#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:07:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180223 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/09/7110977.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_7110977
loop_
_publ_author_name
'Kou, Hui-Zhong'
'Gao, Song'
'Ma, Bao-Qing'
'Liao, Dai-Zheng'
_publ_section_title
;
 A cyano-bridged molecular magnet with a novel two-dimensional brick wall
 structure
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1309
_journal_paper_doi               10.1039/b003089i
_journal_year                    2000
_chemical_formula_sum            'C48 H114 Fe2 N30 Ni3 O12'
_chemical_formula_weight         1591.52
_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                102.06(3)
_cell_angle_beta                 101.24(3)
_cell_angle_gamma                92.67(3)
_cell_formula_units_Z            1
_cell_length_a                   10.018(2)
_cell_length_b                   13.861(3)
_cell_length_c                   15.162(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2011.0(8)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.2777
_diffrn_reflns_av_sigmaI/netI    0.3537
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26679
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   SORTAV
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.2819
_refine_ls_R_factor_gt           0.0850
_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)+(0.1011P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.2489
_reflns_number_gt                2227
_reflns_number_total             7004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003089isup1.cif
_cod_data_source_block           B003089I
_cod_original_cell_volume        2011.0(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110977
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
Fe Fe 0.33443(15) 0.28106(10) 0.18608(10) 0.0443(5) Uani 1 1 d .
Ni2 Ni 0.0000 0.0000 0.0000 0.0473(6) Uani 1 2 d S
Ni3 Ni 0.5000 0.5000 0.0000 0.0436(6) Uani 1 2 d S
Ni1 Ni 0.5000 0.5000 0.5000 0.0571(7) Uani 1 2 d S
N5 N 0.1659(11) 0.2164(8) 0.3168(7) 0.085(4) Uani 1 1 d .
C2 C 0.4680(12) 0.1946(8) 0.2118(9) 0.057(4) Uani 1 1 d .
N1 N 0.1642(9) 0.1131(6) 0.0335(7) 0.060(3) Uani 1 1 d .
N4 N 0.4781(9) 0.4392(7) 0.3557(7) 0.061(3) Uani 1 1 d .
N3 N 0.4769(9) 0.3750(6) 0.0568(7) 0.054(3) Uani 1 1 d .
C1 C 0.2336(10) 0.1771(7) 0.0893(8) 0.044(3) Uani 1 1 d .
N2 N 0.5512(12) 0.1426(8) 0.2283(8) 0.081(3) Uani 1 1 d .
C4 C 0.4275(11) 0.3806(9) 0.2877(9) 0.055(3) Uani 1 1 d .
C5 C 0.2293(13) 0.2382(8) 0.2667(8) 0.061(4) Uani 1 1 d .
C3 C 0.4302(11) 0.3325(8) 0.1043(8) 0.054(3) Uani 1 1 d .
N10 N 0.1419(8) -0.1004(6) 0.0156(7) 0.056(3) Uani 1 1 d .
H12 H 0.2243 -0.0647 0.0394 0.067 Uiso 1 1 calc R
N13 N 0.3090(8) 0.5349(6) 0.0213(6) 0.042(2) Uani 1 1 d .
N8 N 0.3376(9) 0.5850(7) 0.4760(6) 0.064(3) Uani 1 1 d .
H8 H 0.3354 0.6267 0.5306 0.077 Uiso 1 1 calc R
C6 C 0.2014(12) 0.3720(9) 0.1569(9) 0.055(4) Uani 1 1 d .
N11 N -0.0136(9) 0.0309(7) 0.1363(6) 0.058(3) Uani 1 1 d .
H11 H 0.0595 0.0738 0.1685 0.070 Uiso 1 1 calc R
N9 N 0.4759(14) 0.7126(8) 0.4340(8) 0.078(3) Uani 1 1 d .
N7 N 0.6461(10) 0.6110(7) 0.5001(7) 0.065(3) Uani 1 1 d .
H10 H 0.6636 0.6537 0.5563 0.078 Uiso 1 1 calc R
N14 N 0.5747(9) 0.5906(6) 0.1288(6) 0.050(3) Uani 1 1 d .
H14 H 0.6080 0.6498 0.1211 0.061 Uiso 1 1 calc R
C16 C 0.1188(13) -0.1594(9) 0.0819(12) 0.083(4) Uani 1 1 d .
H9A H 0.0363 -0.2035 0.0547 0.100 Uiso 1 1 calc R
H9B H 0.1940 -0.2005 0.0902 0.100 Uiso 1 1 calc R
C20 C 0.3352(10) 0.6223(8) 0.0991(8) 0.055(3) Uani 1 1 d .
H13A H 0.2540 0.6317 0.1247 0.066 Uiso 1 1 calc R
H13B H 0.3568 0.6811 0.0775 0.066 Uiso 1 1 calc R
C21 C 0.4540(10) 0.6074(8) 0.1733(8) 0.052(3) Uani 1 1 d .
H14A H 0.4741 0.6655 0.2237 0.062 Uiso 1 1 calc R
H14B H 0.4314 0.5507 0.1975 0.062 Uiso 1 1 calc R
C9 C 0.3517(14) 0.6471(10) 0.4093(8) 0.075(4) Uani 1 1 d .
H19A H 0.3482 0.6040 0.3495 0.090 Uiso 1 1 calc R
H19B H 0.2743 0.6865 0.4035 0.090 Uiso 1 1 calc R
N15 N 0.8039(8) 0.5264(7) 0.1420(6) 0.056(3) Uani 1 1 d .
O4 O 0.2250(9) 0.7085(7) 0.6371(6) 0.106(3) Uani 1 1 d .
O6 O -0.0737(9) 0.4025(7) 0.2741(7) 0.109(3) Uani 1 1 d .
N12 N 0.1057(13) -0.1068(9) 0.1710(9) 0.082(4) Uani 1 1 d .
N6 N 0.1242(11) 0.4283(9) 0.1370(9) 0.090(4) Uani 1 1 d .
C23 C 0.8895(12) 0.6109(9) 0.1347(9) 0.075(4) Uani 1 1 d .
H17A H 0.8317 0.6570 0.1094 0.090 Uiso 1 1 calc R
H17B H 0.9484 0.5884 0.0922 0.090 Uiso 1 1 calc R
C13 C -0.1356(14) 0.0816(10) 0.1422(9) 0.079(4) Uani 1 1 d .
H7A H -0.1307 0.1177 0.2050 0.095 Uiso 1 1 calc R
H7B H -0.2155 0.0341 0.1242 0.095 Uiso 1 1 calc R
C10 C 0.5966(16) 0.6679(11) 0.4279(9) 0.083(5) Uani 1 1 d .
H20A H 0.6680 0.7189 0.4309 0.099 Uiso 1 1 calc R
H20B H 0.5835 0.6231 0.3678 0.099 Uiso 1 1 calc R
C22 C 0.6876(12) 0.5483(9) 0.1852(8) 0.063(4) Uani 1 1 d .
H16A H 0.7196 0.5949 0.2439 0.076 Uiso 1 1 calc R
H16B H 0.6508 0.4878 0.1978 0.076 Uiso 1 1 calc R
C19 C 0.2195(12) 0.5560(8) -0.0628(9) 0.064(4) Uani 1 1 d .
H15A H 0.1321 0.5731 -0.0485 0.076 Uiso 1 1 calc R
H15B H 0.2614 0.6129 -0.0784 0.076 Uiso 1 1 calc R
C14 C 0.1458(13) -0.1525(10) -0.0784(11) 0.084(4) Uani 1 1 d .
H8A H 0.0707 -0.2040 -0.1007 0.101 Uiso 1 1 calc R
H8B H 0.2306 -0.1837 -0.0779 0.101 Uiso 1 1 calc R
C8 C 0.7693(14) 0.5599(10) 0.4894(10) 0.083(4) Uani 1 1 d .
H24A H 0.8486 0.6080 0.5069 0.099 Uiso 1 1 calc R
H24B H 0.7612 0.5268 0.4253 0.099 Uiso 1 1 calc R
C7 C 0.2116(12) 0.5164(10) 0.4500(9) 0.084(4) Uani 1 1 d .
H23A H 0.1961 0.4835 0.3854 0.101 Uiso 1 1 calc R
H23B H 0.1333 0.5527 0.4601 0.101 Uiso 1 1 calc R
C17 C 0.2359(16) -0.0515(11) 0.2284(13) 0.112(6) Uani 1 1 d .
H11A H 0.2810 -0.0182 0.1905 0.134 Uiso 1 1 calc R
H11B H 0.2153 -0.0014 0.2777 0.134 Uiso 1 1 calc R
C15 C -0.0137(14) -0.0533(10) 0.1772(9) 0.075(4) Uani 1 1 d .
H10A H -0.0948 -0.0977 0.1467 0.090 Uiso 1 1 calc R
H10B H -0.0180 -0.0314 0.2416 0.090 Uiso 1 1 calc R
C11 C 0.4803(18) 0.7913(10) 0.5151(11) 0.115(6) Uani 1 1 d .
H21A H 0.3908 0.8157 0.5130 0.138 Uiso 1 1 calc R
H21B H 0.5036 0.7651 0.5702 0.138 Uiso 1 1 calc R
O2 O 0.4642(10) -0.0451(10) 0.0659(10) 0.172(5) Uani 1 1 d .
O3 O 0.6284(12) 0.8122(7) 0.1362(10) 0.169(6) Uani 1 1 d .
O5 O -0.0089(16) 0.1754(15) 0.4337(12) 0.261(9) Uani 1 1 d .
C24 C 0.9772(16) 0.6645(12) 0.2270(11) 0.141(7) Uani 1 1 d .
H18A H 1.0305 0.7200 0.2188 0.211 Uiso 1 1 calc R
H18B H 1.0371 0.6199 0.2514 0.211 Uiso 1 1 calc R
H18C H 0.9194 0.6873 0.2692 0.211 Uiso 1 1 calc R
O1 O 0.710(2) -0.063(3) 0.298(2) 0.47(2) Uani 1 1 d .
C18 C 0.322(2) -0.1125(15) 0.2654(17) 0.208(11) Uani 1 1 d .
H12A H 0.4030 -0.0742 0.3031 0.312 Uiso 1 1 calc R
H12B H 0.3459 -0.1604 0.2168 0.312 Uiso 1 1 calc R
H12C H 0.2772 -0.1462 0.3025 0.312 Uiso 1 1 calc R
C12 C 0.577(3) 0.8697(14) 0.5197(14) 0.279(17) Uani 1 1 d .
H22A H 0.5769 0.9209 0.5731 0.418 Uiso 1 1 calc R
H22B H 0.5539 0.8957 0.4653 0.418 Uiso 1 1 calc R
H22C H 0.6660 0.8461 0.5237 0.418 Uiso 1 1 calc R
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
C2 Fe C4 90.6(5) . .
C2 Fe C1 89.3(5) . .
C4 Fe C1 175.9(4) . .
C2 Fe C5 92.0(5) . .
C4 Fe C5 88.3(5) . .
C1 Fe C5 87.6(4) . .
C2 Fe C6 177.8(5) . .
C4 Fe C6 89.2(5) . .
C1 Fe C6 91.0(5) . .
C5 Fe C6 90.2(5) . .
C2 Fe C3 92.6(5) . .
C4 Fe C3 90.9(4) . .
C1 Fe C3 93.1(4) . .
C5 Fe C3 175.3(5) . .
C6 Fe C3 85.2(5) . .
N10 Ni2 N10 180.0(7) . 2
N10 Ni2 N11 94.4(4) . .
N10 Ni2 N11 85.6(4) 2 .
N10 Ni2 N11 85.6(4) . 2
N10 Ni2 N11 94.4(4) 2 2
N11 Ni2 N11 180.0(5) . 2
N10 Ni2 N1 88.3(3) . .
N10 Ni2 N1 91.7(3) 2 .
N11 Ni2 N1 88.7(4) . .
N11 Ni2 N1 91.3(4) 2 .
N10 Ni2 N1 91.7(3) . 2
N10 Ni2 N1 88.3(3) 2 2
N11 Ni2 N1 91.3(4) . 2
N11 Ni2 N1 88.7(4) 2 2
N1 Ni2 N1 180.0(3) . 2
N13 Ni3 N13 180.0(4) 2_665 .
N13 Ni3 N14 94.0(3) 2_665 .
N13 Ni3 N14 86.0(3) . .
N13 Ni3 N14 86.0(3) 2_665 2_665
N13 Ni3 N14 94.0(3) . 2_665
N14 Ni3 N14 180.000(1) . 2_665
N13 Ni3 N3 91.3(3) 2_665 .
N13 Ni3 N3 88.7(3) . .
N14 Ni3 N3 92.0(3) . .
N14 Ni3 N3 88.0(3) 2_665 .
N13 Ni3 N3 88.7(3) 2_665 2_665
N13 Ni3 N3 91.3(3) . 2_665
N14 Ni3 N3 88.0(3) . 2_665
N14 Ni3 N3 92.0(3) 2_665 2_665
N3 Ni3 N3 180.0(5) . 2_665
N8 Ni1 N8 180.000(2) 2_666 .
N8 Ni1 N7 85.8(4) 2_666 .
N8 Ni1 N7 94.2(4) . .
N8 Ni1 N7 94.2(4) 2_666 2_666
N8 Ni1 N7 85.8(4) . 2_666
N7 Ni1 N7 180.000(1) . 2_666
N8 Ni1 N4 91.6(4) 2_666 2_666
N8 Ni1 N4 88.4(4) . 2_666
N7 Ni1 N4 87.2(4) . 2_666
N7 Ni1 N4 92.8(4) 2_666 2_666
N8 Ni1 N4 88.4(4) 2_666 .
N8 Ni1 N4 91.6(4) . .
N7 Ni1 N4 92.8(4) . .
N7 Ni1 N4 87.2(4) 2_666 .
N4 Ni1 N4 180.000(1) 2_666 .
N2 C2 Fe 179.1(12) . .
C1 N1 Ni2 148.5(9) . .
C4 N4 Ni1 151.4(9) . .
C3 N3 Ni3 152.1(9) . .
N1 C1 Fe 175.0(9) . .
N4 C4 Fe 173.9(10) . .
N5 C5 Fe 177.3(11) . .
N3 C3 Fe 170.2(11) . .
C14 N10 C16 118.4(11) . .
C14 N10 Ni2 105.2(7) . .
C16 N10 Ni2 112.5(8) . .
C20 N13 C19 111.6(8) . .
C20 N13 Ni3 105.0(6) . .
C19 N13 Ni3 112.5(6) . .
C9 N8 C7 114.5(10) . .
C9 N8 Ni1 113.3(8) . .
C7 N8 Ni1 106.8(7) . .
N6 C6 Fe 177.2(12) . .
C15 N11 C13 111.3(10) . .
C15 N11 Ni2 115.0(8) . .
C13 N11 Ni2 106.9(8) . .
C10 N9 C9 116.3(11) . .
C10 N9 C11 116.5(13) . .
C9 N9 C11 113.0(12) . .
C8 N7 C10 115.3(11) . .
C8 N7 Ni1 104.7(7) . .
C10 N7 Ni1 111.3(7) . .
C22 N14 C21 113.0(8) . .
C22 N14 Ni3 112.7(7) . .
C21 N14 Ni3 106.0(6) . .
N12 C16 N10 117.2(10) . .
N13 C20 C21 109.7(9) . .
N14 C21 C20 107.1(9) . .
N9 C9 N8 114.4(10) . .
C19 N15 C23 114.8(9) 2_665 .
C19 N15 C22 116.1(8) 2_665 .
C23 N15 C22 116.6(9) . .
C16 N12 C15 117.8(11) . .
C16 N12 C17 113.5(13) . .
C15 N12 C17 114.2(12) . .
N15 C23 C24 112.6(10) . .
N11 C13 C14 108.3(10) . 2
N9 C10 N7 116.2(12) . .
N15 C22 N14 114.5(9) . .
N15 C19 N13 113.5(9) 2_665 .
N10 C14 C13 110.8(10) . 2
N7 C8 C7 110.5(11) . 2_666
N8 C7 C8 107.5(10) . 2_666
C18 C17 N12 111.9(14) . .
N11 C15 N12 112.8(11) . .
C12 C11 N9 111.1(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe C2 1.876(14) .
Fe C4 1.892(12) .
Fe C1 1.911(11) .
Fe C5 1.924(13) .
Fe C6 1.929(14) .
Fe C3 1.934(13) .
Ni2 N10 2.050(9) .
Ni2 N10 2.050(9) 2
Ni2 N11 2.053(9) .
Ni2 N11 2.053(9) 2
Ni2 N1 2.126(8) .
Ni2 N1 2.126(8) 2
Ni3 N13 2.064(8) 2_665
Ni3 N13 2.064(8) .
Ni3 N14 2.066(8) .
Ni3 N14 2.066(8) 2_665
Ni3 N3 2.111(9) .
Ni3 N3 2.111(9) 2_665
Ni1 N8 2.072(10) 2_666
Ni1 N8 2.072(10) .
Ni1 N7 2.074(8) .
Ni1 N7 2.074(8) 2_666
Ni1 N4 2.139(10) 2_666
Ni1 N4 2.139(10) .
N5 C5 1.156(13) .
C2 N2 1.152(13) .
N1 C1 1.178(11) .
N4 C4 1.177(12) .
N3 C3 1.169(12) .
N10 C14 1.466(14) .
N10 C16 1.466(14) .
N13 C20 1.477(12) .
N13 C19 1.499(13) .
N8 C9 1.479(13) .
N8 C7 1.480(13) .
C6 N6 1.167(13) .
N11 C15 1.431(14) .
N11 C13 1.447(14) .
N9 C10 1.395(15) .
N9 C9 1.444(14) .
N9 C11 1.456(16) .
N7 C8 1.470(15) .
N7 C10 1.500(15) .
N14 C22 1.499(13) .
N14 C21 1.500(11) .
C16 N12 1.428(16) .
C20 C21 1.524(13) .
N15 C19 1.447(13) 2_665
N15 C23 1.455(12) .
N15 C22 1.459(13) .
N12 C15 1.444(15) .
N12 C17 1.494(16) .
C23 C24 1.519(16) .
C13 C14 1.509(17) 2
C19 N15 1.447(13) 2_665
C14 C13 1.509(17) 2
C8 C7 1.535(16) 2_666
C7 C8 1.535(16) 2_666
C17 C18 1.36(2) .
C11 C12 1.40(2) .
