#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:56:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/29/4332986.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332986
loop_
_publ_author_name
'Rodríguez-Diéguez, Antonio'
'Kivekäs, Raikko'
'Sillanpää, Reijo'
'Cano, Joan'
'Lloret, Francesc'
'McKee, Vickie'
'Stoeckli-Evans, Helen'
'Colacio, Enrique'
_publ_section_title
;
 Structural and Magnetic Diversity in Cyano-Bridged Bi- and Trimetallic
 Complexes Assembled from Cyanometalates and [M(rac-CTH)]n+Building Blocks
 (CTH =d,l-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10537
_journal_page_last               10551
_journal_paper_doi               10.1021/ic061187j
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C42 H72 Cu3 Fe2 N24, 5(H2 O)'
_chemical_formula_sum            'C42 H82 Cu3 Fe2 N24 O5'
_chemical_formula_weight         1305.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.357(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7784(8)
_cell_length_b                   33.112(3)
_cell_length_c                   9.7326(9)
_cell_measurement_reflns_used    5091
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.41
_cell_volume                     2811.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       ω--θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17862
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.788056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (G.M. Sheldrick, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1362.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.385
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0544P)²+5.3866P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                5465
_reflns_number_total             6443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061187jsup1.cif
_cod_data_source_block           compound_9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2811.6(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4332986
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Cu1 Cu 0.68406(4) 0.185505(11) 0.58777(4) 0.01362(11) Uani 1 1 d .
Fe1 Fe 0.71318(5) 0.126597(13) 0.09882(4) 0.01205(11) Uani 1 1 d .
Cu2 Cu 1.0000 0.0000 0.0000 0.01654(13) Uani 1 2 d S
N15 N 0.6389(3) 0.18922(8) 0.3174(3) 0.0182(6) Uani 1 1 d .
N4 N 0.7099(3) 0.24612(8) 0.5903(3) 0.0155(5) Uani 1 1 d .
N19 N 0.7378(3) 0.18544(8) -0.1469(3) 0.0188(6) Uani 1 1 d .
N14 N 0.9088(3) 0.17368(8) 0.5810(3) 0.0149(5) Uani 1 1 d .
N11 N 0.6530(3) 0.12493(8) 0.5743(3) 0.0150(5) Uani 1 1 d .
C15 C 0.6647(3) 0.16722(9) 0.2304(3) 0.0140(6) Uani 1 1 d .
N7 N 0.4585(3) 0.19658(8) 0.5927(3) 0.0150(5) Uani 1 1 d .
N17 N 0.8350(3) 0.05764(8) -0.0721(3) 0.0198(6) Uani 1 1 d .
C18 C 0.4971(4) 0.12225(9) 0.0324(3) 0.0155(6) Uani 1 1 d .
N18 N 0.3681(3) 0.12134(9) -0.0081(3) 0.0219(6) Uani 1 1 d .
C19 C 0.7308(3) 0.16454(9) -0.0520(3) 0.0134(6) Uani 1 1 d .
C17 C 0.7808(4) 0.08356(9) -0.0144(3) 0.0153(6) Uani 1 1 d .
C13 C 0.9201(4) 0.13111(10) 0.5359(3) 0.0173(6) Uani 1 1 d .
H13A H 1.0255 0.1209 0.5612 0.021 Uiso 1 1 calc R
H13B H 0.8962 0.1292 0.4343 0.021 Uiso 1 1 calc R
C5 C 0.5552(4) 0.26315(10) 0.5532(3) 0.0187(6) Uani 1 1 d .
H5A H 0.5255 0.2608 0.4524 0.022 Uiso 1 1 calc R
H5B H 0.5537 0.2921 0.5788 0.022 Uiso 1 1 calc R
C20 C 0.6854(3) 0.08617(9) 0.2395(3) 0.0151(6) Uani 1 1 d .
N16 N 1.0557(3) 0.13895(9) 0.2014(3) 0.0204(6) Uani 1 1 d .
C2 C 0.9807(4) 0.24481(10) 0.5404(3) 0.0195(7) Uani 1 1 d .
H2A H 1.0567 0.2610 0.4965 0.023 Uiso 1 1 calc R
H2B H 1.0080 0.2462 0.6418 0.023 Uiso 1 1 calc R
C16 C 0.9277(4) 0.13409(9) 0.1636(3) 0.0151(6) Uani 1 1 d .
C12 C 0.8072(4) 0.10624(10) 0.6064(3) 0.0176(6) Uani 1 1 d .
H12A H 0.8059 0.0781 0.5722 0.021 Uiso 1 1 calc R
H12B H 0.8367 0.1059 0.7076 0.021 Uiso 1 1 calc R
C10 C 0.5391(4) 0.10591(10) 0.6564(3) 0.0200(7) Uani 1 1 d .
H10A H 0.5767 0.1078 0.7559 0.024 Uiso 1 1 calc R
H10B H 0.5291 0.0769 0.6319 0.024 Uiso 1 1 calc R
N20 N 0.6666(3) 0.06193(9) 0.3220(3) 0.0238(6) Uani 1 1 d .
C9 C 0.3828(4) 0.12589(10) 0.6311(3) 0.0215(7) Uani 1 1 d .
H9A H 0.3489 0.1255 0.5306 0.026 Uiso 1 1 calc R
H9B H 0.3084 0.1098 0.6777 0.026 Uiso 1 1 calc R
C8 C 0.3800(4) 0.16910(10) 0.6819(3) 0.0198(7) Uani 1 1 d .
H8A H 0.2724 0.1779 0.6830 0.024 Uiso 1 1 calc R
H8B H 0.4310 0.1705 0.7778 0.024 Uiso 1 1 calc R
C3 C 0.8229(4) 0.26341(10) 0.5048(3) 0.0184(6) Uani 1 1 d .
H3A H 0.8293 0.2930 0.5198 0.022 Uiso 1 1 calc R
H3B H 0.7881 0.2586 0.4059 0.022 Uiso 1 1 calc R
C6 C 0.4454(4) 0.23961(10) 0.6313(3) 0.0199(7) Uani 1 1 d .
H6A H 0.4719 0.2431 0.7321 0.024 Uiso 1 1 calc R
H6B H 0.3392 0.2493 0.6063 0.024 Uiso 1 1 calc R
C1 C 0.9913(4) 0.20139(10) 0.4947(3) 0.0178(6) Uani 1 1 d .
H1A H 0.9472 0.1990 0.3970 0.021 Uiso 1 1 calc R
H1B H 1.1004 0.1933 0.5007 0.021 Uiso 1 1 calc R
N27 N 0.9581(3) 0.00964(9) 0.1991(3) 0.0223(6) Uani 1 1 d .
N24 N 1.1900(3) 0.03545(9) 0.0165(3) 0.0227(6) Uani 1 1 d .
C25 C 1.2710(4) 0.02614(12) -0.1057(4) 0.0289(8) Uani 1 1 d .
H25A H 1.3294 0.0006 -0.0906 0.035 Uiso 1 1 calc R
H25B H 1.3438 0.0481 -0.1212 0.035 Uiso 1 1 calc R
C22 C 1.2094(5) 0.04245(11) 0.2723(4) 0.0317(9) Uani 1 1 d .
H22A H 1.2861 0.0457 0.3541 0.038 Uiso 1 1 calc R
H22B H 1.1570 0.0687 0.2550 0.038 Uiso 1 1 calc R
C23 C 1.2930(4) 0.03206(11) 0.1479(4) 0.0287(8) Uani 1 1 d .
H23A H 1.3812 0.0506 0.1448 0.034 Uiso 1 1 calc R
H23B H 1.3332 0.0042 0.1578 0.034 Uiso 1 1 calc R
C21 C 1.0924(4) 0.01147(11) 0.3056(3) 0.0271(8) Uani 1 1 d .
H21A H 1.1417 -0.0154 0.3139 0.032 Uiso 1 1 calc R
H21B H 1.0570 0.0181 0.3960 0.032 Uiso 1 1 calc R
C26 C 1.1520(4) 0.02210(11) -0.2300(4) 0.0285(8) Uani 1 1 d .
H26A H 1.0979 0.0481 -0.2485 0.034 Uiso 1 1 calc R
H26B H 1.2018 0.0146 -0.3127 0.034 Uiso 1 1 calc R
O2 O 0.3015(3) 0.18903(7) 0.3065(2) 0.0210(5) Uiso 1 1 d .
O1 O 0.0807(3) 0.14314(8) 0.8473(3) 0.0283(6) Uiso 1 1 d .
O3 O 0.5341(14) 0.9898(4) 0.4537(13) 0.119(4) Uiso 0.50 1 d P
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'
Fe Fe 0.3463 0.8444 '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'
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
N7 Cu1 N4 85.91(11) . .
N7 Cu1 N14 179.12(11) . .
N4 Cu1 N14 94.81(10) . .
N7 Cu1 N11 93.22(11) . .
N4 Cu1 N11 176.86(10) . .
N14 Cu1 N11 86.04(11) . .
C16 Fe1 C17 86.03(13) . .
C16 Fe1 C15 88.45(12) . .
C17 Fe1 C15 172.75(13) . .
C16 Fe1 C18 176.87(13) . .
C17 Fe1 C18 96.08(13) . .
C15 Fe1 C18 89.63(13) . .
C16 Fe1 C20 93.00(13) . .
C17 Fe1 C20 87.96(12) . .
C15 Fe1 C20 87.63(13) . .
C18 Fe1 C20 89.39(13) . .
C16 Fe1 C19 90.39(12) . .
C17 Fe1 C19 89.47(12) . .
C15 Fe1 C19 95.27(12) . .
C18 Fe1 C19 87.33(12) . .
C20 Fe1 C19 175.60(12) . .
N24 Cu2 N24 180.00(16) 3_755 .
N24 Cu2 N27 93.88(12) 3_755 3_755
N24 Cu2 N27 86.12(12) . 3_755
N24 Cu2 N27 86.12(12) 3_755 .
N24 Cu2 N27 93.88(12) . .
N27 Cu2 N27 180.0(2) 3_755 .
N24 Cu2 N17 88.49(10) 3_755 .
N24 Cu2 N17 91.51(10) . .
N27 Cu2 N17 90.74(10) 3_755 .
N27 Cu2 N17 89.26(10) . .
N24 Cu2 N17 91.51(10) 3_755 3_755
N24 Cu2 N17 88.49(10) . 3_755
N27 Cu2 N17 89.26(10) 3_755 3_755
N27 Cu2 N17 90.74(10) . 3_755
N17 Cu2 N17 180.00(14) . 3_755
C5 N4 C3 111.7(2) . .
C5 N4 Cu1 106.08(19) . .
C3 N4 Cu1 117.37(19) . .
C13 N14 C1 111.6(2) . .
C13 N14 Cu1 106.93(19) . .
C1 N14 Cu1 115.97(19) . .
C10 N11 C12 111.1(2) . .
C10 N11 Cu1 118.6(2) . .
C12 N11 Cu1 106.58(19) . .
N15 C15 Fe1 174.4(3) . .
C8 N7 C6 112.9(2) . .
C8 N7 Cu1 115.08(19) . .
C6 N7 Cu1 106.54(19) . .
C17 N17 Cu2 134.5(2) . .
N18 C18 Fe1 177.2(3) . .
N19 C19 Fe1 176.1(3) . .
N17 C17 Fe1 172.7(3) . .
N14 C13 C12 108.4(2) . .
N4 C5 C6 107.5(2) . .
N20 C20 Fe1 178.9(3) . .
C1 C2 C3 113.8(3) . .
N16 C16 Fe1 179.3(3) . .
N11 C12 C13 107.7(2) . .
N11 C10 C9 112.2(3) . .
C8 C9 C10 113.9(3) . .
N7 C8 C9 111.3(3) . .
N4 C3 C2 111.4(3) . .
N7 C6 C5 107.3(3) . .
N14 C1 C2 111.8(3) . .
C26 N27 C21 111.9(3) 3_755 .
C26 N27 Cu2 105.8(2) 3_755 .
C21 N27 Cu2 117.3(2) . .
C25 N24 C23 111.9(3) . .
C25 N24 Cu2 106.2(2) . .
C23 N24 Cu2 116.1(2) . .
N24 C25 C26 108.0(3) . .
C21 C22 C23 114.6(3) . .
N24 C23 C22 111.5(3) . .
N27 C21 C22 112.6(3) . .
N27 C26 C25 108.0(3) 3_755 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N7 2.019(3) .
Cu1 N4 2.020(3) .
Cu1 N14 2.020(3) .
Cu1 N11 2.026(3) .
Fe1 C16 1.935(3) .
Fe1 C17 1.935(3) .
Fe1 C15 1.937(3) .
Fe1 C18 1.940(3) .
Fe1 C20 1.949(3) .
Fe1 C19 1.951(3) .
Cu2 N24 2.031(3) 3_755
Cu2 N24 2.031(3) .
Cu2 N27 2.037(3) 3_755
Cu2 N27 2.037(3) .
Cu2 N17 2.451(3) .
Cu2 N17 2.451(3) 3_755
N15 C15 1.158(4) .
N4 C5 1.478(4) .
N4 C3 1.478(4) .
N19 C19 1.161(4) .
N14 C13 1.483(4) .
N14 C1 1.485(4) .
N11 C10 1.487(4) .
N11 C12 1.490(4) .
N7 C8 1.480(4) .
N7 C6 1.481(4) .
N17 C17 1.156(4) .
C18 N18 1.157(4) .
C13 C12 1.511(4) .
C5 C6 1.509(5) .
C20 N20 1.160(4) .
N16 C16 1.154(4) .
C2 C1 1.511(5) .
C2 C3 1.521(5) .
C10 C9 1.519(5) .
C9 C8 1.515(5) .
N27 C26 1.481(5) 3_755
N27 C21 1.483(5) .
N24 C25 1.484(5) .
N24 C23 1.487(4) .
C25 C26 1.514(5) .
C22 C21 1.512(6) .
C22 C23 1.523(6) .
C26 N27 1.481(5) 3_755
O3 O3 1.32(2) 3_676
