#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:47:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179394 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/91/4329117.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_4329117
loop_
_publ_author_name
'Subrata Naiya'
'Saptarshi Biswas'
'Michael G. B. Drew'
'Carlos J. Gómez-García'
'Ashutosh Ghosh'
_publ_section_title
;
 A Ferromagnetic Methoxido-Bridged Mn(III) Dimer and a Spin-Canted
 Metamagnetic μ1,3-Azido-Bridged Chain
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5332
_journal_page_last               5341
_journal_paper_doi               10.1021/ic300274n
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C22 H32 Mn2 N10 O4'
_chemical_formula_weight         610.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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(13)
_cell_angle_beta                 96.52(10)
_cell_angle_gamma                90.00(8)
_cell_formula_units_Z            2
_cell_length_a                   9.036(5)
_cell_length_b                   11.590(14)
_cell_length_c                   13.339(15)
_cell_measurement_reflns_used    8588
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.27
_cell_volume                     1388(2)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.0721
_diffrn_reflns_av_sigmaI/netI    0.1534
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8588
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.749
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         4011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.749
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[σ²(Fo²)+(0.0367P)²+0.0000P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                1691
_reflns_number_total             4011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300274n_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4329117
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.47061(5) 0.13332(4) 0.97281(3) 0.03590(15) Uani 1 1 d .
N1 N 0.3221(3) 0.2389(2) 0.87109(19) 0.0532(8) Uani 1 1 d .
N2 N 0.3365(3) 0.3343(2) 0.84428(18) 0.0445(7) Uani 1 1 d .
N3 N 0.3445(4) 0.4270(3) 0.8148(2) 0.0802(11) Uani 1 1 d .
N19 N 0.5497(3) 0.2724(2) 1.04874(17) 0.0431(7) Uani 1 1 d .
O11 O 0.6297(2) 0.13598(18) 0.89255(14) 0.0494(6) Uani 1 1 d .
O31 O 0.4031(2) -0.01137(16) 0.91970(16) 0.0452(5) Uani 1 1 d .
N22 N 0.3116(3) 0.1436(2) 1.07549(17) 0.0406(6) Uani 1 1 d .
H22 H 0.3468 0.1006 1.1301 0.049 Uiso 1 1 calc R
C12 C 0.7344(4) 0.2131(3) 0.8872(2) 0.0442(8) Uani 1 1 d .
C13 C 0.8367(4) 0.1956(3) 0.8170(2) 0.0559(9) Uani 1 1 d .
H13 H 0.8297 0.1299 0.7768 0.067 Uiso 1 1 calc R
C14 C 0.9467(4) 0.2744(4) 0.8072(3) 0.0729(12) Uani 1 1 d .
H14 H 1.0135 0.2610 0.7604 0.087 Uiso 1 1 calc R
C15 C 0.9611(4) 0.3728(4) 0.8648(3) 0.0840(13) Uani 1 1 d .
H15 H 1.0360 0.4258 0.8567 0.101 Uiso 1 1 calc R
C16 C 0.8635(4) 0.3913(3) 0.9340(3) 0.0747(12) Uani 1 1 d .
H16 H 0.8723 0.4581 0.9729 0.090 Uiso 1 1 calc R
C17 C 0.7497(4) 0.3119(3) 0.9483(2) 0.0487(9) Uani 1 1 d .
C18 C 0.6578(4) 0.3354(3) 1.0261(2) 0.0491(9) Uani 1 1 d .
H18 H 0.6780 0.4023 1.0638 0.059 Uiso 1 1 calc R
C20 C 0.4681(4) 0.3033(3) 1.1345(2) 0.0577(10) Uani 1 1 d .
H20A H 0.4716 0.3861 1.1453 0.069 Uiso 1 1 calc R
H20B H 0.5127 0.2657 1.1955 0.069 Uiso 1 1 calc R
C21 C 0.3100(4) 0.2644(3) 1.1094(2) 0.0523(9) Uani 1 1 d .
H21A H 0.2570 0.2705 1.1685 0.063 Uiso 1 1 calc R
H21B H 0.2599 0.3125 1.0566 0.063 Uiso 1 1 calc R
C23 C 0.1610(4) 0.1012(3) 1.0417(3) 0.0603(10) Uani 1 1 d .
H23A H 0.0982 0.1126 1.0943 0.090 Uiso 1 1 calc R
H23B H 0.1653 0.0204 1.0262 0.090 Uiso 1 1 calc R
H23C H 0.1210 0.1428 0.9825 0.090 Uiso 1 1 calc R
C32 C 0.3124(4) -0.0269(3) 0.8311(3) 0.0759(13) Uani 1 1 d .
H32A H 0.2358 0.0309 0.8253 0.114 Uiso 1 1 calc R
H32B H 0.2676 -0.1021 0.8308 0.114 Uiso 1 1 calc R
H32C H 0.3702 -0.0204 0.7753 0.114 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'
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'
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
O11 Mn1 O31 92.07(13) . .
O11 Mn1 N19 91.32(13) . .
O31 Mn1 N19 171.09(10) . .
O11 Mn1 N22 172.51(10) . .
O31 Mn1 N22 94.52(13) . .
N19 Mn1 N22 81.66(13) . .
O11 Mn1 N1 95.32(13) . .
O31 Mn1 N1 96.61(14) . .
N19 Mn1 N1 91.28(14) . .
N22 Mn1 N1 87.46(13) . .
O11 Mn1 O31 90.45(12) . 3_657
O31 Mn1 O31 78.42(14) . 3_657
N19 Mn1 O31 93.32(13) . 3_657
N22 Mn1 O31 87.40(12) . 3_657
N1 Mn1 O31 172.54(9) . 3_657
O11 Mn1 Mn1 91.53(12) . 3_657
O31 Mn1 Mn1 43.03(10) . 3_657
N19 Mn1 Mn1 128.63(11) . 3_657
N22 Mn1 Mn1 90.86(12) . 3_657
N1 Mn1 Mn1 139.35(11) . 3_657
O31 Mn1 Mn1 35.38(9) 3_657 3_657
N2 N1 Mn1 129.7(3) . .
N3 N2 N1 176.7(4) . .
C18 N19 C20 120.3(3) . .
C18 N19 Mn1 125.5(2) . .
C20 N19 Mn1 114.2(2) . .
C12 O11 Mn1 130.1(2) . .
C32 O31 Mn1 125.0(2) . .
C32 O31 Mn1 133.0(2) . 3_657
Mn1 O31 Mn1 101.58(14) . 3_657
C23 N22 C21 111.8(3) . .
C23 N22 Mn1 117.4(2) . .
C21 N22 Mn1 106.6(2) . .
C23 N22 H22 106.8 . .
C21 N22 H22 106.8 . .
Mn1 N22 H22 106.8 . .
O11 C12 C13 118.2(3) . .
O11 C12 C17 123.4(3) . .
C13 C12 C17 118.4(3) . .
C14 C13 C12 120.6(4) . .
C14 C13 H13 119.7 . .
C12 C13 H13 119.7 . .
C13 C14 C15 121.7(4) . .
C13 C14 H14 119.1 . .
C15 C14 H14 119.1 . .
C16 C15 C14 118.8(4) . .
C16 C15 H15 120.6 . .
C14 C15 H15 120.6 . .
C15 C16 C17 121.8(4) . .
C15 C16 H16 119.1 . .
C17 C16 H16 119.1 . .
C12 C17 C16 118.7(3) . .
C12 C17 C18 123.4(3) . .
C16 C17 C18 117.9(3) . .
N19 C18 C17 125.7(3) . .
N19 C18 H18 117.2 . .
C17 C18 H18 117.2 . .
N19 C20 C21 107.5(3) . .
N19 C20 H20A 110.2 . .
C21 C20 H20A 110.2 . .
N19 C20 H20B 110.2 . .
C21 C20 H20B 110.2 . .
H20A C20 H20B 108.5 . .
N22 C21 C20 108.2(3) . .
N22 C21 H21A 110.1 . .
C20 C21 H21A 110.1 . .
N22 C21 H21B 110.1 . .
C20 C21 H21B 110.1 . .
H21A C21 H21B 108.4 . .
N22 C23 H23A 109.5 . .
N22 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
N22 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
O31 C32 H32A 109.5 . .
O31 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
O31 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O11 1.887(3) .
Mn1 O31 1.894(3) .
Mn1 N19 1.992(4) .
Mn1 N22 2.098(3) .
Mn1 N1 2.174(4) .
Mn1 O31 2.233(4) 3_657
Mn1 Mn1 3.205(4) 3_657
N1 N2 1.174(3) .
N2 N3 1.149(4) .
N19 C18 1.283(4) .
N19 C20 1.474(4) .
O11 C12 1.309(4) .
O31 C32 1.371(4) .
O31 Mn1 2.233(4) 3_657
N22 C23 1.469(4) .
N22 C21 1.472(4) .
N22 H22 0.9100 .
C12 C13 1.404(4) .
C12 C17 1.403(5) .
C13 C14 1.367(5) .
C13 H13 0.9300 .
C14 C15 1.372(5) .
C14 H14 0.9300 .
C15 C16 1.365(5) .
C15 H15 0.9300 .
C16 C17 1.408(4) .
C16 H16 0.9300 .
C17 C18 1.428(4) .
C18 H18 0.9300 .
C20 C21 1.500(5) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
