#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:49:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179308 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/05/4320566.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_4320566
loop_
_publ_author_name
'Hui-Zhong Kou'
'Song Gao'
'Xianglin Jin'
_publ_contact_author_address
;
State Key Laboratory of Rare Earth Materials Chemistry and Applications
PKU-HKU Joint Laboratory on Rare Earth Materials and Bioinorganic Chemistry
College of Chemistry and Molecular Engineering
Peking University
Beijing 100871
People's Republic of China
;
_publ_contact_author_email       gaosong@chem.pku.edu.cn
_publ_contact_author_fax         86(10)62751708
_publ_contact_author_name        'Song Gao'
_publ_contact_author_phone       86(10)62756320
_publ_section_title
;
 Synthesis, Crystal Structure, and Magnetic Properties of Two
 Cyano-Bridged Bimetallic 4f-3d Arrays with One-Dimensional Chain and
 Two-Dimensional Brick Wall Molecular Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6295
_journal_page_last               6300
_journal_paper_doi               10.1021/ic0103042
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C12 H22 Cr N8 O6 Sm'
_chemical_formula_weight         576.73
_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                94.1590(14)
_cell_angle_beta                 100.0597(18)
_cell_angle_gamma                100.9154(18)
_cell_formula_units_Z            2
_cell_length_a                   7.75350(10)
_cell_length_b                   9.4307(3)
_cell_length_c                   16.2905(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1144.75(5)
_computing_cell_refinement       'HKL Scalepack'
_computing_data_collection       'NONIUS Kappa CCD'
_computing_data_reduction        'HKL Denzo & Maxus'
_computing_molecular_graphics    'Siemens SHELXL (1990)'
_computing_publication_material  'Siemens SHELXL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.71
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'NONIUS Kappa CCD'
_diffrn_measurement_method       CCD
_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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17175
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    3.055
_exptl_absorpt_correction_T_max  0.643
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   SORTAV
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.765
_refine_diff_density_min         -2.051
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       0.0236(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0589P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                3728
_reflns_number_total             4015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0103042_1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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               4320566
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
Sm Sm 0.46323(2) 0.206986(19) 0.244323(11) 0.02106(12) Uani 1 1 d . . .
Cr Cr 0.85207(8) 0.75180(6) 0.22969(4) 0.02063(16) Uani 1 1 d . . .
C6 C 0.6430(5) 0.5809(4) 0.2345(3) 0.0281(9) Uani 1 1 d . . .
O4 O 0.7836(5) 0.2908(5) 0.2985(3) 0.0469(9) Uani 1 1 d . . .
O5 O 0.2654(4) 0.3172(4) 0.3191(2) 0.0369(8) Uani 1 1 d . . .
C4 C 1.0766(5) 0.9124(5) 0.2293(3) 0.0291(9) Uani 1 1 d . . .
C3 C 0.6883(5) 0.9011(4) 0.2336(3) 0.0284(9) Uani 1 1 d . . .
O1 O 0.5176(5) 0.1664(4) 0.38703(19) 0.0458(8) Uani 1 1 d . . .
O3 O 0.2277(5) 0.2619(5) 0.1382(3) 0.0439(9) Uani 1 1 d . . .
O2 O 0.5824(5) 0.2144(4) 0.1215(2) 0.0425(8) Uani 1 1 d . . .
C5 C 1.0008(5) 0.5916(5) 0.2247(3) 0.0304(9) Uani 1 1 d . . .
C1 C 0.7909(6) 0.7291(5) 0.1006(3) 0.0327(9) Uani 1 1 d . . .
C2 C 0.9142(6) 0.7800(5) 0.3597(3) 0.0388(10) Uani 1 1 d . . .
C10 C 0.6279(6) 0.2856(5) 0.0666(3) 0.0375(10) Uani 1 1 d . . .
H10A H 0.6037 0.3785 0.0663 0.045 Uiso 1 1 calc R . .
N5 N 1.0665(6) 0.4920(5) 0.2217(3) 0.0522(11) Uani 1 1 d . . .
N8 N 0.7076(5) 0.2425(5) 0.0082(2) 0.0419(9) Uani 1 1 d . . .
N1 N 0.7624(6) 0.7177(5) 0.0289(3) 0.0554(11) Uani 1 1 d . . .
C7 C 0.4968(7) 0.1732(6) 0.4608(3) 0.0478(12) Uani 1 1 d . . .
H7A H 0.4117 0.1001 0.4747 0.057 Uiso 1 1 calc R . .
N7 N 0.5830(6) 0.2732(6) 0.5203(3) 0.0595(13) Uani 1 1 d . . .
N2 N 0.9483(8) 0.8011(6) 0.4309(3) 0.0707(15) Uani 1 1 d . . .
C11 C 0.7466(9) 0.3299(8) -0.0588(4) 0.0730(18) Uani 1 1 d . . .
H11A H 0.7124 0.4216 -0.0498 0.110 Uiso 1 1 calc R . .
H11B H 0.6807 0.2798 -0.1117 0.110 Uiso 1 1 calc R . .
H11C H 0.8725 0.3460 -0.0592 0.110 Uiso 1 1 calc R . .
C12 C 0.7514(10) 0.0985(7) 0.0051(5) 0.078(2) Uani 1 1 d . . .
H12A H 0.7188 0.0515 0.0521 0.118 Uiso 1 1 calc R . .
H12B H 0.8776 0.1078 0.0072 0.118 Uiso 1 1 calc R . .
H12C H 0.6866 0.0416 -0.0460 0.118 Uiso 1 1 calc R . .
C8 C 0.5608(12) 0.2646(12) 0.6069(4) 0.103(3) Uani 1 1 d . . .
H8A H 0.4732 0.1793 0.6100 0.155 Uiso 1 1 calc R . .
H8B H 0.5214 0.3493 0.6266 0.155 Uiso 1 1 calc R . .
H8C H 0.6730 0.2597 0.6413 0.155 Uiso 1 1 calc R . .
C9 C 0.7089(10) 0.3953(9) 0.5033(5) 0.086(2) Uani 1 1 d . . .
H9A H 0.7102 0.3891 0.4443 0.129 Uiso 1 1 calc R . .
H9B H 0.8262 0.3945 0.5340 0.129 Uiso 1 1 calc R . .
H9C H 0.6742 0.4838 0.5202 0.129 Uiso 1 1 calc R . .
O6 O 0.9822(5) 0.8469(5) 0.6042(3) 0.0454(9) Uani 1 1 d . . .
N6 N 0.5454(5) 0.4773(4) 0.2388(3) 0.0383(9) Uani 1 1 d . . .
N4 N 1.2010(5) 0.9988(4) 0.2325(2) 0.0364(8) Uani 1 1 d . . .
N3 N 0.5977(5) 0.9839(4) 0.2364(2) 0.0385(9) Uani 1 1 d . . .
H501 H 0.222(7) 0.371(6) 0.302(3) 0.036(16) Uiso 1 1 d . . .
H500 H 0.191(7) 0.266(6) 0.341(3) 0.038(14) Uiso 1 1 d . . .
H600 H 0.965(9) 0.840(7) 0.563(4) 0.05(2) Uiso 1 1 d . . .
H300 H 0.238(9) 0.277(8) 0.103(5) 0.06(3) Uiso 1 1 d . . .
H401 H 0.835(11) 0.256(9) 0.322(5) 0.08(3) Uiso 1 1 d . . .
H301 H 0.20(3) 0.19(2) 0.141(11) 0.29(11) Uiso 1 1 d . . .
H601 H 0.988(10) 0.918(8) 0.625(5) 0.08(3) Uiso 1 1 d . . .
H400 H 0.859(12) 0.340(9) 0.287(5) 0.10(3) Uiso 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'
Sm Sm -0.1638 3.4418 '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
O2 Sm O1 144.73(12) . . ?
O2 Sm O4 77.41(14) . . ?
O1 Sm O4 72.53(14) . . ?
O2 Sm O3 75.19(14) . . ?
O1 Sm O3 140.06(13) . . ?
O4 Sm O3 139.30(15) . . ?
O2 Sm O5 142.10(12) . . ?
O1 Sm O5 69.91(12) . . ?
O4 Sm O5 115.78(13) . . ?
O3 Sm O5 72.96(13) . . ?
O2 Sm N4 112.16(12) . 1_445 ?
O1 Sm N4 83.98(13) . 1_445 ?
O4 Sm N4 144.70(14) . 1_445 ?
O3 Sm N4 74.57(14) . 1_445 ?
O5 Sm N4 78.35(13) . 1_445 ?
O2 Sm N6 79.27(12) . . ?
O1 Sm N6 107.17(13) . . ?
O4 Sm N6 70.96(14) . . ?
O3 Sm N6 74.79(14) . . ?
O5 Sm N6 73.02(13) . . ?
N4 Sm N6 142.88(12) 1_445 . ?
O2 Sm N3 75.24(12) . 1_545 ?
O1 Sm N3 79.12(12) . 1_545 ?
O4 Sm N3 74.15(14) . 1_545 ?
O3 Sm N3 125.53(14) . 1_545 ?
O5 Sm N3 141.31(13) . 1_545 ?
N4 Sm N3 75.83(12) 1_445 1_545 ?
N6 Sm N3 140.34(12) . 1_545 ?
C1 Cr C3 90.04(16) . . ?
C1 Cr C5 89.40(16) . . ?
C3 Cr C5 176.20(16) . . ?
C1 Cr C2 178.61(18) . . ?
C3 Cr C2 88.93(17) . . ?
C5 Cr C2 91.69(18) . . ?
C1 Cr C6 91.29(17) . . ?
C3 Cr C6 91.69(15) . . ?
C5 Cr C6 84.57(16) . . ?
C2 Cr C6 89.67(18) . . ?
C1 Cr C4 90.78(17) . . ?
C3 Cr C4 92.73(16) . . ?
C5 Cr C4 91.03(16) . . ?
C2 Cr C4 88.35(18) . . ?
C6 Cr C4 175.12(16) . . ?
N6 C6 Cr 171.2(4) . . ?
N4 C4 Cr 177.0(4) . . ?
N3 C3 Cr 179.5(4) . . ?
C7 O1 Sm 156.6(3) . . ?
C10 O2 Sm 147.6(3) . . ?
N5 C5 Cr 172.6(4) . . ?
N1 C1 Cr 177.9(4) . . ?
N2 C2 Cr 177.3(5) . . ?
O2 C10 N8 125.5(5) . . ?
C10 N8 C11 122.3(5) . . ?
C10 N8 C12 120.3(4) . . ?
C11 N8 C12 117.3(5) . . ?
O1 C7 N7 125.8(5) . . ?
C7 N7 C9 120.8(5) . . ?
C7 N7 C8 121.6(6) . . ?
C9 N7 C8 117.5(6) . . ?
C6 N6 Sm 152.7(3) . . ?
C4 N4 Sm 175.0(3) . 1_665 ?
C3 N3 Sm 167.1(3) . 1_565 ?
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
Sm O2 2.345(3) . ?
Sm O1 2.361(3) . ?
Sm O4 2.442(3) . ?
Sm O3 2.445(4) . ?
Sm O5 2.447(3) . ?
Sm N4 2.514(4) 1_445 ?
Sm N6 2.520(4) . ?
Sm N3 2.524(4) 1_545 ?
Cr C1 2.059(4) . ?
Cr C3 2.071(4) . ?
Cr C5 2.072(4) . ?
Cr C2 2.074(5) . ?
Cr C6 2.075(4) . ?
Cr C4 2.081(4) . ?
C6 N6 1.131(5) . ?
C4 N4 1.129(5) . ?
C3 N3 1.149(5) . ?
O1 C7 1.239(6) . ?
O2 C10 1.218(5) . ?
C5 N5 1.152(6) . ?
C1 N1 1.144(6) . ?
C2 N2 1.138(6) . ?
C10 N8 1.302(6) . ?
N8 C11 1.454(7) . ?
N8 C12 1.461(8) . ?
C7 N7 1.295(7) . ?
N7 C9 1.439(9) . ?
N7 C8 1.458(8) . ?
N4 Sm 2.514(4) 1_665 ?
N3 Sm 2.524(4) 1_565 ?
