#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:07:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179232 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/52/4315223.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_4315223
loop_
_publ_author_name
'Sumit Saha'
'Lei Zhu'
'Burjor Captain'
_publ_section_title
;
 Synthesis and Structural Characterization of Bimetallic Iron-Nickel
 Carbido Cluster Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3465
_journal_page_last               3472
_journal_paper_doi               10.1021/ic100057x
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C17 H6 Fe4 N2 Ni O12'
_chemical_formula_weight         712.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.2706(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6040(3)
_cell_length_b                   15.3859(6)
_cell_length_c                   16.0687(6)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.63
_cell_measurement_theta_min      2.21
_cell_volume                     2279.31(14)
_computing_cell_refinement       'SAINT+  V7.46A (Bruker, 2007)'
_computing_data_collection       'APEX2 v2.2-0 (Bruker, 2007)'
_computing_data_reduction        'SAINT+  V7.46A (Bruker, 2007)'
_computing_molecular_graphics    'XSHELL v4.02 (Bruker, 2000)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'omega 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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37035
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    3.362
_exptl_absorpt_correction_T_max  0.8773
_exptl_absorpt_correction_T_min  0.3774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2007/4 Bruker)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         7260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0207P)²+1.1435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0492
_reflns_number_gt                6821
_reflns_number_total             7260
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100057x_si_001_4.cif
_cod_data_source_block           collect_0m_Compound7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315223
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'
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
Ni1 Ni 0.776671(17) 0.132444(10) 0.958728(10) 0.01116(4) Uani 1 1 d . . .
Fe3 Fe 0.687598(18) 0.361771(11) 0.978310(11) 0.00994(4) Uani 1 1 d . . .
Fe4 Fe 0.539668(18) 0.215978(11) 0.952479(11) 0.01001(4) Uani 1 1 d . . .
Fe2 Fe 0.925454(18) 0.280841(11) 0.972444(11) 0.00921(4) Uani 1 1 d . . .
Fe1 Fe 0.689749(18) 0.256007(11) 0.849727(11) 0.00930(4) Uani 1 1 d . . .
N1 N 0.82214(12) 0.06823(7) 1.06790(7) 0.01431(19) Uani 1 1 d . . .
N2 N 0.80277(12) 0.03631(7) 0.88787(7) 0.01421(19) Uani 1 1 d . . .
O42 O 0.49356(11) 0.03010(6) 0.91383(7) 0.01906(19) Uani 1 1 d . . .
O23 O 1.08815(12) 0.31893(7) 1.15230(6) 0.0223(2) Uani 1 1 d . . .
O41 O 0.24748(11) 0.24864(7) 0.83673(7) 0.0203(2) Uani 1 1 d . . .
O11 O 0.49870(13) 0.13151(7) 0.73086(7) 0.0251(2) Uani 1 1 d . . .
O21 O 1.06754(11) 0.41414(7) 0.89215(7) 0.0208(2) Uani 1 1 d . . .
O22 O 1.11931(11) 0.13603(6) 0.96337(8) 0.0228(2) Uani 1 1 d . . .
O31 O 0.79903(13) 0.52109(7) 0.91816(7) 0.0250(2) Uani 1 1 d . . .
C1 C 0.74026(12) 0.24623(7) 0.97739(7) 0.00954(19) Uani 1 1 d . . .
O33 O 0.77493(13) 0.41088(7) 1.16201(7) 0.0249(2) Uani 1 1 d . . .
O43 O 0.44194(14) 0.20746(8) 1.10961(7) 0.0299(2) Uani 1 1 d . . .
C2 C 0.83145(14) 0.02880(8) 1.12936(8) 0.0149(2) Uani 1 1 d . . .
O32 O 0.38798(12) 0.42416(7) 0.94469(9) 0.0297(3) Uani 1 1 d . . .
O13 O 0.54295(13) 0.41176(7) 0.76150(7) 0.0263(2) Uani 1 1 d . . .
C21 C 1.01548(13) 0.36224(8) 0.92480(8) 0.0139(2) Uani 1 1 d . . .
O12 O 0.90243(13) 0.26622(9) 0.74984(7) 0.0305(3) Uani 1 1 d . . .
C41 C 0.36135(14) 0.23696(8) 0.88223(8) 0.0131(2) Uani 1 1 d . . .
C42 C 0.53155(13) 0.10042(8) 0.93176(8) 0.0138(2) Uani 1 1 d . . .
C23 C 1.02347(14) 0.30417(8) 1.08242(8) 0.0142(2) Uani 1 1 d . . .
C13 C 0.60041(15) 0.35249(8) 0.79963(8) 0.0164(2) Uani 1 1 d . . .
C33 C 0.73948(15) 0.39190(8) 1.09049(9) 0.0158(2) Uani 1 1 d . . .
C4 C 0.80566(14) -0.02399(8) 0.84728(8) 0.0145(2) Uani 1 1 d . . .
C31 C 0.75812(15) 0.45945(8) 0.94279(8) 0.0160(2) Uani 1 1 d . . .
C43 C 0.48292(15) 0.21044(9) 1.04955(9) 0.0170(2) Uani 1 1 d . . .
C22 C 1.03409(14) 0.18834(8) 0.96463(8) 0.0152(2) Uani 1 1 d . . .
C11 C 0.57105(14) 0.17964(8) 0.77774(8) 0.0157(2) Uani 1 1 d . . .
C12 C 0.82741(15) 0.26130(9) 0.79391(9) 0.0178(2) Uani 1 1 d . . .
C5 C 0.80831(16) -0.10129(9) 0.79516(9) 0.0198(3) Uani 1 1 d . . .
H5A H 0.7427 -0.1439 0.8062 0.030 Uiso 1 1 calc R . .
H5B H 0.9048 -0.1248 0.8102 0.030 Uiso 1 1 calc R . .
H5C H 0.7792 -0.0860 0.7348 0.030 Uiso 1 1 calc R . .
C3 C 0.84541(17) -0.02211(10) 1.20805(9) 0.0218(3) Uani 1 1 d . . .
H3A H 0.8717 -0.0808 1.1987 0.033 Uiso 1 1 calc R . .
H3B H 0.7546 -0.0220 1.2221 0.033 Uiso 1 1 calc R . .
H3C H 0.9191 0.0030 1.2550 0.033 Uiso 1 1 calc R . .
C32 C 0.50185(15) 0.39422(9) 0.95720(9) 0.0184(2) 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'
Fe Fe 0.3463 0.8444 '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
C1 Ni1 N2 153.65(5) . . ?
C1 Ni1 N1 110.02(5) . . ?
N2 Ni1 N1 96.27(5) . . ?
C1 Ni1 Fe1 50.21(4) . . ?
N2 Ni1 Fe1 103.73(3) . . ?
N1 Ni1 Fe1 159.67(3) . . ?
C1 Ni1 Fe4 47.50(4) . . ?
N2 Ni1 Fe4 128.07(3) . . ?
N1 Ni1 Fe4 104.99(3) . . ?
Fe1 Ni1 Fe4 59.394(6) . . ?
C1 Ni1 Fe2 44.71(4) . . ?
N2 Ni1 Fe2 123.40(3) . . ?
N1 Ni1 Fe2 112.25(3) . . ?
Fe1 Ni1 Fe2 59.068(6) . . ?
Fe4 Ni1 Fe2 91.320(7) . . ?
C32 Fe3 C33 95.74(6) . . ?
C32 Fe3 C31 98.63(6) . . ?
C33 Fe3 C31 94.56(6) . . ?
C32 Fe3 C1 121.77(6) . . ?
C33 Fe3 C1 104.90(5) . . ?
C31 Fe3 C1 132.06(6) . . ?
C32 Fe3 Fe4 75.05(4) . . ?
C33 Fe3 Fe4 111.46(4) . . ?
C31 Fe3 Fe4 153.58(4) . . ?
C1 Fe3 Fe4 46.73(4) . . ?
C32 Fe3 Fe2 162.85(4) . . ?
C33 Fe3 Fe2 99.16(4) . . ?
C31 Fe3 Fe2 88.64(4) . . ?
C1 Fe3 Fe2 45.69(4) . . ?
Fe4 Fe3 Fe2 91.538(8) . . ?
C32 Fe3 Fe1 104.47(4) . . ?
C33 Fe3 Fe1 152.60(4) . . ?
C31 Fe3 Fe1 100.38(4) . . ?
C1 Fe3 Fe1 48.53(4) . . ?
Fe4 Fe3 Fe1 58.067(6) . . ?
Fe2 Fe3 Fe1 58.737(6) . . ?
C43 Fe4 C41 94.97(6) . . ?
C43 Fe4 C42 96.06(6) . . ?
C41 Fe4 C42 94.40(6) . . ?
C43 Fe4 C1 111.32(6) . . ?
C41 Fe4 C1 144.58(5) . . ?
C42 Fe4 C1 105.49(5) . . ?
C43 Fe4 Fe1 159.83(4) . . ?
C41 Fe4 Fe1 99.31(4) . . ?
C42 Fe4 Fe1 96.97(4) . . ?
C1 Fe4 Fe1 50.08(3) . . ?
C43 Fe4 Ni1 114.87(4) . . ?
C41 Fe4 Ni1 141.79(4) . . ?
C42 Fe4 Ni1 60.73(4) . . ?
C1 Fe4 Ni1 44.77(3) . . ?
Fe1 Fe4 Ni1 59.716(6) . . ?
C43 Fe4 Fe3 100.72(4) . . ?
C41 Fe4 Fe3 108.92(4) . . ?
C42 Fe4 Fe3 149.72(4) . . ?
C1 Fe4 Fe3 44.77(3) . . ?
Fe1 Fe4 Fe3 61.151(7) . . ?
Ni1 Fe4 Fe3 89.260(8) . . ?
C22 Fe2 C23 94.19(6) . . ?
C22 Fe2 C21 99.42(6) . . ?
C23 Fe2 C21 95.59(6) . . ?
C22 Fe2 C1 110.78(5) . . ?
C23 Fe2 C1 104.90(5) . . ?
C21 Fe2 C1 141.64(5) . . ?
C22 Fe2 Fe1 103.44(4) . . ?
C23 Fe2 Fe1 152.88(4) . . ?
C21 Fe2 Fe1 101.54(4) . . ?
C1 Fe2 Fe1 49.63(4) . . ?
C22 Fe2 Fe3 155.43(4) . . ?
C23 Fe2 Fe3 95.26(4) . . ?
C21 Fe2 Fe3 102.16(4) . . ?
C1 Fe2 Fe3 44.76(3) . . ?
Fe1 Fe2 Fe3 60.789(7) . . ?
C22 Fe2 Ni1 67.86(4) . . ?
C23 Fe2 Ni1 111.98(4) . . ?
C21 Fe2 Ni1 149.92(4) . . ?
C1 Fe2 Ni1 43.13(3) . . ?
Fe1 Fe2 Ni1 58.370(6) . . ?
Fe3 Fe2 Ni1 87.572(8) . . ?
C13 Fe1 C12 93.73(6) . . ?
C13 Fe1 C11 96.56(6) . . ?
C12 Fe1 C11 97.48(6) . . ?
C13 Fe1 C1 118.51(5) . . ?
C12 Fe1 C1 121.39(6) . . ?
C11 Fe1 C1 122.75(5) . . ?
C13 Fe1 Fe4 101.81(4) . . ?
C12 Fe1 Fe4 164.22(5) . . ?
C11 Fe1 Fe4 83.58(4) . . ?
C1 Fe1 Fe4 47.89(3) . . ?
C13 Fe1 Ni1 161.25(4) . . ?
C12 Fe1 Ni1 103.34(5) . . ?
C11 Fe1 Ni1 88.94(4) . . ?
C1 Fe1 Ni1 45.23(3) . . ?
Fe4 Fe1 Ni1 60.890(7) . . ?
C13 Fe1 Fe2 115.37(4) . . ?
C12 Fe1 Fe2 76.34(4) . . ?
C11 Fe1 Fe2 147.64(4) . . ?
C1 Fe1 Fe2 46.42(3) . . ?
Fe4 Fe1 Fe2 94.295(8) . . ?
Ni1 Fe1 Fe2 62.562(7) . . ?
C13 Fe1 Fe3 74.47(4) . . ?
C12 Fe1 Fe3 122.17(4) . . ?
C11 Fe1 Fe3 139.45(4) . . ?
C1 Fe1 Fe3 44.51(3) . . ?
Fe4 Fe1 Fe3 60.783(7) . . ?
Ni1 Fe1 Fe3 89.704(8) . . ?
Fe2 Fe1 Fe3 60.473(7) . . ?
C2 N1 Ni1 171.86(11) . . ?
C4 N2 Ni1 173.02(11) . . ?
Ni1 C1 Fe3 171.13(7) . . ?
Ni1 C1 Fe2 92.16(5) . . ?
Fe3 C1 Fe2 89.55(5) . . ?
Ni1 C1 Fe4 87.73(5) . . ?
Fe3 C1 Fe4 88.50(5) . . ?
Fe2 C1 Fe4 165.93(7) . . ?
Ni1 C1 Fe1 84.56(5) . . ?
Fe3 C1 Fe1 86.96(5) . . ?
Fe2 C1 Fe1 83.95(4) . . ?
Fe4 C1 Fe1 82.03(4) . . ?
N1 C2 C3 179.19(15) . . ?
O21 C21 Fe2 177.35(12) . . ?
O41 C41 Fe4 178.58(12) . . ?
O42 C42 Fe4 164.68(11) . . ?
O23 C23 Fe2 178.88(12) . . ?
O13 C13 Fe1 174.81(12) . . ?
O33 C33 Fe3 178.84(13) . . ?
N2 C4 C5 179.62(14) . . ?
O31 C31 Fe3 177.88(13) . . ?
O43 C43 Fe4 177.60(13) . . ?
O22 C22 Fe2 171.01(12) . . ?
O11 C11 Fe1 178.08(12) . . ?
O12 C12 Fe1 172.12(13) . . ?
O32 C32 Fe3 172.59(12) . . ?
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
Ni1 C1 1.8264(11) . ?
Ni1 N2 1.9254(11) . ?
Ni1 N1 1.9532(11) . ?
Ni1 Fe1 2.5612(2) . ?
Ni1 Fe4 2.5913(2) . ?
Ni1 Fe2 2.6696(2) . ?
Fe3 C32 1.7909(14) . ?
Fe3 C33 1.7914(13) . ?
Fe3 C31 1.8055(13) . ?
Fe3 C1 1.8495(11) . ?
Fe3 Fe4 2.6253(2) . ?
Fe3 Fe2 2.6265(2) . ?
Fe3 Fe1 2.6346(2) . ?
Fe4 C43 1.7927(14) . ?
Fe4 C41 1.7967(13) . ?
Fe4 C42 1.8065(13) . ?
Fe4 C1 1.9121(11) . ?
Fe4 Fe1 2.5527(2) . ?
Fe2 C22 1.7898(13) . ?
Fe2 C23 1.7904(13) . ?
Fe2 C21 1.8092(13) . ?
Fe2 C1 1.8795(11) . ?
Fe2 Fe1 2.5802(2) . ?
Fe1 C13 1.7891(13) . ?
Fe1 C12 1.7954(14) . ?
Fe1 C11 1.8109(13) . ?
Fe1 C1 1.9769(11) . ?
N1 C2 1.1410(17) . ?
N2 C4 1.1389(17) . ?
O42 C42 1.1523(16) . ?
O23 C23 1.1436(16) . ?
O41 C41 1.1466(16) . ?
O11 C11 1.1426(17) . ?
O21 C21 1.1446(16) . ?
O22 C22 1.1521(16) . ?
O31 C31 1.1392(17) . ?
O33 C33 1.1414(17) . ?
O43 C43 1.1407(17) . ?
C2 C3 1.4611(18) . ?
O32 C32 1.1513(17) . ?
O13 C13 1.1498(16) . ?
O12 C12 1.1455(17) . ?
C4 C5 1.4589(18) . ?
