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#$Date: 2016-03-23 15:57:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179355 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/52/4325271.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_4325271
loop_
_publ_author_name
'Minao Tang'
'Dongfeng Li'
'Uma Prasad Mallik'
'Yuan-Zhu Zhang'
'Rodolphe Clérac'
'Gordon T. Yee'
'Myung-Hwan Whangbo'
'Amshumali Mungalimane'
'Stephen M. Holmes'
_publ_section_title
;
 Synthesis and Characterization of Di- and Trivalent Pyrazolylborate
 β-Diketonates and Cyanometalates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5153
_journal_page_last               5164
_journal_paper_doi               10.1021/ic200464t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C20 H40 Mn N6'
_chemical_formula_weight         419.52
_chemical_name_common            '[NEt4]2[Mn(CN)4]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 99.1750(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4590(4)
_cell_length_b                   10.3260(3)
_cell_length_c                   15.6990(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2473.96(12)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'ω scans at fixed χ = 55°'
_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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5502
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.9222
_exptl_absorpt_correction_T_min  0.8751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'scalepack (otwinowski & Minor, 1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_description       'tetragonal prism'
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0510P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                1862
_reflns_number_total             2832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200464t_si_002_5.cif
_cod_data_source_block           5_k07258
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4325271
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.5000 -0.33876(4) 0.7500 0.02015(16) Uani 1 2 d S
N1 N 0.34906(12) -0.51914(19) 0.63531(12) 0.0320(5) Uani 1 1 d .
N2 N 0.41651(11) -0.14583(18) 0.88298(12) 0.0282(5) Uani 1 1 d .
N3 N 0.30855(10) 0.05471(16) 0.62002(10) 0.0192(4) Uani 1 1 d .
C1 C 0.40230(14) -0.4552(2) 0.67431(14) 0.0242(5) Uani 1 1 d .
C2 C 0.44367(13) -0.2136(2) 0.83598(13) 0.0207(5) Uani 1 1 d .
C3 C 0.21434(12) 0.0760(2) 0.57799(12) 0.0217(5) Uani 1 1 d .
H3A H 0.1969 0.1624 0.5927 0.026 Uiso 1 1 calc R
H3B H 0.2119 0.0731 0.5159 0.026 Uiso 1 1 calc R
C4 C 0.14832(13) -0.0192(2) 0.60232(14) 0.0289(5) Uani 1 1 d .
H4A H 0.0910 0.0024 0.5725 0.043 Uiso 1 1 calc R
H4B H 0.1484 -0.0155 0.6634 0.043 Uiso 1 1 calc R
H4C H 0.1635 -0.1051 0.5865 0.043 Uiso 1 1 calc R
C5 C 0.31835(14) 0.0642(2) 0.71792(13) 0.0232(5) Uani 1 1 d .
H5A H 0.2809 -0.0004 0.7382 0.028 Uiso 1 1 calc R
H5B H 0.3784 0.0433 0.7423 0.028 Uiso 1 1 calc R
C6 C 0.29620(14) 0.1944(2) 0.75164(13) 0.0273(5) Uani 1 1 d .
H6A H 0.3046 0.1921 0.8135 0.041 Uiso 1 1 calc R
H6B H 0.2362 0.2149 0.7298 0.041 Uiso 1 1 calc R
H6C H 0.3337 0.2591 0.7331 0.041 Uiso 1 1 calc R
C7 C 0.34035(13) -0.0799(2) 0.60136(13) 0.0230(5) Uani 1 1 d .
H7A H 0.4006 -0.0890 0.6295 0.028 Uiso 1 1 calc R
H7B H 0.3057 -0.1430 0.6269 0.028 Uiso 1 1 calc R
C8 C 0.33585(15) -0.1122(2) 0.50654(14) 0.0294(5) Uani 1 1 d .
H8A H 0.3578 -0.1983 0.5008 0.044 Uiso 1 1 calc R
H8B H 0.3708 -0.0515 0.4805 0.044 Uiso 1 1 calc R
H8C H 0.2761 -0.1074 0.4782 0.044 Uiso 1 1 calc R
C9 C 0.36131(13) 0.15870(19) 0.58266(14) 0.0227(5) Uani 1 1 d .
H9A H 0.3532 0.1478 0.5205 0.027 Uiso 1 1 calc R
H9B H 0.3374 0.2426 0.5942 0.027 Uiso 1 1 calc R
C10 C 0.45858(13) 0.1600(2) 0.61630(15) 0.0322(6) Uani 1 1 d .
H10A H 0.4858 0.2291 0.5893 0.048 Uiso 1 1 calc R
H10B H 0.4838 0.0789 0.6033 0.048 Uiso 1 1 calc R
H10C H 0.4679 0.1728 0.6776 0.048 Uiso 1 1 calc R
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'
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
C1 Mn1 C1 111.54(11) 2_656 .
C1 Mn1 C2 111.47(7) 2_656 2_656
C1 Mn1 C2 108.06(8) . 2_656
C1 Mn1 C2 108.06(8) 2_656 .
C1 Mn1 C2 111.47(7) . .
C2 Mn1 C2 106.12(11) 2_656 .
C3 N3 C7 111.52(15) . .
C3 N3 C9 105.46(15) . .
C7 N3 C9 111.21(15) . .
C3 N3 C5 111.34(14) . .
C7 N3 C5 105.70(14) . .
C9 N3 C5 111.73(15) . .
N1 C1 Mn1 178.33(19) . .
N2 C2 Mn1 177.68(18) . .
C4 C3 N3 115.90(17) . .
C4 C3 H3A 108.3 . .
N3 C3 H3A 108.3 . .
C4 C3 H3B 108.3 . .
N3 C3 H3B 108.3 . .
H3A C3 H3B 107.4 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C6 C5 N3 114.92(16) . .
C6 C5 H5A 108.5 . .
N3 C5 H5A 108.5 . .
C6 C5 H5B 108.5 . .
N3 C5 H5B 108.5 . .
H5A C5 H5B 107.5 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C8 C7 N3 115.16(17) . .
C8 C7 H7A 108.5 . .
N3 C7 H7A 108.5 . .
C8 C7 H7B 108.5 . .
N3 C7 H7B 108.5 . .
H7A C7 H7B 107.5 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C10 C9 N3 115.84(17) . .
C10 C9 H9A 108.3 . .
N3 C9 H9A 108.3 . .
C10 C9 H9B 108.3 . .
N3 C9 H9B 108.3 . .
H9A C9 H9B 107.4 . .
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 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 C1 2.137(2) 2_656
Mn1 C1 2.137(2) .
Mn1 C2 2.151(2) 2_656
Mn1 C2 2.151(2) .
N1 C1 1.152(3) .
N2 C2 1.144(3) .
N3 C3 1.516(2) .
N3 C7 1.519(3) .
N3 C9 1.521(2) .
N3 C5 1.523(2) .
C3 C4 1.510(3) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 C6 1.504(3) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.516(3) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 C10 1.512(3) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
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 Mn1 C1 N1 63(7) 2_656
C2 Mn1 C1 N1 -174(100) 2_656
C2 Mn1 C1 N1 -58(7) .
C1 Mn1 C2 N2 50(5) 2_656
C1 Mn1 C2 N2 173(5) .
C2 Mn1 C2 N2 -70(5) 2_656
C7 N3 C3 C4 57.1(2) .
C9 N3 C3 C4 177.91(16) .
C5 N3 C3 C4 -60.7(2) .
C3 N3 C5 C6 -62.8(2) .
C7 N3 C5 C6 175.97(17) .
C9 N3 C5 C6 54.9(2) .
C3 N3 C7 C8 58.3(2) .
C9 N3 C7 C8 -59.1(2) .
C5 N3 C7 C8 179.48(17) .
C3 N3 C9 C10 178.73(17) .
C7 N3 C9 C10 -60.2(2) .
C5 N3 C9 C10 57.6(2) .
