#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/77/1517701.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_1517701
loop_
_publ_author_name
'Hui Chen'
'Bao-Xi Miao'
'Li-Fang Zhang'
'Guo-Ling Li'
'Zhong-Hai Ni'
_publ_section_title
;
 Syntheses, crystal structures, and magnetic properties of a series of
 cyanide-bridged trinuclear chromate(III)-nickel(II)-chromate(III)
 complexes based on dicyanidechromate(III) building blocks
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              34
_journal_page_last               39
_journal_volume                  404
_journal_year                    2013
_chemical_formula_moiety         'C54 H56 Cr2 N16 Ni O4'
_chemical_formula_sum            'C54 H56 Cr2 N16 Ni O4'
_chemical_formula_weight         1155.86
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0535(18)
_cell_length_b                   14.211(3)
_cell_length_c                   20.331(4)
_cell_measurement_reflns_used    2530
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.55
_cell_measurement_theta_min      3.01
_cell_volume                     2615.7(9)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       'ω 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  0.0836
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29269
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.02
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         5679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1079P)²+1.2891P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                5303
_reflns_number_total             5679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-404-34-39-4.cif
_cod_data_source_block           dmbpb
_cod_original_cell_volume        2615.8(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1517701
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
Ni1 Ni 0.5000 0.5000 0.5000 0.01521(13) Uani 1 2 d S
Cr1 Cr 0.28717(3) 0.34432(2) 0.290286(14) 0.01319(12) Uani 1 1 d .
O1 O 0.57677(19) 0.13154(13) 0.33274(9) 0.0335(4) Uani 1 1 d .
O2 O -0.11525(18) 0.35276(12) 0.38098(8) 0.0288(4) Uani 1 1 d .
N1 N 0.4435(2) 0.47707(13) 0.40001(9) 0.0221(4) Uani 1 1 d .
N2 N 0.1235(2) 0.23099(15) 0.17308(10) 0.0319(5) Uani 1 1 d .
N3 N 0.4875(2) 0.33771(12) 0.24052(8) 0.0170(3) Uani 1 1 d .
N4 N 0.37896(18) 0.23564(12) 0.33541(8) 0.0164(3) Uani 1 1 d .
N5 N 0.12634(18) 0.31500(12) 0.35242(8) 0.0156(3) Uani 1 1 d .
N6 N 0.13409(19) 0.44700(11) 0.26300(8) 0.0169(3) Uani 1 1 d .
N7 N 0.71236(19) 0.45259(14) 0.48200(9) 0.0226(4) Uani 1 1 d .
H7 H 0.7127 0.4292 0.4403 0.027 Uiso 1 1 calc R
N8 N 0.5849(2) 0.63354(13) 0.48067(9) 0.0228(4) Uani 1 1 d .
H8 H 0.6053 0.6609 0.5202 0.027 Uiso 1 1 calc R
C1 C 0.3891(2) 0.43633(14) 0.35698(9) 0.0157(4) Uani 1 1 d .
C2 C 0.1899(2) 0.26743(14) 0.21462(10) 0.0195(4) Uani 1 1 d .
C3 C 0.5403(2) 0.39553(15) 0.19362(10) 0.0212(4) Uani 1 1 d .
H3 H 0.4840 0.4471 0.1807 0.025 Uiso 1 1 calc R
C4 C 0.6754(2) 0.38040(17) 0.16423(11) 0.0249(5) Uani 1 1 d .
H4 H 0.7091 0.4211 0.1318 0.030 Uiso 1 1 calc R
C5 C 0.7606(3) 0.30388(17) 0.18360(11) 0.0266(5) Uani 1 1 d .
H5 H 0.8518 0.2925 0.1644 0.032 Uiso 1 1 calc R
C6 C 0.7071(2) 0.24472(17) 0.23216(11) 0.0269(5) Uani 1 1 d .
H6 H 0.7624 0.1932 0.2461 0.032 Uiso 1 1 calc R
C7 C 0.5699(2) 0.26314(15) 0.25975(10) 0.0201(4) Uani 1 1 d .
C8 C 0.5086(2) 0.20167(15) 0.31405(10) 0.0203(4) Uani 1 1 d .
C9 C 0.2970(2) 0.19877(14) 0.38854(9) 0.0165(4) Uani 1 1 d .
C10 C 0.3408(2) 0.12723(17) 0.43165(11) 0.0253(5) Uani 1 1 d .
H10 H 0.4317 0.0980 0.4257 0.030 Uiso 1 1 calc R
C11 C 0.2506(3) 0.09881(17) 0.48349(11) 0.0261(5) Uani 1 1 d .
C12 C 0.3035(3) 0.0227(3) 0.53019(16) 0.0522(9) Uani 1 1 d .
H12A H 0.3188 0.0491 0.5731 0.078 Uiso 1 1 calc R
H12B H 0.3947 -0.0031 0.5145 0.078 Uiso 1 1 calc R
H12C H 0.2306 -0.0262 0.5325 0.078 Uiso 1 1 calc R
C13 C 0.0143(3) 0.11303(17) 0.54820(11) 0.0265(5) Uani 1 1 d .
H13A H 0.0061 0.0457 0.5498 0.040 Uiso 1 1 calc R
H13B H -0.0820 0.1401 0.5421 0.040 Uiso 1 1 calc R
H13C H 0.0564 0.1355 0.5887 0.040 Uiso 1 1 calc R
C14 C 0.1119(2) 0.14087(15) 0.49184(10) 0.0197(4) Uani 1 1 d .
C15 C 0.0669(2) 0.21171(14) 0.44830(10) 0.0178(4) Uani 1 1 d .
H15 H -0.0256 0.2390 0.4535 0.021 Uiso 1 1 calc R
C16 C 0.1571(2) 0.24231(13) 0.39738(9) 0.0148(4) Uani 1 1 d .
C17 C -0.0011(2) 0.36284(15) 0.34813(10) 0.0184(4) Uani 1 1 d .
C18 C 0.0043(2) 0.43724(14) 0.29518(10) 0.0191(4) Uani 1 1 d .
C19 C -0.1179(3) 0.49096(16) 0.27951(11) 0.0254(5) Uani 1 1 d .
H19 H -0.2055 0.4837 0.3026 0.031 Uiso 1 1 calc R
C20 C -0.1080(3) 0.55630(16) 0.22867(11) 0.0285(5) Uani 1 1 d .
H20 H -0.1893 0.5928 0.2170 0.034 Uiso 1 1 calc R
C21 C 0.0239(3) 0.56618(15) 0.19585(11) 0.0254(5) Uani 1 1 d .
H21 H 0.0327 0.6094 0.1618 0.030 Uiso 1 1 calc R
C22 C 0.1439(3) 0.51065(14) 0.21438(11) 0.0215(4) Uani 1 1 d .
H22 H 0.2332 0.5178 0.1925 0.026 Uiso 1 1 calc R
C23 C 0.3368(3) 0.70787(18) 0.47787(13) 0.0357(6) Uani 1 1 d .
H23A H 0.2857 0.7612 0.4585 0.043 Uiso 1 1 calc R
H23B H 0.3540 0.7224 0.5239 0.043 Uiso 1 1 calc R
C24 C 0.4858(3) 0.69795(17) 0.44449(12) 0.0317(5) Uani 1 1 d .
H24A H 0.4710 0.6744 0.4001 0.038 Uiso 1 1 calc R
H24B H 0.5320 0.7594 0.4414 0.038 Uiso 1 1 calc R
C25 C 0.7274(3) 0.61689(18) 0.44768(12) 0.0291(5) Uani 1 1 d .
H25A H 0.7872 0.6735 0.4494 0.035 Uiso 1 1 calc R
H25B H 0.7104 0.6009 0.4019 0.035 Uiso 1 1 calc R
C26 C 0.8074(2) 0.53694(19) 0.48206(12) 0.0306(5) Uani 1 1 d .
H26A H 0.8991 0.5234 0.4595 0.037 Uiso 1 1 calc R
H26B H 0.8310 0.5549 0.5270 0.037 Uiso 1 1 calc R
C27 C 0.7639(3) 0.37637(19) 0.52597(12) 0.0317(5) Uani 1 1 d .
H27A H 0.7675 0.3993 0.5709 0.038 Uiso 1 1 calc R
H27B H 0.8631 0.3579 0.5136 0.038 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'
Cr Cr 0.3209 0.6236 '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
N7 Ni1 N7 180.0 . 3_666
N7 Ni1 N8 94.63(8) . 3_666
N7 Ni1 N8 85.37(8) 3_666 3_666
N7 Ni1 N8 85.37(8) . .
N7 Ni1 N8 94.63(8) 3_666 .
N8 Ni1 N8 180.0 3_666 .
N7 Ni1 N1 89.94(7) . .
N7 Ni1 N1 90.06(7) 3_666 .
N8 Ni1 N1 87.36(7) 3_666 .
N8 Ni1 N1 92.64(7) . .
N7 Ni1 N1 90.06(7) . 3_666
N7 Ni1 N1 89.94(7) 3_666 3_666
N8 Ni1 N1 92.64(7) 3_666 3_666
N8 Ni1 N1 87.36(7) . 3_666
N1 Ni1 N1 180.0 . 3_666
N5 Cr1 N4 81.26(7) . .
N5 Cr1 C2 92.96(8) . .
N4 Cr1 C2 96.18(8) . .
N5 Cr1 N6 80.02(7) . .
N4 Cr1 N6 161.25(7) . .
C2 Cr1 N6 83.87(8) . .
N5 Cr1 N3 161.21(7) . .
N4 Cr1 N3 79.95(7) . .
C2 Cr1 N3 89.02(8) . .
N6 Cr1 N3 118.77(7) . .
N5 Cr1 C1 92.36(7) . .
N4 Cr1 C1 90.29(8) . .
C2 Cr1 C1 172.17(8) . .
N6 Cr1 C1 91.42(7) . .
N3 Cr1 C1 87.77(7) . .
C1 N1 Ni1 154.42(17) . .
C3 N3 C7 118.98(18) . .
C3 N3 Cr1 128.98(15) . .
C7 N3 Cr1 112.04(13) . .
C8 N4 C9 125.24(17) . .
C8 N4 Cr1 119.75(13) . .
C9 N4 Cr1 114.99(13) . .
C17 N5 C16 125.53(17) . .
C17 N5 Cr1 119.20(14) . .
C16 N5 Cr1 115.26(13) . .
C22 N6 C18 119.08(18) . .
C22 N6 Cr1 128.30(15) . .
C18 N6 Cr1 112.12(13) . .
C27 N7 C26 114.38(19) . .
C27 N7 Ni1 114.92(14) . .
C26 N7 Ni1 106.11(14) . .
C27 N7 H7 107.0 . .
C26 N7 H7 107.0 . .
Ni1 N7 H7 107.0 . .
C24 N8 C25 113.77(19) . .
C24 N8 Ni1 115.80(15) . .
C25 N8 Ni1 105.29(14) . .
C24 N8 H8 107.2 . .
C25 N8 H8 107.2 . .
Ni1 N8 H8 107.2 . .
N1 C1 Cr1 170.50(18) . .
N2 C2 Cr1 172.92(19) . .
N3 C3 C4 122.0(2) . .
N3 C3 H3 119.0 . .
C4 C3 H3 119.0 . .
C3 C4 C5 119.4(2) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
C6 C5 C4 118.8(2) . .
C6 C5 H5 120.6 . .
C4 C5 H5 120.6 . .
C7 C6 C5 119.3(2) . .
C7 C6 H6 120.3 . .
C5 C6 H6 120.3 . .
N3 C7 C6 121.56(19) . .
N3 C7 C8 117.25(18) . .
C6 C7 C8 121.17(19) . .
O1 C8 N4 128.94(19) . .
O1 C8 C7 120.37(18) . .
N4 C8 C7 110.68(17) . .
C10 C9 N4 126.84(18) . .
C10 C9 C16 119.11(18) . .
N4 C9 C16 114.04(17) . .
C11 C10 C9 121.2(2) . .
C11 C10 H10 119.4 . .
C9 C10 H10 119.4 . .
C10 C11 C14 119.8(2) . .
C10 C11 C12 119.7(2) . .
C14 C11 C12 120.5(2) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C14 C13 H13A 109.5 . .
C14 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C14 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C15 C14 C11 119.18(19) . .
C15 C14 C13 120.03(19) . .
C11 C14 C13 120.76(19) . .
C16 C15 C14 121.68(19) . .
C16 C15 H15 119.2 . .
C14 C15 H15 119.2 . .
C15 C16 N5 126.76(18) . .
C15 C16 C9 119.02(18) . .
N5 C16 C9 114.21(17) . .
O2 C17 N5 128.66(19) . .
O2 C17 C18 119.65(18) . .
N5 C17 C18 111.69(18) . .
N6 C18 C19 121.9(2) . .
N6 C18 C17 116.61(18) . .
C19 C18 C17 121.5(2) . .
C18 C19 C20 119.0(2) . .
C18 C19 H19 120.5 . .
C20 C19 H19 120.5 . .
C21 C20 C19 119.1(2) . .
C21 C20 H20 120.4 . .
C19 C20 H20 120.4 . .
C20 C21 C22 119.2(2) . .
C20 C21 H21 120.4 . .
C22 C21 H21 120.4 . .
N6 C22 C21 121.7(2) . .
N6 C22 H22 119.2 . .
C21 C22 H22 119.2 . .
C24 C23 C27 116.2(2) . 3_666
C24 C23 H23A 108.2 . .
C27 C23 H23A 108.2 3_666 .
C24 C23 H23B 108.2 . .
C27 C23 H23B 108.2 3_666 .
H23A C23 H23B 107.4 . .
N8 C24 C23 111.91(19) . .
N8 C24 H24A 109.2 . .
C23 C24 H24A 109.2 . .
N8 C24 H24B 109.2 . .
C23 C24 H24B 109.2 . .
H24A C24 H24B 107.9 . .
N8 C25 C26 109.08(18) . .
N8 C25 H25A 109.9 . .
C26 C25 H25A 109.9 . .
N8 C25 H25B 109.9 . .
C26 C25 H25B 109.9 . .
H25A C25 H25B 108.3 . .
N7 C26 C25 109.37(18) . .
N7 C26 H26A 109.8 . .
C25 C26 H26A 109.8 . .
N7 C26 H26B 109.8 . .
C25 C26 H26B 109.8 . .
H26A C26 H26B 108.2 . .
N7 C27 C23 111.2(2) . 3_666
N7 C27 H27A 109.4 . .
C23 C27 H27A 109.4 3_666 .
N7 C27 H27B 109.4 . .
C23 C27 H27B 109.4 3_666 .
H27A C27 H27B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N7 2.0720(18) .
Ni1 N7 2.0720(18) 3_666
Ni1 N8 2.0857(19) 3_666
Ni1 N8 2.0857(19) .
Ni1 N1 2.1183(18) .
Ni1 N1 2.1183(18) 3_666
Cr1 N5 1.9782(17) .
Cr1 N4 1.9767(17) .
Cr1 C2 2.078(2) .
Cr1 N6 2.0851(17) .
Cr1 N3 2.0846(19) .
Cr1 C1 2.094(2) .
O1 C8 1.231(3) .
O2 C17 1.243(3) .
N1 C1 1.156(3) .
N2 C2 1.156(3) .
N3 C3 1.349(3) .
N3 C7 1.352(3) .
N4 C8 1.343(3) .
N4 C9 1.415(2) .
N5 C17 1.341(3) .
N5 C16 1.406(2) .
N6 C22 1.343(3) .
N6 C18 1.356(3) .
N7 C27 1.478(3) .
N7 C26 1.476(3) .
N7 H7 0.9100 .
N8 C24 1.475(3) .
N8 C25 1.477(3) .
N8 H8 0.9100 .
C3 C4 1.382(3) .
C3 H3 0.9300 .
C4 C5 1.388(3) .
C4 H4 0.9300 .
C5 C6 1.387(3) .
C5 H5 0.9300 .
C6 C7 1.391(3) .
C6 H6 0.9300 .
C7 C8 1.516(3) .
C9 C10 1.398(3) .
C9 C16 1.422(3) .
C10 C11 1.397(3) .
C10 H10 0.9300 .
C11 C14 1.402(3) .
C11 C12 1.515(3) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 C14 1.505(3) .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 C15 1.400(3) .
C15 C16 1.392(3) .
C15 H15 0.9300 .
C17 C18 1.510(3) .
C18 C19 1.380(3) .
C19 C20 1.393(3) .
C19 H19 0.9300 .
C20 C21 1.379(4) .
C20 H20 0.9300 .
C21 C22 1.393(3) .
C21 H21 0.9300 .
C22 H22 0.9300 .
C23 C24 1.521(4) .
C23 C27 1.507(4) 3_666
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 C26 1.516(4) .
C25 H25A 0.9700 .
C25 H25B 0.9700 .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
C27 C23 1.507(4) 3_666
C27 H27A 0.9700 .
C27 H27B 0.9700 .
