#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:19:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179407 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/04/4330438.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_4330438
loop_
_publ_author_name
'Sandeep K. Kondaveeti'
'Shivaiah Vaddypally'
'Carol Lam'
'Daigorou Hirai'
'Ni Ni'
'Robert J. Cava'
'Michael J. Zdilla'
_publ_section_title
;
 Synthesis, Structure, and Magnetic Studies of Manganese-Oxygen Clusters
 of Reduced Coordination Number, Featuring an Unchelated, 5-Coordinate
 Octanuclear Manganese Cluster with Water-Derived Oxo Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10095
_journal_page_last               10104
_journal_paper_doi               10.1021/ic202448c
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C32 H62 Mn2 N2 O4 Si4'
_chemical_formula_sum            'C32 H62 Mn2 N2 O4 Si4'
_chemical_formula_weight         761.08
_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                97.530(2)
_cell_angle_beta                 106.0430(10)
_cell_angle_gamma                107.005(2)
_cell_formula_units_Z            1
_cell_length_a                   8.8769(7)
_cell_length_b                   10.9042(8)
_cell_length_c                   12.3175(9)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0585
_cell_measurement_theta_min      2.6415
_cell_volume                     1066.23(14)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       'COSMO (Bruker-AXS)'
_computing_data_reduction        'SADABS (Bruker-AXS)'
_computing_molecular_graphics    XP
_computing_publication_material  'APEX II report generator (Bruker-AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Kappa APEX II DUO'
_diffrn_measurement_method       '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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14471
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.9434
_exptl_absorpt_correction_T_min  0.7984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Estimated minimum and maximum transmission:  0.6204  0.7456
 The ratio of these values is more reliable than their absolute values!
 Additional spherical absorption correction applied with mu*r =  0.2000
 Lambda/2 correction factor = 0.0015 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       needle
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         5028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0366P)²+0.5566P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1089
_reflns_number_gt                3999
_reflns_number_total             5028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202448c_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4330438
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 0.46947(4) 0.04807(3) 0.11829(3) 0.04658(11) Uani 1 1 d .
Si1 Si 0.32868(9) 0.21485(7) 0.26661(6) 0.05402(17) Uani 1 1 d .
Si2 Si 0.70063(9) 0.27324(8) 0.34940(5) 0.05955(19) Uani 1 1 d .
O1 O 0.3851(2) 0.04568(16) -0.05644(12) 0.0516(4) Uani 1 1 d .
O3 O 0.3209(3) -0.13315(17) 0.14473(15) 0.0680(5) Uani 1 1 d .
N1 N 0.5054(2) 0.19154(18) 0.25315(14) 0.0468(4) Uani 1 1 d .
C1 C 0.3271(3) 0.1326(2) -0.10867(19) 0.0525(5) Uani 1 1 d .
C2 C 0.2279(4) 0.0943(4) -0.2239(2) 0.0822(9) Uani 1 1 d .
H2 H 0.1978 0.0080 -0.2648 0.099 Uiso 1 1 calc R
C3 C 0.1731(6) 0.1831(5) -0.2788(3) 0.1132(14) Uani 1 1 d .
H3 H 0.1092 0.1566 -0.3572 0.136 Uiso 1 1 calc R
C4 C 0.2108(6) 0.3087(5) -0.2206(4) 0.1139(15) Uani 1 1 d .
H4 H 0.1723 0.3677 -0.2582 0.137 Uiso 1 1 calc R
C5 C 0.3062(6) 0.3470(4) -0.1057(4) 0.1064(13) Uani 1 1 d .
H5 H 0.3326 0.4328 -0.0651 0.128 Uiso 1 1 calc R
C6 C 0.3640(4) 0.2594(3) -0.0490(3) 0.0748(8) Uani 1 1 d .
H6 H 0.4278 0.2865 0.0293 0.090 Uiso 1 1 calc R
C13 C 0.2119(5) -0.2498(3) 0.0587(3) 0.0984(11) Uani 1 1 d .
H13A H 0.2633 -0.2695 0.0018 0.118 Uiso 1 1 calc R
H13B H 0.1076 -0.2388 0.0191 0.118 Uiso 1 1 calc R
C14 C 0.1820(7) -0.3562(4) 0.1200(4) 0.1372(19) Uani 1 1 d .
H14A H 0.0635 -0.3958 0.1070 0.165 Uiso 1 1 calc R
H14B H 0.2222 -0.4239 0.0928 0.165 Uiso 1 1 calc R
C15 C 0.2716(9) -0.2974(4) 0.2419(4) 0.162(3) Uani 1 1 d .
H15A H 0.1974 -0.3204 0.2866 0.194 Uiso 1 1 calc R
H15B H 0.3628 -0.3299 0.2688 0.194 Uiso 1 1 calc R
C16 C 0.3339(6) -0.1611(3) 0.2567(3) 0.1044(13) Uani 1 1 d .
H16A H 0.4496 -0.1261 0.3069 0.125 Uiso 1 1 calc R
H16B H 0.2701 -0.1206 0.2923 0.125 Uiso 1 1 calc R
C21 C 0.1410(3) 0.0976(3) 0.1460(3) 0.0798(8) Uani 1 1 d .
H21A H 0.1244 0.0093 0.1559 0.120 Uiso 1 1 calc R
H21B H 0.1580 0.1037 0.0729 0.120 Uiso 1 1 calc R
H21C H 0.0443 0.1196 0.1473 0.120 Uiso 1 1 calc R
C22 C 0.3237(5) 0.3832(3) 0.2544(3) 0.0858(9) Uani 1 1 d .
H22A H 0.3534 0.4045 0.1882 0.129 Uiso 1 1 calc R
H22B H 0.4018 0.4468 0.3234 0.129 Uiso 1 1 calc R
H22C H 0.2133 0.3846 0.2454 0.129 Uiso 1 1 calc R
C23 C 0.2963(5) 0.1887(4) 0.4071(3) 0.0871(9) Uani 1 1 d .
H23A H 0.3878 0.2512 0.4706 0.131 Uiso 1 1 calc R
H23B H 0.2905 0.1009 0.4139 0.131 Uiso 1 1 calc R
H23C H 0.1939 0.2007 0.4087 0.131 Uiso 1 1 calc R
C24 C 0.7276(4) 0.4365(3) 0.4388(3) 0.0926(11) Uani 1 1 d .
H24A H 0.6526 0.4234 0.4828 0.139 Uiso 1 1 calc R
H24B H 0.7034 0.4934 0.3884 0.139 Uiso 1 1 calc R
H24C H 0.8406 0.4760 0.4908 0.139 Uiso 1 1 calc R
C25 C 0.7644(6) 0.1759(5) 0.4580(3) 0.1116(14) Uani 1 1 d .
H25A H 0.7639 0.0939 0.4182 0.167 Uiso 1 1 calc R
H25B H 0.6871 0.1586 0.5002 0.167 Uiso 1 1 calc R
H25C H 0.8745 0.2254 0.5112 0.167 Uiso 1 1 calc R
C26 C 0.8546(4) 0.3067(4) 0.2703(3) 0.0921(11) Uani 1 1 d .
H26A H 0.8330 0.3663 0.2221 0.138 Uiso 1 1 calc R
H26B H 0.8443 0.2255 0.2228 0.138 Uiso 1 1 calc R
H26C H 0.9656 0.3455 0.3253 0.138 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'
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'
Si Si 0.0817 0.0704 '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
N1 Mn1 O1 127.46(7) . .
N1 Mn1 O1 137.17(7) . 2_655
O1 Mn1 O1 79.33(6) . 2_655
N1 Mn1 O3 106.70(7) . .
O1 Mn1 O3 108.03(7) . .
O1 Mn1 O3 91.62(7) 2_655 .
N1 Mn1 Mn1 150.69(6) . 2_655
O1 Mn1 Mn1 40.01(4) . 2_655
O1 Mn1 Mn1 39.31(4) 2_655 2_655
O3 Mn1 Mn1 102.59(5) . 2_655
N1 Si1 C23 113.33(13) . .
N1 Si1 C21 109.90(11) . .
C23 Si1 C21 107.60(16) . .
N1 Si1 C22 113.15(13) . .
C23 Si1 C22 107.09(16) . .
C21 Si1 C22 105.33(16) . .
N1 Si2 C26 109.76(12) . .
N1 Si2 C25 111.93(17) . .
C26 Si2 C25 108.35(19) . .
N1 Si2 C24 114.64(13) . .
C26 Si2 C24 106.73(17) . .
C25 Si2 C24 105.09(18) . .
C1 O1 Mn1 129.27(13) . .
C1 O1 Mn1 122.41(13) . 2_655
Mn1 O1 Mn1 100.67(6) . 2_655
C13 O3 C16 108.2(2) . .
C13 O3 Mn1 127.63(19) . .
C16 O3 Mn1 123.71(18) . .
Si2 N1 Si1 124.39(10) . .
Si2 N1 Mn1 119.91(10) . .
Si1 N1 Mn1 115.57(10) . .
O1 C1 C2 120.0(2) . .
O1 C1 C6 121.5(2) . .
C2 C1 C6 118.6(3) . .
C3 C2 C1 120.4(3) . .
C3 C2 H2 119.8 . .
C1 C2 H2 119.8 . .
C4 C3 C2 121.1(4) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
C3 C4 C5 119.0(3) . .
C3 C4 H4 120.5 . .
C5 C4 H4 120.5 . .
C4 C5 C6 120.8(4) . .
C4 C5 H5 119.6 . .
C6 C5 H5 119.6 . .
C1 C6 C5 120.1(3) . .
C1 C6 H6 120.0 . .
C5 C6 H6 120.0 . .
O3 C13 C14 106.5(3) . .
O3 C13 H13A 110.4 . .
C14 C13 H13A 110.4 . .
O3 C13 H13B 110.4 . .
C14 C13 H13B 110.4 . .
H13A C13 H13B 108.6 . .
C15 C14 C13 106.7(3) . .
C15 C14 H14A 110.4 . .
C13 C14 H14A 110.4 . .
C15 C14 H14B 110.4 . .
C13 C14 H14B 110.4 . .
H14A C14 H14B 108.6 . .
C16 C15 C14 108.5(4) . .
C16 C15 H15A 110.0 . .
C14 C15 H15A 110.0 . .
C16 C15 H15B 110.0 . .
C14 C15 H15B 110.0 . .
H15A C15 H15B 108.4 . .
C15 C16 O3 108.0(3) . .
C15 C16 H16A 110.1 . .
O3 C16 H16A 110.1 . .
C15 C16 H16B 110.1 . .
O3 C16 H16B 110.1 . .
H16A C16 H16B 108.4 . .
Si1 C21 H21A 109.5 . .
Si1 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
Si1 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
Si1 C22 H22A 109.5 . .
Si1 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
Si1 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
Si1 C23 H23A 109.5 . .
Si1 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
Si1 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
Si2 C24 H24A 109.5 . .
Si2 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
Si2 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
Si2 C25 H25A 109.5 . .
Si2 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
Si2 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
Si2 C26 H26A 109.5 . .
Si2 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
Si2 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N1 2.0106(17) .
Mn1 O1 2.0680(14) .
Mn1 O1 2.0987(15) 2_655
Mn1 O3 2.1523(18) .
Mn1 Mn1 3.2077(6) 2_655
Si1 N1 1.7089(19) .
Si1 C23 1.875(3) .
Si1 C21 1.873(3) .
Si1 C22 1.874(3) .
Si2 N1 1.6989(19) .
Si2 C26 1.868(3) .
Si2 C25 1.882(4) .
Si2 C24 1.879(3) .
O1 C1 1.356(3) .
O1 Mn1 2.0987(15) 2_655
O3 C13 1.427(4) .
O3 C16 1.432(3) .
C1 C2 1.380(4) .
C1 C6 1.377(4) .
C2 C3 1.377(5) .
C2 H2 0.9300 .
C3 C4 1.358(6) .
C3 H3 0.9300 .
C4 C5 1.367(6) .
C4 H4 0.9300 .
C5 C6 1.388(4) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C13 C14 1.465(5) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 C15 1.444(6) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C16 1.393(5) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 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
_geom_torsion_site_symmetry_4
N1 Mn1 O1 C1 -6.4(2) . .
O1 Mn1 O1 C1 -149.2(2) 2_655 .
O3 Mn1 O1 C1 122.62(19) . .
Mn1 Mn1 O1 C1 -149.2(2) 2_655 .
N1 Mn1 O1 Mn1 142.73(8) . 2_655
O1 Mn1 O1 Mn1 0.0 2_655 2_655
O3 Mn1 O1 Mn1 -88.22(8) . 2_655
N1 Mn1 O3 C13 154.4(3) . .
O1 Mn1 O3 C13 14.4(3) . .
O1 Mn1 O3 C13 -64.9(3) 2_655 .
Mn1 Mn1 O3 C13 -26.8(3) 2_655 .
N1 Mn1 O3 C16 -34.3(3) . .
O1 Mn1 O3 C16 -174.3(3) . .
O1 Mn1 O3 C16 106.4(3) 2_655 .
Mn1 Mn1 O3 C16 144.5(3) 2_655 .
C26 Si2 N1 Si1 -143.75(18) . .
C25 Si2 N1 Si1 95.90(19) . .
C24 Si2 N1 Si1 -23.7(2) . .
C26 Si2 N1 Mn1 40.62(19) . .
C25 Si2 N1 Mn1 -79.73(18) . .
C24 Si2 N1 Mn1 160.71(15) . .
C23 Si1 N1 Si2 -56.31(19) . .
C21 Si1 N1 Si2 -176.72(16) . .
C22 Si1 N1 Si2 65.86(19) . .
C23 Si1 N1 Mn1 119.50(15) . .
C21 Si1 N1 Mn1 -0.92(17) . .
C22 Si1 N1 Mn1 -118.33(15) . .
O1 Mn1 N1 Si2 -116.21(11) . .
O1 Mn1 N1 Si2 2.70(18) 2_655 .
O3 Mn1 N1 Si2 114.23(12) . .
Mn1 Mn1 N1 Si2 -63.52(18) 2_655 .
O1 Mn1 N1 Si1 67.78(14) . .
O1 Mn1 N1 Si1 -173.31(8) 2_655 .
O3 Mn1 N1 Si1 -61.77(12) . .
Mn1 Mn1 N1 Si1 120.47(10) 2_655 .
Mn1 O1 C1 C2 -158.9(2) . .
Mn1 O1 C1 C2 57.7(3) 2_655 .
Mn1 O1 C1 C6 20.7(3) . .
Mn1 O1 C1 C6 -122.7(2) 2_655 .
O1 C1 C2 C3 -177.8(3) . .
C6 C1 C2 C3 2.6(5) . .
C1 C2 C3 C4 -2.0(7) . .
C2 C3 C4 C5 0.7(7) . .
C3 C4 C5 C6 0.0(7) . .
O1 C1 C6 C5 178.4(3) . .
C2 C1 C6 C5 -2.0(5) . .
C4 C5 C6 C1 0.7(6) . .
C16 O3 C13 C14 -9.8(5) . .
Mn1 O3 C13 C14 162.6(3) . .
O3 C13 C14 C15 1.5(6) . .
C13 C14 C15 C16 7.6(8) . .
C14 C15 C16 O3 -13.7(7) . .
C13 O3 C16 C15 14.8(6) . .
Mn1 O3 C16 C15 -158.0(4) . .
