#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:16:45 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179888 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/84/7018420.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_7018420
loop_
_publ_author_name
'Li, Xiu-Bing'
'Wang, Kun'
'Ma, Yu'
'Gao, En-Qing'
'Liu, Cai-Ming'
_publ_section_title
;
 Three-dimensional networks based on trinuclear motifs with tricomponent
 azide-carboxylate-tetrazolate cobridges: synthesis, structure and
 magnetic properties.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4188
_journal_page_last               4194
_journal_paper_doi               10.1039/c2dt11966h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C16 H16 Mn3 N22 O6, 4(H2 O)'
_chemical_formula_sum            'C16 H24 Mn3 N22 O10'
_chemical_formula_weight         849.39
_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                62.913(2)
_cell_angle_beta                 80.351(2)
_cell_angle_gamma                85.288(2)
_cell_formula_units_Z            1
_cell_length_a                   7.6829(17)
_cell_length_b                   10.533(2)
_cell_length_c                   11.055(2)
_cell_measurement_reflns_used    2893
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.17
_cell_volume                     785.2(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0130
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3960
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             429
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2765
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0256
_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)+(0.0389P)²+0.2596P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0727
_reflns_number_gt                2434
_reflns_number_total             2765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt11966h.txt
_cod_data_source_block           Mn_1
_cod_database_code               7018420
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 0.70449(4) 0.84415(3) -0.24329(3) 0.02317(11) Uani 1 1 d .
Mn2 Mn 0.5000 0.5000 0.0000 0.01937(12) Uani 1 2 d S
C1 C 0.8488(3) 0.6224(2) 0.02276(19) 0.0218(4) Uani 1 1 d .
C2 C 0.9604(3) 0.6083(2) 0.13042(19) 0.0235(4) Uani 1 1 d .
H2B H 1.0763 0.5715 0.1116 0.028 Uiso 1 1 calc R
H2A H 0.9756 0.7019 0.1238 0.028 Uiso 1 1 calc R
C3 C 0.8315(3) 0.5647(2) 0.36323(19) 0.0226(4) Uani 1 1 d .
H3A H 0.8538 0.6597 0.3379 0.027 Uiso 1 1 calc R
C4 C 0.7506(3) 0.4789(2) 0.4941(2) 0.0238(4) Uani 1 1 d .
C5 C 0.7106(3) 0.3392(2) 0.5269(2) 0.0325(5) Uani 1 1 d .
H5A H 0.6501 0.2808 0.6129 0.039 Uiso 1 1 calc R
C6 C 0.7607(3) 0.2881(2) 0.4323(2) 0.0327(5) Uani 1 1 d .
H6A H 0.7354 0.1945 0.4544 0.039 Uiso 1 1 calc R
C7 C 0.8482(3) 0.3750(2) 0.3048(2) 0.0272(5) Uani 1 1 d .
H7A H 0.8865 0.3395 0.2416 0.033 Uiso 1 1 calc R
C8 C 0.7114(3) 0.5344(2) 0.59648(19) 0.0234(4) Uani 1 1 d .
O1 O 0.8795(2) 0.72893(16) -0.09018(14) 0.0327(4) Uani 1 1 d .
O2 O 0.7447(2) 0.52419(15) 0.05382(15) 0.0326(4) Uani 1 1 d .
O3 O 0.6833(2) 0.99438(17) -0.15246(17) 0.0391(4) Uani 1 1 d .
H3C H 0.7837 1.0387 -0.1756 0.059 Uiso 1 1 d R
H3B H 0.5908 1.0504 -0.1782 0.059 Uiso 1 1 d R
O4 O 0.5857(2) 0.80700(18) 0.15024(17) 0.0448(4) Uani 1 1 d .
H4A H 0.5089 0.7555 0.1568 0.067 Uiso 1 1 d R
H4B H 0.5987 0.8613 0.0738 0.067 Uiso 1 1 d R
O5 O 0.0225(3) 0.1089(2) 0.7720(2) 0.0560(5) Uani 1 1 d .
H5B H 0.0748 0.0478 0.8520 0.084 Uiso 1 1 d R
H5C H 0.0341 0.0876 0.7044 0.084 Uiso 1 1 d R
N1 N 0.2382(3) 0.8764(3) -0.0498(3) 0.0579(7) Uani 1 1 d U
N2 N 0.3505(3) 0.80560(19) -0.06993(19) 0.0311(4) Uani 1 1 d U
N3 N 0.4698(2) 0.73375(17) -0.08836(18) 0.0294(4) Uani 1 1 d U
N7 N 0.6267(2) 0.45854(18) 0.72322(17) 0.0271(4) Uani 1 1 d .
N6 N 0.6250(2) 0.54369(18) 0.78304(16) 0.0263(4) Uani 1 1 d .
N5 N 0.7051(2) 0.66435(19) 0.69586(17) 0.0279(4) Uani 1 1 d .
N4 N 0.7620(3) 0.66163(19) 0.57567(17) 0.0296(4) Uani 1 1 d .
N8 N 0.5000 1.0000 -0.5000 0.0404(7) Uani 1 2 d S
N9 N 0.5359(4) 0.9777(2) -0.3941(2) 0.0590(7) Uani 1 1 d .
N10 N 1.0000 1.0000 -0.5000 0.0315(6) Uani 1 2 d S
N11 N 0.9465(3) 0.9470(2) -0.3828(2) 0.0460(5) Uani 1 1 d .
N12 N 0.8784(2) 0.51227(17) 0.27178(15) 0.0212(4) 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'
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'
O O 0.0106 0.0060 '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
N9 Mn1 O1 174.33(8) . .
N9 Mn1 N11 92.50(10) . .
O1 Mn1 N11 85.51(7) . .
N9 Mn1 O3 91.86(8) . 1
O1 Mn1 O3 82.91(6) . 1
N11 Mn1 O3 92.01(7) . 1
N9 Mn1 O3 91.86(8) . .
O1 Mn1 O3 82.91(6) . .
N11 Mn1 O3 92.01(7) . .
O3 Mn1 O3 0.00(4) 1 .
N9 Mn1 N3 91.51(9) . .
O1 Mn1 N3 90.37(6) . .
N11 Mn1 N3 175.75(8) . .
O3 Mn1 N3 86.46(6) 1 .
O3 Mn1 N3 86.46(6) . .
N9 Mn1 N5 92.24(8) . 1_554
O1 Mn1 N5 93.24(6) . 1_554
N11 Mn1 N5 95.79(7) . 1_554
O3 Mn1 N5 171.02(6) 1 1_554
O3 Mn1 N5 171.02(6) . 1_554
N3 Mn1 N5 85.45(6) . 1_554
O2 Mn2 O2 180.00(9) 2_665 .
O2 Mn2 N3 87.47(6) 2_665 2_665
O2 Mn2 N3 92.53(6) . 2_665
O2 Mn2 N3 92.53(6) 2_665 .
O2 Mn2 N3 87.47(6) . .
N3 Mn2 N3 180.0 2_665 .
O2 Mn2 N6 87.33(6) 2_665 1_554
O2 Mn2 N6 92.67(6) . 1_554
N3 Mn2 N6 95.50(6) 2_665 1_554
N3 Mn2 N6 84.50(6) . 1_554
O2 Mn2 N6 92.67(6) 2_665 2_666
O2 Mn2 N6 87.33(6) . 2_666
N3 Mn2 N6 84.50(6) 2_665 2_666
N3 Mn2 N6 95.50(6) . 2_666
N6 Mn2 N6 180.0 1_554 2_666
O1 C1 O2 126.87(19) . .
O1 C1 C2 115.43(18) . .
O2 C1 C2 117.58(17) . .
N12 C2 C1 112.11(16) . .
N12 C2 H2B 109.2 . .
C1 C2 H2B 109.2 . .
N12 C2 H2A 109.2 . .
C1 C2 H2A 109.2 . .
H2B C2 H2A 107.9 . .
N12 C3 C4 120.49(18) . .
N12 C3 H3A 119.8 . .
C4 C3 H3A 119.8 . .
C3 C4 C5 118.43(18) . .
C3 C4 C8 120.05(18) . .
C5 C4 C8 121.50(18) . .
C6 C5 C4 119.9(2) . .
C6 C5 H5A 120.1 . .
C4 C5 H5A 120.1 . .
C5 C6 C7 120.0(2) . .
C5 C6 H6A 120.0 . .
C7 C6 H6A 120.0 . .
N12 C7 C6 119.56(19) . .
N12 C7 H7A 120.2 . .
C6 C7 H7A 120.2 . .
N4 C8 N7 112.75(17) . .
N4 C8 C4 124.28(18) . .
N7 C8 C4 122.92(18) . .
C1 O1 Mn1 129.27(14) . .
C1 O2 Mn2 137.36(13) . .
O3 O3 Mn1 0(10) 1 .
O3 O3 H3C 0.0 1 .
Mn1 O3 H3C 108.6 . .
O3 O3 H3B 0.0 1 .
Mn1 O3 H3B 108.4 . .
H3C O3 H3B 114.9 . .
H4A O4 H4B 104.0 . .
H5B O5 H5C 119.1 . .
N1 N2 N3 177.8(3) . .
N2 N3 Mn2 130.66(15) . .
N2 N3 Mn1 118.02(13) . .
Mn2 N3 Mn1 111.27(8) . .
N6 N7 C8 103.89(16) . .
N5 N6 N7 109.89(15) . .
N5 N6 Mn2 122.65(12) . 1_556
N7 N6 Mn2 127.44(13) . 1_556
N6 N5 N4 109.64(16) . .
N6 N5 Mn1 119.49(12) . 1_556
N4 N5 Mn1 130.57(13) . 1_556
C8 N4 N5 103.83(16) . .
N9 N8 N9 180.000(1) 2_674 .
N8 N9 Mn1 141.9(2) . .
N11 N10 N11 180.00(12) . 2_774
N10 N11 Mn1 139.27(17) . .
C3 N12 C7 121.50(17) . .
C3 N12 C2 119.27(16) . .
C7 N12 C2 119.20(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N9 2.174(2) .
Mn1 O1 2.1843(15) .
Mn1 N11 2.204(2) .
Mn1 O3 2.2109(16) 1
Mn1 O3 2.2109(16) .
Mn1 N3 2.2434(18) .
Mn1 N5 2.2797(18) 1_554
Mn2 O2 2.1320(15) 2_665
Mn2 O2 2.1320(15) .
Mn2 N3 2.2049(17) 2_665
Mn2 N3 2.2049(17) .
Mn2 N6 2.2765(17) 1_554
Mn2 N6 2.2765(17) 2_666
C1 O1 1.242(2) .
C1 O2 1.245(2) .
C1 C2 1.527(3) .
C2 N12 1.482(2) .
C2 H2B 0.9700 .
C2 H2A 0.9700 .
C3 N12 1.346(2) .
C3 C4 1.377(3) .
C3 H3A 0.9300 .
C4 C5 1.393(3) .
C4 C8 1.475(3) .
C5 C6 1.370(3) .
C5 H5A 0.9300 .
C6 C7 1.373(3) .
C6 H6A 0.9300 .
C7 N12 1.351(3) .
C7 H7A 0.9300 .
C8 N4 1.332(3) .
C8 N7 1.336(3) .
O3 O3 0.000(4) 1
O3 H3C 0.8730 .
O3 H3B 0.8836 .
O4 H4A 0.8060 .
O4 H4B 0.7697 .
O5 H5B 0.9566 .
O5 H5C 0.8624 .
N1 N2 1.153(3) .
N2 N3 1.191(3) .
N7 N6 1.333(2) .
N6 N5 1.318(2) .
N6 Mn2 2.2765(17) 1_556
N5 N4 1.340(2) .
N5 Mn1 2.2797(18) 1_556
N8 N9 1.161(2) 2_674
N8 N9 1.161(2) .
N10 N11 1.1661(19) .
N10 N11 1.1661(19) 2_774
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3C O5 0.87 1.93 2.796(3) 170.6 1_664
O3 H3B O4 0.88 2.03 2.823(3) 148.1 2_675
O5 H5B N1 0.96 2.08 2.943(3) 149.7 1_546
O4 H4B O3 0.77 2.25 3.007(2) 168.9 1
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_4
O1 C1 C2 N12 160.05(17) . .
O2 C1 C2 N12 -23.6(3) . .
N12 C3 C4 C5 -3.3(3) . .
N12 C3 C4 C8 175.58(19) . .
C3 C4 C5 C6 3.6(3) . .
C8 C4 C5 C6 -175.2(2) . .
C4 C5 C6 C7 -0.8(4) . .
C5 C6 C7 N12 -2.5(4) . .
C3 C4 C8 N4 -5.8(3) . .
C5 C4 C8 N4 173.0(2) . .
C3 C4 C8 N7 177.1(2) . .
C5 C4 C8 N7 -4.1(3) . .
O2 C1 O1 Mn1 31.0(3) . .
C2 C1 O1 Mn1 -152.99(14) . .
N9 Mn1 O1 C1 123.9(8) . .
N11 Mn1 O1 C1 -166.47(19) . .
O3 Mn1 O1 C1 100.94(18) 1 .
O3 Mn1 O1 C1 100.94(18) . .
N3 Mn1 O1 C1 14.55(18) . .
N5 Mn1 O1 C1 -70.91(18) 1_554 .
O1 C1 O2 Mn2 -32.2(3) . .
C2 C1 O2 Mn2 151.94(16) . .
O2 Mn2 O2 C1 -25(100) 2_665 .
N3 Mn2 O2 C1 164.3(2) 2_665 .
N3 Mn2 O2 C1 -15.7(2) . .
N6 Mn2 O2 C1 68.6(2) 1_554 .
N6 Mn2 O2 C1 -111.4(2) 2_666 .
N9 Mn1 O3 O3 0.0(4) . 1
O1 Mn1 O3 O3 0.0(4) . 1
N11 Mn1 O3 O3 0.0(4) . 1
N3 Mn1 O3 O3 0.0(4) . 1
N5 Mn1 O3 O3 0.0(4) 1_554 1
N1 N2 N3 Mn2 109(6) . .
N1 N2 N3 Mn1 -74(6) . .
O2 Mn2 N3 N2 52.0(2) 2_665 .
O2 Mn2 N3 N2 -128.0(2) . .
N3 Mn2 N3 N2 -68(100) 2_665 .
N6 Mn2 N3 N2 139.1(2) 1_554 .
N6 Mn2 N3 N2 -40.9(2) 2_666 .
O2 Mn2 N3 Mn1 -125.17(8) 2_665 .
O2 Mn2 N3 Mn1 54.83(8) . .
N3 Mn2 N3 Mn1 114(100) 2_665 .
N6 Mn2 N3 Mn1 -38.10(8) 1_554 .
N6 Mn2 N3 Mn1 141.90(8) 2_666 .
N9 Mn1 N3 N2 -48.12(18) . .
O1 Mn1 N3 N2 126.53(17) . .
N11 Mn1 N3 N2 112.6(10) . .
O3 Mn1 N3 N2 43.65(17) 1 .
O3 Mn1 N3 N2 43.65(17) . .
N5 Mn1 N3 N2 -140.25(17) 1_554 .
N9 Mn1 N3 Mn2 129.49(10) . .
O1 Mn1 N3 Mn2 -55.86(8) . .
N11 Mn1 N3 Mn2 -69.8(10) . .
O3 Mn1 N3 Mn2 -138.74(9) 1 .
O3 Mn1 N3 Mn2 -138.74(9) . .
N5 Mn1 N3 Mn2 37.36(8) 1_554 .
N4 C8 N7 N6 0.1(2) . .
C4 C8 N7 N6 177.50(19) . .
C8 N7 N6 N5 0.0(2) . .
C8 N7 N6 Mn2 178.38(14) . 1_556
N7 N6 N5 N4 0.0(2) . .
Mn2 N6 N5 N4 -178.55(14) 1_556 .
N7 N6 N5 Mn1 174.27(14) . 1_556
Mn2 N6 N5 Mn1 -4.2(2) 1_556 1_556
N7 C8 N4 N5 -0.1(2) . .
C4 C8 N4 N5 -177.5(2) . .
N6 N5 N4 C8 0.1(2) . .
Mn1 N5 N4 C8 -173.37(15) 1_556 .
N9 N8 N9 Mn1 -28(100) 2_674 .
O1 Mn1 N9 N8 136.5(7) . .
N11 Mn1 N9 N8 67.2(3) . .
O3 Mn1 N9 N8 159.3(3) 1 .
O3 Mn1 N9 N8 159.3(3) . .
N3 Mn1 N9 N8 -114.2(3) . .
N5 Mn1 N9 N8 -28.6(3) 1_554 .
N11 N10 N11 Mn1 -163(100) 2_774 .
N9 Mn1 N11 N10 -32.2(3) . .
O1 Mn1 N11 N10 153.1(3) . .
O3 Mn1 N11 N10 -124.1(2) 1 .
O3 Mn1 N11 N10 -124.1(2) . .
N3 Mn1 N11 N10 167.1(8) . .
N5 Mn1 N11 N10 60.3(2) 1_554 .
C4 C3 N12 C7 0.0(3) . .
C4 C3 N12 C2 178.19(18) . .
C6 C7 N12 C3 3.0(3) . .
C6 C7 N12 C2 -175.2(2) . .
C1 C2 N12 C3 -118.07(19) . .
C1 C2 N12 C7 60.2(2) . .
