#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/99/4309903.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_4309903
loop_
_publ_author_name
'Jung Hee Yoon'
'Hyoung Chan Kim'
'Chang Seop Hong'
_publ_section_title
;
Cyanide-Bridged W(V)-Mn(II) Bimetallic Double-Zigzag Chains with a
Metamagnetic Nature
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7714
_journal_page_last               7716
_journal_paper_doi               10.1021/ic051415u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C16 H14 Mn0.5 N8 O3 W'
_chemical_formula_weight         577.67
_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                99.290(4)
_cell_angle_beta                 100.791(4)
_cell_angle_gamma                107.102(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4715(12)
_cell_length_b                   10.5250(15)
_cell_length_c                   11.9813(16)
_cell_measurement_temperature    293(2)
_cell_volume                     976.0(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12476
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    6.262
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             553
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.932
_refine_diff_density_min         -2.594
_refine_diff_density_rms         0.350
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0634
_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)+(0.0939P)²+23.1347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1839
_refine_ls_wR_factor_ref         0.1858
_reflns_number_gt                4221
_reflns_number_total             4525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051415usi20050819_022934.cif
_cod_data_source_block           complex1
_cod_original_formula_sum        'C16 H14 Mn0.50 N8 O3 W'
_cod_database_code               4309903
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
W1 W 0.65378(5) 0.18957(4) 0.27440(3) 0.02455(17) Uani 1 1 d . . .
C1 C 0.6471(16) 0.2085(14) 0.0999(12) 0.038(3) Uani 1 1 d . . .
N1 N 0.6575(18) 0.2215(16) 0.0060(10) 0.053(3) Uani 1 1 d . . .
C2 C 0.8033(15) 0.0815(13) 0.2018(10) 0.030(2) Uani 1 1 d . . .
N2 N 0.8852(14) 0.0274(12) 0.1573(10) 0.038(2) Uani 1 1 d . . .
C3 C 0.5325(16) -0.0199(14) 0.2728(11) 0.038(3) Uani 1 1 d . . .
N3 N 0.4673(19) -0.1325(13) 0.2780(11) 0.054(3) Uani 1 1 d . . .
C4 C 0.5083(14) 0.2056(13) 0.4017(11) 0.033(2) Uani 1 1 d . . .
N4 N 0.4295(17) 0.2164(15) 0.4682(12) 0.051(3) Uani 1 1 d . . .
C5 C 0.5908(16) 0.3733(14) 0.2816(11) 0.037(3) Uani 1 1 d . . .
N5 N 0.5602(17) 0.4737(14) 0.2893(13) 0.051(3) Uani 1 1 d . . .
C6 C 0.3964(15) 0.1230(13) 0.1735(11) 0.035(3) Uani 1 1 d . . .
N6 N 0.2569(14) 0.0914(13) 0.1162(10) 0.043(3) Uani 1 1 d . . .
N7 N 0.9024(12) 0.3564(10) 0.3035(9) 0.032(2) Uani 1 1 d . . .
C7 C 0.9316(16) 0.4475(14) 0.2380(13) 0.040(3) Uani 1 1 d . . .
H7 H 0.8410 0.4472 0.1804 0.048 Uiso 1 1 calc R . .
C8 C 1.0902(17) 0.5420(16) 0.2518(12) 0.042(3) Uani 1 1 d . . .
H8 H 1.1071 0.6027 0.2032 0.050 Uiso 1 1 calc R . .
C9 C 1.2250(19) 0.5446(15) 0.3405(13) 0.048(3) Uani 1 1 d . . .
H9 H 1.3328 0.6091 0.3537 0.058 Uiso 1 1 calc R . .
C10 C 1.1960(15) 0.4516(14) 0.4070(11) 0.038(3) Uani 1 1 d . . .
H10 H 1.2857 0.4511 0.4649 0.045 Uiso 1 1 calc R . .
C11 C 1.0346(14) 0.3569(12) 0.3902(10) 0.030(2) Uani 1 1 d . . .
C12 C 0.9908(14) 0.2608(12) 0.4638(10) 0.030(2) Uani 1 1 d . . .
C13 C 1.1090(16) 0.2537(14) 0.5587(12) 0.038(3) Uani 1 1 d . . .
H13 H 1.2241 0.3040 0.5733 0.046 Uiso 1 1 calc R . .
C14 C 1.0501(18) 0.1699(16) 0.6303(11) 0.044(3) Uani 1 1 d . . .
H14 H 1.1243 0.1713 0.6987 0.052 Uiso 1 1 calc R . .
C15 C 0.890(2) 0.0878(15) 0.6030(10) 0.042(3) Uani 1 1 d . . .
H15 H 0.8553 0.0241 0.6467 0.051 Uiso 1 1 calc R . .
C16 C 0.7727(16) 0.0973(14) 0.5082(10) 0.037(3) Uani 1 1 d . . .
H16 H 0.6580 0.0459 0.4937 0.044 Uiso 1 1 calc R . .
N8 N 0.8243(12) 0.1802(10) 0.4375(9) 0.030(2) Uani 1 1 d . . .
Mn1 Mn 1.0000 0.0000 0.0000 0.0251(5) Uani 1 2 d S . .
O1 O 1.0122(15) -0.1944(11) 0.0256(13) 0.059(3) Uani 1 1 d . . .
O2 O 0.492(4) 0.373(2) 0.8741(17) 0.129(9) Uani 1 1 d . . .
O3 O 0.758(2) 0.5914(17) 0.0367(18) 0.096(5) Uani 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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
C1 W1 C6 69.8(5) . . ?
C1 W1 C3 108.8(5) . . ?
C6 W1 C3 70.7(5) . . ?
C1 W1 C2 70.0(5) . . ?
C6 W1 C2 112.8(5) . . ?
C3 W1 C2 74.5(5) . . ?
C1 W1 C5 80.6(5) . . ?
C6 W1 C5 75.6(5) . . ?
C3 W1 C5 138.4(5) . . ?
C2 W1 C5 142.9(5) . . ?
C1 W1 C4 139.5(5) . . ?
C6 W1 C4 75.7(5) . . ?
C3 W1 C4 78.1(5) . . ?
C2 W1 C4 145.9(4) . . ?
C5 W1 C4 70.5(5) . . ?
C1 W1 N7 80.1(4) . . ?
C6 W1 N7 140.6(4) . . ?
C3 W1 N7 145.7(5) . . ?
C2 W1 N7 78.1(4) . . ?
C5 W1 N7 74.9(4) . . ?
C4 W1 N7 117.3(4) . . ?
C1 W1 N8 142.8(4) . . ?
C6 W1 N8 144.5(4) . . ?
C3 W1 N8 81.8(4) . . ?
C2 W1 N8 79.4(4) . . ?
C5 W1 N8 115.5(4) . . ?
C4 W1 N8 76.9(4) . . ?
N7 W1 N8 73.1(4) . . ?
N1 C1 W1 174.5(12) . . ?
N2 C2 W1 175.9(10) . . ?
C2 N2 Mn1 145.6(10) . . ?
N3 C3 W1 176.6(11) . . ?
N4 C4 W1 178.3(12) . . ?
N5 C5 W1 177.7(12) . . ?
N6 C6 W1 177.1(13) . . ?
C6 N6 Mn1 170.8(12) . 1_455 ?
C7 N7 C11 119.2(10) . . ?
C7 N7 W1 124.1(8) . . ?
C11 N7 W1 116.5(8) . . ?
N7 C7 C8 122.8(12) . . ?
C7 C8 C9 118.5(13) . . ?
C10 C9 C8 118.8(12) . . ?
C9 C10 C11 121.2(13) . . ?
N7 C11 C10 119.4(11) . . ?
N7 C11 C12 116.1(10) . . ?
C10 C11 C12 124.3(11) . . ?
N8 C12 C13 121.0(11) . . ?
N8 C12 C11 116.1(10) . . ?
C13 C12 C11 122.9(10) . . ?
C14 C13 C12 118.1(12) . . ?
C15 C14 C13 121.0(12) . . ?
C14 C15 C16 119.7(13) . . ?
N8 C16 C15 120.8(12) . . ?
C16 N8 C12 118.9(11) . . ?
C16 N8 W1 124.0(8) . . ?
C12 N8 W1 117.1(8) . . ?
O1 Mn1 O1 180.0(6) 2_755 . ?
O1 Mn1 N6 87.3(5) 2_755 2_655 ?
O1 Mn1 N6 92.7(5) . 2_655 ?
O1 Mn1 N6 92.7(5) 2_755 1_655 ?
O1 Mn1 N6 87.3(5) . 1_655 ?
N6 Mn1 N6 180.0(6) 2_655 1_655 ?
O1 Mn1 N2 90.9(5) 2_755 2_755 ?
O1 Mn1 N2 89.1(5) . 2_755 ?
N6 Mn1 N2 90.0(4) 2_655 2_755 ?
N6 Mn1 N2 90.0(4) 1_655 2_755 ?
O1 Mn1 N2 89.1(5) 2_755 . ?
O1 Mn1 N2 90.9(5) . . ?
N6 Mn1 N2 90.0(4) 2_655 . ?
N6 Mn1 N2 90.0(4) 1_655 . ?
N2 Mn1 N2 180.0(5) 2_755 . ?
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
W1 C1 2.124(14) . ?
W1 C6 2.133(12) . ?
W1 C3 2.136(14) . ?
W1 C2 2.143(12) . ?
W1 C5 2.145(14) . ?
W1 C4 2.148(13) . ?
W1 N7 2.235(10) . ?
W1 N8 2.237(10) . ?
C1 N1 1.170(19) . ?
C2 N2 1.167(16) . ?
N2 Mn1 2.293(11) . ?
C3 N3 1.169(18) . ?
C4 N4 1.143(18) . ?
C5 N5 1.153(19) . ?
C6 N6 1.170(17) . ?
N6 Mn1 2.191(10) 1_455 ?
N7 C7 1.331(17) . ?
N7 C11 1.375(15) . ?
C7 C8 1.379(18) . ?
C8 C9 1.40(2) . ?
C9 C10 1.36(2) . ?
C10 C11 1.391(15) . ?
C11 C12 1.459(17) . ?
C12 N8 1.361(14) . ?
C12 C13 1.395(17) . ?
C13 C14 1.38(2) . ?
C14 C15 1.32(2) . ?
C15 C16 1.400(19) . ?
C16 N8 1.350(16) . ?
Mn1 O1 2.146(10) 2_755 ?
Mn1 O1 2.146(10) . ?
Mn1 N6 2.191(10) 2_655 ?
Mn1 N6 2.191(10) 1_655 ?
Mn1 N2 2.293(11) 2_755 ?
