip, 2009)'
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH and CH~2~
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~)
and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~),
with U~iso~(H) = 1.2U~eq~(CH).
H atoms on the amin nitrogen atoms were found and
refined with U~iso~(H) = 1.2U~eq~(N).
;
_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^)+(0.1212P)^2^+1.1685P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.00(1)
_refine_ls_number_reflns 2177
_refine_ls_number_parameters 198
_refine_ls_number_restraints 297
_refine_ls_R_factor_all 0.0602
_refine_ls_R_factor_gt 0.0558
_refine_ls_wR_factor_ref 0.1606
_refine_ls_wR_factor_gt 0.1550
_refine_ls_goodness_of_fit_ref 1.058
_refine_ls_restrained_S_all 1.196
_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
Cu Cu 0.40171(10) 0.40025(13) 0.48842(19) 0.0518(4) Uani 1 1 d D . .
O3A O 0.4371(9) 0.4402(12) 0.875(2) 0.109(6) Uani 0.77(3) 1 d PDU A 1
H31 H 0.482(4) 0.424(5) 0.940(12) 0.164 Uiso 0.77(3) 1 d PD A 1
H32 H 0.420(5) 0.485(4) 0.936(12) 0.164 Uiso 0.77(3) 1 d PD A 1
O3B O 0.4657(15) 0.4665(15) 0.805(6) 0.109(6) Uani 0.23(3) 1 d PDU . 2
H33 H 0.5000 0.5000 0.786(13) 0.164 Uiso 0.23(3) 1 d PD A 2
H34 H 0.4520(17) 0.4551(17) 0.944(8) 0.164 Uiso 0.23(3) 1 d PD A 2
O1 O 0.5044(8) 0.3887(6) 0.3285(15) 0.062(3) Uani 1 1 d DU A .
H11 H 0.538(7) 0.427(3) 0.28(5) 0.094 Uiso 0.50 1 d PD B -3
N1 N 0.4190(5) 0.2837(5) 0.5952(16) 0.041(2) Uani 1 1 d DU A .
H1C H 0.4146 0.2776 0.7580 0.049 Uiso 1 1 d R . .
H1D H 0.3853 0.2467 0.5180 0.049 Uiso 1 1 d R . .
C1 C 0.5324(10) 0.3057(8) 0.332(4) 0.088(6) Uani 1 1 d DU A 2
H1A H 0.5933 0.3044 0.3195 0.105 Uiso 1 1 calc R A 2
H1B H 0.5092 0.2753 0.1947 0.105 Uiso 1 1 calc R A 2
C2 C 0.5068(7) 0.2664(6) 0.554(3) 0.051(3) Uani 1 1 d DU A 2
H2 H 0.5390 0.2917 0.6875 0.061 Uiso 1 1 calc R A 2
C3 C 0.5242(9) 0.1749(7) 0.552(3) 0.071(5) Uani 1 1 d DU A 2
H3C H 0.4899 0.1485 0.4274 0.085 Uiso 1 1 calc R A 2
H3D H 0.5827 0.1659 0.5091 0.085 Uiso 1 1 calc R A 2
C4 C 0.507(2) 0.1343(9) 0.786(4) 0.093(6) Uani 1 1 d DU A 2
H4A H 0.5177 0.0750 0.7722 0.140 Uiso 1 1 calc R A 2
H4B H 0.4496 0.1434 0.8307 0.140 Uiso 1 1 calc R A 2
H4C H 0.5435 0.1578 0.9084 0.140 Uiso 1 1 calc R A 2
N2 N 0.2882(8) 0.4140(7) 0.568(2) 0.077(4) Uani 1 1 d DU A .
H2C H 0.2571 0.3797 0.4736 0.093 Uiso 1 1 calc R . .
H2D H 0.2804 0.3982 0.7245 0.093 Uiso 1 1 calc R . .
O2 O 0.3853(7) 0.5081(10) 0.331(2) 0.113(6) Uani 1 1 d DU A .
H21 H 0.4274 0.5409 0.2614 0.136 Uiso 0.50 1 d PRD . .
C5 C 0.3061(10) 0.5417(13) 0.362(5) 0.120(9) Uani 1 1 d DU . .
H5A H 0.2764 0.5397 0.2073 0.144 Uiso 1 1 calc R A .
H5B H 0.3115 0.6003 0.4085 0.144 Uiso 1 1 calc R . .
C6 C 0.2584(8) 0.4993(10) 0.539(3) 0.071(4) Uani 1 1 d DU A .
H6A H 0.2796 0.5254 0.6883 0.085 Uiso 1 1 calc R . .
C7 C 0.1698(8) 0.5212(13) 0.553(3) 0.078(5) Uani 1 1 d DU . .
H7A H 0.1645 0.5809 0.5205 0.094 Uiso 1 1 calc R A .
H7B H 0.1406 0.4918 0.4230 0.094 Uiso 1 1 calc R . .
C8 C 0.1271(11) 0.5033(17) 0.778(3) 0.081(5) Uani 1 1 d DU A .
H8A H 0.0720 0.5279 0.7744 0.121 Uiso 1 1 calc R . .
H8B H 0.1585 0.5265 0.9112 0.121 Uiso 1 1 calc R . .
H8C H 0.1223 0.4435 0.7981 0.121 Uiso 1 1 calc R . .
Cl Cl 0.2565(5) 0.2550(7) 0.0684(19) 0.047(2) Uani 0.546(8) 1 d PD C 1
O11 O 0.2354(14) 0.3375(9) 0.100(5) 0.0850(18) Uani 0.546(8) 1 d PDU C 1
O12 O 0.3427(8) 0.2421(15) 0.095(5) 0.0850(18) Uani 0.546(8) 1 d PDU C 1
O13 O 0.2099(12) 0.1945(12) 0.176(2) 0.0850(18) Uani 0.546(8) 1 d PDU C 1
O14 O 0.2461(14) 0.2414(16) -0.193(2) 0.0850(18) Uani 0.546(8) 1 d PDU C 1
ClA Cl 0.2624(8) 0.2653(8) 0.119(2) 0.067(5) Uani 0.454(8) 1 d PD C 2
O12A O 0.3390(8) 0.3073(11) 0.093(3) 0.0850(18) Uani 0.454(8) 1 d PDU C 2
O13A O 0.2025(10) 0.3267(11) 0.055(4) 0.0850(18) Uani 0.454(8) 1 d PDU C 2
O11A O 0.2577(11) 0.1995(10) -0.046(3) 0.0850(18) Uani 0.454(8) 1 d PDU C 2
O14A O 0.2471(13) 0.2369(14) 0.351(3) 0.0850(18) Uani 0.454(8) 1 d PDU C 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu 0.0305(13) 0.0551(18) 0.0699(6) 0.0142(10) 0.0097(10) 0.0117(4)
O3A 0.034(8) 0.209(18) 0.083(8) -0.021(12) -0.014(7) 0.012(8)
O3B 0.034(8) 0.209(18) 0.083(8) -0.021(12) -0.014(7) 0.012(8)
O1 0.055(6) 0.034(5) 0.099(8) -0.002(5) 0.022(6) 0.004(4)
N1 0.044(5) 0.032(5) 0.046(5) 0.021(5) 0.008(5) 0.014(4)
C1 0.061(9) 0.037(7) 0.165(15) 0.014(8) 0.065(10) 0.018(7)
C2 0.038(5) 0.015(4) 0.099(8) -0.014(5) -0.011(7) 0.008(4)
C3 0.047(7) 0.028(6) 0.138(14) -0.002(8) 0.016(11) 0.002(5)
C4 0.131(16) 0.033(8) 0.115(14) 0.005(8) -0.004(14) 0.021(9)
N2 0.095(10) 0.053(7) 0.084(10) -0.003(7) 0.003(9) 0.015(7)
O2 0.064(7) 0.065(9) 0.210(17) 0.080(11) 0.030(9) 0.013(6)
C5 0.058(9) 0.085(13) 0.22(2) 0.063(14) 0.040(12) 0.000(8)
C6 0.073(7) 0.063(9) 0.077(10) 0.024(9) 0.006(8) 0.024(8)
C7 0.065(7) 0.077(13) 0.092(12) -0.009(10) 0.015(9) 0.007(8)
C8 0.085(8) 0.080(9) 0.077(8) -0.002(9) 0.008(7) 0.025(8)
Cl 0.029(4) 0.058(6) 0.055(4) -0.026(4) 0.002(3) 0.006(2)
O11 0.080(6) 0.092(6) 0.082(4) 0.015(5) -0.001(4) -0.008(4)
O12 0.080(6) 0.092(6) 0.082(4) 0.015(5) -0.001(4) -0.008(4)
O13 0.080(6) 0.092(6) 0.082(4) 0.015(5) -0.001(4) -0.008(4)
O14 0.080(6) 0.092(6) 0.082(4) 0.015(5) -0.001(4) -0.008(4)
ClA 0.089(9) 0.045(7) 0.067(7) 0.009(6) -0.025(6) -0.003(4)
O12A 0.080(6) 0.092(6) 0.082(4) 0.015(5) -0.001(4) -0.008(4)
O13A 0.080(6) 0.092(6) 0.082(4) 0.015(5) -0.001(4) -0.008(4)
O11A 0.080(6) 0.092(6) 0.082(4) 0.015(5) -0.001(4) -0.008(4)
O14A 0.080(6) 0.092(6) 0.082(4) 0.015(5) -0.001(4) -0.008(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu O1 1.901(12) . ?
Cu N2 1.909(14) . ?
Cu O2 1.977(12) . ?
Cu N1 2.003(9) . ?
Cu O3B 2.32(2) . ?
Cu O3A 2.331(11) . ?
O3A H31 0.86(2) . ?
O3A H32 0.84(2) . ?
O3A H34 0.52(4) . ?
O3B O3B 1.56(5) 2_665 ?
O3B H31 1.06(8) . ?
O3B H32 1.08(8) . ?
O3B H33 0.79(2) . ?
O3B H34 0.83(2) . ?
O1 C1 1.421(13) . ?
O1 H11 0.86(2) . ?
N1 C2 1.470(12) . ?
N1 H1C 0.9200 . ?
N1 H1D 0.9200 . ?
C1 C2 1.455(16) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.512(12) . ?
C2 H2 1.0000 . ?
C3 C4 1.492(17) . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N2 C6 1.476(14) . ?
N2 H2C 0.9200 . ?
N2 H2D 0.9200 . ?
O2 C5 1.406(14) . ?
O2 H21 0.9500 . ?
C5 C6 1.434(16) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.482(14) . ?
C6 H6A 1.0000 . ?
C7 C8 1.467(16) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Cl O13 1.380(13) . ?
Cl O11 1.392(14) . ?
Cl O12 1.422(13) . ?
Cl O14 1.490(14) . ?
ClA O14A 1.399(14) . ?
ClA O11A 1.413(14) . ?
ClA O12A 1.425(14) . ?
ClA O13A 1.437(15) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu N2 165.5(5) . . ?
O1 Cu O2 89.8(3) . . ?
N2 Cu O2 82.6(5) . . ?
O1 Cu N1 85.7(4) . . ?
N2 Cu N1 100.1(3) . . ?
O2 Cu N1 170.9(5) . . ?
O1 Cu O3B 90.8(8) . . ?
N2 Cu O3B 101.4(8) . . ?
O2 Cu O3B 89.5(8) . . ?
N1 Cu O3B 98.4(7) . . ?
O1 Cu O3A 104.4(5) . . ?
N2 Cu O3A 89.3(5) . . ?
O2 Cu O3A 101.6(6) . . ?
N1 Cu O3A 87.2(5) . . ?
O3B Cu O3A 18.3(8) . . ?
Cu O3A H31 121(3) . . ?
Cu O3A H32 123(3) . . ?
H31 O3A H32 111(5) . . ?
Cu O3A H34 160(4) . . ?
H31 O3A H34 55(3) . . ?
H32 O3A H34 56(3) . . ?
O3B O3B Cu 130.1(9) 2_665 . ?
O3B O3B H31 106(5) 2_665 . ?
Cu O3B H31 111(3) . . ?
O3B O3B H32 107(5) 2_665 . ?
Cu O3B H32 110(3) . . ?
H31 O3B H32 82(7) . . ?
O3B O3B H33 8(4) 2_665 . ?
Cu O3B H33 122(4) . . ?
H31 O3B H33 112(6) . . ?
H32 O3B H33 113(6) . . ?
O3B O3B H34 110(3) 2_665 . ?
Cu O3B H34 120(3) . . ?
H31 O3B H34 42(4) . . ?
H32 O3B H34 41(4) . . ?
H33 O3B H34 118(6) . . ?
C1 O1 Cu 111.5(7) . . ?
C1 O1 H11 119(4) . . ?
Cu O1 H11 128(4) . . ?
C2 N1 Cu 105.6(6) . . ?
C2 N1 H1C 102.1 . . ?
Cu N1 H1C 112.8 . . ?
C2 N1 H1D 112.2 . . ?
Cu N1 H1D 113.1 . . ?
H1C N1 H1D 110.4 . . ?
O1 C1 C2 109.7(10) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C1 C2 N1 109.1(9) . . ?
C1 C2 C3 111.8(11) . . ?
N1 C2 C3 111.6(10) . . ?
C1 C2 H2 108.1 . . ?
N1 C2 H2 108.1 . . ?
C3 C2 H2 108.1 . . ?
C4 C3 C2 113.2(12) . . ?
C4 C3 H3C 108.9 . . ?
C2 C3 H3C 108.9 . . ?
C4 C3 H3D 108.9 . . ?
C2 C3 H3D 108.9 . . ?
H3C C3 H3D 107.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 N2 Cu 113.6(9) . . ?
C6 N2 H2C 108.8 . . ?
Cu N2 H2C 108.8 . . ?
C6 N2 H2D 108.8 . . ?
Cu N2 H2D 108.8 . . ?
H2C N2 H2D 107.7 . . ?
C5 O2 Cu 114.4(8) . . ?
C5 O2 H21 119.3 . . ?
Cu O2 H21 125.5 . . ?
O2 C5 C6 113.0(12) . . ?
O2 C5 H5A 109.0 . . ?
C6 C5 H5A 109.0 . . ?
O2 C5 H5B 109.0 . . ?
C6 C5 H5B 109.0 . . ?
H5A C5 H5B 107.8 . . ?
C5 C6 N2 110.5(11) . . ?
C5 C6 C7 116.5(11) . . ?
N2 C6 C7 122.5(14) . . ?
C5 C6 H6A 100.9 . . ?
N2 C6 H6A 100.9 . . ?
C7 C6 H6A 100.9 . . ?
C8 C7 C6 117.1(14) . . ?
C8 C7 H7A 108.0 . . ?
C6 C7 H7A 108.0 . . ?
C8 C7 H7B 108.0 . . ?
C6 C7 H7B 108.0 . . ?
H7A C7 H7B 107.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O13 Cl O11 119.6(10) . . ?
O13 Cl O12 112.9(11) . . ?
O11 Cl O12 111.7(10) . . ?
O13 Cl O14 105.1(10) . . ?
O11 Cl O14 103.8(11) . . ?
O12 Cl O14 101.2(10) . . ?
O14A ClA O11A 110.3(12) . . ?
O14A ClA O12A 113.9(12) . . ?
O11A ClA O12A 110.0(11) . . ?
O14A ClA O13A 109.8(12) . . ?
O11A ClA O13A 108.9(12) . . ?
O12A ClA O13A 103.6(11) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3A H31 O1 0.86(2) 2.28(7) 2.890(17) 128(8) 1_556
O3A H32 O2 0.84(2) 2.32(7) 2.91(2) 128(8) 1_556
O3B H34 O1 0.83(2) 2.55(4) 3.25(3) 143(2) 1_556
O3B H34 O1 0.83(2) 2.55(4) 3.25(3) 143(2) 1_556
N1 H1C O12 0.92 2.29 3.14(3) 152.0 1_556
N2 H2D O11 0.92 2.43 3.34(3) 167.2 1_556
N1 H1C O12A 0.92 2.30 3.10(2) 146.1 1_556
N2 H2D O13A 0.92 2.53 3.37(3) 153.4 1_556
N1 H1D O14A 0.92 2.44 3.20(2) 140.4 .
N2 H2C O14A 0.92 2.42 3.19(2) 141.2 .
N2 H2C O11 0.92 2.23 3.03(3) 144.5 .
N1 H1D O12 0.92 2.47 3.13(2) 129.5 .
O3B H33 O3A 0.79(2) 1.49(2) 2.22(3) 152(6) 2_665
O1 H11 O2 0.86(2) 1.66(14) 2.452(11) 151(27) 2_665
O2 H21 O1 0.95 1.64 2.452(11) 141.6 2_665
O3A H31 O3A 0.86(2) 2.59(11) 2.82(4) 96(7) 2_665
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 23.49
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 1.260
_refine_diff_density_min -0.340
_refine_diff_density_rms 0.103
#===END