#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:39:36 +0100 (vie 25 de mar de 2016) $
#$Revision: 179758 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/54/7005410.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7005410
loop_
_publ_author_name
'Burrows, Andrew D.'
'Cassar, Kevin'
'Mahon, Mary F.'
'Warren, John E.'
_publ_section_title
;
 The stepwise formation of mixed-metal coordination networks using
 complexes of 3-cyanoacetylacetonate.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2499
_journal_page_last               2509
_journal_paper_doi               10.1039/b702074k
_journal_year                    2007
_chemical_formula_sum            'C42 H54 Cu6 N6 O18'
_chemical_formula_weight         1312.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.936(1)
_cell_angle_beta                 100.006(1)
_cell_angle_gamma                104.594(1)
_cell_formula_units_Z            1
_cell_length_a                   8.6030(1)
_cell_length_b                   10.6410(2)
_cell_length_c                   14.7610(3)
_cell_measurement_reflns_used    17677
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     1235.97(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32325
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         5.62
_exptl_absorpt_coefficient_mu    2.613
_exptl_absorpt_correction_T_max  00.84
_exptl_absorpt_correction_T_min  00.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
?
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0140(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         7172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0495P)²+0.0758P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                5097
_reflns_number_total             7172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702074k.txt
_cod_data_source_block           compound_2_h06kc2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7005410
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.56988(3) 0.51048(3) 0.602018(18) 0.02098(9) Uani 1 1 d . . .
O1 O 0.7680(2) 0.48357(16) 0.66652(11) 0.0239(3) Uani 1 1 d . . .
N1 N 0.7934(3) 0.4517(3) 0.98198(16) 0.0405(6) Uani 1 1 d . . .
C1 C 0.9677(3) 0.4525(3) 0.78349(18) 0.0309(5) Uani 1 1 d . . .
H1A H 1.0309 0.4609 0.7348 0.046 Uiso 1 1 calc R . .
H1B H 0.9518 0.3625 0.7935 0.046 Uiso 1 1 calc R . .
H1C H 1.0286 0.5217 0.8438 0.046 Uiso 1 1 calc R . .
Cu2 Cu 0.47683(3) 0.77389(3) 0.576952(18) 0.02201(9) Uani 1 1 d . . .
O2 O 0.4712(2) 0.50383(18) 0.70915(12) 0.0287(4) Uani 1 1 d . . .
N2 N 0.8820(3) 0.8380(3) 1.17903(17) 0.0438(6) Uani 1 1 d . . .
C2 C 0.8019(3) 0.4712(2) 0.75039(16) 0.0226(4) Uani 1 1 d . . .
Cu3 Cu 0.61955(3) 0.80809(3) 0.781103(18) 0.02297(9) Uani 1 1 d . . .
O3 O 0.37927(18) 0.53214(16) 0.52255(11) 0.0211(3) Uani 1 1 d . . .
N3 N 0.3008(3) 0.9380(2) 0.23019(15) 0.0348(5) Uani 1 1 d . . .
C3 C 0.6933(3) 0.4728(2) 0.81230(16) 0.0238(5) Uani 1 1 d . . .
O4 O 0.67087(18) 0.75480(16) 0.65743(11) 0.0226(3) Uani 1 1 d . . .
C4 C 0.5335(3) 0.4885(2) 0.78880(16) 0.0237(5) Uani 1 1 d . . .
O5 O 0.4166(2) 0.78827(19) 0.69619(11) 0.0287(4) Uani 1 1 d . . .
C5 C 0.4268(3) 0.4879(3) 0.85834(17) 0.0315(5) Uani 1 1 d . . .
H5A H 0.3659 0.5535 0.8536 0.047 Uiso 1 1 calc R . .
H5B H 0.4963 0.5124 0.9235 0.047 Uiso 1 1 calc R . .
H5C H 0.3481 0.3973 0.8436 0.047 Uiso 1 1 calc R . .
O6 O 0.8316(2) 0.81327(17) 0.85157(11) 0.0268(4) Uani 1 1 d . . .
C6 C 0.7494(3) 0.4608(3) 0.90617(17) 0.0304(5) Uani 1 1 d . . .
O7 O 0.5363(2) 0.83329(18) 0.89384(11) 0.0281(4) Uani 1 1 d . . .
C7 C 0.2155(3) 0.4883(3) 0.53609(17) 0.0286(5) Uani 1 1 d . . .
H7A H 0.1863 0.3921 0.5330 0.043 Uiso 1 1 calc R . .
H7B H 0.1366 0.5022 0.4856 0.043 Uiso 1 1 calc R . .
H7C H 0.2114 0.5408 0.5989 0.043 Uiso 1 1 calc R . .
O8 O 0.5787(2) 0.79313(17) 0.47198(11) 0.0268(4) Uani 1 1 d . . .
C8 C 1.0457(3) 0.8122(3) 0.97508(18) 0.0305(5) Uani 1 1 d . . .
H8A H 1.0384 0.7242 0.9872 0.046 Uiso 1 1 calc R . .
H8B H 1.1019 0.8845 1.0346 0.046 Uiso 1 1 calc R . .
H8C H 1.1086 0.8230 0.9265 0.046 Uiso 1 1 calc R . .
O9 O 0.2825(2) 0.80866(17) 0.51497(11) 0.0251(3) Uani 1 1 d . . .
C9 C 0.8746(3) 0.8194(2) 0.93980(16) 0.0242(5) Uani 1 1 d . . .
C10 C 0.7710(3) 0.8298(2) 1.00336(16) 0.0240(5) Uani 1 1 d . . .
C11 C 0.6077(3) 0.8373(2) 0.97805(16) 0.0243(5) Uani 1 1 d . . .
C12 C 0.5097(3) 0.8515(3) 1.05154(17) 0.0326(6) Uani 1 1 d . . .
H12A H 0.5551 0.9427 1.0961 0.049 Uiso 1 1 calc R . .
H12B H 0.5156 0.7845 1.0870 0.049 Uiso 1 1 calc R . .
H12C H 0.3940 0.8366 1.0199 0.049 Uiso 1 1 calc R . .
C13 C 0.8341(3) 0.8347(3) 1.10085(17) 0.0298(5) Uani 1 1 d . . .
C14 C 0.2671(3) 0.7977(3) 0.71993(18) 0.0305(5) Uani 1 1 d . . .
H14A H 0.2290 0.7291 0.7524 0.046 Uiso 1 1 calc R . .
H14B H 0.1829 0.7827 0.6613 0.046 Uiso 1 1 calc R . .
H14C H 0.2855 0.8879 0.7626 0.046 Uiso 1 1 calc R . .
C15 C 0.8390(3) 0.8046(2) 0.65182(17) 0.0266(5) Uani 1 1 d . . .
H15A H 0.8892 0.8968 0.6944 0.040 Uiso 1 1 calc R . .
H15B H 0.8413 0.8051 0.5858 0.040 Uiso 1 1 calc R . .
H15C H 0.9016 0.7458 0.6715 0.040 Uiso 1 1 calc R . .
C16 C 0.6425(3) 0.8544(3) 0.33644(18) 0.0316(5) Uani 1 1 d . . .
H16A H 0.7125 0.9489 0.3571 0.047 Uiso 1 1 calc R . .
H16B H 0.5777 0.8330 0.2704 0.047 Uiso 1 1 calc R . .
H16C H 0.7125 0.7949 0.3396 0.047 Uiso 1 1 calc R . .
C17 C 0.5282(3) 0.8337(2) 0.40065(16) 0.0232(4) Uani 1 1 d . . .
C18 C 0.3726(3) 0.8584(2) 0.38096(16) 0.0234(5) Uani 1 1 d . . .
C19 C 0.2577(3) 0.8427(2) 0.43866(16) 0.0226(4) Uani 1 1 d . . .
C20 C 0.0947(3) 0.8691(3) 0.41088(18) 0.0295(5) Uani 1 1 d . . .
H20A H 0.0125 0.8158 0.4370 0.044 Uiso 1 1 calc R . .
H20B H 0.0570 0.8431 0.3409 0.044 Uiso 1 1 calc R . .
H20C H 0.1085 0.9655 0.4367 0.044 Uiso 1 1 calc R . .
C21 C 0.3314(3) 0.9019(2) 0.29670(17) 0.0268(5) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O2 92.53(7) . . ?
O1 Cu1 O3 172.90(6) . . ?
O2 Cu1 O3 94.32(7) . . ?
O1 Cu1 O3 93.03(6) . 2_666 ?
O2 Cu1 O3 163.62(8) . 2_666 ?
O3 Cu1 O3 79.88(7) . 2_666 ?
O1 Cu1 O4 95.26(6) . . ?
O2 Cu1 O4 91.01(7) . . ?
O3 Cu1 O4 86.46(6) . . ?
O3 Cu1 O4 103.80(6) 2_666 . ?
O1 Cu1 Cu1 132.89(5) . 2_666 ?
O2 Cu1 Cu1 132.51(5) . 2_666 ?
O3 Cu1 Cu1 40.01(5) . 2_666 ?
O3 Cu1 Cu1 39.86(4) 2_666 2_666 ?
O4 Cu1 Cu1 96.63(4) . 2_666 ?
C2 O1 Cu1 127.53(15) . . ?
O5 Cu2 O9 94.08(7) . . ?
O5 Cu2 O8 167.47(8) . . ?
O9 Cu2 O8 91.66(7) . . ?
O5 Cu2 O4 78.55(7) . . ?
O9 Cu2 O4 171.57(7) . . ?
O8 Cu2 O4 94.81(6) . . ?
O5 Cu2 O3 95.67(7) . . ?
O9 Cu2 O3 98.08(6) . . ?
O8 Cu2 O3 94.54(6) . . ?
O4 Cu2 O3 86.81(6) . . ?
O5 Cu2 Cu3 38.95(5) . . ?
O9 Cu2 Cu3 131.19(5) . . ?
O8 Cu2 Cu3 131.79(5) . . ?
O4 Cu2 Cu3 40.74(5) . . ?
O3 Cu2 Cu3 98.98(4) . . ?
C4 O2 Cu1 127.67(16) . . ?
O1 C2 C3 124.0(2) . . ?
O1 C2 C1 116.4(2) . . ?
C3 C2 C1 119.6(2) . . ?
O5 Cu3 O7 94.88(7) . . ?
O5 Cu3 O6 171.91(7) . . ?
O7 Cu3 O6 92.42(7) . . ?
O5 Cu3 O4 78.95(7) . . ?
O7 Cu3 O4 170.08(7) . . ?
O6 Cu3 O4 93.33(7) . . ?
O5 Cu3 Cu2 39.12(5) . . ?
O7 Cu3 Cu2 133.89(5) . . ?
O6 Cu3 Cu2 133.69(5) . . ?
O4 Cu3 Cu2 40.97(4) . . ?
C7 O3 Cu1 122.57(13) . . ?
C7 O3 Cu1 123.04(13) . 2_666 ?
Cu1 O3 Cu1 100.12(7) . 2_666 ?
C7 O3 Cu2 108.26(14) . . ?
Cu1 O3 Cu2 93.99(6) . . ?
Cu1 O3 Cu2 103.88(7) 2_666 . ?
C2 C3 C4 124.7(2) . . ?
C2 C3 C6 118.0(2) . . ?
C4 C3 C6 117.3(2) . . ?
C15 O4 Cu3 117.95(13) . . ?
C15 O4 Cu2 125.81(13) . . ?
Cu3 O4 Cu2 98.29(7) . . ?
C15 O4 Cu1 111.32(13) . . ?
Cu3 O4 Cu1 106.91(7) . . ?
Cu2 O4 Cu1 92.74(6) . . ?
O2 C4 C3 123.6(2) . . ?
O2 C4 C5 115.4(2) . . ?
C3 C4 C5 121.1(2) . . ?
C14 O5 Cu3 127.54(14) . . ?
C14 O5 Cu2 130.19(14) . . ?
Cu3 O5 Cu2 101.93(8) . . ?
C9 O6 Cu3 127.58(16) . . ?
N1 C6 C3 179.3(3) . . ?
C11 O7 Cu3 127.75(16) . . ?
C17 O8 Cu2 127.77(15) . . ?
C19 O9 Cu2 128.34(15) . . ?
O6 C9 C10 123.9(2) . . ?
O6 C9 C8 116.4(2) . . ?
C10 C9 C8 119.7(2) . . ?
C9 C10 C11 124.6(2) . . ?
C9 C10 C13 118.3(2) . . ?
C11 C10 C13 117.1(2) . . ?
O7 C11 C10 123.5(2) . . ?
O7 C11 C12 116.2(2) . . ?
C10 C11 C12 120.3(2) . . ?
N2 C13 C10 178.8(3) . . ?
O8 C17 C18 123.4(2) . . ?
O8 C17 C16 116.1(2) . . ?
C18 C17 C16 120.5(2) . . ?
C19 C18 C17 124.1(2) . . ?
C19 C18 C21 118.8(2) . . ?
C17 C18 C21 117.1(2) . . ?
O9 C19 C18 124.1(2) . . ?
O9 C19 C20 115.7(2) . . ?
C18 C19 C20 120.13(19) . . ?
N3 C21 C18 179.0(3) . . ?
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 O1 1.9232(15) . ?
Cu1 O2 1.9269(16) . ?
Cu1 O3 1.9394(15) . ?
Cu1 O3 1.9453(16) 2_666 ?
Cu1 O4 2.4178(17) . ?
Cu1 Cu1 2.9786(5) 2_666 ?
O1 C2 1.265(3) . ?
N1 C6 1.151(3) . ?
C1 C2 1.503(3) . ?
Cu2 O5 1.9042(16) . ?
Cu2 O9 1.9235(16) . ?
Cu2 O8 1.9325(16) . ?
Cu2 O4 1.9567(15) . ?
Cu2 O3 2.3916(17) . ?
Cu2 Cu3 2.9528(4) . ?
O2 C4 1.268(3) . ?
N2 C13 1.146(3) . ?
C2 C3 1.416(3) . ?
Cu3 O5 1.8973(16) . ?
Cu3 O7 1.9146(17) . ?
Cu3 O6 1.9173(16) . ?
Cu3 O4 1.9472(16) . ?
O3 C7 1.432(3) . ?
O3 Cu1 1.9453(16) 2_666 ?
N3 C21 1.145(3) . ?
C3 C4 1.419(3) . ?
C3 C6 1.431(3) . ?
O4 C15 1.434(3) . ?
C4 C5 1.491(3) . ?
O5 C14 1.412(3) . ?
O6 C9 1.273(3) . ?
O7 C11 1.274(3) . ?
O8 C17 1.274(3) . ?
C8 C9 1.501(3) . ?
O9 C19 1.258(3) . ?
C9 C10 1.408(3) . ?
C10 C11 1.417(3) . ?
C10 C13 1.431(3) . ?
C11 C12 1.489(3) . ?
C16 C17 1.490(3) . ?
C17 C18 1.423(3) . ?
C18 C19 1.416(3) . ?
C18 C21 1.440(3) . ?
C19 C20 1.504(3) . ?
