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#$Date: 2022-03-31 10:27:45 +0300 (Thu, 31 Mar 2022) $
#$Revision: 274162 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/49/8104968.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_8104968
loop_
_publ_author_name
'Ikarugi, Riko'
'Fujisawa, Kiyoshi'
'Tiekink, Edward R. T.'
_publ_section_title
;
 Crystal structure of
 bis{hydridotris(3-trifluoromethyl-5-methylpyrazolyl-1-yl)borato-\kN
 3}manganese(II), C30H26B2F18MnN12
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              85
_journal_page_last               87
_journal_paper_doi               10.1515/ncrs-2021-0395
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C30 H26 B2 F18 Mn N12'
_chemical_formula_sum            'C30 H26 B2 F18 Mn N12'
_chemical_formula_weight         973.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                111.755(3)
_cell_angle_beta                 99.100(2)
_cell_angle_gamma                112.740(3)
_cell_formula_units_Z            1
_cell_length_a                   10.5322(3)
_cell_length_b                   10.6475(4)
_cell_length_c                   10.9890(4)
_cell_measurement_reflns_used    18541
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     988.07(8)
_computing_cell_refinement       'CrysAlisPro [1]'
_computing_data_collection       'CrysAlisPro [1]'
_computing_data_reduction        'CrysAlisPro [1]'
_computing_molecular_graphics    'ORTEP-3 for Windows [4]'
_computing_publication_material  'SHELXL-2018/3 [3]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SIR2014 [2]'
_diffrn_ambient_temperature      178(2)
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33278
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.845
_diffrn_reflns_theta_min         2.309
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro [1]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       prism
_exptl_crystal_F_000             487
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0417P)²+0.4002P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4626
_reflns_number_total             5266
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0395_suppl.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        988.07(7)
_cod_database_code               8104968
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.970
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn 0.500000 0.500000 0.500000 0.01844(8) Uani 1 2 d S . P . .
F1 F 0.60801(11) 0.71851(11) 0.85888(9) 0.0374(2) Uani 1 1 d . . . . .
F2 F 0.67936(11) 0.95268(11) 0.90127(10) 0.0433(2) Uani 1 1 d . . . . .
F3 F 0.51403(12) 0.84652(12) 0.97520(9) 0.0425(2) Uani 1 1 d . . . . .
F4 F 0.78545(10) 0.59124(12) 0.37393(11) 0.0403(2) Uani 1 1 d . . . . .
F5 F 0.84302(11) 0.72809(13) 0.26869(13) 0.0509(3) Uani 1 1 d . . . . .
F6 F 0.69270(12) 0.48517(13) 0.15174(11) 0.0489(3) Uani 1 1 d . . . . .
F7 F 0.30670(10) 0.10565(10) 0.38839(11) 0.0394(2) Uani 1 1 d . . . . .
F8 F 0.10751(12) 0.06504(12) 0.43182(12) 0.0465(3) Uani 1 1 d . . . . .
F9 F 0.09797(11) -0.06723(10) 0.22527(11) 0.0457(3) Uani 1 1 d . . . . .
N11 N 0.42836(11) 0.67497(12) 0.60777(11) 0.0206(2) Uani 1 1 d . . . . .
N12 N 0.31723(11) 0.66981(13) 0.51944(11) 0.0214(2) Uani 1 1 d . . . . .
N21 N 0.51569(11) 0.59428(12) 0.34249(11) 0.0208(2) Uani 1 1 d . . . . .
N22 N 0.41056(12) 0.63583(13) 0.31681(11) 0.0216(2) Uani 1 1 d . . . . .
N31 N 0.25589(11) 0.33975(12) 0.36216(11) 0.0218(2) Uani 1 1 d . . . . .
N32 N 0.19692(11) 0.40706(13) 0.30356(11) 0.0223(2) Uani 1 1 d . . . . .
C1 C 0.56021(16) 0.81846(16) 0.86567(14) 0.0286(3) Uani 1 1 d . . . . .
C2 C 0.44229(15) 0.76831(15) 0.73625(14) 0.0247(3) Uani 1 1 d . . . . .
C3 C 0.34203(18) 0.8224(2) 0.73256(16) 0.0373(4) Uani 1 1 d . . . . .
H3 H 0.329747 0.889214 0.809885 0.045 Uiso 1 1 calc R U . . .
C4 C 0.26415(17) 0.75839(19) 0.59259(16) 0.0346(3) Uani 1 1 d . . . . .
C5 C 0.1424(3) 0.7777(3) 0.5260(2) 0.0685(7) Uani 1 1 d . . . . .
H5A H 0.124316 0.848799 0.598896 0.103 Uiso 1 1 calc R U . . .
H5B H 0.052787 0.677053 0.472567 0.103 Uiso 1 1 calc R U . . .
H5C H 0.170334 0.819961 0.463073 0.103 Uiso 1 1 calc R U . . .
C6 C 0.73202(16) 0.61327(18) 0.26985(16) 0.0304(3) Uani 1 1 d . . . . .
C7 C 0.60701(15) 0.64516(16) 0.27949(14) 0.0250(3) Uani 1 1 d . . . . .
C8 C 0.56450(19) 0.7197(2) 0.21522(19) 0.0389(4) Uani 1 1 d . . . . .
H8 H 0.611906 0.766133 0.164661 0.047 Uiso 1 1 calc R U . . .
C9 C 0.43846(18) 0.7118(2) 0.24071(18) 0.0351(3) Uani 1 1 d . . . . .
C10 C 0.3439(3) 0.7737(3) 0.1975(3) 0.0628(7) Uani 1 1 d . . . . .
H10A H 0.385423 0.826195 0.145310 0.094 Uiso 1 1 calc R U . . .
H10B H 0.339972 0.847296 0.280923 0.094 Uiso 1 1 calc R U . . .
H10C H 0.244290 0.688148 0.137939 0.094 Uiso 1 1 calc R U . . .
C11 C 0.16908(16) 0.07481(16) 0.33558(17) 0.0313(3) Uani 1 1 d . . . . .
C12 C 0.15652(14) 0.18939(15) 0.29447(15) 0.0263(3) Uani 1 1 d . . . . .
C13 C 0.03585(16) 0.15804(17) 0.19204(16) 0.0347(3) Uani 1 1 d . . . . .
H13 H -0.048269 0.060414 0.129803 0.042 Uiso 1 1 calc R U . . .
C14 C 0.06480(16) 0.29914(17) 0.20045(15) 0.0316(3) Uani 1 1 d . . . . .
C15 C -0.0263(2) 0.3365(2) 0.1154(2) 0.0529(5) Uani 1 1 d . . . . .
H15A H -0.115493 0.241067 0.045501 0.079 Uiso 1 1 calc R U . . .
H15B H 0.030551 0.385493 0.067998 0.079 Uiso 1 1 calc R U . . .
H15C H -0.053518 0.407377 0.176997 0.079 Uiso 1 1 calc R U . . .
B1 B 0.27407(15) 0.58382(17) 0.35890(15) 0.0208(3) Uani 1 1 d . . . . .
H1 H 0.195363 0.613257 0.310404 0.025 Uiso 1 1 calc R U . . .
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'
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'
N N 0.0061 0.0033 '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
N11 Mn N11 180.00(7) . 2_666
N11 Mn N31 85.43(4) . .
N11 Mn N31 94.57(4) 2_666 .
N11 Mn N31 94.57(4) . 2_666
N11 Mn N31 85.43(4) 2_666 2_666
N31 Mn N31 180.0 . 2_666
N11 Mn N21 94.24(4) . 2_666
N11 Mn N21 85.76(4) 2_666 2_666
N31 Mn N21 94.30(4) . 2_666
N31 Mn N21 85.70(4) 2_666 2_666
N11 Mn N21 85.76(4) . .
N11 Mn N21 94.24(4) 2_666 .
N31 Mn N21 85.70(4) . .
N31 Mn N21 94.30(4) 2_666 .
N21 Mn N21 180.0 2_666 .
C2 N11 N12 105.04(10) . .
C2 N11 Mn 139.97(9) . .
N12 N11 Mn 113.83(8) . .
C4 N12 N11 110.75(11) . .
C4 N12 B1 127.31(11) . .
N11 N12 B1 121.72(10) . .
C7 N21 N22 104.91(10) . .
C7 N21 Mn 140.84(9) . .
N22 N21 Mn 113.30(7) . .
C9 N22 N21 110.62(11) . .
C9 N22 B1 127.38(11) . .
N21 N22 B1 121.70(10) . .
C12 N31 N32 105.11(10) . .
C12 N31 Mn 139.79(9) . .
N32 N31 Mn 113.15(8) . .
C14 N32 N31 110.61(11) . .
C14 N32 B1 127.67(11) . .
N31 N32 B1 121.65(10) . .
F1 C1 F3 107.28(12) . .
F1 C1 F2 106.35(12) . .
F3 C1 F2 105.33(12) . .
F1 C1 C2 115.02(12) . .
F3 C1 C2 110.53(12) . .
F2 C1 C2 111.76(12) . .
N11 C2 C3 111.66(12) . .
N11 C2 C1 123.58(12) . .
C3 C2 C1 124.54(13) . .
C4 C3 C2 105.07(13) . .
C4 C3 H3 127.5 . .
C2 C3 H3 127.5 . .
N12 C4 C3 107.47(12) . .
N12 C4 C5 123.79(14) . .
C3 C4 C5 128.74(14) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
F5 C6 F4 107.48(12) . .
F5 C6 F6 106.35(12) . .
F4 C6 F6 105.67(13) . .
F5 C6 C7 111.43(12) . .
F4 C6 C7 113.69(12) . .
F6 C6 C7 111.78(12) . .
N21 C7 C8 111.93(12) . .
N21 C7 C6 123.56(12) . .
C8 C7 C6 124.33(13) . .
C9 C8 C7 104.86(13) . .
C9 C8 H8 127.6 . .
C7 C8 H8 127.6 . .
N22 C9 C8 107.67(12) . .
N22 C9 C10 123.22(14) . .
C8 C9 C10 129.11(14) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
F7 C11 F9 107.09(12) . .
F7 C11 F8 106.59(13) . .
F9 C11 F8 106.20(12) . .
F7 C11 C12 114.15(11) . .
F9 C11 C12 110.70(13) . .
F8 C11 C12 111.67(12) . .
N31 C12 C13 111.60(13) . .
N31 C12 C11 123.11(12) . .
C13 C12 C11 125.02(13) . .
C14 C13 C12 105.01(12) . .
C14 C13 H13 127.5 . .
C12 C13 H13 127.5 . .
N32 C14 C13 107.67(12) . .
N32 C14 C15 123.35(14) . .
C13 C14 C15 128.98(14) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N22 B1 N12 110.55(10) . .
N22 B1 N32 110.38(10) . .
N12 B1 N32 110.62(10) . .
N22 B1 H1 108.4 . .
N12 B1 H1 108.4 . .
N32 B1 H1 108.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn N11 2.2751(11) .
Mn N11 2.2751(11) 2_666
Mn N31 2.2971(11) .
Mn N31 2.2971(11) 2_666
Mn N21 2.2981(11) 2_666
Mn N21 2.2981(11) .
F1 C1 1.3262(17) .
F2 C1 1.3468(17) .
F3 C1 1.3437(17) .
F4 C6 1.3331(17) .
F5 C6 1.3314(17) .
F6 C6 1.3407(19) .
F7 C11 1.3304(17) .
F8 C11 1.3403(18) .
F9 C11 1.3400(17) .
N11 C2 1.3358(17) .
N11 N12 1.3662(14) .
N12 C4 1.3550(18) .
N12 B1 1.5442(18) .
N21 C7 1.3355(17) .
N21 N22 1.3689(14) .
N22 C9 1.3549(17) .
N22 B1 1.5401(18) .
N31 C12 1.3369(17) .
N31 N32 1.3689(15) .
N32 C14 1.3567(17) .
N32 B1 1.5444(18) .
C1 C2 1.4886(19) .
C2 C3 1.387(2) .
C3 C4 1.376(2) .
C3 H3 0.9500 .
C4 C5 1.497(2) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C7 1.4910(19) .
C7 C8 1.386(2) .
C8 C9 1.377(2) .
C8 H8 0.9500 .
C9 C10 1.497(2) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.491(2) .
C12 C13 1.391(2) .
C13 C14 1.376(2) .
C13 H13 0.9500 .
C14 C15 1.496(2) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
B1 H1 1.1200 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C2 N11 N12 C4 0.00(15) . . . .
Mn N11 N12 C4 170.23(10) . . . .
C2 N11 N12 B1 174.99(11) . . . .
Mn N11 N12 B1 -14.78(14) . . . .
C7 N21 N22 C9 -0.56(15) . . . .
Mn N21 N22 C9 170.68(10) . . . .
C7 N21 N22 B1 173.61(11) . . . .
Mn N21 N22 B1 -15.14(14) . . . .
C12 N31 N32 C14 -0.89(15) . . . .
Mn N31 N32 C14 166.48(9) . . . .
C12 N31 N32 B1 176.26(11) . . . .
Mn N31 N32 B1 -16.36(14) . . . .
N12 N11 C2 C3 0.40(16) . . . .
Mn N11 C2 C3 -165.64(12) . . . .
N12 N11 C2 C1 -174.41(12) . . . .
Mn N11 C2 C1 19.6(2) . . . .
F1 C1 C2 N11 -29.6(2) . . . .
F3 C1 C2 N11 -151.25(13) . . . .
F2 C1 C2 N11 91.79(16) . . . .
F1 C1 C2 C3 156.26(15) . . . .
F3 C1 C2 C3 34.6(2) . . . .
F2 C1 C2 C3 -82.35(19) . . . .
N11 C2 C3 C4 -0.63(19) . . . .
C1 C2 C3 C4 174.12(14) . . . .
N11 N12 C4 C3 -0.39(18) . . . .
B1 N12 C4 C3 -175.03(14) . . . .
N11 N12 C4 C5 179.62(19) . . . .
B1 N12 C4 C5 5.0(3) . . . .
C2 C3 C4 N12 0.60(19) . . . .
C2 C3 C4 C5 -179.4(2) . . . .
N22 N21 C7 C8 0.63(16) . . . .
Mn N21 C7 C8 -166.58(12) . . . .
N22 N21 C7 C6 -174.57(13) . . . .
Mn N21 C7 C6 18.2(2) . . . .
F5 C6 C7 N21 -149.07(14) . . . .
F4 C6 C7 N21 -27.4(2) . . . .
F6 C6 C7 N21 92.09(17) . . . .
F5 C6 C7 C8 36.3(2) . . . .
F4 C6 C7 C8 157.96(15) . . . .
F6 C6 C7 C8 -82.52(19) . . . .
N21 C7 C8 C9 -0.5(2) . . . .
C6 C7 C8 C9 174.69(15) . . . .
N21 N22 C9 C8 0.29(19) . . . .
B1 N22 C9 C8 -173.47(14) . . . .
N21 N22 C9 C10 -179.23(18) . . . .
B1 N22 C9 C10 7.0(3) . . . .
C7 C8 C9 N22 0.1(2) . . . .
C7 C8 C9 C10 179.6(2) . . . .
N32 N31 C12 C13 0.93(16) . . . .
Mn N31 C12 C13 -160.93(11) . . . .
N32 N31 C12 C11 -173.27(13) . . . .
Mn N31 C12 C11 24.9(2) . . . .
F7 C11 C12 N31 -33.0(2) . . . .
F9 C11 C12 N31 -153.89(13) . . . .
F8 C11 C12 N31 88.00(16) . . . .
F7 C11 C12 C13 153.60(15) . . . .
F9 C11 C12 C13 32.7(2) . . . .
F8 C11 C12 C13 -85.42(19) . . . .
N31 C12 C13 C14 -0.63(18) . . . .
C11 C12 C13 C14 173.44(14) . . . .
N31 N32 C14 C13 0.53(17) . . . .
B1 N32 C14 C13 -176.41(13) . . . .
N31 N32 C14 C15 -179.28(16) . . . .
B1 N32 C14 C15 3.8(2) . . . .
C12 C13 C14 N32 0.05(18) . . . .
C12 C13 C14 C15 179.85(18) . . . .
C9 N22 B1 N12 -115.43(15) . . . .
N21 N22 B1 N12 71.43(14) . . . .
C9 N22 B1 N32 121.87(15) . . . .
N21 N22 B1 N32 -51.27(15) . . . .
C4 N12 B1 N22 122.74(15) . . . .
N11 N12 B1 N22 -51.37(15) . . . .
C4 N12 B1 N32 -114.69(15) . . . .
N11 N12 B1 N32 71.20(14) . . . .
C14 N32 B1 N22 -110.39(15) . . . .
N31 N32 B1 N22 72.97(14) . . . .
C14 N32 B1 N12 126.94(14) . . . .
N31 N32 B1 N12 -49.69(15) . . . .
