#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:23:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179375 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/72/4327237.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_4327237
loop_
_publ_author_name
'Ferdaus Hossain'
'Matthew A. Rigsby'
'Cole T. Duncan'
'Paul L. Milligan'
'Richard L. Lord'
'Mu-Hyun Baik'
'Franklin A. Schultz'
_publ_section_title
;
 Synthesis, Structure, and Properties of Low-Spin
 Manganese(III)-Poly(pyrazolyl)borate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2596
_journal_page_last               2603
_journal_paper_doi               10.1021/ic062224+
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C18 H20 B2 Mn N12, F6 Sb'
_chemical_formula_sum            'C18 H20 B2 F6 Mn N12 Sb'
_chemical_formula_weight         716.77
_chemical_name_systematic
; 
 ? 
;
_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                99.0970(10)
_cell_angle_beta                 91.7820(10)
_cell_angle_gamma                108.5160(10)
_cell_formula_units_Z            1
_cell_length_a                   7.5518(2)
_cell_length_b                   8.8710(2)
_cell_length_c                   9.9838(3)
_cell_measurement_reflns_used    6983
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      2.9
_cell_volume                     623.87(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'XTEL (local library)'
_computing_publication_material  'XCIF (Bruker, 1999), XTEL (local library)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'0.30 degree frames measured for 3 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       ω-scans
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13743
_diffrn_reflns_theta_full        32.53
_diffrn_reflns_theta_max         32.53
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  329
_diffrn_standards_number         152
_exptl_absorpt_coefficient_mu    1.670
_exptl_absorpt_correction_T_max  0.8508
_exptl_absorpt_correction_T_min  0.7206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing (1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       plate
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         4529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0210
_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)+(0.0282P)²+0.2010P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                4248
_reflns_number_total             4529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0622242Bsi20061121_122147_1.cif
_cod_data_source_block           03238
_cod_database_code               4327237
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
Mn1 Mn 1.0000 0.5000 0.5000 0.01069(5) Uani 1 2 d S
N1 N 0.74404(15) 0.41422(13) 0.25477(10) 0.01357(18) Uani 1 1 d .
N2 N 0.79436(15) 0.35728(13) 0.36410(10) 0.01353(18) Uani 1 1 d .
N3 N 0.84144(15) 0.70252(13) 0.36540(10) 0.01331(18) Uani 1 1 d .
N4 N 0.89064(15) 0.67347(13) 0.48907(10) 0.01392(18) Uani 1 1 d .
N5 N 1.06387(15) 0.59713(13) 0.23527(10) 0.01328(18) Uani 1 1 d .
N6 N 1.14805(15) 0.56494(13) 0.34509(10) 0.01375(18) Uani 1 1 d .
C1 C 0.60145(17) 0.29774(16) 0.17826(13) 0.0164(2) Uani 1 1 d .
H1 H 0.5409 0.3077 0.0969 0.024(5) Uiso 1 1 calc R
C2 C 0.55715(19) 0.16081(16) 0.23739(14) 0.0189(2) Uani 1 1 d .
H2 H 0.4628 0.0597 0.2057 0.023(5) Uiso 1 1 calc R
C3 C 0.68131(18) 0.20401(16) 0.35350(13) 0.0165(2) Uani 1 1 d .
H3 H 0.6855 0.1349 0.4163 0.029(5) Uiso 1 1 calc R
C4 C 0.77802(17) 0.82925(15) 0.38368(13) 0.0147(2) Uani 1 1 d .
H4 H 0.7366 0.8741 0.3134 0.033(6) Uiso 1 1 calc R
C5 C 0.78331(19) 0.88336(16) 0.52244(13) 0.0166(2) Uani 1 1 d .
H5 H 0.7460 0.9703 0.5659 0.025(5) Uiso 1 1 calc R
C6 C 0.85537(18) 0.78231(15) 0.58426(13) 0.0155(2) Uani 1 1 d .
H6 H 0.8763 0.7896 0.6797 0.022(5) Uiso 1 1 calc R
C7 C 1.18728(18) 0.63473(16) 0.14218(13) 0.0162(2) Uani 1 1 d .
H7 H 1.1624 0.6620 0.0569 0.032(6) Uiso 1 1 calc R
C8 C 1.35772(19) 0.62709(18) 0.19155(13) 0.0196(2) Uani 1 1 d .
H8 H 1.4710 0.6475 0.1481 0.024(5) Uiso 1 1 calc R
C9 C 1.32593(18) 0.58287(17) 0.31879(13) 0.0173(2) Uani 1 1 d .
H9 H 1.4170 0.5676 0.3782 0.028(5) Uiso 1 1 calc R
B1 B 0.85606(19) 0.58780(17) 0.23600(13) 0.0137(2) Uani 1 1 d .
H1B H 0.808(3) 0.617(2) 0.1475(19) 0.020(4) Uiso 1 1 d .
Sb1 Sb 1.0000 1.0000 0.0000 0.01392(4) Uani 1 2 d S
F1 F 1.00198(13) 0.79953(10) -0.09430(9) 0.02283(17) Uani 1 1 d .
F2 F 1.10096(13) 0.95866(11) 0.15929(8) 0.02167(16) Uani 1 1 d .
F3 F 1.24316(12) 1.09959(12) -0.04762(10) 0.02496(18) 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'
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'
Sb Sb -0.5866 1.5461 '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
N4 Mn1 N4 180.0 . 2_766
N4 Mn1 N2 92.59(4) . 2_766
N4 Mn1 N2 87.41(4) 2_766 2_766
N4 Mn1 N2 87.41(4) . .
N4 Mn1 N2 92.59(4) 2_766 .
N2 Mn1 N2 180.0 2_766 .
N4 Mn1 N6 91.27(4) . 2_766
N4 Mn1 N6 88.73(4) 2_766 2_766
N2 Mn1 N6 87.78(4) 2_766 2_766
N2 Mn1 N6 92.22(4) . 2_766
N4 Mn1 N6 88.73(4) . .
N4 Mn1 N6 91.27(4) 2_766 .
N2 Mn1 N6 92.22(4) 2_766 .
N2 Mn1 N6 87.78(4) . .
N6 Mn1 N6 180.0 2_766 .
C1 N1 N2 109.32(10) . .
C1 N1 B1 131.81(11) . .
N2 N1 B1 118.83(10) . .
C3 N2 N1 106.84(10) . .
C3 N2 Mn1 133.25(9) . .
N1 N2 Mn1 119.91(8) . .
C4 N3 N4 109.41(10) . .
C4 N3 B1 131.96(11) . .
N4 N3 B1 118.54(10) . .
C6 N4 N3 107.16(10) . .
C6 N4 Mn1 132.58(9) . .
N3 N4 Mn1 120.22(8) . .
C7 N5 N6 109.75(10) . .
C7 N5 B1 131.18(11) . .
N6 N5 B1 119.07(10) . .
C9 N6 N5 106.87(10) . .
C9 N6 Mn1 133.45(9) . .
N5 N6 Mn1 119.66(8) . .
N1 C1 C2 108.86(11) . .
N1 C1 H1 125.6 . .
C2 C1 H1 125.6 . .
C1 C2 C3 104.72(11) . .
C1 C2 H2 127.6 . .
C3 C2 H2 127.6 . .
N2 C3 C2 110.26(11) . .
N2 C3 H3 124.9 . .
C2 C3 H3 124.9 . .
N3 C4 C5 108.51(11) . .
N3 C4 H4 125.7 . .
C5 C4 H4 125.7 . .
C4 C5 C6 104.98(11) . .
C4 C5 H5 127.5 . .
C6 C5 H5 127.5 . .
N4 C6 C5 109.94(11) . .
N4 C6 H6 125.0 . .
C5 C6 H6 125.0 . .
N5 C7 C8 108.45(11) . .
N5 C7 H7 125.8 . .
C8 C7 H7 125.8 . .
C7 C8 C9 104.84(11) . .
C7 C8 H8 127.6 . .
C9 C8 H8 127.6 . .
N6 C9 C8 110.09(11) . .
N6 C9 H9 125.0 . .
C8 C9 H9 125.0 . .
N3 B1 N5 106.61(10) . .
N3 B1 N1 106.87(10) . .
N5 B1 N1 106.53(10) . .
N3 B1 H1B 112.0(10) . .
N5 B1 H1B 112.2(10) . .
N1 B1 H1B 112.2(10) . .
F2 Sb1 F2 180.000(1) . 2_775
F2 Sb1 F3 89.85(4) . 2_775
F2 Sb1 F3 90.15(4) 2_775 2_775
F2 Sb1 F3 90.15(4) . .
F2 Sb1 F3 89.85(4) 2_775 .
F3 Sb1 F3 180.0 2_775 .
F2 Sb1 F1 90.21(4) . 2_775
F2 Sb1 F1 89.79(4) 2_775 2_775
F3 Sb1 F1 90.19(4) 2_775 2_775
F3 Sb1 F1 89.81(4) . 2_775
F2 Sb1 F1 89.79(4) . .
F2 Sb1 F1 90.21(4) 2_775 .
F3 Sb1 F1 89.81(4) 2_775 .
F3 Sb1 F1 90.19(4) . .
F1 Sb1 F1 180.0 2_775 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N4 1.9790(11) .
Mn1 N4 1.9790(11) 2_766
Mn1 N2 1.9831(10) 2_766
Mn1 N2 1.9831(10) .
Mn1 N6 1.9885(10) 2_766
Mn1 N6 1.9885(10) .
N1 C1 1.3428(16) .
N1 N2 1.3643(14) .
N1 B1 1.5478(18) .
N2 C3 1.3418(16) .
N3 C4 1.3450(16) .
N3 N4 1.3645(14) .
N3 B1 1.5432(17) .
N4 C6 1.3399(16) .
N5 C7 1.3409(16) .
N5 N6 1.3634(14) .
N5 B1 1.5454(17) .
N6 C9 1.3410(16) .
C1 C2 1.3845(19) .
C1 H1 0.9500 .
C2 C3 1.3905(18) .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 C5 1.3876(17) .
C4 H4 0.9500 .
C5 C6 1.3944(18) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.3895(18) .
C7 H7 0.9500 .
C8 C9 1.3936(18) .
C8 H8 0.9500 .
C9 H9 0.9500 .
B1 H1B 1.047(19) .
Sb1 F2 1.8792(8) .
Sb1 F2 1.8792(8) 2_775
Sb1 F3 1.8803(9) 2_775
Sb1 F3 1.8803(9) .
Sb1 F1 1.8808(8) 2_775
Sb1 F1 1.8808(8) .
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
C1 N1 N2 C3 0.24(14) .
B1 N1 N2 C3 -177.63(11) .
C1 N1 N2 Mn1 -179.27(8) .
B1 N1 N2 Mn1 2.86(14) .
N4 Mn1 N2 C3 -136.46(12) .
N4 Mn1 N2 C3 43.54(12) 2_766
N2 Mn1 N2 C3 127(100) 2_766
N6 Mn1 N2 C3 -45.29(12) 2_766
N6 Mn1 N2 C3 134.71(12) .
N4 Mn1 N2 N1 42.90(9) .
N4 Mn1 N2 N1 -137.10(9) 2_766
N2 Mn1 N2 N1 -54(100) 2_766
N6 Mn1 N2 N1 134.07(9) 2_766
N6 Mn1 N2 N1 -45.93(9) .
C4 N3 N4 C6 0.62(14) .
B1 N3 N4 C6 -176.37(11) .
C4 N3 N4 Mn1 -177.49(8) .
B1 N3 N4 Mn1 5.52(14) .
N4 Mn1 N4 C6 -142(100) 2_766
N2 Mn1 N4 C6 -45.15(12) 2_766
N2 Mn1 N4 C6 134.85(12) .
N6 Mn1 N4 C6 42.68(12) 2_766
N6 Mn1 N4 C6 -137.32(12) .
N4 Mn1 N4 N3 36(100) 2_766
N2 Mn1 N4 N3 132.40(9) 2_766
N2 Mn1 N4 N3 -47.60(9) .
N6 Mn1 N4 N3 -139.77(9) 2_766
N6 Mn1 N4 N3 40.23(9) .
C7 N5 N6 C9 -0.09(14) .
B1 N5 N6 C9 -179.46(11) .
C7 N5 N6 Mn1 -178.61(9) .
B1 N5 N6 Mn1 2.02(14) .
N4 Mn1 N6 C9 137.79(13) .
N4 Mn1 N6 C9 -42.21(13) 2_766
N2 Mn1 N6 C9 45.25(13) 2_766
N2 Mn1 N6 C9 -134.75(13) .
N6 Mn1 N6 C9 -106(100) 2_766
N4 Mn1 N6 N5 -44.16(9) .
N4 Mn1 N6 N5 135.84(9) 2_766
N2 Mn1 N6 N5 -136.70(9) 2_766
N2 Mn1 N6 N5 43.30(9) .
N6 Mn1 N6 N5 72(100) 2_766
N2 N1 C1 C2 -0.37(14) .
B1 N1 C1 C2 177.13(12) .
N1 C1 C2 C3 0.34(15) .
N1 N2 C3 C2 -0.02(15) .
Mn1 N2 C3 C2 179.40(10) .
C1 C2 C3 N2 -0.19(16) .
N4 N3 C4 C5 -0.80(14) .
B1 N3 C4 C5 175.65(12) .
N3 C4 C5 C6 0.65(14) .
N3 N4 C6 C5 -0.20(14) .
Mn1 N4 C6 C5 177.58(9) .
C4 C5 C6 N4 -0.27(15) .
N6 N5 C7 C8 0.06(15) .
B1 N5 C7 C8 179.33(13) .
N5 C7 C8 C9 -0.01(16) .
N5 N6 C9 C8 0.08(15) .
Mn1 N6 C9 C8 178.31(10) .
C7 C8 C9 N6 -0.05(16) .
C4 N3 B1 N5 123.64(13) .
N4 N3 B1 N5 -60.18(13) .
C4 N3 B1 N1 -122.74(14) .
N4 N3 B1 N1 53.43(13) .
C7 N5 B1 N3 -123.49(14) .
N6 N5 B1 N3 55.73(14) .
C7 N5 B1 N1 122.66(14) .
N6 N5 B1 N1 -58.12(13) .
C1 N1 B1 N3 124.27(13) .
N2 N1 B1 N3 -58.43(13) .
C1 N1 B1 N5 -122.06(14) .
N2 N1 B1 N5 55.24(13) .
