#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/08/4320824.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_4320824
loop_
_publ_author_name
'Sheyi Wang'
'Michael S. Wemple'
'Jae Yoo'
'Kirsten Folting'
'John C. Huffman'
'Karl S. Hagen'
'David N. Hendrickson'
'George Christou'
_publ_section_title
;
 Tetranuclear Manganese Carboxylate Complexes with a Trigonal Pyramidal
 Metal Topology via Controlled Potential Electrolysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1501
_journal_page_last               1513
_journal_paper_doi               10.1021/ic991068m
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C52 H50 Mn4 N2 O18'
_chemical_formula_weight         1210.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.1 BETA  output'
_cell_angle_alpha                108.622(15)
_cell_angle_beta                 118.977(14)
_cell_angle_gamma                89.344(16)
_cell_formula_units_Z            1
_cell_length_a                   10.868(3)
_cell_length_b                   13.864(3)
_cell_length_c                   10.625(3)
_cell_measurement_reflns_used    100
_cell_measurement_theta_max      22.06
_cell_measurement_theta_min      9.02
_cell_volume                     1307.2(6)
_computing_cell_refinement       'XTEL, local package'
_computing_data_collection       'NPS, local program'
_computing_data_reduction        'XTEL, local package'
_computing_molecular_graphics    'XTEL, local package'
_computing_publication_material  'XTEL, local package'
_computing_structure_refinement  'XTEL, local package'
_computing_structure_solution    MULTAN78
_diffrn_measured_fraction_theta_full 0
_diffrn_measurement_device_type  'refurbished Picker diffractometer'
_diffrn_measurement_method       'θ/2θ scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_number            4089
_diffrn_reflns_theta_full        0
_diffrn_standards_decay_%        -0.2
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.0197
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             620
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       0.6349E-6
_refine_ls_extinction_expression
;

Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)

;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   1.2355
_refine_ls_matrix_type           full
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          2.9647
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w⁻¹=σ²(F)+(.07F)²
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.037
_reflns_number_gt                2987
_reflns_number_total             3432
_reflns_threshold_expression     F²>2.33σ(F²)
_cod_data_source_file            ic991068m_1.cif
_cod_data_source_block           '[Mn4O2(O2CMe)6(py)2(dbm)2]'
_cod_database_code               4320824
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_disorder_group
_atom_site_disorder_assembly
Mn1 Mn 0.29890(4) 0.14576(3) 0.88876(5) 0.0176(3) Uani 1 0 .
Mn2 Mn 0.49255(5) -0.03575(3) 0.85332(5) 0.0173(3) Uani 1 0 .
O3 O 0.4489(2) 0.07545(10) 0.9738(2) 0.0181(9) Uani 1 0 .
O4 O 0.3303(3) 0.1396(2) 0.7030(3) 0.0326(9) Uani 1 0 .
C5 C 0.3801(4) 0.0778(3) 0.6360(4) 0.0339(19) Uani 1 0 .
O6 O 0.4413(3) 0.0062(2) 0.6772(3) 0.0324(12) Uani 1 0 .
C7 C 0.3670(8) 0.0838(5) 0.4919(7) 0.079(4) Uani 1 0 .
O8 O 0.1532(2) 0.0238(2) 0.7667(2) 0.0273(9) Uani 1 0 .
C9 C 0.1600(3) -0.0722(2) 0.7129(4) 0.0265(16) Uani 1 0 .
O10 O 0.2684(2) 0.8913(2) 0.7275(2) 0.0262(9) Uani 1 0 .
C11 C 0.0194(4) -0.1441(3) 0.6262(6) 0.043(2) Uani 1 0 .
O12 O 0.2609(2) 0.1805(2) 1.0834(2) 0.0250(9) Uani 1 0 .
C13 C 0.3599(3) 0.2047(2) 1.2180(4) 0.0238(18) Uani 1 0 .
O14 O 0.5333(2) 0.84157(10) 0.7356(2) 0.0214(9) Uani 1 0 .
C15 C 0.3579(4) 0.2963(3) 1.3400(4) 0.0314(19) Uani 1 0 .
O16 O 0.4362(2) 0.27254(10) 1.0147(2) 0.0234(9) Uani 1 0 .
C17 C 0.4107(3) 0.3650(2) 1.0558(3) 0.0229(16) Uani 1 0 .
C18 C 0.2763(3) 0.3911(2) 0.9929(4) 0.0249(18) Uani 1 0 .
C19 C 0.1537(3) 0.3221(2) 0.8701(3) 0.0235(16) Uani 1 0 .
O20 O 0.1504(2) 0.22421(10) 0.8119(2) 0.0238(9) Uani 1 0 .
C21 C 0.5413(3) 0.4428(2) 1.1789(3) 0.0241(16) Uani 1 0 .
C22 C 0.5494(4) 0.5480(2) 1.2012(4) 0.0300(19) Uani 1 0 .
C23 C 0.6750(4) 0.6155(3) 1.3123(4) 0.038(2) Uani 1 0 .
C24 C 0.7923(4) 0.5817(3) 1.4019(4) 0.0406(19) Uani 1 0 .
C25 C 0.7864(4) 0.4785(3) 1.3844(5) 0.0409(19) Uani 1 0 .
C26 C 0.6612(4) 0.4090(3) 1.2716(4) 0.0331(19) Uani 1 0 .
C27 C 0.0136(3) 0.3558(2) 0.7944(4) 0.0251(18) Uani 1 0 .
C28 C 0.9996(4) 0.4598(3) 0.8315(4) 0.0367(19) Uani 1 0 .
C29 C -0.1323(4) 0.4876(3) 0.7618(5) 0.0413(19) Uani 1 0 .
C30 C 0.7486(4) 0.4138(3) 0.6535(4) 0.0409(19) Uani 1 0 .
C31 C 0.7614(4) 0.3107(3) 0.6126(4) 0.0411(19) Uani 1 0 .
C32 C -0.1071(4) 0.2826(3) 0.6833(4) 0.0336(19) Uani 1 0 .
N33 N 0.7119(3) 0.0729(2) 0.9441(3) 0.0336(16) Uani 1 0 .
C34 C 0.7191(4) 0.1761(3) 1.0064(5) 0.0424(19) Uani 1 0 .
C35 C 0.8263(5) 0.2478(3) 1.0358(5) 0.049(2) Uani 1 0 .
C36 C 0.9283(4) 0.2141(3) 1.0007(5) 0.051(2) Uani 1 0 .
C37 C 0.9208(4) 0.1104(3) 0.9342(5) 0.048(2) Uani 1 0 .
C38 C 0.8149(4) 0.0441(3) 0.9127(4) 0.0400(19) Uani 1 0 .
H1 H 0.304(6) 0.127(4) 0.453(6) 0.087(13) Uiso 1 0 .
H2 H 0.490(8) 0.136(5) 0.575(8) 0.133(13) Uiso 1 0 .
H3 H 0.366(10) 0.028(7) 0.430(10) 0.204(13) Uiso 1 0 .
H4 H 0.981(5) 0.866(4) 0.691(6) 0.082(13) Uiso 1 0 .
H5 H 0.963(5) 0.873(3) 0.551(5) 0.055(11) Uiso 1 0 .
H6 H 0.031(5) -0.204(4) 0.597(6) 0.084(13) Uiso 1 0 .
H7 H 0.420(4) 0.298(3) 1.442(5) 0.046(10) Uiso 1 0 .
H8 H 0.387(5) 0.355(4) 1.326(5) 0.068(11) Uiso 1 0 .
H9 H 0.269(5) 0.295(3) 1.331(5) 0.055(11) Uiso 1 0 .
H10 H 0.271(4) 0.459(3) 1.029(4) 0.034(9) Uiso 1 0 .
H11 H 0.472(4) 0.569(3) 1.143(4) 0.025(9) Uiso 1 0 .
H12 H 0.679(4) 0.673(3) 1.316(4) 0.040(10) Uiso 1 0 .
H13 H 0.878(5) 0.623(3) 1.475(5) 0.058(11) Uiso 1 0 .
H14 H 0.865(5) 0.458(3) 1.450(5) 0.061(11) Uiso 1 0 .
H15 H 0.655(4) 0.341(3) 1.265(4) 0.035(9) Uiso 1 0 .
H16 H 0.077(4) 0.511(3) 0.905(4) 0.038(9) Uiso 1 0 .
H17 H 0.861(4) 0.555(3) 0.797(4) 0.050(10) Uiso 1 0 .
H18 H -0.337(4) 0.433(3) 0.610(4) 0.039(9) Uiso 1 0 .
H19 H -0.320(5) 0.262(3) 0.543(5) 0.056(11) Uiso 1 0 .
H20 H -0.099(4) 0.217(3) 0.666(4) 0.037(9) Uiso 1 0 .
H21 H 0.638(4) 0.196(3) 1.031(4) 0.055(10) Uiso 1 0 .
H22 H 0.828(5) 0.309(4) 1.075(6) 0.081(13) Uiso 1 0 .
H23 H 1.006(5) 0.262(4) 1.022(5) 0.072(11) Uiso 1 0 .
H24 H 0.991(5) 0.085(3) 0.905(5) 0.074(11) Uiso 1 0 .
H25 H 0.806(5) 0.972(4) 0.870(6) 0.080(13) Uiso 1 0 .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn Mn 0.295 0.729 'International Tables Vol. IV (1974) Table 2.2B'
O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B'
N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B'
C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B'
H H 0 0 'International Tables Vol. IV (1974) Table 2.2B'
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mn1 O4 94.72(8) . . . no
O3 Mn1 O8 95.01(9) . . . no
O3 Mn1 O12 92.88(8) . . . no
O3 Mn1 O16 87.74(8) . . . no
O3 Mn1 O20 176.89(8) . . . no
O4 Mn1 O8 93.37(9) . . . no
O4 Mn1 O12 169.81(8) . . . no
O4 Mn1 O16 88.96(9) . . . no
O4 Mn1 O20 86.79(9) . . . no
O8 Mn1 O12 92.71(9) . . . no
O8 Mn1 O16 176.23(8) . . . no
O8 Mn1 O20 87.60(9) . . . no
O12 Mn1 O16 84.57(8) . . . no
O12 Mn1 O20 85.30(8) . . . no
O16 Mn1 O20 89.58(9) . . . no
Mn2 Mn2 O3 40.35(6) 2_657 . 2_657 no
Mn2 Mn2 O3 40.58(6) 2_657 . . no
Mn2 Mn2 O6 140.66(7) 2_657 . . no
Mn2 Mn2 O10 93.45(6) 2_657 . 1_545 no
Mn2 Mn2 O14 135.34(6) 2_657 . 1_545 no
Mn2 Mn2 N33 94.67(7) 2_657 . . no
O3 Mn2 O3 80.93(9) . . 2_657 no
O3 Mn2 O3 80.93(9) 2_657 . . no
O3 Mn2 O6 177.33(9) 2_657 . . no
O3 Mn2 O6 100.14(9) . . . no
O3 Mn2 O10 96.97(9) 2_657 . 1_545 no
O3 Mn2 O10 88.27(8) . . 1_545 no
O3 Mn2 O14 175.15(9) . . 1_545 no
O3 Mn2 O14 95.05(9) 2_657 . 1_545 no
O3 Mn2 N33 98.52(9) 2_657 . . no
O3 Mn2 N33 88.59(9) . . . no
O6 Mn2 O10 85.53(9) . . 1_545 no
O6 Mn2 O14 84.00(9) . . 1_545 no
O6 Mn2 N33 79.09(10) . . . no
O10 Mn2 O14 89.54(8) 1_545 . 1_545 no
O10 Mn2 N33 163.50(9) 1_545 . . no
O14 Mn2 N33 94.72(9) 1_545 . . no
Mn1 O3 Mn2 123.17(10) . . . no
Mn1 O3 Mn2 128.61(10) . . 2_657 no
Mn2 O3 Mn2 99.07(9) . . 2_657 no
Mn2 O3 Mn2 99.07(9) 2_657 . . no
Mn1 O4 C5 131.4(2) . . . no
Mn2 O6 C5 133.7(2) . . . no
Mn1 O8 C9 131.5(2) . . . no
Mn2 O10 C9 131.32(19) 1_565 . 1_565 no
Mn1 O12 C13 122.08(19) . . . no
Mn2 O14 C13 129.04(19) 1_565 . 2_667 no
Mn1 O16 C17 127.39(19) . . . no
Mn1 O20 C19 127.83(19) . . . no
Mn2 N33 C34 116.5(2) . . . no
Mn2 N33 C38 126.1(2) . . . no
C34 N33 C38 116.0(3) . . . no
O4 C5 O6 125.2(3) . . . no
O4 C5 C7 119.2(3) . . . no
O6 C5 C7 115.6(3) . . . no
O8 C9 O10 126.6(3) . . 1_545 no
O8 C9 C11 114.4(3) . . . no
O10 C9 C11 119.0(3) 1_545 . . no
O12 C13 O14 125.4(3) . . 2_667 no
O12 C13 C15 118.6(3) . . . no
O14 C13 C15 116.0(3) 2_667 . . no
O16 C17 C18 124.0(3) . . . no
O16 C17 C21 113.5(3) . . . no
C18 C17 C21 122.5(3) . . . no
C17 C18 C19 123.9(3) . . . no
O20 C19 C18 123.7(3) . . . no
O20 C19 C27 114.1(3) . . . no
C18 C19 C27 122.3(3) . . . no
C17 C21 C22 122.6(3) . . . no
C17 C21 C26 118.7(3) . . . no
C22 C21 C26 118.7(3) . . . no
C21 C22 C23 120.0(4) . . . no
C22 C23 C24 121.0(3) . . . no
C23 C24 C25 120.2(3) . . . no
C24 C25 C26 119.6(4) . . . no
C21 C26 C25 120.5(3) . . . no
C19 C27 C28 122.1(3) . . 1_455 no
C19 C27 C32 119.6(3) . . . no
C28 C27 C32 118.3(3) 1_455 . . no
C27 C28 C29 120.4(3) 1_655 . 1_655 no
C28 C29 C30 120.6(4) 1_455 . 1_455 no
C29 C30 C31 119.7(3) 1_655 . . no
C30 C31 C32 119.8(4) . . 1_655 no
C27 C32 C31 121.2(3) . . 1_455 no
N33 C34 C35 122.2(4) . . . no
C34 C35 C36 119.2(4) . . . no
C35 C36 C37 119.4(4) . . . no
C36 C37 C38 118.2(4) . . . no
N33 C38 C37 124.8(4) . . . no
C5 C7 H1 113(3) . . . no
C5 C7 H2 87(3) . . . no
C5 C7 H3 115(6) . . . no
H1 C7 H2 108(4) . . . no
H1 C7 H3 119(7) . . . no
H2 C7 H3 110(7) . . . no
C9 C11 H4 109(3) . . 1_445 no
C9 C11 H5 108(3) . . 1_445 no
C9 C11 H6 109(4) . . . no
H4 C11 H5 107(4) 1_445 . 1_445 no
H4 C11 H6 112(5) 1_445 . . no
H5 C11 H6 111(5) 1_445 . . no
C13 C15 H7 114(2) . . . no
C13 C15 H8 104(3) . . . no
C13 C15 H9 112(3) . . . no
H7 C15 H8 111(3) . . . no
H7 C15 H9 104(3) . . . no
H8 C15 H9 113(4) . . . no
C17 C18 H10 117(2) . . . no
C19 C18 H10 119(2) . . . no
C21 C22 H11 118(2) . . . no
C23 C22 H11 122(2) . . . no
C22 C23 H12 117(3) . . . no
C24 C23 H12 121(3) . . . no
C23 C24 H13 124(3) . . . no
C25 C24 H13 115(3) . . . no
C24 C25 H14 119(3) . . . no
C26 C25 H14 122(3) . . . no
C21 C26 H15 120(2) . . . no
C25 C26 H15 120(2) . . . no
C27 C28 H16 121(2) 1_655 . 1_655 no
C29 C28 H16 119(2) 1_655 . 1_655 no
C28 C29 H17 118(3) 1_455 . 1_455 no
C30 C29 H17 121(3) 1_455 . 1_455 no
C29 C30 H18 119(2) 1_655 . 1_655 no
C31 C30 H18 121(2) . . 1_655 no
C30 C31 H19 119(3) . . 1_655 no
C32 C31 H19 121(3) 1_655 . 1_655 no
C27 C32 H20 118(2) . . . no
C31 C32 H20 121(2) 1_455 . . no
N33 C34 H21 114(2) . . . no
C35 C34 H21 124(2) . . . no
C34 C35 H22 120(4) . . . no
C36 C35 H22 121(4) . . . no
C35 C36 H23 122(3) . . . no
C37 C36 H23 119(3) . . . no
C36 C37 H24 121(3) . . . no
C38 C37 H24 121(3) . . . no
N33 C38 H25 113(3) . . 1_545 no
C37 C38 H25 122(3) . . 1_545 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O3 1.8768(19) . . no
Mn1 O4 2.136(2) . . no
Mn1 O8 1.928(2) . . no
Mn1 O12 2.205(2) . . no
Mn1 O16 1.931(2) . . no
Mn1 O20 1.9248(19) . . no
Mn2 Mn2 2.8749(11) . 2_657 no
Mn2 O3 1.8848(19) . . no
Mn2 O3 1.894(2) . 2_657 no
Mn2 O6 1.957(2) . . no
Mn2 O10 2.187(2) . 1_545 no
Mn2 O14 1.953(2) . 1_545 no
Mn2 N33 2.410(3) . . no
O4 C5 1.228(4) . . no
O6 C5 1.264(4) . . no
O8 C9 1.287(4) . . no
O10 C9 1.235(4) . 1_565 no
O12 C13 1.236(4) . . no
O14 C13 1.277(4) . 2_667 no
O16 C17 1.290(4) . . no
O20 C19 1.292(4) . . no
N33 C34 1.357(4) . . no
N33 C38 1.338(4) . . no
C5 C7 1.497(6) . . no
C9 C11 1.504(5) . . no
C13 C15 1.506(5) . . no
C17 C18 1.381(4) . . no
C17 C21 1.491(4) . . no
C18 C19 1.393(5) . . no
C19 C27 1.490(4) . . no
C21 C22 1.397(4) . . no
C21 C26 1.387(5) . . no
C22 C23 1.377(5) . . no
C23 C24 1.360(6) . . no
C24 C25 1.380(5) . . no
C25 C26 1.389(5) . . no
C27 C28 1.396(5) . 1_455 no
C27 C32 1.382(5) . . no
C28 C29 1.376(5) . 1_655 no
C29 C30 1.372(6) . 1_455 no
C30 C31 1.381(5) . . no
C31 C32 1.375(5) . 1_655 no
C34 C35 1.385(5) . . no
C35 C36 1.366(6) . . no
C36 C37 1.367(6) . . no
C37 C38 1.363(5) . . no
C7 H1 0.94(6) . . no
C7 H2 1.25(7) . . no
C7 H3 0.83(9) . . no
C11 H4 0.94(5) . 1_445 no
C11 H5 0.84(4) . 1_445 no
C11 H6 0.82(6) . . no
C15 H7 0.95(4) . . no
C15 H8 0.96(5) . . no
C15 H9 0.92(4) . . no
C18 H10 0.91(4) . . no
C22 H11 0.88(3) . . no
C23 H12 0.79(4) . . no
C24 H13 0.91(4) . . no
C25 H14 0.92(4) . . no
C26 H15 0.93(4) . . no
C28 H16 0.92(4) . 1_655 no
C29 H17 0.90(4) . 1_455 no
C30 H18 0.90(4) . 1_655 no
C31 H19 0.92(4) . 1_655 no
C32 H20 0.87(4) . . no
C34 H21 1.05(4) . . no
C35 H22 0.81(5) . . no
C36 H23 0.97(5) . . no
C37 H24 0.98(5) . . no
C38 H25 0.94(5) . 1_545 no
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139134051
