#------------------------------------------------------------------------------
#$Date: 2018-08-21 13:35:45 +0300 (Tue, 21 Aug 2018) $
#$Revision: 210018 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/23/4302381.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_4302381
loop_
_publ_author_name
'Zhang, Daopeng'
'Wang, Hailong'
'Chen, Yuting'
'Ni, Zhong-Hai'
'Tian, Laijin'
'Jiang, Jianzhuang'
_publ_section_title
;
 Rational Design and Assembly of a New Series of Cyanide-Bridged
 FeIII--MnII One-Dimensional Single Chain Complexes:
 Synthesis, Crystal Structures, and Magnetic Properties
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5488
_journal_page_last               5496
_journal_paper_doi               10.1021/ic900483z
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C16 H27 Cl2 Mn N3 O8'
_chemical_formula_weight         515.25
_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                69.3660(10)
_cell_angle_beta                 81.1560(10)
_cell_angle_gamma                85.8990(10)
_cell_formula_units_Z            2
_cell_length_a                   7.1991(6)
_cell_length_b                   11.6817(10)
_cell_length_c                   14.5535(11)
_cell_measurement_temperature    273(2)
_cell_volume                     1131.59(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5678
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             534
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0514
_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)+(0.0982P)²+0.9493P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1590
_reflns_number_gt                3351
_reflns_number_total             3955
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4338602
_cod_data_source_file            ic900483z_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4302381
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
Mn1 Mn 0.84444(6) 0.20970(4) 0.20847(3) 0.0381(2) Uani 1 1 d . . .
Cl1 Cl 0.52134(16) 0.78508(11) 0.21375(10) 0.0706(3) Uani 1 1 d . . .
Cl2 Cl 1.16674(12) 0.28447(9) 0.20984(8) 0.0530(3) Uani 1 1 d . . .
O1 O 0.7992(4) 0.3915(2) 0.08437(19) 0.0550(7) Uani 1 1 d . . .
O2 O 0.9398(4) 0.1806(3) 0.06219(18) 0.0542(7) Uani 1 1 d . . .
O3 O 0.7028(6) 0.7562(5) 0.1833(5) 0.146(2) Uani 1 1 d . . .
O4 O 0.3915(9) 0.7447(5) 0.1719(6) 0.159(2) Uani 1 1 d . . .
O5 O 0.4932(10) 0.8997(5) 0.2135(8) 0.205(4) Uani 1 1 d . . .
O6 O 0.4903(13) 0.7074(8) 0.3144(5) 0.210(4) Uani 1 1 d . . .
O7 O 0.0711(7) 0.3792(3) 0.3893(3) 0.1037(13) Uani 1 1 d . . .
H7 H 0.1795 0.3532 0.3833 0.124 Uiso 1 1 d R . .
O8 O 0.5655(3) 0.1533(3) 0.1836(2) 0.0578(7) Uani 1 1 d . . .
H8C H 0.4813 0.1993 0.1955 0.069 Uiso 1 1 d R . .
H8D H 0.5364 0.1153 0.1500 0.069 Uiso 1 1 d R . .
N1 N 0.7793(4) 0.1105(2) 0.36990(19) 0.0393(6) Uani 1 1 d . . .
N2 N 0.9480(4) 0.0156(3) 0.2426(2) 0.0430(7) Uani 1 1 d . . .
N3 N 0.6804(4) 0.3344(3) 0.2798(2) 0.0463(7) Uani 1 1 d . . .
C1 C 0.6968(5) 0.1700(3) 0.4283(2) 0.0437(8) Uani 1 1 d . . .
C2 C 0.6597(5) 0.1113(4) 0.5303(3) 0.0558(10) Uani 1 1 d . . .
H2 H 0.6037 0.1535 0.5711 0.067 Uiso 1 1 calc R . .
C3 C 0.7075(6) -0.0101(4) 0.5692(3) 0.0607(11) Uani 1 1 d . . .
H3 H 0.6833 -0.0509 0.6372 0.073 Uiso 1 1 calc R . .
C4 C 0.7915(5) -0.0725(4) 0.5082(3) 0.0543(10) Uani 1 1 d . . .
H4 H 0.8232 -0.1552 0.5343 0.065 Uiso 1 1 calc R . .
C5 C 0.8274(5) -0.0086(3) 0.4069(2) 0.0418(8) Uani 1 1 d . . .
C6 C 0.9180(5) -0.0611(3) 0.3304(3) 0.0453(8) Uani 1 1 d . . .
C7 C 1.0292(6) -0.0192(4) 0.1574(3) 0.0574(10) Uani 1 1 d . . .
H7A H 0.9363 -0.0611 0.1398 0.069 Uiso 1 1 calc R . .
H7B H 1.1356 -0.0746 0.1743 0.069 Uiso 1 1 calc R . .
C8 C 1.0915(5) 0.0924(4) 0.0718(3) 0.0563(10) Uani 1 1 d . . .
H8A H 1.2026 0.1249 0.0834 0.068 Uiso 1 1 calc R . .
H8B H 1.1219 0.0729 0.0117 0.068 Uiso 1 1 calc R . .
C9 C 0.9708(7) 0.2928(4) -0.0193(3) 0.0702(12) Uani 1 1 d . . .
H9A H 0.9800 0.2785 -0.0816 0.084 Uiso 1 1 calc R . .
H9B H 1.0867 0.3291 -0.0176 0.084 Uiso 1 1 calc R . .
C10 C 0.8070(7) 0.3758(4) -0.0095(3) 0.0691(12) Uani 1 1 d . . .
H10A H 0.8225 0.4543 -0.0628 0.083 Uiso 1 1 calc R . .
H10B H 0.6916 0.3402 -0.0127 0.083 Uiso 1 1 calc R . .
C11 C 0.6370(6) 0.4559(4) 0.1113(3) 0.0580(10) Uani 1 1 d . . .
H11A H 0.5242 0.4152 0.1114 0.070 Uiso 1 1 calc R . .
H11B H 0.6341 0.5386 0.0639 0.070 Uiso 1 1 calc R . .
C12 C 0.6449(6) 0.4592(4) 0.2132(3) 0.0618(11) Uani 1 1 d . . .
H12A H 0.7446 0.5124 0.2105 0.074 Uiso 1 1 calc R . .
H12B H 0.5267 0.4909 0.2375 0.074 Uiso 1 1 calc R . .
C13 C 0.6477(5) 0.3012(3) 0.3733(3) 0.0488(9) Uani 1 1 d . . .
C14 C 0.5662(8) 0.3813(5) 0.4317(4) 0.0783(14) Uani 1 1 d . . .
H14A H 0.5602 0.4647 0.3878 0.117 Uiso 1 1 calc R . .
H14B H 0.6444 0.3756 0.4810 0.117 Uiso 1 1 calc R . .
H14C H 0.4419 0.3548 0.4635 0.117 Uiso 1 1 calc R . .
C15 C 0.9614(7) -0.1960(4) 0.3610(4) 0.0674(12) Uani 1 1 d . . .
H15A H 0.8515 -0.2385 0.3619 0.101 Uiso 1 1 calc R . .
H15B H 0.9989 -0.2246 0.4260 0.101 Uiso 1 1 calc R . .
H15C H 1.0616 -0.2110 0.3147 0.101 Uiso 1 1 calc R . .
C16 C 0.0706(10) 0.5056(5) 0.3559(5) 0.1013(19) Uani 1 1 d . . .
H16A H 0.0480 0.5331 0.4116 0.152 Uiso 1 1 calc R . .
H16B H -0.0268 0.5372 0.3148 0.152 Uiso 1 1 calc R . .
H16C H 0.1902 0.5344 0.3181 0.152 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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
N1 Mn1 N2 71.03(10) . . ?
N1 Mn1 N3 70.80(11) . . ?
N2 Mn1 N3 141.65(11) . . ?
N1 Mn1 O2 142.50(11) . . ?
N2 Mn1 O2 72.29(10) . . ?
N3 Mn1 O2 144.35(11) . . ?
N1 Mn1 O8 90.60(10) . . ?
N2 Mn1 O8 89.02(10) . . ?
N3 Mn1 O8 87.75(11) . . ?
O2 Mn1 O8 81.20(10) . . ?
N1 Mn1 O1 143.64(11) . . ?
N2 Mn1 O1 144.93(11) . . ?
N3 Mn1 O1 72.88(10) . . ?
O2 Mn1 O1 72.65(10) . . ?
O8 Mn1 O1 86.23(10) . . ?
N1 Mn1 Cl2 97.39(7) . . ?
N2 Mn1 Cl2 92.56(8) . . ?
N3 Mn1 Cl2 95.86(8) . . ?
O2 Mn1 Cl2 91.75(7) . . ?
O8 Mn1 Cl2 171.94(8) . . ?
O1 Mn1 Cl2 87.95(7) . . ?
O5 Cl1 O3 115.2(4) . . ?
O5 Cl1 O4 115.3(4) . . ?
O3 Cl1 O4 112.5(4) . . ?
O5 Cl1 O6 106.4(5) . . ?
O3 Cl1 O6 103.0(5) . . ?
O4 Cl1 O6 102.6(5) . . ?
C11 O1 C10 114.9(3) . . ?
C11 O1 Mn1 111.5(2) . . ?
C10 O1 Mn1 111.8(2) . . ?
C9 O2 C8 115.6(3) . . ?
C9 O2 Mn1 112.7(2) . . ?
C8 O2 Mn1 110.5(2) . . ?
C16 O7 H7 109.5 . . ?
Mn1 O8 H8C 109.5 . . ?
Mn1 O8 H8D 133.8 . . ?
H8C O8 H8D 113.1 . . ?
C1 N1 C5 121.4(3) . . ?
C1 N1 Mn1 119.5(2) . . ?
C5 N1 Mn1 119.1(2) . . ?
C6 N2 C7 123.0(3) . . ?
C6 N2 Mn1 120.4(2) . . ?
C7 N2 Mn1 116.2(2) . . ?
C13 N3 C12 123.6(3) . . ?
C13 N3 Mn1 119.7(2) . . ?
C12 N3 Mn1 115.9(2) . . ?
N1 C1 C2 120.8(4) . . ?
N1 C1 C13 113.8(3) . . ?
C2 C1 C13 125.4(3) . . ?
C3 C2 C1 118.6(4) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 120.6(4) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C5 118.3(4) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 120.3(3) . . ?
N1 C5 C6 114.2(3) . . ?
C4 C5 C6 125.5(3) . . ?
N2 C6 C5 115.1(3) . . ?
N2 C6 C15 125.6(4) . . ?
C5 C6 C15 119.3(3) . . ?
N2 C7 C8 109.5(3) . . ?
N2 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
N2 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
O2 C8 C7 107.5(3) . . ?
O2 C8 H8A 110.2 . . ?
C7 C8 H8A 110.2 . . ?
O2 C8 H8B 110.2 . . ?
C7 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
O2 C9 C10 107.0(3) . . ?
O2 C9 H9A 110.3 . . ?
C10 C9 H9A 110.3 . . ?
O2 C9 H9B 110.3 . . ?
C10 C9 H9B 110.3 . . ?
H9A C9 H9B 108.6 . . ?
O1 C10 C9 107.6(3) . . ?
O1 C10 H10A 110.2 . . ?
C9 C10 H10A 110.2 . . ?
O1 C10 H10B 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
O1 C11 C12 108.5(3) . . ?
O1 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
O1 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
N3 C12 C11 108.7(3) . . ?
N3 C12 H12A 109.9 . . ?
C11 C12 H12A 109.9 . . ?
N3 C12 H12B 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
N3 C13 C1 115.4(3) . . ?
N3 C13 C14 125.7(4) . . ?
C1 C13 C14 118.9(4) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 H15A 109.5 . . ?
C6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O7 C16 H16A 109.5 . . ?
O7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
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
Mn1 N1 2.214(3) . ?
Mn1 N2 2.241(3) . ?
Mn1 N3 2.244(3) . ?
Mn1 O2 2.269(3) . ?
Mn1 O8 2.276(3) . ?
Mn1 O1 2.293(2) . ?
Mn1 Cl2 2.5423(10) . ?
Cl1 O5 1.339(5) . ?
Cl1 O3 1.372(4) . ?
Cl1 O4 1.381(5) . ?
Cl1 O6 1.418(7) . ?
O1 C11 1.423(5) . ?
O1 C10 1.433(5) . ?
O2 C9 1.429(5) . ?
O2 C8 1.435(5) . ?
O7 C16 1.383(6) . ?
O7 H7 0.8200 . ?
O8 H8C 0.8200 . ?
O8 H8D 0.8219 . ?
N1 C1 1.328(4) . ?
N1 C5 1.344(4) . ?
N2 C6 1.273(5) . ?
N2 C7 1.463(5) . ?
N3 C13 1.265(5) . ?
N3 C12 1.469(5) . ?
C1 C2 1.389(5) . ?
C1 C13 1.503(5) . ?
C2 C3 1.369(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.384(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.496(5) . ?
C6 C15 1.502(5) . ?
C7 C8 1.490(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.495(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.506(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.506(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
