#------------------------------------------------------------------------------
#$Date: 2016-03-21 11:04:52 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178679 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/90/4079090.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_4079090
loop_
_publ_author_name
'Engerer, Laura K.'
'Carlson, Christin N.'
'Hanusa, Timothy P.'
'Brennessel, William W.'
'Young, Victor G.'
_publ_section_title
;
 σ- vs π-Bonding in Manganese(II) Allyl Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6131
_journal_paper_doi               10.1021/om300478v
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C26 H58 Mn O2 Si4'
_chemical_formula_sum            'C26 H58 Mn O2 Si4'
_chemical_formula_weight         570.02
_chemical_name_common            02082
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   9.820(1)
_cell_length_b                   9.820(1)
_cell_length_c                   32.530(8)
_cell_measurement_reflns_used    3758
_cell_measurement_temperature    173(2)
_cell_volume                     2716.7(8)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, 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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            16226
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.899735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             933
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.138
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.43(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3218
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0330
_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)+(0.0483P)²+0.7784P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                3006
_reflns_number_total             3218
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300478v_si_002.cif
_cod_data_source_block           02082
_cod_original_sg_symbol_H-M      P3(1)21
_cod_database_code               4079090
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
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 0.18638(5) 0.18638(5) 0.0000 0.03675(13) Uani 1 2 d S A .
C1 C 0.1501(3) 0.3843(3) 0.01106(7) 0.0412(5) Uani 1 1 d . . .
H1 H 0.039(3) 0.336(3) 0.0146(6) 0.033(6) Uiso 1 1 d . . .
C2 C 0.2313(3) 0.4618(3) 0.04939(7) 0.0405(5) Uani 1 1 d . A .
H2 H 0.343(3) 0.518(3) 0.0489(7) 0.045(7) Uiso 1 1 d . . .
C3 C 0.1728(3) 0.4663(3) 0.08611(7) 0.0453(6) Uani 1 1 d . . .
H3 H 0.071(3) 0.422(3) 0.0888(7) 0.033(6) Uiso 1 1 d . . .
Si1 Si 0.2150(5) 0.5144(5) -0.03380(16) 0.0553(5) Uani 0.815(11) 1 d PDU A 1
C4 C 0.1271(11) 0.6458(9) -0.03419(18) 0.104(2) Uani 0.815(11) 1 d PDU A 1
H4A H 0.1661 0.7157 -0.0581 0.156 Uiso 0.815(11) 1 calc PR A 1
H4B H 0.1570 0.7089 -0.0090 0.156 Uiso 0.815(11) 1 calc PR A 1
H4C H 0.0122 0.5814 -0.0357 0.156 Uiso 0.815(11) 1 calc PR A 1
C5 C 0.1763(11) 0.4117(15) -0.0844(3) 0.0762(18) Uani 0.815(11) 1 d PDU A 1
H5A H 0.2152 0.4895 -0.1066 0.114 Uiso 0.815(11) 1 calc PR A 1
H5B H 0.0629 0.3408 -0.0878 0.114 Uiso 0.815(11) 1 calc PR A 1
H5C H 0.2304 0.3507 -0.0854 0.114 Uiso 0.815(11) 1 calc PR A 1
C6 C 0.4361(7) 0.6518(7) -0.03219(17) 0.098(2) Uani 0.815(11) 1 d PDU A 1
H6A H 0.4687 0.7221 -0.0561 0.147 Uiso 0.815(11) 1 calc PR A 1
H6B H 0.4893 0.5899 -0.0328 0.147 Uiso 0.815(11) 1 calc PR A 1
H6C H 0.4643 0.7144 -0.0069 0.147 Uiso 0.815(11) 1 calc PR A 1
Si1' Si 0.206(2) 0.532(2) -0.0339(8) 0.0553(5) Uani 0.185(11) 1 d PDU A 5
C4' C 0.034(3) 0.563(4) -0.0425(9) 0.104(2) Uani 0.185(11) 1 d PDU A 5
H4'1 H 0.0537 0.6309 -0.0666 0.156 Uiso 0.185(11) 1 calc PR A 5
H4'2 H 0.0188 0.6138 -0.0183 0.156 Uiso 0.185(11) 1 calc PR A 5
H4'3 H -0.0616 0.4616 -0.0472 0.156 Uiso 0.185(11) 1 calc PR A 5
C5' C 0.215(5) 0.431(7) -0.0817(16) 0.0762(18) Uani 0.185(11) 1 d PDU A 5
H5'1 H 0.2422 0.5029 -0.1051 0.114 Uiso 0.185(11) 1 calc PR A 5
H5'2 H 0.1129 0.3373 -0.0865 0.114 Uiso 0.185(11) 1 calc PR A 5
H5'3 H 0.2958 0.4010 -0.0784 0.114 Uiso 0.185(11) 1 calc PR A 5
C6' C 0.395(3) 0.712(3) -0.0245(8) 0.098(2) Uani 0.185(11) 1 d PDU A 5
H6'1 H 0.4239 0.7811 -0.0485 0.147 Uiso 0.185(11) 1 calc PR A 5
H6'2 H 0.4768 0.6834 -0.0198 0.147 Uiso 0.185(11) 1 calc PR A 5
H6'3 H 0.3867 0.7660 -0.0003 0.147 Uiso 0.185(11) 1 calc PR A 5
Si2 Si 0.29101(9) 0.55806(9) 0.13261(2) 0.05045(19) Uani 1 1 d . A .
C7 C 0.2517(5) 0.4059(5) 0.17226(10) 0.0866(12) Uani 1 1 d . . .
H7A H 0.3227 0.4548 0.1956 0.130 Uiso 1 1 calc R A .
H7B H 0.2691 0.3242 0.1604 0.130 Uiso 1 1 calc R . .
H7C H 0.1425 0.3588 0.1816 0.130 Uiso 1 1 calc R . .
C8 C 0.5046(4) 0.6602(4) 0.12040(10) 0.0741(9) Uani 1 1 d . . .
H8A H 0.5654 0.7069 0.1455 0.111 Uiso 1 1 calc R A .
H8B H 0.5290 0.7431 0.1001 0.111 Uiso 1 1 calc R . .
H8C H 0.5319 0.5844 0.1091 0.111 Uiso 1 1 calc R . .
C9 C 0.2445(5) 0.7041(6) 0.15546(12) 0.1016(14) Uani 1 1 d . . .
H9A H 0.3072 0.7487 0.1804 0.152 Uiso 1 1 calc R A .
H9B H 0.1324 0.6520 0.1624 0.152 Uiso 1 1 calc R . .
H9C H 0.2694 0.7884 0.1356 0.152 Uiso 1 1 calc R . .
O1 O 0.0387(2) 0.0130(2) 0.04540(5) 0.0533(5) Uani 1 1 d U . .
C10 C -0.0282(4) 0.0379(4) 0.08173(9) 0.0650(8) Uani 1 1 d U A .
H10A H -0.1341 0.0224 0.0760 0.078 Uiso 1 1 calc R . .
H10B H 0.0395 0.1454 0.0926 0.078 Uiso 1 1 calc R . .
C11 C -0.0373(5) -0.0811(5) 0.11104(11) 0.0981(13) Uani 1 1 d U . .
H11A H 0.0597 -0.0379 0.1278 0.118 Uiso 1 1 calc R A .
H11B H -0.1284 -0.1155 0.1297 0.118 Uiso 1 1 calc R . .
C12 C -0.0550(6) -0.2104(5) 0.08626(13) 0.1086(15) Uani 1 1 d U A .
H12A H -0.1674 -0.2914 0.0837 0.130 Uiso 1 1 calc R . .
H12B H 0.0022 -0.2593 0.0988 0.130 Uiso 1 1 calc R . .
C13 C 0.0104(6) -0.1451(4) 0.04633(12) 0.1007(14) Uani 1 1 d U A .
H13A H 0.1100 -0.1456 0.0420 0.121 Uiso 1 1 calc R . .
H13B H -0.0642 -0.2083 0.0243 0.121 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'
Si Si 0.0817 0.0704 '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
O1 Mn1 O1 86.87(10) 4 .
O1 Mn1 C1 106.59(8) 4 .
O1 Mn1 C1 104.17(8) . .
O1 Mn1 C1 104.17(8) 4 4
O1 Mn1 C1 106.59(8) . 4
C1 Mn1 C1 137.16(14) . 4
C2 C1 Si1 113.9(2) . .
C2 C1 Si1' 112.0(6) . .
C2 C1 Mn1 108.32(16) . .
Si1 C1 Mn1 109.67(17) . .
Si1' C1 Mn1 115.7(6) . .
C2 C1 H1 110.2(13) . .
Si1 C1 H1 111.0(13) . .
Si1' C1 H1 106.9(15) . .
Mn1 C1 H1 103.3(14) . .
C3 C2 C1 130.1(2) . .
C3 C2 H2 112.7(15) . .
C1 C2 H2 117.2(15) . .
C2 C3 Si2 125.0(2) . .
C2 C3 H3 118.7(15) . .
Si2 C3 H3 116.3(15) . .
C1 Si1 C5 114.8(5) . .
C1 Si1 C4 111.5(3) . .
C5 Si1 C4 109.0(4) . .
C1 Si1 C6 110.4(3) . .
C5 Si1 C6 105.0(3) . .
C4 Si1 C6 105.5(3) . .
Si1 C4 H4A 109.5 . .
Si1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
Si1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
Si1 C5 H5A 109.5 . .
Si1 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
Si1 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
Si1 C6 H6A 109.5 . .
Si1 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
Si1 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C6' Si1' C5' 110.6(17) . .
C6' Si1' C4' 115.6(14) . .
C5' Si1' C4' 104.4(16) . .
C6' Si1' C1 111.3(13) . .
C5' Si1' C1 107(3) . .
C4' Si1' C1 107.0(14) . .
Si1' C4' H4'1 109.5 . .
Si1' C4' H4'2 109.5 . .
H4'1 C4' H4'2 109.5 . .
Si1' C4' H4'3 109.5 . .
H4'1 C4' H4'3 109.5 . .
H4'2 C4' H4'3 109.5 . .
Si1' C5' H5'1 109.5 . .
Si1' C5' H5'2 109.5 . .
H5'1 C5' H5'2 109.5 . .
Si1' C5' H5'3 109.5 . .
H5'1 C5' H5'3 109.5 . .
H5'2 C5' H5'3 109.5 . .
Si1' C6' H6'1 109.5 . .
Si1' C6' H6'2 109.5 . .
H6'1 C6' H6'2 109.5 . .
Si1' C6' H6'3 109.5 . .
H6'1 C6' H6'3 109.5 . .
H6'2 C6' H6'3 109.5 . .
C3 Si2 C8 110.67(13) . .
C3 Si2 C7 110.42(14) . .
C8 Si2 C7 107.84(17) . .
C3 Si2 C9 111.49(15) . .
C8 Si2 C9 108.33(19) . .
C7 Si2 C9 108.0(2) . .
Si2 C7 H7A 109.5 . .
Si2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
Si2 C8 H8A 109.5 . .
Si2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
Si2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
Si2 C9 H9A 109.5 . .
Si2 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
Si2 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C10 O1 C13 108.1(2) . .
C10 O1 Mn1 127.68(16) . .
C13 O1 Mn1 123.73(18) . .
O1 C10 C11 104.5(3) . .
O1 C10 H10A 110.9 . .
C11 C10 H10A 110.9 . .
O1 C10 H10B 110.9 . .
C11 C10 H10B 110.9 . .
H10A C10 H10B 108.9 . .
C12 C11 C10 105.6(3) . .
C12 C11 H11A 110.6 . .
C10 C11 H11A 110.6 . .
C12 C11 H11B 110.6 . .
C10 C11 H11B 110.6 . .
H11A C11 H11B 108.7 . .
C11 C12 C13 106.2(3) . .
C11 C12 H12A 110.5 . .
C13 C12 H12A 110.5 . .
C11 C12 H12B 110.5 . .
C13 C12 H12B 110.5 . .
H12A C12 H12B 108.7 . .
O1 C13 C12 107.6(3) . .
O1 C13 H13A 110.2 . .
C12 C13 H13A 110.2 . .
O1 C13 H13B 110.2 . .
C12 C13 H13B 110.2 . .
H13A C13 H13B 108.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.1713(17) 4
Mn1 O1 2.1713(17) .
Mn1 C1 2.174(2) .
Mn1 C1 2.174(2) 4
C1 C2 1.470(3) .
C1 Si1 1.831(6) .
C1 Si1' 1.94(2) .
C1 H1 0.95(2) .
C2 C3 1.336(3) .
C2 H2 0.95(3) .
C3 Si2 1.845(3) .
C3 H3 0.87(3) .
Si1 C5 1.869(5) .
Si1 C4 1.877(5) .
Si1 C6 1.899(6) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
Si1' C6' 1.838(17) .
Si1' C5' 1.870(16) .
Si1' C4' 1.885(16) .
C4' H4'1 0.9800 .
C4' H4'2 0.9800 .
C4' H4'3 0.9800 .
C5' H5'1 0.9800 .
C5' H5'2 0.9800 .
C5' H5'3 0.9800 .
C6' H6'1 0.9800 .
C6' H6'2 0.9800 .
C6' H6'3 0.9800 .
Si2 C8 1.860(3) .
Si2 C7 1.862(3) .
Si2 C9 1.863(4) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
O1 C10 1.431(3) .
O1 C13 1.434(4) .
C10 C11 1.476(5) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.440(6) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.449(5) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
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
O1 Mn1 C1 C2 163.82(16) 4
O1 Mn1 C1 C2 72.87(18) .
C1 Mn1 C1 C2 -61.99(16) 4
O1 Mn1 C1 Si1 -71.32(19) 4
O1 Mn1 C1 Si1 -162.27(18) .
C1 Mn1 C1 Si1 62.87(17) 4
O1 Mn1 C1 Si1' -69.4(7) 4
O1 Mn1 C1 Si1' -160.4(7) .
C1 Mn1 C1 Si1' 64.8(7) 4
Si1 C1 C2 C3 128.3(3) .
Si1' C1 C2 C3 121.8(7) .
Mn1 C1 C2 C3 -109.3(3) .
C1 C2 C3 Si2 175.6(2) .
C2 C1 Si1 C5 157.7(4) .
Si1' C1 Si1 C5 -128(7) .
Mn1 C1 Si1 C5 36.2(4) .
C2 C1 Si1 C4 -77.7(4) .
Si1' C1 Si1 C4 -4(7) .
Mn1 C1 Si1 C4 160.7(4) .
C2 C1 Si1 C6 39.2(4) .
Si1' C1 Si1 C6 113(7) .
Mn1 C1 Si1 C6 -82.3(3) .
C2 C1 Si1' C6' 22.1(15) .
Si1 C1 Si1' C6' -86(7) .
Mn1 C1 Si1' C6' -102.8(14) .
C2 C1 Si1' C5' 143.3(15) .
Si1 C1 Si1' C5' 35(7) .
Mn1 C1 Si1' C5' 18.4(16) .
C2 C1 Si1' C4' -105.1(13) .
Si1 C1 Si1' C4' 146(8) .
Mn1 C1 Si1' C4' 130.1(13) .
C2 C3 Si2 C8 5.3(3) .
C2 C3 Si2 C7 -114.1(3) .
C2 C3 Si2 C9 125.9(3) .
O1 Mn1 O1 C10 -123.4(3) 4
C1 Mn1 O1 C10 -17.1(2) .
C1 Mn1 O1 C10 132.7(2) 4
O1 Mn1 O1 C13 65.8(3) 4
C1 Mn1 O1 C13 172.1(3) .
C1 Mn1 O1 C13 -38.1(3) 4
C13 O1 C10 C11 22.5(4) .
Mn1 O1 C10 C11 -149.5(2) .
O1 C10 C11 C12 -28.8(4) .
C10 C11 C12 C13 24.2(5) .
C10 O1 C13 C12 -7.9(5) .
Mn1 O1 C13 C12 164.5(3) .
C11 C12 C13 O1 -10.4(6) .
