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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/4/11/21/4112169.cif $
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#
# 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_4112169
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 H24 Cl Mn2 N21 O5'
_chemical_formula_weight         831.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4368(3)
_cell_length_b                   14.5844(3)
_cell_length_c                   17.5169(4)
_cell_measurement_reflns_used    63162
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     3688.22(14)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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        27.49
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.71
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.0217(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         8384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0972P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                3129
_reflns_number_total             4137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039104asi20031017_103420_3.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 2 2 2'
_cod_database_code               4112169
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'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 0.84066(5) 0.12085(5) 0.54250(4) 0.0652(2) Uani 1 1 d .
Mn2 Mn 0.67628(5) -0.08432(5) 0.39096(4) 0.0661(2) Uani 1 1 d .
N1 N 0.7101(3) 0.1912(3) 0.5913(2) 0.0690(10) Uani 1 1 d .
N2 N 0.7229(3) 0.0151(2) 0.5529(2) 0.0618(9) Uani 1 1 d .
N3 N 0.7234(3) -0.0698(2) 0.5141(2) 0.0622(9) Uani 1 1 d .
N4 N 0.7677(3) -0.2087(3) 0.4217(2) 0.0702(10) Uani 1 1 d .
N5 N 0.5608(3) 0.0026(3) 0.5470(3) 0.0846(13) Uani 1 1 d .
H5A H 0.5629 -0.0514 0.5274 0.102 Uiso 1 1 calc R
H5B H 0.5082 0.0281 0.5558 0.102 Uiso 1 1 calc R
N6 N 0.8435(3) -0.1103(3) 0.5968(2) 0.0826(12) Uani 1 1 d .
H6A H 0.8382 -0.0612 0.6237 0.099 Uiso 1 1 calc R
H6B H 0.8848 -0.1505 0.6083 0.099 Uiso 1 1 calc R
N7 N 0.9807(3) 0.0545(3) 0.5181(2) 0.0685(10) Uani 1 1 d .
N8 N 0.8390(3) 0.0648(3) 0.42145(19) 0.0637(9) Uani 1 1 d .
N9 N 0.7549(3) 0.0480(3) 0.3818(2) 0.0648(9) Uani 1 1 d .
N10 N 0.5794(3) 0.0282(3) 0.3408(2) 0.0719(11) Uani 1 1 d .
N11 N 0.9047(3) -0.0483(3) 0.3436(2) 0.0802(12) Uani 1 1 d .
H11B H 0.8560 -0.0532 0.3157 0.096 Uiso 1 1 calc R
H11C H 0.9525 -0.0816 0.3343 0.096 Uiso 1 1 calc R
N12 N 0.7432(4) 0.2058(3) 0.3740(3) 0.0976(15) Uani 1 1 d .
H12B H 0.7964 0.2132 0.3952 0.117 Uiso 1 1 calc R
H12C H 0.7112 0.2528 0.3603 0.117 Uiso 1 1 calc R
N13 N 0.8939(5) 0.2481(4) 0.5093(4) 0.119(2) Uani 1 1 d .
N14 N 0.8903(3) 0.3277(3) 0.5047(3) 0.0835(12) Uani 1 1 d .
N15 N 0.8859(4) 0.4056(3) 0.4949(5) 0.135(3) Uani 1 1 d .
N16 N 0.5540(4) -0.1596(4) 0.4158(4) 0.1011(16) Uani 1 1 d .
N17 N 0.5459(3) -0.2376(3) 0.4277(3) 0.0864(14) Uani 1 1 d .
N18 N 0.5339(5) -0.3128(4) 0.4390(6) 0.152(3) Uani 1 1 d .
N19 N 0.7076(4) -0.1229(4) 0.2720(3) 0.0939(15) Uani 1 1 d .
N20 N 0.6644(3) -0.1107(3) 0.2175(3) 0.0713(10) Uani 1 1 d .
N21 N 0.6201(3) -0.0975(4) 0.1636(3) 0.0912(13) Uani 1 1 d .
C1 C 0.7107(5) 0.2730(3) 0.6261(3) 0.0873(16) Uani 1 1 d .
H1A H 0.7631 0.3097 0.6215 0.105 Uiso 1 1 calc R
C2 C 0.6380(5) 0.3051(4) 0.6679(3) 0.097(2) Uani 1 1 d .
H2A H 0.6416 0.3622 0.6914 0.116 Uiso 1 1 calc R
C3 C 0.5590(5) 0.2524(5) 0.6753(4) 0.105(2) Uani 1 1 d .
H3A H 0.5089 0.2729 0.7039 0.126 Uiso 1 1 calc R
C4 C 0.5564(4) 0.1678(4) 0.6386(4) 0.0920(17) Uani 1 1 d .
H4A H 0.5036 0.1313 0.6408 0.110 Uiso 1 1 calc R
C5 C 0.6326(3) 0.1393(3) 0.5995(3) 0.0662(11) Uani 1 1 d .
C6 C 0.6399(3) 0.0472(3) 0.5639(3) 0.0637(11) Uani 1 1 d .
C7 C 0.7879(3) -0.1239(3) 0.5376(3) 0.0648(11) Uani 1 1 d .
C8 C 0.7985(3) -0.2117(3) 0.4933(3) 0.0652(11) Uani 1 1 d .
C9 C 0.8356(4) -0.2902(3) 0.5263(3) 0.0723(12) Uani 1 1 d .
H9A H 0.8548 -0.2909 0.5769 0.087 Uiso 1 1 calc R
C10 C 0.8429(4) -0.3674(3) 0.4806(4) 0.0856(15) Uani 1 1 d .
H10A H 0.8676 -0.4212 0.5005 0.103 Uiso 1 1 calc R
C11 C 0.8150(4) -0.3648(3) 0.4096(4) 0.0910(17) Uani 1 1 d .
H11A H 0.8214 -0.4166 0.3791 0.109 Uiso 1 1 calc R
C12 C 0.7756(4) -0.2848(4) 0.3785(4) 0.0874(16) Uani 1 1 d .
H12A H 0.7550 -0.2844 0.3283 0.105 Uiso 1 1 calc R
C13 C 1.0566(4) 0.0629(4) 0.5607(3) 0.0792(14) Uani 1 1 d .
H13A H 1.0497 0.0840 0.6105 0.095 Uiso 1 1 calc R
C14 C 1.1435(4) 0.0428(4) 0.5361(3) 0.0863(15) Uani 1 1 d .
H14A H 1.1946 0.0525 0.5675 0.104 Uiso 1 1 calc R
C15 C 1.1540(4) 0.0089(5) 0.4660(4) 0.0917(16) Uani 1 1 d .
H15A H 1.2129 -0.0058 0.4484 0.110 Uiso 1 1 calc R
C16 C 1.0774(4) -0.0049(4) 0.4189(3) 0.0797(14) Uani 1 1 d .
H16A H 1.0839 -0.0291 0.3701 0.096 Uiso 1 1 calc R
C17 C 0.9921(3) 0.0185(3) 0.4470(3) 0.0656(11) Uani 1 1 d .
C18 C 0.9061(3) 0.0108(3) 0.4014(3) 0.0643(11) Uani 1 1 d .
C19 C 0.7108(4) 0.1232(3) 0.3627(3) 0.0692(12) Uani 1 1 d .
C20 C 0.6178(4) 0.1113(4) 0.3317(3) 0.0752(13) Uani 1 1 d .
C21 C 0.5701(5) 0.1803(4) 0.2945(4) 0.0936(18) Uani 1 1 d .
H21A H 0.5968 0.2380 0.2889 0.112 Uiso 1 1 calc R
C22 C 0.4806(5) 0.1633(5) 0.2648(4) 0.107(2) Uani 1 1 d .
H22A H 0.4477 0.2086 0.2392 0.128 Uiso 1 1 calc R
C23 C 0.4446(5) 0.0780(5) 0.2754(4) 0.104(2) Uani 1 1 d .
H23A H 0.3859 0.0646 0.2565 0.125 Uiso 1 1 calc R
C24 C 0.4933(4) 0.0114(4) 0.3134(4) 0.0951(17) Uani 1 1 d .
H24A H 0.4668 -0.0461 0.3205 0.114 Uiso 1 1 calc R
O1 O 0.7624(8) 0.3622(11) 0.1844(5) 0.333(9) Uani 1 1 d .
O2 O 0.6875(4) 0.3843(3) 0.2911(3) 0.1278(18) Uani 1 1 d .
O3 O 0.7761(6) 0.4958(5) 0.2379(6) 0.211(4) Uani 1 1 d .
O4 O 0.8420(6) 0.3761(10) 0.2842(8) 0.290(7) Uani 1 1 d .
O5 O 1.0304(5) -0.2118(5) 0.3577(7) 0.212(4) Uani 1 1 d .
Cl1 Cl 0.76623(11) 0.40387(10) 0.24796(9) 0.0899(4) 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'
Mn Mn 0.3368 0.7283 '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'
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
N13 Mn1 N21 108.0(3) . 2_655
N13 Mn1 N8 93.6(2) . .
N21 Mn1 N8 146.99(17) 2_655 .
N13 Mn1 N7 89.9(2) . .
N21 Mn1 N7 83.60(17) 2_655 .
N8 Mn1 N7 71.45(15) . .
N13 Mn1 N2 152.6(2) . .
N21 Mn1 N2 90.56(18) 2_655 .
N8 Mn1 N2 79.93(14) . .
N7 Mn1 N2 112.62(13) . .
N13 Mn1 N1 90.5(2) . .
N21 Mn1 N1 85.57(17) 2_655 .
N8 Mn1 N1 119.74(15) . .
N7 Mn1 N1 168.75(14) . .
N2 Mn1 N1 70.46(13) . .
N16 Mn2 N19 103.4(2) . .
N16 Mn2 N9 151.59(18) . .
N19 Mn2 N9 92.76(18) . .
N16 Mn2 N3 95.9(2) . .
N19 Mn2 N3 149.27(17) . .
N9 Mn2 N3 80.57(13) . .
N16 Mn2 N4 91.20(18) . .
N19 Mn2 N4 84.41(17) . .
N9 Mn2 N4 113.79(15) . .
N3 Mn2 N4 71.36(14) . .
N16 Mn2 N10 86.71(18) . .
N19 Mn2 N10 86.93(17) . .
N9 Mn2 N10 70.78(14) . .
N3 Mn2 N10 118.19(14) . .
N4 Mn2 N10 170.38(15) . .
C1 N1 C5 116.9(5) . .
C1 N1 Mn1 124.0(4) . .
C5 N1 Mn1 117.7(3) . .
C6 N2 N3 113.0(4) . .
C6 N2 Mn1 116.8(3) . .
N3 N2 Mn1 123.0(3) . .
C7 N3 N2 112.7(4) . .
C7 N3 Mn2 117.6(3) . .
N2 N3 Mn2 122.5(3) . .
C8 N4 C12 118.3(4) . .
C8 N4 Mn2 115.9(3) . .
C12 N4 Mn2 124.4(4) . .
C13 N7 C17 116.6(4) . .
C13 N7 Mn1 125.8(3) . .
C17 N7 Mn1 116.3(3) . .
C18 N8 N9 113.6(4) . .
C18 N8 Mn1 117.6(3) . .
N9 N8 Mn1 121.9(3) . .
C19 N9 N8 113.3(4) . .
C19 N9 Mn2 119.5(3) . .
N8 N9 Mn2 123.1(3) . .
C20 N10 C24 120.0(5) . .
C20 N10 Mn2 115.7(3) . .
C24 N10 Mn2 123.9(4) . .
N14 N13 Mn1 152.5(5) . .
N15 N14 N13 175.3(8) . .
N17 N16 Mn2 128.8(4) . .
N18 N17 N16 176.9(7) . .
N20 N19 Mn2 129.2(4) . .
N21 N20 N19 178.8(5) . .
N20 N21 Mn1 127.8(4) . 2_654
N1 C1 C2 123.1(6) . .
C1 C2 C3 119.7(5) . .
C2 C3 C4 118.2(6) . .
C5 C4 C3 118.8(6) . .
N1 C5 C4 123.4(5) . .
N1 C5 C6 113.6(4) . .
C4 C5 C6 123.0(5) . .
N2 C6 N5 125.1(4) . .
N2 C6 C5 116.9(4) . .
N5 C6 C5 118.0(4) . .
N3 C7 N6 126.5(4) . .
N3 C7 C8 115.4(4) . .
N6 C7 C8 118.0(4) . .
N4 C8 C9 123.2(4) . .
N4 C8 C7 115.1(4) . .
C9 C8 C7 121.7(5) . .
C10 C9 C8 117.3(5) . .
C11 C10 C9 120.2(5) . .
C10 C11 C12 121.1(5) . .
N4 C12 C11 120.0(6) . .
N7 C13 C14 124.2(5) . .
C15 C14 C13 118.5(5) . .
C14 C15 C16 120.6(5) . .
C17 C16 C15 117.7(5) . .
N7 C17 C16 122.3(5) . .
N7 C17 C18 114.9(4) . .
C16 C17 C18 122.8(5) . .
N8 C18 N11 126.1(5) . .
N8 C18 C17 115.7(4) . .
N11 C18 C17 118.2(4) . .
N12 C19 N9 124.0(5) . .
N12 C19 C20 119.7(5) . .
N9 C19 C20 116.2(4) . .
N10 C20 C21 120.5(5) . .
N10 C20 C19 116.4(4) . .
C21 C20 C19 123.1(6) . .
C20 C21 C22 120.0(6) . .
C23 C22 C21 117.4(6) . .
C22 C23 C24 121.1(6) . .
N10 C24 C23 121.0(6) . .
O1 Cl1 O4 108.0(10) . .
O1 Cl1 O3 111.3(9) . .
O4 Cl1 O3 106.1(7) . .
O1 Cl1 O2 110.0(5) . .
O4 Cl1 O2 110.4(6) . .
O3 Cl1 O2 111.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N13 2.091(5) .
Mn1 N21 2.222(5) 2_655
Mn1 N8 2.273(4) .
Mn1 N7 2.282(4) .
Mn1 N2 2.303(4) .
Mn1 N1 2.309(4) .
Mn2 N16 2.124(5) .
Mn2 N19 2.205(5) .
Mn2 N9 2.245(4) .
Mn2 N3 2.271(4) .
Mn2 N4 2.308(4) .
Mn2 N10 2.328(4) .
N1 C1 1.341(6) .
N1 C5 1.358(6) .
N2 C6 1.301(6) .
N2 N3 1.413(5) .
N3 C7 1.289(6) .
N4 C8 1.331(6) .
N4 C12 1.347(7) .
N5 C6 1.346(7) .
N6 C7 1.326(6) .
N7 C13 1.333(7) .
N7 C17 1.361(6) .
N8 C18 1.297(6) .
N8 N9 1.420(5) .
N9 C19 1.312(6) .
N10 C20 1.342(7) .
N10 C24 1.355(7) .
N11 C18 1.329(6) .
N12 C19 1.307(7) .
N13 N14 1.165(7) .
N14 N15 1.151(7) .
N16 N17 1.162(7) .
N17 N18 1.128(7) .
N19 N20 1.155(6) .
N20 N21 1.156(6) .
N21 Mn1 2.222(5) 2_654
C1 C2 1.362(9) .
C2 C3 1.382(10) .
C3 C4 1.392(9) .
C4 C5 1.361(7) .
C5 C6 1.486(6) .
C7 C8 1.505(6) .
C8 C9 1.389(6) .
C9 C10 1.385(7) .
C10 C11 1.307(9) .
C11 C12 1.407(8) .
C13 C14 1.359(8) .
C14 C15 1.333(8) .
C15 C16 1.395(8) .
C16 C17 1.368(7) .
C17 C18 1.482(7) .
C19 C20 1.459(7) .
C20 C21 1.384(8) .
C21 C22 1.414(9) .
C22 C23 1.361(10) .
C23 C24 1.372(9) .
O1 Cl1 1.270(7) .
O2 Cl1 1.394(5) .
O3 Cl1 1.360(7) .
O4 Cl1 1.328(8) .
