#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:40:30 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301839 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/11/4331132.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_4331132
loop_
_publ_author_name
'Shengwen Liang'
'Haoshuang Wang'
'Tapash Deb'
'Jeffrey L. Petersen'
'Gordon T. Yee'
'Michael P. Jensen'
_publ_section_title
;
 Structural and Spectroscopic Trends in a Series of Half-Sandwich
 Scorpionate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12707
_journal_page_last               12719
_journal_paper_doi               10.1021/ic301409s
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C34 H31 B2 F8 Mn N9'
_chemical_formula_weight         794.24
_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                67.315(1)
_cell_angle_beta                 70.336(1)
_cell_angle_gamma                73.350(1)
_cell_formula_units_Z            2
_cell_length_a                   12.6467(9)
_cell_length_b                   12.9873(9)
_cell_length_c                   13.4015(9)
_cell_measurement_reflns_used    8848
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.66
_cell_volume                     1881.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13066
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale amber'
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         8270
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0932P)²+0.2493P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1642
_reflns_number_gt                6823
_reflns_number_total             8270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301409s_si_002_1.cif
_cod_data_source_block           2Mn
_cod_database_code               4331132
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
Mn1 Mn 0.20735(3) 0.39910(2) 0.20222(2) 0.04855(12) Uani 1 1 d . . .
N1 N 0.22536(17) 0.54403(14) 0.25116(14) 0.0551(4) Uani 1 1 d . . .
N2 N 0.21546(18) 0.64962(15) 0.17534(15) 0.0595(4) Uani 1 1 d . . .
N3 N 0.05834(15) 0.53347(13) 0.14440(14) 0.0504(4) Uani 1 1 d . . .
N4 N 0.07462(16) 0.64340(14) 0.09787(15) 0.0555(4) Uani 1 1 d . . .
N5 N 0.30413(15) 0.50075(14) 0.02986(13) 0.0511(4) Uani 1 1 d . . .
N6 N 0.27146(16) 0.61584(14) -0.00064(14) 0.0543(4) Uani 1 1 d . . .
N7 N 0.20936(17) 0.26718(17) 0.13539(18) 0.0627(4) Uani 1 1 d . . .
N8 N 0.34995(18) 0.28999(16) 0.27678(16) 0.0618(4) Uani 1 1 d . . .
N9 N 0.09330(19) 0.30549(18) 0.35926(17) 0.0662(5) Uani 1 1 d . . .
C1 C 0.2566(2) 0.5560(2) 0.33189(18) 0.0602(5) Uani 1 1 d . . .
C2 C 0.2663(3) 0.6691(2) 0.3050(2) 0.0802(8) Uani 1 1 d . . .
H2 H 0.2871 0.6992 0.3469 0.096 Uiso 1 1 calc R . .
C3 C 0.2394(3) 0.7254(2) 0.2060(2) 0.0741(7) Uani 1 1 d . . .
H3 H 0.2378 0.8023 0.1665 0.089 Uiso 1 1 calc R . .
C4 C 0.2783(2) 0.4597(2) 0.42998(18) 0.0638(5) Uani 1 1 d . . .
C5 C 0.1966(3) 0.3937(3) 0.4986(2) 0.0787(7) Uani 1 1 d . . .
H5 H 0.1250 0.4116 0.4851 0.094 Uiso 1 1 calc R . .
C6 C 0.2225(4) 0.2997(3) 0.5886(3) 0.0975(10) Uani 1 1 d . . .
H6 H 0.1680 0.2546 0.6348 0.117 Uiso 1 1 calc R . .
C7 C 0.3261(4) 0.2738(3) 0.6090(3) 0.1039(11) Uani 1 1 d . . .
H7 H 0.3432 0.2098 0.6678 0.125 Uiso 1 1 calc R . .
C8 C 0.4063(3) 0.3411(3) 0.5438(3) 0.0978(10) Uani 1 1 d . . .
H8 H 0.4765 0.3241 0.5600 0.117 Uiso 1 1 calc R . .
C9 C 0.3829(3) 0.4337(3) 0.4544(2) 0.0809(7) Uani 1 1 d . . .
H9 H 0.4375 0.4792 0.4102 0.097 Uiso 1 1 calc R . .
C10 C -0.05445(18) 0.54031(19) 0.16942(17) 0.0551(4) Uani 1 1 d . . .
C11 C -0.1083(2) 0.6550(2) 0.1405(2) 0.0730(6) Uani 1 1 d . . .
H11 H -0.1862 0.6824 0.1502 0.088 Uiso 1 1 calc R . .
C12 C -0.0248(2) 0.7172(2) 0.0962(2) 0.0690(6) Uani 1 1 d . . .
H12 H -0.0341 0.7960 0.0695 0.083 Uiso 1 1 calc R . .
C13 C -0.10550(18) 0.43757(19) 0.22224(17) 0.0554(5) Uani 1 1 d . . .
C14 C -0.0655(2) 0.3498(2) 0.1773(2) 0.0647(5) Uani 1 1 d . . .
H14 H -0.0101 0.3583 0.1096 0.078 Uiso 1 1 calc R . .
C15 C -0.1076(2) 0.2493(2) 0.2323(3) 0.0794(7) Uani 1 1 d . . .
H15 H -0.0795 0.1901 0.2023 0.095 Uiso 1 1 calc R . .
C16 C -0.1916(3) 0.2373(3) 0.3320(3) 0.0868(8) Uani 1 1 d . . .
H16 H -0.2190 0.1695 0.3700 0.104 Uiso 1 1 calc R . .
C17 C -0.2346(3) 0.3266(3) 0.3749(2) 0.0832(8) Uani 1 1 d . . .
H17 H -0.2925 0.3195 0.4408 0.100 Uiso 1 1 calc R . .
C18 C -0.1921(2) 0.4257(2) 0.32091(19) 0.0693(6) Uani 1 1 d . . .
H18 H -0.2213 0.4853 0.3504 0.083 Uiso 1 1 calc R . .
C19 C 0.37385(18) 0.48082(19) -0.06349(16) 0.0537(4) Uani 1 1 d . . .
C20 C 0.3840(2) 0.5830(2) -0.15250(19) 0.0670(6) Uani 1 1 d . . .
H20 H 0.4276 0.5916 -0.2257 0.080 Uiso 1 1 calc R . .
C21 C 0.3174(2) 0.6666(2) -0.11001(18) 0.0649(6) Uani 1 1 d . . .
H21 H 0.3057 0.7439 -0.1488 0.078 Uiso 1 1 calc R . .
C22 C 0.42676(17) 0.36591(19) -0.06807(17) 0.0541(4) Uani 1 1 d . . .
C23 C 0.4765(2) 0.2847(2) 0.0144(2) 0.0696(6) Uani 1 1 d . . .
H23 H 0.4801 0.3032 0.0735 0.083 Uiso 1 1 calc R . .
C24 C 0.5212(2) 0.1754(3) 0.0088(3) 0.0851(8) Uani 1 1 d . . .
H24 H 0.5536 0.1207 0.0648 0.102 Uiso 1 1 calc R . .
C25 C 0.5175(3) 0.1480(3) -0.0785(3) 0.0858(8) Uani 1 1 d . . .
H25 H 0.5475 0.0747 -0.0816 0.103 Uiso 1 1 calc R . .
C26 C 0.4699(3) 0.2277(3) -0.1619(3) 0.0799(7) Uani 1 1 d . . .
H26 H 0.4680 0.2086 -0.2213 0.096 Uiso 1 1 calc R . .
C27 C 0.4249(2) 0.3367(2) -0.1572(2) 0.0654(5) Uani 1 1 d . . .
H27 H 0.3931 0.3909 -0.2139 0.078 Uiso 1 1 calc R . .
C28 C 0.1849(2) 0.67166(16) 0.07339(17) 0.0556(5) Uani 1 1 d . . .
H28 H 0.1783 0.7535 0.0343 0.067 Uiso 1 1 calc R . .
C29 C 0.2085(2) 0.1874(2) 0.1213(2) 0.0627(5) Uani 1 1 d . . .
C30 C 0.2045(3) 0.0850(3) 0.1035(3) 0.0938(10) Uani 1 1 d . . .
H30A H 0.1266 0.0756 0.1242 0.141 Uiso 1 1 calc R . .
H30B H 0.2468 0.0206 0.1486 0.141 Uiso 1 1 calc R . .
H30C H 0.2376 0.0913 0.0260 0.141 Uiso 1 1 calc R . .
C31 C 0.4100(2) 0.2206(2) 0.32259(19) 0.0618(5) Uani 1 1 d . . .
C32 C 0.4884(3) 0.1316(3) 0.3817(3) 0.0962(10) Uani 1 1 d . . .
H32A H 0.5399 0.0902 0.3331 0.144 Uiso 1 1 calc R . .
H32B H 0.4460 0.0810 0.4464 0.144 Uiso 1 1 calc R . .
H32C H 0.5311 0.1649 0.4046 0.144 Uiso 1 1 calc R . .
C33 C 0.0590(2) 0.2339(2) 0.4342(2) 0.0682(6) Uani 1 1 d . . .
C34 C 0.0171(4) 0.1429(3) 0.5320(3) 0.1114(12) Uani 1 1 d . . .
H34A H 0.0762 0.0768 0.5398 0.167 Uiso 1 1 calc R . .
H34B H -0.0478 0.1256 0.5238 0.167 Uiso 1 1 calc R . .
H34C H -0.0048 0.1659 0.5972 0.167 Uiso 1 1 calc R . .
B1 B 0.3170(3) 0.9501(2) 0.3641(2) 0.0710(7) Uani 1 1 d D . .
F1 F 0.3798(2) 1.01155(19) 0.26572(16) 0.1073(6) Uani 1 1 d D A .
F2 F 0.2465(8) 1.0182(5) 0.4165(8) 0.160(4) Uani 0.566(15) 1 d PD A 1
F3 F 0.2601(9) 0.8916(6) 0.3412(5) 0.145(4) Uani 0.566(15) 1 d PD A 1
F4 F 0.3888(5) 0.8768(8) 0.4243(7) 0.156(5) Uani 0.566(15) 1 d PD A 1
F2' F 0.2079(6) 0.9667(14) 0.3611(7) 0.176(8) Uani 0.434(15) 1 d PD A 2
F3' F 0.3147(10) 0.9765(10) 0.4548(5) 0.130(5) Uani 0.434(15) 1 d PD A 2
F4' F 0.3570(10) 0.8372(4) 0.3901(7) 0.130(5) Uani 0.434(15) 1 d PD A 2
B2 B 0.8238(4) 0.0091(3) 0.1487(3) 0.1035(13) Uani 1 1 d D . .
F5 F 0.7428(3) 0.0548(3) 0.2208(3) 0.1908(16) Uani 1 1 d DU B .
F6 F 0.9146(5) -0.0440(6) 0.1935(6) 0.217(3) Uani 0.731(9) 1 d PDU B 1
F7 F 0.7883(5) -0.0777(3) 0.1434(4) 0.1389(19) Uani 0.731(9) 1 d PDU B 1
F8 F 0.8483(7) 0.0804(3) 0.0500(5) 0.233(5) Uani 0.731(9) 1 d PDU B 1
F6' F 0.9104(8) 0.0793(10) 0.1061(9) 0.126(5) Uani 0.269(9) 1 d PDU B 2
F7' F 0.8735(14) -0.0919(6) 0.1832(10) 0.275(18) Uani 0.269(9) 1 d PDU B 2
F8' F 0.7908(12) 0.0364(16) 0.0551(9) 0.282(16) Uani 0.269(9) 1 d PDU B 2
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
N7 Mn1 N8 90.27(7)
N7 Mn1 N9 86.01(8)
N8 Mn1 N9 85.88(8)
N7 Mn1 N5 90.81(7)
N8 Mn1 N5 101.42(7)
N9 Mn1 N5 172.07(7)
N7 Mn1 N3 100.64(7)
N8 Mn1 N3 168.96(6)
N9 Mn1 N3 93.12(7)
N5 Mn1 N3 80.32(6)
N7 Mn1 N1 172.26(7)
N8 Mn1 N1 88.65(7)
N9 Mn1 N1 101.55(7)
N5 Mn1 N1 81.90(6)
N3 Mn1 N1 80.77(6)
C1 N1 N2 104.48(16)
C1 N1 Mn1 138.21(15)
N2 N1 Mn1 116.81(11)
C3 N2 N1 112.28(18)
C3 N2 C28 126.29(19)
N1 N2 C28 121.41(15)
C10 N3 N4 104.88(16)
C10 N3 Mn1 135.43(14)
N4 N3 Mn1 116.86(12)
C12 N4 N3 111.90(19)
C12 N4 C28 125.95(19)
N3 N4 C28 121.31(16)
C19 N5 N6 104.59(16)
C19 N5 Mn1 137.67(14)
N6 N5 Mn1 116.47(12)
C21 N6 N5 111.99(18)
C21 N6 C28 125.25(19)
N5 N6 C28 122.14(16)
C29 N7 Mn1 167.2(2)
C31 N8 Mn1 167.6(2)
C33 N9 Mn1 161.0(2)
N1 C1 C2 110.1(2)
N1 C1 C4 121.85(19)
C2 C1 C4 128.1(2)
C3 C2 C1 106.2(2)
N2 C3 C2 107.0(2)
C5 C4 C9 119.2(3)
C5 C4 C1 121.3(2)
C9 C4 C1 119.5(2)
C4 C5 C6 119.5(3)
C7 C6 C5 120.4(3)
C6 C7 C8 120.5(3)
C7 C8 C9 120.0(3)
C8 C9 C4 120.3(3)
N3 C10 C11 109.8(2)
N3 C10 C13 120.92(18)
C11 C10 C13 129.3(2)
C12 C11 C10 106.7(2)
N4 C12 C11 106.8(2)
C14 C13 C18 119.2(2)
C14 C13 C10 120.66(19)
C18 C13 C10 120.1(2)
C13 C14 C15 120.4(2)
C16 C15 C14 119.8(3)
C17 C16 C15 119.7(3)
C18 C17 C16 120.4(3)
C17 C18 C13 120.4(3)
N5 C19 C20 110.6(2)
N5 C19 C22 122.49(19)
C20 C19 C22 126.92(19)
C21 C20 C19 106.04(19)
N6 C21 C20 106.8(2)
C23 C22 C27 118.9(2)
C23 C22 C19 122.15(19)
C27 C22 C19 118.9(2)
C22 C23 C24 120.0(2)
C25 C24 C23 120.3(3)
C24 C25 C26 120.6(3)
C25 C26 C27 119.7(3)
C26 C27 C22 120.5(2)
N6 C28 N4 111.96(16)
N6 C28 N2 112.36(18)
N4 C28 N2 110.82(17)
N7 C29 C30 178.7(3)
N8 C31 C32 179.4(3)
N9 C33 C34 178.2(3)
F2 B1 F4 111.1(5)
F2 B1 F2' 65.7(5)
F4 B1 F2' 139.2(5)
F2 B1 F4' 136.3(5)
F4 B1 F4' 45.1(4)
F2' B1 F4' 107.0(5)
F2 B1 F3 110.8(5)
F4 B1 F3 109.1(5)
F2' B1 F3 47.2(5)
F4' B1 F3 65.1(5)
F2 B1 F1 109.3(4)
F4 B1 F1 108.2(4)
F2' B1 F1 111.0(4)
F4' B1 F1 113.2(4)
F3 B1 F1 108.4(4)
F2 B1 F3' 46.5(4)
F4 B1 F3' 66.0(5)
F2' B1 F3' 107.0(5)
F4' B1 F3' 104.7(5)
F3 B1 F3' 137.2(4)
F1 B1 F3' 113.5(4)
F7' B2 F8 127.3(6)
F7' B2 F5 119.4(6)
F8 B2 F5 113.0(4)
F7' B2 F8' 115.2(7)
F8 B2 F8' 45.5(6)
F5 B2 F8' 110.0(7)
F7' B2 F6 44.1(9)
F8 B2 F6 114.2(6)
F5 B2 F6 108.1(5)
F8' B2 F6 141.7(8)
F7' B2 F7 59.1(10)
F8 B2 F7 108.9(5)
F5 B2 F7 108.8(4)
F8' B2 F7 67.4(8)
F6 B2 F7 103.1(4)
F7' B2 F6' 106.4(8)
F8 B2 F6' 54.0(5)
F5 B2 F6' 103.6(4)
F8' B2 F6' 99.3(6)
F6 B2 F6' 68.2(6)
F7 B2 F6' 147.5(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mn1 N7 2.2094(18)
Mn1 N8 2.2170(19)
Mn1 N9 2.231(2)
Mn1 N5 2.2908(17)
Mn1 N3 2.2918(17)
Mn1 N1 2.3072(16)
N1 C1 1.343(3)
N1 N2 1.357(2)
N2 C3 1.340(3)
N2 C28 1.445(3)
N3 C10 1.336(3)
N3 N4 1.366(2)
N4 C12 1.346(3)
N4 C28 1.442(3)
N5 C19 1.336(3)
N5 N6 1.364(2)
N6 C21 1.350(3)
N6 C28 1.441(3)
N7 C29 1.127(3)
N8 C31 1.123(3)
N9 C33 1.131(3)
C1 C2 1.403(3)
C1 C4 1.465(3)
C2 C3 1.351(4)
C4 C5 1.381(4)
C4 C9 1.386(4)
C5 C6 1.397(4)
C6 C7 1.350(6)
C7 C8 1.370(6)
C8 C9 1.376(5)
C10 C11 1.408(3)
C10 C13 1.468(3)
C11 C12 1.348(4)
C13 C14 1.383(3)
C13 C18 1.391(3)
C14 C15 1.387(4)
C15 C16 1.385(5)
C16 C17 1.383(5)
C17 C18 1.373(4)
C19 C20 1.405(3)
C19 C22 1.466(3)
C20 C21 1.357(4)
C22 C23 1.385(3)
C22 C27 1.394(3)
C23 C24 1.391(4)
C24 C25 1.366(4)
C25 C26 1.373(4)
C26 C27 1.384(4)
C29 C30 1.455(3)
C31 C32 1.453(4)
C33 C34 1.446(4)
B1 F2 1.294(5)
B1 F4 1.336(5)
B1 F2' 1.347(5)
B1 F4' 1.352(5)
B1 F3 1.354(5)
B1 F1 1.361(3)
B1 F3' 1.373(5)
B2 F7' 1.260(7)
B2 F8 1.283(5)
B2 F5 1.328(4)
B2 F8' 1.341(8)
B2 F6 1.359(6)
B2 F7 1.361(5)
B2 F6' 1.451(7)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139138074
