#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:13:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179099 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/61/4306104.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_4306104
loop_
_publ_author_name
'Ying-Bing Lu'
'Ming-Sheng Wang'
'Wei-Wei Zhou'
'Gang Xu'
'Guo-Cong Guo'
'Jin-Shun Huang'
_publ_section_title
;
Novel 3-D PtS-like Tetrazolate-Bridged Manganese(II) Complex Exhibiting
Spin-Canted Antiferromagnetism and Field-Induced Spin-Flop Transition
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8935
_journal_page_last               8942
_journal_paper_doi               10.1021/ic801026y
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         Mn3(C8N36O6H18)
_chemical_formula_sum            'C8 H18 Mn3 N36 O6'
_chemical_formula_weight         879.40
_chemical_melting_point          ?
_chemical_name_common            Mn3(C8N36O6H18)
_chemical_name_systematic        Mn3(C8N36O6H18)
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.286(3)
_cell_length_b                   11.406(4)
_cell_length_c                   25.703(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2722.4(16)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2002)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Siemens SHELXTLTM 5'
_computing_structure_refinement  'Siemens SHELXTLTM 5'
_computing_structure_solution    'Siemens SHELXTLTM 5'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_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  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0085
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            8344
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sphere (Rigaku CrystalClear)'
_exptl_crystal_colour            'pale red'
_exptl_crystal_density_diffrn    2.146
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       blcok
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0067(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1262
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0303
_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)+(0.1400P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                1246
_reflns_number_total             1262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801026y_si_002_1.cif
_cod_data_source_block           72
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2722.5(15)
_cod_database_code               4306104
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.0000 0.5000 0.0000 0.0132(3) Uani 1 4 d S . .
Mn2 Mn 0.5000 0.5000 0.176271(13) 0.0132(3) Uani 1 2 d S . .
N1 N 0.33489(14) 0.43581(12) 0.11825(5) 0.0157(4) Uani 1 1 d . . .
N2 N 0.24409(16) 0.50344(10) 0.09019(6) 0.0160(5) Uani 1 1 d . . .
N3 N 0.16391(13) 0.43645(13) 0.06099(5) 0.0184(4) Uani 1 1 d . . .
N4 N 0.19808(15) 0.32308(11) 0.06762(5) 0.0182(4) Uani 1 1 d . . .
N5 N 0.36353(15) 0.22502(12) 0.12157(5) 0.0173(4) Uani 1 1 d . . .
H5A H 0.3324 0.1598 0.1091 0.021 Uiso 1 1 calc R . .
N6 N 0.52328(16) 0.12043(17) 0.17635(5) 0.0147(4) Uani 1 1 d . . .
H6A H 0.4975 0.0504 0.1682 0.018 Uiso 1 1 calc R . .
N7 N 0.62781(14) 0.15201(12) 0.21091(5) 0.0178(4) Uani 1 1 d . . .
N8 N 0.63446(15) 0.26468(13) 0.21259(5) 0.0196(4) Uani 1 1 d . . .
N9 N 0.53582(18) 0.31197(12) 0.17922(5) 0.0149(4) Uani 1 1 d . . .
C1 C 0.30252(17) 0.32608(13) 0.10349(6) 0.0138(4) Uani 1 1 d . . .
C2 C 0.46943(19) 0.21984(15) 0.15776(6) 0.0132(4) Uani 1 1 d . . .
O1 O 0.3486(2) 0.5000 0.2500 0.0160(5) Uani 1 2 d S . .
H1A H 0.2485 0.5000 0.2500 0.024 Uiso 1 2 calc SR . .
O1W O -0.1030(3) 0.33254(18) 0.0000 0.0398(6) Uani 1 2 d SD . .
HW1 H -0.1944(11) 0.328(3) 0.0000 0.060 Uiso 1 2 d SD . .
HW2 H -0.080(3) 0.2603(13) 0.0000 0.060 Uiso 1 2 d SD . .
O2W O 0.0452(4) 0.1246(3) 0.0000 0.0674(8) Uani 1 2 d SD . .
HW3 H 0.108(3) 0.152(4) 0.0212(13) 0.101 Uiso 1 1 d 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
O1W Mn1 O1W 180.0 . 9_565 ?
O1W Mn1 N3 89.16(7) . 9_565 ?
O1W Mn1 N3 90.84(7) 9_565 9_565 ?
O1W Mn1 N3 90.84(7) . . ?
O1W Mn1 N3 89.16(7) 9_565 . ?
N3 Mn1 N3 180.00(8) 9_565 . ?
O1W Mn1 N3 89.16(7) . 2_565 ?
O1W Mn1 N3 90.84(7) 9_565 2_565 ?
N3 Mn1 N3 85.84(7) 9_565 2_565 ?
N3 Mn1 N3 94.16(7) . 2_565 ?
O1W Mn1 N3 90.84(7) . 10 ?
O1W Mn1 N3 89.16(7) 9_565 10 ?
N3 Mn1 N3 94.16(7) 9_565 10 ?
N3 Mn1 N3 85.84(7) . 10 ?
N3 Mn1 N3 180.00(5) 2_565 10 ?
N9 Mn2 N9 176.00(7) 2_665 . ?
N9 Mn2 N1 103.83(5) 2_665 . ?
N9 Mn2 N1 78.87(5) . . ?
N9 Mn2 N1 78.87(5) 2_665 2_665 ?
N9 Mn2 N1 103.83(6) . 2_665 ?
N1 Mn2 N1 97.46(7) . 2_665 ?
N9 Mn2 O1 93.63(4) 2_665 2_665 ?
N9 Mn2 O1 83.15(4) . 2_665 ?
N1 Mn2 O1 159.04(4) . 2_665 ?
N1 Mn2 O1 97.22(5) 2_665 2_665 ?
N9 Mn2 O1 83.15(4) 2_665 . ?
N9 Mn2 O1 93.63(4) . . ?
N1 Mn2 O1 97.22(5) . . ?
N1 Mn2 O1 159.04(4) 2_665 . ?
O1 Mn2 O1 73.13(8) 2_665 . ?
C1 N1 N2 103.99(12) . . ?
C1 N1 Mn2 129.83(10) . . ?
N2 N1 Mn2 126.18(10) . . ?
N3 N2 N1 109.20(13) . . ?
N2 N3 N4 110.88(12) . . ?
N2 N3 Mn1 125.78(11) . . ?
N4 N3 Mn1 123.10(10) . . ?
C1 N4 N3 103.54(12) . . ?
C2 N5 C1 124.85(14) . . ?
C2 N5 H5A 117.6 . . ?
C1 N5 H5A 117.6 . . ?
C2 N6 N7 106.07(16) . . ?
C2 N6 H6A 127.0 . . ?
N7 N6 H6A 127.0 . . ?
N8 N7 N6 108.64(13) . . ?
N7 N8 N9 109.93(12) . . ?
C2 N9 N8 104.94(13) . . ?
C2 N9 Mn2 133.71(12) . . ?
N8 N9 Mn2 120.97(10) . . ?
N4 C1 N1 112.39(13) . . ?
N4 C1 N5 120.88(13) . . ?
N1 C1 N5 126.72(14) . . ?
N6 C2 N9 110.42(15) . . ?
N6 C2 N5 123.88(16) . . ?
N9 C2 N5 125.69(15) . . ?
Mn2 O1 Mn2 106.87(8) 7_545 . ?
Mn2 O1 H1A 126.6 7_545 . ?
Mn2 O1 H1A 126.6 . . ?
Mn1 O1W HW1 120(2) . . ?
Mn1 O1W HW2 139(2) . . ?
HW1 O1W HW2 101(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1W 2.1364(19) . ?
Mn1 O1W 2.1364(19) 9_565 ?
Mn1 N3 2.3022(13) 9_565 ?
Mn1 N3 2.3022(13) . ?
Mn1 N3 2.3022(13) 2_565 ?
Mn1 N3 2.3022(13) 10 ?
Mn2 N9 2.1717(15) 2_665 ?
Mn2 N9 2.1717(15) . ?
Mn2 N1 2.2607(13) . ?
Mn2 N1 2.2607(13) 2_665 ?
Mn2 O1 2.3595(13) 2_665 ?
Mn2 O1 2.3595(13) . ?
N1 C1 1.342(2) . ?
N1 N2 1.3515(19) . ?
N2 N3 1.304(2) . ?
N3 N4 1.342(2) . ?
N4 C1 1.339(2) . ?
N5 C2 1.355(2) . ?
N5 C1 1.366(2) . ?
N5 H5A 0.8600 . ?
N6 C2 1.328(2) . ?
N6 N7 1.3643(19) . ?
N6 H6A 0.8600 . ?
N7 N8 1.2873(19) . ?
N8 N9 1.3660(19) . ?
N9 C2 1.337(2) . ?
O1 Mn2 2.3595(13) 7_545 ?
O1 H1A 0.9300 . ?
O1W HW1 0.850(10) . ?
O1W HW2 0.852(10) . ?
O2W HW3 0.856(10) . ?
