#------------------------------------------------------------------------------
#$Date: 2019-11-25 00:51:48 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239810 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/02/4350250.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_4350250
loop_
_publ_author_name
'Tao, Jun'
'Zhang, Yuan-Zhu'
'Bai, Yue-Lin'
'Sato, Osamu'
_publ_section_title
;
 One-dimensional ferromagnetic complexes built with Mn(III)3O units.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4877
_journal_page_last               4879
_journal_paper_doi               10.1021/ic060159y
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C32 H33 Mn3 N6 O9'
_chemical_formula_weight         810.46
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.78(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.309(4)
_cell_length_b                   7.6251(15)
_cell_length_c                   21.554(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3336.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6555
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    1.182
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.0028(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0502
_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)+(0.1124P)²+0.3040P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1559
_reflns_number_gt                5911
_reflns_number_total             6555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060159ysi20060127_093058.cif
_cod_data_source_block           complex_1
_cod_original_cell_volume        3336.2(12)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4350250
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Mn1 Mn 0.181719(18) 0.05752(5) 0.108078(17) 0.02550(15) Uani 1 1 d .
Mn2 Mn 0.223720(18) 0.30009(5) -0.010999(17) 0.02618(15) Uani 1 1 d .
Mn3 Mn 0.338222(18) 0.14451(5) 0.085411(17) 0.02743(15) Uani 1 1 d .
O4 O 0.24729(8) 0.1787(2) 0.06390(8) 0.0257(4) Uani 1 1 d .
O1 O 0.11863(9) -0.0077(3) 0.16329(8) 0.0334(4) Uani 1 1 d .
N1 N 0.11295(10) 0.1729(3) 0.05811(10) 0.0277(4) Uani 1 1 d .
N2 N 0.12882(11) 0.2768(3) 0.00900(10) 0.0288(5) Uani 1 1 d .
C1 C 0.05246(13) -0.0284(3) 0.15526(12) 0.0298(5) Uani 1 1 d .
C2 C 0.02119(14) -0.1403(4) 0.19679(13) 0.0374(6) Uani 1 1 d .
H2A H 0.0460 -0.1996 0.2271 0.045 Uiso 1 1 calc R
C3 C -0.04620(16) -0.1628(4) 0.19295(15) 0.0435(7) Uani 1 1 d .
H3A H -0.0665 -0.2373 0.2207 0.052 Uiso 1 1 calc R
C4 C -0.08411(15) -0.0747(5) 0.14789(15) 0.0462(7) Uani 1 1 d .
H4A H -0.1296 -0.0885 0.1459 0.055 Uiso 1 1 calc R
C5 C -0.05349(14) 0.0331(4) 0.10629(14) 0.0396(7) Uani 1 1 d .
H5A H -0.0789 0.0910 0.0760 0.048 Uiso 1 1 calc R
C6 C 0.01493(13) 0.0576(3) 0.10851(12) 0.0309(6) Uani 1 1 d .
C7 C 0.04653(13) 0.1654(3) 0.06173(12) 0.0302(5) Uani 1 1 d .
C8 C 0.01940(13) 0.2676(4) 0.01396(14) 0.0363(6) Uani 1 1 d .
H8A H -0.0251 0.2877 0.0050 0.044 Uiso 1 1 calc R
C9 C 0.07237(14) 0.3331(4) -0.01736(14) 0.0357(6) Uani 1 1 d .
H9A H 0.0692 0.4061 -0.0519 0.043 Uiso 1 1 calc R
O2 O 0.19947(9) 0.4157(3) -0.08307(9) 0.0351(4) Uani 1 1 d .
N3 N 0.31610(10) 0.3292(3) -0.03113(10) 0.0269(4) Uani 1 1 d .
N4 N 0.36444(11) 0.2591(3) 0.00632(10) 0.0305(5) Uani 1 1 d .
C10 C 0.23407(13) 0.4930(3) -0.12755(12) 0.0294(5) Uani 1 1 d .
C11 C 0.19764(14) 0.5816(4) -0.17405(13) 0.0346(6) Uani 1 1 d .
H11A H 0.1519 0.5827 -0.1731 0.041 Uiso 1 1 calc R
C12 C 0.22886(15) 0.6674(4) -0.22139(12) 0.0366(6) Uani 1 1 d .
H12A H 0.2040 0.7273 -0.2515 0.044 Uiso 1 1 calc R
C13 C 0.29675(15) 0.6648(4) -0.22421(13) 0.0365(6) Uani 1 1 d .
H13A H 0.3176 0.7217 -0.2563 0.044 Uiso 1 1 calc R
C14 C 0.33351(14) 0.5766(4) -0.17872(12) 0.0341(6) Uani 1 1 d .
H14A H 0.3792 0.5748 -0.1808 0.041 Uiso 1 1 calc R
C15 C 0.30334(13) 0.4901(3) -0.12968(11) 0.0288(5) Uani 1 1 d .
C16 C 0.34408(13) 0.4020(3) -0.08161(11) 0.0286(5) Uani 1 1 d .
C17 C 0.41215(14) 0.3782(4) -0.07571(13) 0.0366(6) Uani 1 1 d .
H17A H 0.4439 0.4144 -0.1031 0.044 Uiso 1 1 calc R
C18 C 0.42203(14) 0.2892(4) -0.02035(14) 0.0385(7) Uani 1 1 d .
H18A H 0.4629 0.2550 -0.0039 0.046 Uiso 1 1 calc R
O3 O 0.42647(9) 0.1217(3) 0.10846(9) 0.0368(5) Uani 1 1 d .
N5 N 0.31414(11) 0.0197(3) 0.16026(10) 0.0305(5) Uani 1 1 d .
N6 N 0.24955(11) -0.0103(3) 0.17230(10) 0.0323(5) Uani 1 1 d .
C19 C 0.45752(14) 0.0335(4) 0.15468(12) 0.0321(6) Uani 1 1 d .
C20 C 0.52645(15) 0.0313(4) 0.15500(14) 0.0406(7) Uani 1 1 d .
H20A H 0.5484 0.0931 0.1247 0.049 Uiso 1 1 calc R
C21 C 0.56250(15) -0.0613(5) 0.19960(16) 0.0460(8) Uani 1 1 d .
H21A H 0.6083 -0.0629 0.1988 0.055 Uiso 1 1 calc R
C22 C 0.53019(17) -0.1521(4) 0.24572(17) 0.0502(8) Uani 1 1 d .
H22A H 0.5541 -0.2167 0.2753 0.060 Uiso 1 1 calc R
C23 C 0.46217(15) -0.1454(4) 0.24721(14) 0.0410(7) Uani 1 1 d .
H23A H 0.4408 -0.2028 0.2789 0.049 Uiso 1 1 calc R
C24 C 0.42480(14) -0.0540(3) 0.20200(12) 0.0329(6) Uani 1 1 d .
C25 C 0.35267(14) -0.0571(3) 0.20428(13) 0.0327(6) Uani 1 1 d .
C26 C 0.31124(15) -0.1405(4) 0.24596(14) 0.0407(7) Uani 1 1 d .
H26A H 0.3239 -0.2050 0.2810 0.049 Uiso 1 1 calc R
C27 C 0.24781(15) -0.1071(4) 0.22429(13) 0.0395(7) Uani 1 1 d .
H27A H 0.2097 -0.1457 0.2428 0.047 Uiso 1 1 calc R
O5 O 0.19059(11) -0.1681(2) 0.05113(9) 0.0380(5) Uani 1 1 d .
O6 O 0.24073(11) -0.4230(3) 0.04608(11) 0.0433(5) Uani 1 1 d .
C28 C 0.14727(19) -0.4013(4) 0.11031(17) 0.0521(8) Uani 1 1 d .
H28A H 0.1568 -0.5230 0.1176 0.078 Uiso 1 1 calc R
H28B H 0.1035 -0.3897 0.0927 0.078 Uiso 1 1 calc R
H28C H 0.1505 -0.3384 0.1489 0.078 Uiso 1 1 calc R
C29 C 0.19586(14) -0.3273(3) 0.06603(13) 0.0323(6) Uani 1 1 d .
O7 O 0.22029(10) 0.0316(2) -0.05630(8) 0.0337(4) Uani 1 1 d .
H7 H 0.2194 -0.0471 -0.0284 0.040 Uiso 1 1 d R
C30 C 0.26645(17) -0.0177(4) -0.10246(14) 0.0448(7) Uani 1 1 d .
H30A H 0.2575 -0.1355 -0.1160 0.067 Uiso 1 1 calc R
H30B H 0.3104 -0.0113 -0.0850 0.067 Uiso 1 1 calc R
H30C H 0.2623 0.0606 -0.1372 0.067 Uiso 1 1 calc R
O8 O 0.33765(10) -0.1290(3) 0.03508(10) 0.0412(5) Uani 1 1 d .
H8 H 0.3131 -0.2039 0.0522 0.049 Uiso 1 1 d R
C31 C 0.39413(17) -0.2054(5) 0.00905(18) 0.0540(9) Uani 1 1 d .
H31A H 0.3826 -0.3167 -0.0091 0.081 Uiso 1 1 calc R
H31B H 0.4276 -0.2220 0.0410 0.081 Uiso 1 1 calc R
H31C H 0.4105 -0.1292 -0.0224 0.081 Uiso 1 1 calc R
O9 O 0.32981(10) 0.4087(3) 0.13098(9) 0.0374(4) Uani 1 1 d .
H9 H 0.3061 0.4720 0.1067 0.045 Uiso 1 1 d R
C32 C 0.38420(19) 0.5141(5) 0.15173(19) 0.0562(9) Uani 1 1 d .
H32A H 0.3682 0.6208 0.1695 0.084 Uiso 1 1 calc R
H32B H 0.4111 0.5416 0.1172 0.084 Uiso 1 1 calc R
H32C H 0.4099 0.4510 0.1824 0.084 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'
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_3
O1 Mn1 O4 165.04(8) .
O1 Mn1 N1 88.74(9) .
O4 Mn1 N1 90.28(8) .
O1 Mn1 N6 87.76(9) .
O4 Mn1 N6 89.67(8) .
N1 Mn1 N6 166.18(9) .
O1 Mn1 O5 103.15(8) .
O4 Mn1 O5 91.78(8) .
N1 Mn1 O5 96.80(9) .
N6 Mn1 O5 97.02(9) .
O2 Mn2 O4 178.97(8) .
O2 Mn2 N3 89.53(9) .
O4 Mn2 N3 91.46(8) .
O2 Mn2 N2 89.43(9) .
O4 Mn2 N2 89.58(8) .
N3 Mn2 N2 178.53(9) .
O2 Mn2 O7 93.73(9) .
O4 Mn2 O7 86.00(7) .
N3 Mn2 O7 91.36(8) .
N2 Mn2 O7 89.74(8) .
O2 Mn2 O6 92.34(9) 1_565
O4 Mn2 O6 88.02(8) 1_565
N3 Mn2 O6 83.84(8) 1_565
N2 Mn2 O6 95.16(8) 1_565
O7 Mn2 O6 172.23(7) 1_565
O3 Mn3 O4 177.15(9) .
O3 Mn3 N5 89.87(9) .
O4 Mn3 N5 90.12(9) .
O3 Mn3 N4 89.35(9) .
O4 Mn3 N4 90.83(8) .
N5 Mn3 N4 176.61(10) .
O3 Mn3 O9 93.04(9) .
O4 Mn3 O9 84.12(7) .
N5 Mn3 O9 92.95(9) .
N4 Mn3 O9 90.39(8) .
O3 Mn3 O8 91.79(9) .
O4 Mn3 O8 91.05(7) .
N5 Mn3 O8 87.19(9) .
N4 Mn3 O8 89.53(9) .
O9 Mn3 O8 175.17(7) .
Mn1 O4 Mn3 119.97(9) .
Mn1 O4 Mn2 119.88(9) .
Mn3 O4 Mn2 119.16(9) .
C1 O1 Mn1 130.80(16) .
C7 N1 N2 109.1(2) .
C7 N1 Mn1 130.36(18) .
N2 N1 Mn1 120.48(16) .
C9 N2 N1 107.2(2) .
C9 N2 Mn2 134.57(19) .
N1 N2 Mn2 118.08(16) .
O1 C1 C2 117.0(2) .
O1 C1 C6 123.3(2) .
C2 C1 C6 119.7(3) .
C3 C2 C1 120.3(3) .
C2 C3 C4 120.5(3) .
C5 C4 C3 119.4(3) .
C4 C5 C6 121.6(3) .
C5 C6 C1 118.5(2) .
C5 C6 C7 120.4(3) .
C1 C6 C7 121.0(2) .
N1 C7 C8 107.8(2) .
N1 C7 C6 121.5(2) .
C8 C7 C6 130.7(3) .
C9 C8 C7 105.5(2) .
N2 C9 C8 110.3(2) .
C10 O2 Mn2 132.92(17) .
C16 N3 N4 108.8(2) .
C16 N3 Mn2 130.70(18) .
N4 N3 Mn2 120.29(17) .
C18 N4 N3 107.6(2) .
C18 N4 Mn3 134.37(19) .
N3 N4 Mn3 118.05(17) .
O2 C10 C11 116.5(2) .
O2 C10 C15 124.2(2) .
C11 C10 C15 119.3(2) .
C12 C11 C10 120.8(3) .
C13 C12 C11 120.4(3) .
C12 C13 C14 119.4(3) .
C13 C14 C15 121.5(3) .
C14 C15 C10 118.5(2) .
C14 C15 C16 119.8(2) .
C10 C15 C16 121.7(2) .
N3 C16 C17 108.1(2) .
N3 C16 C15 120.7(2) .
C17 C16 C15 131.2(2) .
C18 C17 C16 105.0(2) .
N4 C18 C17 110.5(3) .
C19 O3 Mn3 132.36(18) .
C25 N5 N6 109.5(2) .
C25 N5 Mn3 129.89(19) .
N6 N5 Mn3 120.45(17) .
C27 N6 N5 107.5(2) .
C27 N6 Mn1 133.4(2) .
N5 N6 Mn1 118.22(17) .
O3 C19 C20 117.1(3) .
O3 C19 C24 123.7(2) .
C20 C19 C24 119.1(2) .
C21 C20 C19 121.1(3) .
C20 C21 C22 119.9(3) .
C23 C22 C21 119.4(3) .
C22 C23 C24 121.4(3) .
C19 C24 C23 118.9(3) .
C19 C24 C25 121.8(2) .
C23 C24 C25 119.2(3) .
N5 C25 C26 107.6(3) .
N5 C25 C24 121.9(2) .
C26 C25 C24 130.4(3) .
C27 C26 C25 105.8(2) .
N6 C27 C26 109.6(3) .
C29 O5 Mn1 129.89(18) .
C29 O6 Mn2 125.32(19) 1_545
O6 C29 O5 122.0(3) .
O6 C29 C28 119.9(3) .
O5 C29 C28 118.1(3) .
C30 O7 Mn2 121.46(18) .
C31 O8 Mn3 123.7(2) .
C32 O9 Mn3 124.9(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 1.8438(19) .
Mn1 O4 1.9008(18) .
Mn1 N1 1.947(2) .
Mn1 N6 1.991(2) .
Mn1 O5 2.1243(19) .
Mn2 O2 1.8399(19) .
Mn2 O4 1.9089(18) .
Mn2 N3 1.951(2) .
Mn2 N2 1.996(2) .
Mn2 O7 2.2684(19) .
Mn2 O6 2.463(2) 1_565
Mn3 O3 1.853(2) .
Mn3 O4 1.9079(18) .
Mn3 N5 1.949(2) .
Mn3 N4 2.002(2) .
Mn3 O9 2.250(2) .
Mn3 O8 2.351(2) .
O1 C1 1.359(3) .
N1 C7 1.355(3) .
N1 N2 1.369(3) .
N2 C9 1.335(4) .
C1 C2 1.403(4) .
C1 C6 1.407(4) .
C2 C3 1.379(4) .
C3 C4 1.393(5) .
C4 C5 1.379(4) .
C5 C6 1.401(4) .
C6 C7 1.464(4) .
C7 C8 1.392(4) .
C8 C9 1.381(4) .
O2 C10 1.342(3) .
N3 C16 1.361(3) .
N3 N4 1.361(3) .
N4 C18 1.339(4) .
C10 C11 1.401(4) .
C10 C15 1.409(4) .
C11 C12 1.383(4) .
C12 C13 1.382(4) .
C13 C14 1.388(4) .
C14 C15 1.403(4) .
C15 C16 1.469(4) .
C16 C17 1.396(4) .
C17 C18 1.382(4) .
O3 C19 1.343(3) .
N5 C25 1.345(3) .
N5 N6 1.364(3) .
N6 C27 1.343(4) .
C19 C20 1.400(4) .
C19 C24 1.403(4) .
C20 C21 1.384(4) .
C21 C22 1.392(5) .
C22 C23 1.384(5) .
C23 C24 1.402(4) .
C24 C25 1.468(4) .
C25 C26 1.402(4) .
C26 C27 1.380(4) .
O5 C29 1.260(3) .
O6 C29 1.254(3) .
O6 Mn2 2.463(2) 1_545
C28 C29 1.503(4) .
O7 C30 1.438(3) .
O8 C31 1.418(4) .
O9 C32 1.427(4) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7 O5 0.85 2.05 2.851(3) 157.4 .
O8 H8 O6 0.85 2.23 2.997(3) 150.9 .
O9 H9 O6 0.85 2.00 2.839(3) 168.7 1_565
