#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:21:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179786 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/82/7008243.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_7008243
loop_
_publ_author_name
'Toma, Liviu'
'Toma, Luminita Marilena'
'Lescouëzec, Rodrigue'
'Armentano, Donatella'
'De Munno, Giovanni'
'Andruh, Marius'
'Cano, Joan'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 Synthesis, crystal structures and magnetic properties of cyanide- and
 phenolate-bridged [M(III)NiII]2 tetranuclear complexes (M=Fe and Cr).
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1357
_journal_page_last               1364
_journal_paper_doi               10.1039/b500168b
_journal_year                    2005
_chemical_formula_sum            'C30 H26 Cr N9 Ni O2'
_chemical_formula_weight         655.31
_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                101.02(2)
_cell_angle_beta                 103.63(2)
_cell_angle_gamma                109.18(2)
_cell_formula_units_Z            2
_cell_length_a                   10.000(3)
_cell_length_b                   11.492(3)
_cell_length_c                   14.669(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      15
_cell_volume                     1479.6(8)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'R3m/V automatic four-circle diffractometer'
_diffrn_measurement_method       omega/2-theta-scans
_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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6213
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        1.3
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.6673
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.644
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5858
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1027P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1541
_reflns_number_gt                4177
_reflns_number_total             5858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b500168b.txt
_cod_data_source_block           3
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1479.6(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008243
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
Cr1 Cr -0.15177(7) 0.21748(6) 0.30276(4) 0.03409(18) Uani 1 1 d . . .
N1 N 0.0607(4) 0.2978(3) 0.4080(2) 0.0389(8) Uani 1 1 d . . .
N2 N -0.1204(4) 0.0508(3) 0.3195(3) 0.0435(8) Uani 1 1 d . . .
C1 C 0.1493(5) 0.4215(5) 0.4520(3) 0.0473(11) Uani 1 1 d . . .
H1A H 0.1119 0.4834 0.4409 0.057 Uiso 1 1 calc R . .
C2 C 0.2944(6) 0.4620(6) 0.5134(4) 0.0627(14) Uani 1 1 d . . .
H2A H 0.3529 0.5494 0.5425 0.075 Uiso 1 1 calc R . .
C3 C 0.3502(6) 0.3724(6) 0.5306(4) 0.0693(16) Uani 1 1 d . . .
H3A H 0.4480 0.3986 0.5712 0.083 Uiso 1 1 calc R . .
C4 C 0.2618(5) 0.2410(5) 0.4877(3) 0.0523(12) Uani 1 1 d . . .
C5 C 0.3085(7) 0.1402(7) 0.5028(4) 0.0694(16) Uani 1 1 d . . .
H5A H 0.4053 0.1609 0.5427 0.083 Uiso 1 1 calc R . .
C6 C 0.2169(7) 0.0166(7) 0.4614(4) 0.0716(17) Uani 1 1 d . . .
H6A H 0.2515 -0.0467 0.4734 0.086 Uiso 1 1 calc R . .
C7 C 0.0684(6) -0.0210(5) 0.3996(4) 0.0547(13) Uani 1 1 d . . .
C8 C -0.0341(8) -0.1488(6) 0.3530(5) 0.0727(18) Uani 1 1 d . . .
H8A H -0.0071 -0.2164 0.3637 0.087 Uiso 1 1 calc R . .
C9 C -0.1730(8) -0.1745(5) 0.2921(5) 0.0695(16) Uani 1 1 d . . .
H9A H -0.2404 -0.2592 0.2608 0.083 Uiso 1 1 calc R . .
C10 C -0.2133(6) -0.0718(5) 0.2771(4) 0.0585(13) Uani 1 1 d . . .
H10A H -0.3087 -0.0903 0.2360 0.070 Uiso 1 1 calc R . .
C11 C 0.0189(5) 0.0765(4) 0.3808(3) 0.0427(10) Uani 1 1 d . . .
C12 C 0.1145(5) 0.2079(4) 0.4263(3) 0.0422(10) Uani 1 1 d . . .
N8 N 0.2354(4) 0.2884(3) 0.0404(3) 0.0438(8) Uani 1 1 d . . .
C13 C -0.2628(5) 0.2175(4) 0.4052(3) 0.0437(10) Uani 1 1 d . . .
N3 N -0.3295(5) 0.2167(5) 0.4580(3) 0.0658(12) Uani 1 1 d . . .
C14 C -0.1606(5) 0.3915(5) 0.2937(3) 0.0452(10) Uani 1 1 d . . .
N4 N -0.1640(6) 0.4879(5) 0.2896(4) 0.0759(14) Uani 1 1 d . . .
C15 C -0.3541(5) 0.1159(4) 0.1925(3) 0.0438(10) Uani 1 1 d . . .
N5 N -0.4625(4) 0.0574(4) 0.1297(3) 0.0588(11) Uani 1 1 d . . .
C16 C -0.0477(4) 0.2116(4) 0.1962(3) 0.0330(8) Uani 1 1 d . . .
N6 N 0.0105(4) 0.1939(3) 0.1399(3) 0.0423(8) Uani 1 1 d . . .
Ni1 Ni 0.13709(5) 0.12287(5) 0.06739(3) 0.03118(16) Uani 1 1 d . . .
N7 N 0.2883(3) 0.1550(3) 0.1980(2) 0.0369(8) Uani 1 1 d . . .
C17 C 0.2980(4) 0.0638(4) 0.2334(3) 0.0403(10) Uani 1 1 d . . .
H17A H 0.3784 0.0878 0.2900 0.048 Uiso 1 1 calc R . .
C18 C 0.2009(5) -0.0721(4) 0.1976(3) 0.0382(9) Uani 1 1 d . . .
C19 C 0.2469(5) -0.1532(5) 0.2468(3) 0.0475(11) Uani 1 1 d . . .
H19A H 0.3384 -0.1166 0.2969 0.057 Uiso 1 1 calc R . .
C20 C 0.1652(6) -0.2831(5) 0.2255(3) 0.0506(11) Uani 1 1 d . . .
C21 C 0.0289(6) -0.3332(5) 0.1536(3) 0.0528(12) Uani 1 1 d . . .
H21A H -0.0308 -0.4199 0.1400 0.063 Uiso 1 1 calc R . .
C22 C -0.0255(5) -0.2604(4) 0.0995(3) 0.0425(10) Uani 1 1 d . . .
C23 C 0.0626(4) -0.1268(4) 0.1190(3) 0.0350(9) Uani 1 1 d . . .
C24 C 0.2220(7) -0.3658(6) 0.2808(4) 0.0735(16) Uani 1 1 d . . .
H24A H 0.1499 -0.4532 0.2559 0.110 Uiso 1 1 calc R . .
H24B H 0.2368 -0.3336 0.3494 0.110 Uiso 1 1 calc R . .
H24C H 0.3151 -0.3628 0.2721 0.110 Uiso 1 1 calc R . .
O1 O 0.0178(3) -0.0573(2) 0.06824(18) 0.0342(6) Uani 1 1 d . . .
O2 O 0.2739(3) 0.0511(3) -0.0002(2) 0.0514(8) Uani 1 1 d D . .
H1W H 0.357(3) 0.040(4) 0.038(3) 0.060 Uiso 1 1 d D . .
H2W H 0.230(4) -0.018(3) -0.0599(18) 0.060 Uiso 1 1 d D . .
C25 C 0.4069(5) 0.2839(4) 0.2522(3) 0.0528(12) Uani 1 1 d . . .
H25A H 0.3996 0.3080 0.3174 0.063 Uiso 1 1 calc R . .
H25B H 0.5029 0.2772 0.2598 0.063 Uiso 1 1 calc R . .
C26 C 0.4062(7) 0.3866(6) 0.2096(5) 0.089(2) Uani 1 1 d . . .
H26A H 0.4986 0.4602 0.2470 0.107 Uiso 1 1 calc R . .
H26B H 0.3255 0.4099 0.2211 0.107 Uiso 1 1 calc R . .
C27 C 0.3910(6) 0.3715(6) 0.1059(4) 0.0767(18) Uani 1 1 d . . .
H27A H 0.4588 0.3339 0.0890 0.092 Uiso 1 1 calc R . .
H27B H 0.4193 0.4558 0.0952 0.092 Uiso 1 1 calc R . .
C28 C 0.1745(5) 0.3272(4) -0.0273(3) 0.0506(11) Uani 1 1 d . . .
H28A H 0.2315 0.4073 -0.0312 0.061 Uiso 1 1 calc R . .
C29 C 0.2908(9) 0.7281(7) -0.0001(6) 0.0828(19) Uani 1 1 d . . .
H29A H 0.334(6) 0.811(5) -0.001(4) 0.060 Uiso 1 1 d . . .
H29B H 0.183(6) 0.716(5) -0.003(4) 0.060 Uiso 1 1 d . . .
H29C H 0.272(5) 0.658(5) -0.071(4) 0.060 Uiso 1 1 d . . .
C30 C 0.3989(8) 0.7094(6) 0.0696(6) 0.0811(18) Uani 1 1 d . . .
N9 N 0.4824(8) 0.6924(7) 0.1252(7) 0.139(3) 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
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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
C14 Cr1 C15 92.10(18) . . ?
C14 Cr1 C13 89.30(17) . . ?
C15 Cr1 C13 89.73(17) . . ?
C14 Cr1 C16 91.47(16) . . ?
C15 Cr1 C16 88.17(16) . . ?
C13 Cr1 C16 177.79(16) . . ?
C14 Cr1 N2 174.36(16) . . ?
C15 Cr1 N2 93.31(17) . . ?
C13 Cr1 N2 92.34(16) . . ?
C16 Cr1 N2 87.10(15) . . ?
C14 Cr1 N1 95.11(16) . . ?
C15 Cr1 N1 171.84(15) . . ?
C13 Cr1 N1 94.18(15) . . ?
C16 Cr1 N1 87.82(14) . . ?
N2 Cr1 N1 79.40(14) . . ?
C1 N1 C12 118.2(4) . . ?
C1 N1 Cr1 129.0(3) . . ?
C12 N1 Cr1 112.6(3) . . ?
C10 N2 C11 118.1(4) . . ?
C10 N2 Cr1 129.1(4) . . ?
C11 N2 Cr1 112.7(3) . . ?
N1 C1 C2 123.1(5) . . ?
C3 C2 C1 119.1(5) . . ?
C2 C3 C4 120.5(5) . . ?
C3 C4 C12 116.8(5) . . ?
C3 C4 C5 124.8(5) . . ?
C12 C4 C5 118.5(5) . . ?
C6 C5 C4 121.7(5) . . ?
C5 C6 C7 121.8(5) . . ?
C8 C7 C11 116.6(5) . . ?
C8 C7 C6 125.1(5) . . ?
C11 C7 C6 118.2(5) . . ?
C9 C8 C7 120.4(5) . . ?
C8 C9 C10 119.4(5) . . ?
N2 C10 C9 122.5(5) . . ?
N2 C11 C7 123.0(5) . . ?
N2 C11 C12 116.8(4) . . ?
C7 C11 C12 120.2(4) . . ?
N1 C12 C4 122.4(4) . . ?
N1 C12 C11 118.0(4) . . ?
C4 C12 C11 119.6(4) . . ?
C28 N8 C27 118.7(4) . . ?
C28 N8 Ni1 124.7(3) . . ?
C27 N8 Ni1 116.6(3) . . ?
N3 C13 Cr1 176.8(4) . . ?
N4 C14 Cr1 179.3(5) . . ?
N5 C15 Cr1 177.0(4) . . ?
N6 C16 Cr1 171.0(4) . . ?
C16 N6 Ni1 160.0(3) . . ?
N8 Ni1 N7 98.61(14) . . ?
N8 Ni1 O1 169.62(12) . . ?
N7 Ni1 O1 91.11(13) . . ?
N8 Ni1 O1 89.64(13) . 2 ?
N7 Ni1 O1 169.69(12) . 2 ?
O1 Ni1 O1 80.31(11) . 2 ?
N8 Ni1 N6 93.77(15) . . ?
N7 Ni1 N6 90.14(13) . . ?
O1 Ni1 N6 89.81(13) . . ?
O1 Ni1 N6 95.50(12) 2 . ?
N8 Ni1 O2 86.84(15) . . ?
N7 Ni1 O2 87.15(13) . . ?
O1 Ni1 O2 90.04(13) . . ?
O1 Ni1 O2 87.15(11) 2 . ?
N6 Ni1 O2 177.27(13) . . ?
C17 N7 C25 115.6(4) . . ?
C17 N7 Ni1 122.4(3) . . ?
C25 N7 Ni1 121.6(3) . . ?
N7 C17 C18 129.0(4) . . ?
C19 C18 C23 118.8(4) . . ?
C19 C18 C17 116.5(4) . . ?
C23 C18 C17 124.6(4) . . ?
C20 C19 C18 124.1(4) . . ?
C21 C20 C19 116.5(4) . . ?
C21 C20 C24 121.9(5) . . ?
C19 C20 C24 121.6(5) . . ?
C20 C21 C22 123.4(4) . . ?
C21 C22 C23 119.9(4) . . ?
C21 C22 C28 116.7(4) . 2 ?
C23 C22 C28 123.5(4) . 2 ?
O1 C23 C18 121.4(4) . . ?
O1 C23 C22 121.5(4) . . ?
C18 C23 C22 117.1(4) . . ?
C23 O1 Ni1 128.0(2) . . ?
C23 O1 Ni1 126.7(2) . 2 ?
Ni1 O1 Ni1 99.69(11) . 2 ?
C26 C25 N7 116.8(4) . . ?
C25 C26 C27 121.7(6) . . ?
C26 C27 N8 112.2(5) . . ?
N8 C28 C22 127.3(4) . 2 ?
N9 C30 C29 178.5(9) . . ?
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
Cr1 C14 2.058(5) . ?
Cr1 C15 2.063(5) . ?
Cr1 C13 2.069(5) . ?
Cr1 C16 2.075(4) . ?
Cr1 N2 2.089(4) . ?
Cr1 N1 2.091(3) . ?
N1 C1 1.332(6) . ?
N1 C12 1.353(5) . ?
N2 C10 1.329(6) . ?
N2 C11 1.369(6) . ?
C1 C2 1.383(6) . ?
C2 C3 1.359(8) . ?
C3 C4 1.398(8) . ?
C4 C12 1.414(6) . ?
C4 C5 1.419(7) . ?
C5 C6 1.334(9) . ?
C6 C7 1.418(8) . ?
C7 C8 1.404(8) . ?
C7 C11 1.413(6) . ?
C8 C9 1.364(8) . ?
C9 C10 1.405(8) . ?
C11 C12 1.416(6) . ?
N8 C28 1.273(6) . ?
N8 C27 1.491(6) . ?
N8 Ni1 1.996(4) . ?
C13 N3 1.133(6) . ?
C14 N4 1.132(6) . ?
C15 N5 1.136(5) . ?
C16 N6 1.141(5) . ?
N6 Ni1 2.093(4) . ?
Ni1 N7 2.022(3) . ?
Ni1 O1 2.026(3) . ?
Ni1 O1 2.033(3) 2 ?
Ni1 O2 2.146(3) . ?
N7 C17 1.276(5) . ?
N7 C25 1.478(5) . ?
C17 C18 1.452(6) . ?
C18 C19 1.409(6) . ?
C18 C23 1.427(6) . ?
C19 C20 1.376(7) . ?
C20 C21 1.370(7) . ?
C20 C24 1.522(6) . ?
C21 C22 1.405(6) . ?
C22 C23 1.428(6) . ?
C22 C28 1.458(6) 2 ?
C23 O1 1.303(5) . ?
O1 Ni1 2.033(3) 2 ?
C25 C26 1.438(8) . ?
C26 C27 1.462(8) . ?
C28 C22 1.458(6) 2 ?
C29 C30 1.405(10) . ?
C30 N9 1.118(9) . ?
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
O2 H1W N5 0.948(10) 1.905(14) 2.835(5) 167(4) 1_655
O2 H2W N6 0.953(10) 2.41(3) 3.162(5) 135(4) 2
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1 C16 N6 Ni1 -21(3) . . . . ?
