#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:28:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179112 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/74/4307447.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_4307447
loop_
_publ_author_name
'Long Jiang'
'Hye Jin Choi'
'Xiao-Long Feng'
'Tong-Bu Lu'
'Jeffrey R. Long'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of the Face-Centered Cubic
Clusters [Tp8(H2O)12M6Fe8(CN)24]4+ (M = Co, Ni)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2181
_journal_page_last               2186
_journal_paper_doi               10.1021/ic061924b
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C144 H214 B8 Cl4 Fe8 N72 Ni6 O47'
_chemical_formula_weight         4733.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           221
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 4 2 3'
_symmetry_space_group_name_H-M   'P m -3 m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   17.5480(12)
_cell_length_b                   17.5480(12)
_cell_length_c                   17.5480(12)
_cell_measurement_reflns_used    5277
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.89
_cell_measurement_theta_min      2.32
_cell_volume                     5403.6(6)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17379
_diffrn_reflns_theta_full        22.99
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.7145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2442
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         737
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      2.891
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0970
_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)+(0.1072P)²+52.1238P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2352
_refine_ls_wR_factor_ref         0.2498
_reflns_number_gt                644
_reflns_number_total             737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061924bsi20061009_012058.cif
_cod_data_source_block           051127cm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' 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_database_code               4307447
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
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
Fe1 Fe 0.1986(2) 0.1986(2) 0.1986(2) 0.055(3) Uani 1 6 d S . .
Ni1 Ni 0.0000 0.2532(4) 0.0000 0.039(2) Uani 1 8 d SD . .
N1 N 0.3143(12) 0.3143(12) 0.216(2) 0.099(10) Uani 1 2 d SDU . .
N2 N 0.2730(13) 0.2730(13) 0.167(2) 0.101(10) Uani 1 2 d SDU . .
C1 C 0.324(3) 0.273(3) 0.097(3) 0.098(12) Uani 0.50 1 d PDU . .
H1A H 0.3122 0.2416 0.0539 0.07(14) Uiso 0.50 1 d PR . .
C3 C 0.386(3) 0.340(3) 0.181(3) 0.100(12) Uani 0.50 1 d PDU . .
H3A H 0.4237 0.3712 0.2052 0.2(4) Uiso 0.50 1 d PR . .
C2 C 0.386(4) 0.310(3) 0.106(4) 0.100(12) Uani 0.50 1 d PDU . .
H2A H 0.4244 0.3208 0.0685 0.2(3) Uiso 0.50 1 d PR . .
C4 C 0.1251(16) 0.231(2) 0.1251(16) 0.082(12) Uani 1 2 d S . .
B1 B 0.299(2) 0.299(2) 0.299(2) 0.09(3) Uani 1 6 d S . .
H1 H 0.3314 0.3314 0.3314 0.106 Uiso 1 6 calc SR . .
N3 N 0.0818(14) 0.250(2) 0.0818(14) 0.111(14) Uani 1 2 d S . .
O1 O 0.0000 0.3809(12) 0.0000 0.19(3) Uani 1 8 d SDU . .
H1B H 0.0000 0.3893 0.0483 0.224 Uiso 0.50 2 d SPRD . .
O2 O 0.0000 0.126(2) 0.0000 0.044(9) Uani 1 8 d SDU . .
H2B H 0.0000 0.1062 0.0448 0.053 Uiso 0.50 2 d SPRD . .
Cl1 Cl 0.5000 0.5000 0.028(3) 0.19(2) Uani 0.44 8 d SPDU . .
O4 O 0.423(2) 0.5000 0.0000 0.19(2) Uani 0.70 4 d SPDU . .
O5 O 0.5000 0.5000 0.110(3) 0.19(2) Uani 0.35 8 d SPDU . .
Cl2 Cl 0.5000 0.5000 0.321(11) 0.20(7) Uani 0.23 8 d SPDU . .
O6 O 0.5000 0.5000 0.239(11) 0.19(8) Uani 0.18 8 d SPDU . .
O8 O 0.5000 0.5000 0.5000 0.3(3) Uani 1 48 d SD . .
H8A H 0.4717 0.5283 0.4717 0.400 Uiso 0.25 6 d SPRD . .
O7 O 0.5000 0.423(3) 0.348(12) 0.20(7) Uani 0.18 2 d SPDU . .
O3 O 0.5000 0.2298 0.1439 0.192 Uani 0.50 2 d SPDU . .
C5 C 0.4377 0.1954 0.1053 0.190 Uani 0.50 1 d PDU . .
H5A H 0.4025 0.1751 0.1427 0.228 Uiso 0.50 1 d P . .
H5B H 0.4110 0.2342 0.0764 0.228 Uiso 0.50 1 d P . .
C6 C 0.4593 0.1367 0.0557 0.189 Uani 0.50 1 d PDU . .
H6A H 0.4387 0.1479 0.0063 0.227 Uiso 0.50 1 d PD . .
H6B H 0.4387 0.0893 0.0732 0.227 Uiso 0.50 1 d PD . .
O9 O 0.5000 0.2905 0.2905 0.250 Uani 0.50 4 d SPU . .
H9A H 0.5000 0.2465 0.2727 0.300 Uiso 0.25 2 d SPR . .
H9B H 0.5000 0.3054 0.3316 0.300 Uiso 0.25 2 d SPR . .
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'
Cl Cl 0.1484 0.1585 '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'
B B 0.0013 0.0007 '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
C4 Fe1 C4 86.7(16) 5 9 ?
C4 Fe1 C4 86.7(16) 5 . ?
C4 Fe1 C4 86.7(16) 9 . ?
C4 Fe1 N2 179.4(16) 5 . ?
C4 Fe1 N2 93.7(10) 9 . ?
C4 Fe1 N2 93.7(10) . . ?
C4 Fe1 N2 93.7(10) 5 9 ?
C4 Fe1 N2 93.7(10) 9 9 ?
C4 Fe1 N2 179.4(16) . 9 ?
N2 Fe1 N2 85.9(15) . 9 ?
C4 Fe1 N2 93.7(10) 5 5 ?
C4 Fe1 N2 179.4(16) 9 5 ?
C4 Fe1 N2 93.7(10) . 5 ?
N2 Fe1 N2 85.9(15) . 5 ?
N2 Fe1 N2 85.9(15) 9 5 ?
N3 Ni1 N3 89.95(7) . 26 ?
N3 Ni1 N3 177(2) . 3 ?
N3 Ni1 N3 89.95(7) 26 3 ?
N3 Ni1 N3 89.95(7) . 28 ?
N3 Ni1 N3 177(2) 26 28 ?
N3 Ni1 N3 89.95(7) 3 28 ?
N3 Ni1 O2 88.3(11) . . ?
N3 Ni1 O2 88.3(11) 26 . ?
N3 Ni1 O2 88.3(11) 3 . ?
N3 Ni1 O2 88.3(11) 28 . ?
N3 Ni1 O1 91.7(11) . . ?
N3 Ni1 O1 91.7(11) 26 . ?
N3 Ni1 O1 91.7(11) 3 . ?
N3 Ni1 O1 91.7(11) 28 . ?
O2 Ni1 O1 180.000(1) . . ?
N2 N1 C3 111(3) . . ?
N2 N1 C3 111(3) . 38 ?
C3 N1 C3 46(3) . 38 ?
N2 N1 B1 115(4) . . ?
C3 N1 B1 127(3) . . ?
C3 N1 B1 127(3) 38 . ?
N1 N2 C1 102(3) . . ?
N1 N2 C1 102(3) . 38 ?
C1 N2 C1 49(3) . 38 ?
N1 N2 Fe1 124(3) . . ?
C1 N2 Fe1 129(3) . . ?
C1 N2 Fe1 129(3) 38 . ?
C1 C1 C2 104.0(18) 38 . ?
C1 C1 N2 65.5(15) 38 . ?
C2 C1 N2 114(6) . . ?
C1 C1 C2 38(2) 38 38 ?
C2 C1 C2 66(3) . 38 ?
N2 C1 C2 83(3) . 38 ?
C3 C3 C2 104.9(18) 38 . ?
C3 C3 N1 67.0(14) 38 . ?
C2 C3 N1 106(5) . . ?
C1 C2 C3 107(6) . . ?
C1 C2 C2 76.0(18) . 38 ?
C3 C2 C2 75.1(18) . 38 ?
C1 C2 C1 38(3) . 38 ?
C3 C2 C1 92(4) . 38 ?
C2 C2 C1 38(2) 38 38 ?
N3 C4 Fe1 180(4) . . ?
N1 B1 N1 108(3) 9 . ?
N1 B1 N1 108(3) 9 5 ?
N1 B1 N1 108(3) . 5 ?
C4 N3 Ni1 164(4) . . ?
Cl1 Cl1 O5 180.000(4) 25_665 . ?
Cl1 Cl1 O4 70(3) 25_665 13 ?
O5 Cl1 O4 110(3) . 13 ?
Cl1 Cl1 O4 70(3) 25_665 . ?
O5 Cl1 O4 110(3) . . ?
O4 Cl1 O4 83.4(17) 13 . ?
Cl1 Cl1 O4 70(3) 25_665 37_665 ?
O5 Cl1 O4 110(3) . 37_665 ?
O4 Cl1 O4 140(5) 13 37_665 ?
O4 Cl1 O4 83.4(17) . 37_665 ?
Cl1 Cl1 O4 70(3) 25_665 25_665 ?
O5 Cl1 O4 110(3) . 25_665 ?
O4 Cl1 O4 83.4(17) 13 25_665 ?
O4 Cl1 O4 140(5) . 25_665 ?
O4 Cl1 O4 83.4(17) 37_665 25_665 ?
Cl1 O4 Cl1 40(5) . 25_665 ?
O7 Cl2 O7 83.6(19) . 37_665 ?
O7 Cl2 O7 141(6) . 2_665 ?
O7 Cl2 O7 83.6(19) 37_665 2_665 ?
O7 Cl2 O7 83.6(19) . 38 ?
O7 Cl2 O7 141(6) 37_665 38 ?
O7 Cl2 O7 83.6(19) 2_665 38 ?
O7 Cl2 O6 110(3) . . ?
O7 Cl2 O6 110(3) 37_665 . ?
O7 Cl2 O6 110(3) 2_665 . ?
O7 Cl2 O6 110(3) 38 . ?
C5 O3 C5 100.6 . 28_655 ?
C6 C5 O3 113.6 . . ?
C5 C6 C6 105.7 . 28_655 ?
C5 C6 C6 128.4 . 26 ?
C6 C6 C6 90.0 28_655 26 ?
C5 C6 C6 94.6 . 43 ?
C6 C6 C6 90.0 28_655 43 ?
C6 C6 C6 135.0 26 43 ?
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
Fe1 C4 1.91(4) 5 ?
Fe1 C4 1.91(4) 9 ?
Fe1 C4 1.91(4) . ?
Fe1 N2 1.93(3) . ?
Fe1 N2 1.93(3) 9 ?
Fe1 N2 1.93(3) 5 ?
Ni1 N3 2.03(4) . ?
Ni1 N3 2.03(4) 26 ?
Ni1 N3 2.03(4) 3 ?
Ni1 N3 2.03(4) 28 ?
Ni1 O2 2.23(4) . ?
Ni1 O1 2.24(2) . ?
N1 N2 1.33(4) . ?
N1 C3 1.46(6) . ?
N1 C3 1.46(6) 38 ?
N1 B1 1.51(4) . ?
N2 C1 1.52(6) . ?
N2 C1 1.52(6) 38 ?
C1 C1 1.26(9) 38 ?
C1 C2 1.28(8) . ?
C1 C2 2.00(9) 38 ?
C3 C3 1.14(8) 38 ?
C3 C2 1.42(9) . ?
C2 C2 1.88(11) 38 ?
C2 C1 2.00(9) 38 ?
C4 N3 1.13(5) . ?
B1 N1 1.51(4) 9 ?
B1 N1 1.51(4) 5 ?
Cl1 Cl1 0.98(11) 25_665 ?
Cl1 O5 1.44(3) . ?
Cl1 O4 1.44(3) 13 ?
Cl1 O4 1.44(3) . ?
Cl1 O4 1.44(3) 37_665 ?
Cl1 O4 1.44(3) 25_665 ?
O4 Cl1 1.44(3) 25_665 ?
Cl2 O7 1.44(3) . ?
Cl2 O7 1.44(3) 37_665 ?
Cl2 O7 1.44(3) 2_665 ?
Cl2 O7 1.44(3) 38 ?
Cl2 O6 1.44(3) . ?
O3 C5 1.4207 . ?
O3 C5 1.4207 28_655 ?
C5 C6 1.3997 . ?
C6 C6 1.4281 28_655 ?
C6 C6 1.9561 26 ?
C6 C6 2.0098 43 ?
