#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:12:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179317 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/14/4321412.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_4321412
loop_
_publ_author_name
'Concepción López'
'Ramon Costa'
'Francesc Illas'
'Elies Molins'
'Enric Espinosa'
_publ_section_title
;
 Ferromagnetic Copper(II) Complex Containing Ferrocenecarboxylato Bridging
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4560
_journal_page_last               4565
_journal_paper_doi               10.1021/ic000521n
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C34 H52 Cu2 Fe2 N6 O4, 2(Cl O4)'
_chemical_formula_sum            'C34 H52 Cl2 Cu2 Fe2 N6 O12'
_chemical_formula_weight         1046.51
_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                 93.170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.920(2)
_cell_length_b                   12.925(2)
_cell_length_c                   15.768(3)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.
_cell_measurement_theta_min      13.
_cell_volume                     2018.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_sigmaI/netI    0.1037
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6280
_diffrn_reflns_theta_full        30.38
_diffrn_reflns_theta_max         30.38
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    1.945
_exptl_absorpt_correction_T_max  0.9986
_exptl_absorpt_correction_T_min  0.8049
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'PSI scan empirical absorption correction'
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.146
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         6087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.1608
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0958P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1609
_reflns_number_gt                3324
_reflns_number_total             6087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000521n.cif
_cod_data_source_block           IC-00-0521-N_(dpt5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4321412
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.09483(5) 0.12828(4) 0.06651(3) 0.02868(14) Uani 1 1 d . . .
N1 N 0.1890(4) 0.0038(3) 0.1178(2) 0.0388(8) Uani 1 1 d . . .
H1A H 0.1987 0.0149 0.1742 0.058(3) Uiso 1 1 calc R . .
H1B H 0.1322 -0.0501 0.1102 0.058(3) Uiso 1 1 calc R . .
N2 N 0.2729(3) 0.2080(3) 0.0615(2) 0.0310(7) Uani 1 1 d . . .
H2 H 0.2955 0.2273 0.1159 0.058(3) Uiso 1 1 calc R . .
N3 N -0.0237(4) 0.2530(3) 0.0402(3) 0.0419(9) Uani 1 1 d . . .
H3A H -0.0874 0.2314 0.0013 0.058(3) Uiso 1 1 calc R . .
H3B H -0.0668 0.2656 0.0879 0.058(3) Uiso 1 1 calc R . .
C12 C 0.3205(5) -0.0300(4) 0.0905(3) 0.0460(11) Uani 1 1 d . . .
H12A H 0.3104 -0.0550 0.0324 0.058(3) Uiso 1 1 calc R . .
H12B H 0.3532 -0.0868 0.1261 0.058(3) Uiso 1 1 calc R . .
C13 C 0.4217(4) 0.0561(4) 0.0954(3) 0.0408(10) Uani 1 1 d . . .
H13A H 0.5094 0.0286 0.0829 0.058(3) Uiso 1 1 calc R . .
H13B H 0.4284 0.0828 0.1530 0.058(3) Uiso 1 1 calc R . .
C14 C 0.3866(4) 0.1441(3) 0.0348(3) 0.0350(9) Uani 1 1 d . . .
H14A H 0.4654 0.1879 0.0304 0.058(3) Uiso 1 1 calc R . .
H14B H 0.3636 0.1158 -0.0211 0.058(3) Uiso 1 1 calc R . .
C15 C 0.2665(5) 0.3045(3) 0.0121(3) 0.0435(11) Uani 1 1 d . . .
H15A H 0.2462 0.2880 -0.0473 0.058(3) Uiso 1 1 calc R . .
H15B H 0.3543 0.3377 0.0165 0.058(3) Uiso 1 1 calc R . .
C16 C 0.1620(5) 0.3794(4) 0.0411(4) 0.0547(13) Uani 1 1 d . . .
H16A H 0.1669 0.3811 0.1027 0.058(3) Uiso 1 1 calc R . .
H16B H 0.1838 0.4481 0.0212 0.058(3) Uiso 1 1 calc R . .
C17 C 0.0201(5) 0.3538(4) 0.0105(4) 0.0603(15) Uani 1 1 d . . .
H17A H -0.0402 0.4066 0.0302 0.058(3) Uiso 1 1 calc R . .
H17B H 0.0138 0.3546 -0.0511 0.058(3) Uiso 1 1 calc R . .
Fe1 Fe 0.19883(6) 0.08446(5) -0.29861(3) 0.02989(16) Uani 1 1 d . . .
O1 O 0.0768(3) -0.0783(2) -0.1115(2) 0.0413(7) Uani 1 1 d . . .
O2 O 0.0942(3) 0.0885(2) -0.07374(18) 0.0362(6) Uani 1 1 d . . .
C1 C 0.1261(4) 0.0121(3) -0.1173(2) 0.0288(8) Uani 1 1 d . . .
C2 C 0.2308(4) 0.0243(3) -0.1802(2) 0.0290(8) Uani 1 1 d . . .
C3 C 0.2666(5) -0.0496(4) -0.2421(3) 0.0405(10) Uani 1 1 d . . .
C4 C 0.3693(5) -0.0063(5) -0.2896(3) 0.0513(14) Uani 1 1 d . . .
C5 C 0.3987(5) 0.0931(5) -0.2583(3) 0.0485(13) Uani 1 1 d . . .
C6 C 0.3138(4) 0.1133(4) -0.1914(3) 0.0374(10) Uani 1 1 d . . .
C7 C 0.1446(5) 0.1186(4) -0.4232(3) 0.0484(12) Uani 1 1 d . . .
H7 H 0.1956 0.1060 -0.4698 0.058(3) Uiso 1 1 calc R . .
C8 C 0.0495(5) 0.0497(4) -0.3889(3) 0.0556(14) Uani 1 1 d . . .
H8 H 0.0273 -0.0161 -0.4089 0.058(3) Uiso 1 1 calc R . .
C9 C -0.0049(5) 0.1001(5) -0.3187(3) 0.0536(14) Uani 1 1 d . . .
H9 H -0.0699 0.0734 -0.2844 0.058(3) Uiso 1 1 calc R . .
C10 C 0.0571(5) 0.1978(4) -0.3102(3) 0.0513(12) Uani 1 1 d . . .
H10 H 0.0404 0.2470 -0.2690 0.058(3) Uiso 1 1 calc R . .
C11 C 0.1474(5) 0.2081(4) -0.3740(3) 0.0485(12) Uani 1 1 d . . .
H11 H 0.2013 0.2657 -0.3824 0.058(3) Uiso 1 1 calc R . .
H3 H 0.223(6) -0.110(5) -0.250(4) 0.058(3) Uiso 1 1 d . . .
H4 H 0.420(6) -0.034(4) -0.327(3) 0.058(3) Uiso 1 1 d . . .
H5 H 0.465(6) 0.136(4) -0.282(3) 0.058(3) Uiso 1 1 d . . .
H6 H 0.309(5) 0.176(4) -0.159(3) 0.058(3) Uiso 1 1 d . . .
Cl1 Cl 0.21836(15) 0.19148(10) -0.68199(8) 0.0540(3) Uani 1 1 d . . .
O3 O 0.3173(8) 0.2491(5) -0.6361(5) 0.161(3) Uani 1 1 d . . .
O4 O 0.1905(7) 0.2412(5) -0.7575(3) 0.121(2) Uani 1 1 d . . .
O5 O 0.2635(7) 0.0892(4) -0.6957(4) 0.112(2) Uani 1 1 d . . .
O6 O 0.1070(9) 0.1956(5) -0.6338(4) 0.152(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
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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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'
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 N1 89.11(13) 3 . ?
O1 Cu1 N3 80.37(14) 3 . ?
N1 Cu1 N3 166.51(16) . . ?
O1 Cu1 N2 159.02(14) 3 . ?
N1 Cu1 N2 92.04(14) . . ?
N3 Cu1 N2 94.80(14) . . ?
O1 Cu1 O2 108.52(12) 3 . ?
N1 Cu1 O2 100.78(14) . . ?
N3 Cu1 O2 90.62(14) . . ?
N2 Cu1 O2 91.84(12) . . ?
C12 N1 Cu1 121.5(3) . . ?
C15 N2 C14 109.5(3) . . ?
C15 N2 Cu1 115.8(3) . . ?
C14 N2 Cu1 113.7(2) . . ?
C17 N3 Cu1 126.6(3) . . ?
N1 C12 C13 111.6(4) . . ?
C12 C13 C14 113.3(4) . . ?
N2 C14 C13 113.1(3) . . ?
N2 C15 C16 113.2(4) . . ?
C17 C16 C15 114.2(5) . . ?
N3 C17 C16 112.7(4) . . ?
C6 Fe1 C2 41.40(16) . . ?
C6 Fe1 C10 107.3(2) . . ?
C2 Fe1 C10 115.53(19) . . ?
C6 Fe1 C9 128.4(2) . . ?
C2 Fe1 C9 106.49(18) . . ?
C10 Fe1 C9 40.5(2) . . ?
C6 Fe1 C11 117.0(2) . . ?
C2 Fe1 C11 149.0(2) . . ?
C10 Fe1 C11 39.9(2) . . ?
C9 Fe1 C11 67.5(2) . . ?
C6 Fe1 C3 68.6(2) . . ?
C2 Fe1 C3 40.90(17) . . ?
C10 Fe1 C3 149.2(2) . . ?
C9 Fe1 C3 116.8(2) . . ?
C11 Fe1 C3 169.6(2) . . ?
C6 Fe1 C8 167.3(2) . . ?
C2 Fe1 C8 128.7(2) . . ?
C10 Fe1 C8 68.0(2) . . ?
C9 Fe1 C8 40.6(2) . . ?
C11 Fe1 C8 67.6(2) . . ?
C3 Fe1 C8 109.0(2) . . ?
C6 Fe1 C5 40.49(18) . . ?
C2 Fe1 C5 68.71(17) . . ?
C10 Fe1 C5 129.8(2) . . ?
C9 Fe1 C5 167.4(2) . . ?
C11 Fe1 C5 110.1(2) . . ?
C3 Fe1 C5 67.8(2) . . ?
C8 Fe1 C5 151.3(2) . . ?
C6 Fe1 C7 149.9(2) . . ?
C2 Fe1 C7 168.4(2) . . ?
C10 Fe1 C7 67.4(2) . . ?
C9 Fe1 C7 68.0(2) . . ?
C11 Fe1 C7 39.8(2) . . ?
C3 Fe1 C7 131.3(2) . . ?
C8 Fe1 C7 40.6(2) . . ?
C5 Fe1 C7 118.8(2) . . ?
C6 Fe1 C4 67.9(2) . . ?
C2 Fe1 C4 68.42(17) . . ?
C10 Fe1 C4 168.5(2) . . ?
C9 Fe1 C4 150.6(3) . . ?
C11 Fe1 C4 131.7(2) . . ?
C3 Fe1 C4 40.3(2) . . ?
C8 Fe1 C4 118.9(2) . . ?
C5 Fe1 C4 39.9(2) . . ?
C7 Fe1 C4 111.0(2) . . ?
C1 O1 Cu1 131.6(3) . 3 ?
C1 O2 Cu1 136.5(3) . . ?
O2 C1 O1 125.1(4) . . ?
O2 C1 C2 119.3(4) . . ?
O1 C1 C2 115.6(4) . . ?
C3 C2 C6 106.7(4) . . ?
C3 C2 C1 126.7(4) . . ?
C6 C2 C1 126.6(4) . . ?
C3 C2 Fe1 70.1(2) . . ?
C6 C2 Fe1 68.9(2) . . ?
C1 C2 Fe1 125.2(3) . . ?
C4 C3 C2 108.2(5) . . ?
C4 C3 Fe1 70.3(3) . . ?
C2 C3 Fe1 69.0(2) . . ?
C5 C4 C3 108.5(4) . . ?
C5 C4 Fe1 69.9(3) . . ?
C3 C4 Fe1 69.4(3) . . ?
C4 C5 C6 108.2(4) . . ?
C4 C5 Fe1 70.3(3) . . ?
C6 C5 Fe1 68.6(2) . . ?
C5 C6 C2 108.3(4) . . ?
C5 C6 Fe1 70.9(3) . . ?
C2 C6 Fe1 69.7(2) . . ?
C11 C7 C8 107.5(4) . . ?
C11 C7 Fe1 69.5(3) . . ?
C8 C7 Fe1 69.4(3) . . ?
C9 C8 C7 107.4(5) . . ?
C9 C8 Fe1 69.4(3) . . ?
C7 C8 Fe1 70.0(3) . . ?
C10 C9 C8 107.6(5) . . ?
C10 C9 Fe1 69.5(3) . . ?
C8 C9 Fe1 70.0(3) . . ?
C11 C10 C9 108.2(5) . . ?
C11 C10 Fe1 70.3(3) . . ?
C9 C10 Fe1 70.0(3) . . ?
C10 C11 C7 109.2(5) . . ?
C10 C11 Fe1 69.8(3) . . ?
C7 C11 Fe1 70.7(3) . . ?
O4 Cl1 O6 109.5(5) . . ?
O4 Cl1 O3 107.5(5) . . ?
O6 Cl1 O3 104.8(5) . . ?
O4 Cl1 O5 110.9(4) . . ?
O6 Cl1 O5 113.0(4) . . ?
O3 Cl1 O5 110.9(4) . . ?
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 1.988(3) 3 ?
Cu1 N1 2.008(4) . ?
Cu1 N3 2.025(3) . ?
Cu1 N2 2.051(3) . ?
Cu1 O2 2.270(3) . ?
N1 C12 1.463(6) . ?
N2 C15 1.470(5) . ?
N2 C14 1.478(5) . ?
N3 C17 1.458(6) . ?
C12 C13 1.498(7) . ?
C13 C14 1.514(6) . ?
C15 C16 1.508(7) . ?
C16 C17 1.499(7) . ?
Fe1 C6 2.021(4) . ?
Fe1 C2 2.031(4) . ?
Fe1 C10 2.032(5) . ?
Fe1 C9 2.039(5) . ?
Fe1 C11 2.039(5) . ?
Fe1 C3 2.045(4) . ?
Fe1 C8 2.047(5) . ?
Fe1 C5 2.052(5) . ?
Fe1 C7 2.055(4) . ?
Fe1 C4 2.057(5) . ?
O1 C1 1.272(5) . ?
O1 Cu1 1.988(3) 3 ?
O2 C1 1.253(5) . ?
C1 C2 1.484(5) . ?
C2 C3 1.424(6) . ?
C2 C6 1.432(6) . ?
C3 C4 1.413(7) . ?
C4 C5 1.402(8) . ?
C5 C6 1.410(6) . ?
C7 C11 1.393(7) . ?
C7 C8 1.425(8) . ?
C8 C9 1.416(8) . ?
C9 C10 1.409(8) . ?
C10 C11 1.390(7) . ?
Cl1 O4 1.368(5) . ?
Cl1 O6 1.376(6) . ?
Cl1 O3 1.401(6) . ?
Cl1 O5 1.416(5) . ?
