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#$Date: 2016-03-22 11:16:28 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178892 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/21/4112168.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_4112168
loop_
_publ_author_name
'En-Qing Gao'
'Yan-Feng Yue'
'Shi-Qiang Bai'
'Zheng He'
'Chun-Hua Yan'
_publ_contact_author_address
;
State Key Lab of Rare Earth Materials Chemistry and Applications & 
PKU-HKU Joint Lab on Rare Earth Materials and Bioinorganic Chemistry, 
College of Chemistry and Molecular Engineering, 
Peking University, 
Beijing 100871, 
China
;
_publ_contact_author_email       chyan@chem.pku.edu.cn
_publ_contact_author_fax         86-(10)-62754179
_publ_contact_author_name        'Prof. Chun-Hua Yan'
_publ_contact_author_phone       86-(10)-62754179
_publ_section_title
;
 From Achiral Ligands to Chiral Coordination Polymers: Spontaneous
 Resolution, Weak Ferromagnetism, and Topological Ferrimagnetism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1419
_journal_page_last               1429
_journal_paper_doi               10.1021/ja039104a
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C24 H22 Mn3 N28'
_chemical_formula_weight         867.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 127.0816(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.1238(4)
_cell_length_b                   10.8439(3)
_cell_length_c                   12.3532(4)
_cell_measurement_reflns_used    17712
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     1829.98(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'NONIUS KappaCCD Diffractometer'
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14935
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.71
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4137
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0385
_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)+(0.0505P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                3129
_reflns_number_total             4137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039104asi20031017_103420_2.cif
_cod_data_source_block           1
_cod_database_code               4112168
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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
Mn1 Mn 0.88867(3) 0.67209(3) 0.47287(5) 0.03769(14) Uani 1 1 d .
Mn2 Mn 1.0000 1.14072(5) 0.5000 0.0424(2) Uani 1 2 d S
N1 N 0.86921(18) 0.7161(2) 0.6353(3) 0.0397(6) Uani 1 1 d .
N2 N 0.88309(19) 0.8826(2) 0.4902(3) 0.0361(6) Uani 1 1 d .
N3 N 0.89101(18) 0.9734(2) 0.4155(3) 0.0359(6) Uani 1 1 d .
N4 N 0.9308(2) 1.1211(3) 0.2791(3) 0.0534(7) Uani 1 1 d .
N5 N 0.8410(2) 1.0420(2) 0.5716(3) 0.0521(7) Uani 1 1 d .
H5A H 0.8400 1.0956 0.5196 0.063 Uiso 1 1 calc R
H5B H 0.8279 1.0640 0.6260 0.063 Uiso 1 1 calc R
N6 N 0.94877(18) 0.6677(3) 0.3593(3) 0.0493(7) Uani 1 1 d .
N7 N 0.9150(2) 0.6713(5) 0.2437(4) 0.0837(12) Uani 1 1 d .
N8 N 0.8837(3) 0.6855(8) 0.1299(5) 0.142(2) Uani 1 1 d .
N9 N 0.73307(19) 0.6767(3) 0.3014(3) 0.0449(6) Uani 1 1 d .
N10 N 0.6798(2) 0.7623(3) 0.2573(3) 0.0506(7) Uani 1 1 d .
N11 N 0.6262(3) 0.8450(4) 0.2094(5) 0.0938(14) Uani 1 1 d .
N12 N 0.8914(2) 1.2661(3) 0.4679(4) 0.0681(10) Uani 1 1 d .
N13 N 0.8840(2) 1.3711(3) 0.4786(3) 0.0481(8) Uani 1 1 d .
N14 N 0.8738(3) 1.4743(3) 0.4907(4) 0.0674(10) Uani 1 1 d .
C1 C 0.8743(2) 0.6323(3) 0.7188(4) 0.0491(8) Uani 1 1 d .
H1A H 0.8789 0.5496 0.7034 0.059 Uiso 1 1 calc R
C2 C 0.8730(3) 0.6614(4) 0.8261(3) 0.0589(9) Uani 1 1 d .
H2A H 0.8762 0.6000 0.8812 0.071 Uiso 1 1 calc R
C3 C 0.8669(3) 0.7836(4) 0.8498(4) 0.0641(11) Uani 1 1 d .
H3A H 0.8660 0.8062 0.9217 0.077 Uiso 1 1 calc R
C4 C 0.8622(3) 0.8728(4) 0.7655(4) 0.0563(10) Uani 1 1 d .
H4A H 0.8576 0.9560 0.7793 0.068 Uiso 1 1 calc R
C5 C 0.8644(2) 0.8355(3) 0.6616(3) 0.0376(7) Uani 1 1 d .
C6 C 0.8623(2) 0.9265(3) 0.5680(3) 0.0350(7) Uani 1 1 d .
C7 C 0.8544(3) 0.9456(3) 0.2930(4) 0.0459(8) Uani 1 1 d .
H7A H 0.8191 0.8729 0.2554 0.055 Uiso 1 1 calc R
C8 C 0.8678(3) 1.0272(4) 0.2121(4) 0.0502(8) Uani 1 1 d .
C9 C 0.8197(3) 1.0058(5) 0.0770(4) 0.0747(12) Uani 1 1 d .
H9A H 0.7774 0.9389 0.0352 0.090 Uiso 1 1 calc R
C10 C 0.8344(4) 1.0841(6) 0.0035(5) 0.0926(16) Uani 1 1 d .
H10A H 0.8013 1.0723 -0.0892 0.111 Uiso 1 1 calc R
C11 C 0.8982(4) 1.1792(6) 0.0686(5) 0.0916(16) Uani 1 1 d .
H11A H 0.9103 1.2322 0.0212 0.110 Uiso 1 1 calc R
C12 C 0.9459(3) 1.1972(5) 0.2086(5) 0.0772(13) Uani 1 1 d .
H12A H 0.9887 1.2633 0.2524 0.093 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'
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
N6 Mn1 N14 99.91(13) . 1_545
N6 Mn1 N9 98.56(10) . .
N14 Mn1 N9 88.39(13) 1_545 .
N6 Mn1 N6 77.99(11) . 2_756
N14 Mn1 N6 92.35(13) 1_545 2_756
N9 Mn1 N6 176.55(10) . 2_756
N6 Mn1 N1 161.40(10) . .
N14 Mn1 N1 91.67(13) 1_545 .
N9 Mn1 N1 96.25(9) . .
N6 Mn1 N1 87.10(9) 2_756 .
N6 Mn1 N2 98.25(11) . .
N14 Mn1 N2 161.84(10) 1_545 .
N9 Mn1 N2 88.45(11) . .
N6 Mn1 N2 91.88(11) 2_756 .
N1 Mn1 N2 70.92(10) . .
N12 Mn2 N12 101.06(18) 2_756 .
N12 Mn2 N4 92.79(12) 2_756 .
N12 Mn2 N4 94.15(12) . .
N12 Mn2 N4 94.15(12) 2_756 2_756
N12 Mn2 N4 92.79(12) . 2_756
N4 Mn2 N4 169.07(16) . 2_756
N12 Mn2 N3 160.50(11) 2_756 .
N12 Mn2 N3 92.27(11) . .
N4 Mn2 N3 71.91(10) . .
N4 Mn2 N3 99.40(10) 2_756 .
N12 Mn2 N3 92.27(11) 2_756 2_756
N12 Mn2 N3 160.50(11) . 2_756
N4 Mn2 N3 99.40(10) . 2_756
N4 Mn2 N3 71.91(10) 2_756 2_756
N3 Mn2 N3 78.84(12) . 2_756
C1 N1 C5 116.9(3) . .
C1 N1 Mn1 124.2(2) . .
C5 N1 Mn1 118.4(2) . .
C6 N2 N3 113.9(2) . .
C6 N2 Mn1 118.5(2) . .
N3 N2 Mn1 127.3(2) . .
C7 N3 N2 116.0(3) . .
C7 N3 Mn2 113.5(2) . .
N2 N3 Mn2 127.8(2) . .
C12 N4 C8 117.8(4) . .
C12 N4 Mn2 124.7(3) . .
C8 N4 Mn2 117.5(2) . .
N7 N6 Mn1 134.6(2) . .
N7 N6 Mn1 123.2(2) . 2_756
Mn1 N6 Mn1 101.96(11) . 2_756
N6 N7 N8 174.1(7) . .
N10 N9 Mn1 128.0(2) . .
N11 N10 N9 177.6(4) . .
N13 N12 Mn2 138.1(3) . .
N14 N13 N12 176.9(4) . .
N13 N14 Mn1 154.2(3) . 1_565
N1 C1 C2 123.7(3) . .
C3 C2 C1 118.3(3) . .
C2 C3 C4 119.3(3) . .
C5 C4 C3 118.4(4) . .
N1 C5 C4 123.3(3) . .
N1 C5 C6 114.9(3) . .
C4 C5 C6 121.8(3) . .
N2 C6 N5 125.4(3) . .
N2 C6 C5 116.0(3) . .
N5 C6 C5 118.6(3) . .
N3 C7 C8 120.3(3) . .
N4 C8 C9 123.5(4) . .
N4 C8 C7 116.0(3) . .
C9 C8 C7 120.5(4) . .
C8 C9 C10 119.2(5) . .
C11 C10 C9 118.7(5) . .
C10 C11 C12 119.8(4) . .
N4 C12 C11 121.1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N6 2.185(2) .
Mn1 N14 2.187(3) 1_545
Mn1 N9 2.187(3) .
Mn1 N6 2.256(3) 2_756
Mn1 N1 2.274(3) .
Mn1 N2 2.300(3) .
Mn2 N12 2.140(3) 2_756
Mn2 N12 2.140(3) .
Mn2 N4 2.235(3) .
Mn2 N4 2.235(3) 2_756
Mn2 N3 2.348(2) .
Mn2 N3 2.348(2) 2_756
N1 C1 1.338(4) .
N1 C5 1.350(4) .
N2 C6 1.300(4) .
N2 N3 1.411(4) .
N3 C7 1.278(4) .
N4 C12 1.334(5) .
N4 C8 1.344(5) .
N5 C6 1.313(4) .
N6 N7 1.173(4) .
N6 Mn1 2.256(3) 2_756
N7 N8 1.175(5) .
N9 N10 1.180(4) .
N10 N11 1.158(5) .
N12 N13 1.161(4) .
N13 N14 1.156(4) .
N14 Mn1 2.187(3) 1_565
C1 C2 1.376(5) .
C2 C3 1.374(6) .
C3 C4 1.388(6) .
C4 C5 1.369(5) .
C5 C6 1.502(4) .
C7 C8 1.452(5) .
C8 C9 1.363(6) .
C9 C10 1.374(7) .
C10 C11 1.357(8) .
C11 C12 1.411(6) .
