#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:42:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178578 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/88/4068861.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_4068861
loop_
_publ_author_name
'Alberola, Antonio'
'Blair, Victoria L.'
'Carrella, Luca M.'
'Clegg, William'
'Kennedy, Alan R.'
'Klett, Jan'
'Mulvey, Robert E.'
'Newton, Sean'
'Rentschler, Eva'
'Russo, Luca'
_publ_section_title
;
 Bis[(trimethylsilyl)methyl]manganese: Structural Variations of Its
 Solvent-Free and TMEDA-, Pyridine-, and Dioxane-Complexed Forms
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2112
_journal_paper_doi               10.1021/om801135d
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C8 H22 Mn Si2'
_chemical_formula_sum            'C8 H22 Mn Si2'
_chemical_formula_weight         229.38
_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                106.652(12)
_cell_angle_beta                 100.101(11)
_cell_angle_gamma                92.256(12)
_cell_formula_units_Z            2
_cell_length_a                   5.7011(5)
_cell_length_b                   10.5246(12)
_cell_length_c                   11.0936(13)
_cell_measurement_reflns_used    2877
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     625.00(13)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'φ and ω 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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7633
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         5.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             246
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0221
_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)+(0.0239P)²+0.3168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                1971
_reflns_number_total             2187
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om801135d_si_001.cif
_cod_data_source_block           rem431
_cod_original_cell_volume        625.00(12)
_cod_database_code               4068861
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 0.25229(4) 0.52264(2) 0.00160(2) 0.01464(9) Uani 1 1 d .
C1 C 0.5599(3) 0.65661(17) 0.12868(15) 0.0179(4) Uani 1 1 d .
H1A H 0.6771 0.6040 0.1650 0.021 Uiso 1 1 d R
H1B H 0.6397 0.7028 0.0786 0.021 Uiso 1 1 d R
C2 C 0.3124(4) 0.7075(2) 0.36758(19) 0.0298(4) Uani 1 1 d .
H2A H 0.1567 0.6612 0.3196 0.045 Uiso 1 1 calc R
H2B H 0.2897 0.7776 0.4435 0.045 Uiso 1 1 calc R
H2C H 0.4143 0.6438 0.3944 0.045 Uiso 1 1 calc R
C3 C 0.2428(4) 0.88963(19) 0.19925(19) 0.0294(4) Uani 1 1 d .
H3A H 0.3162 0.9319 0.1451 0.044 Uiso 1 1 calc R
H3B H 0.2021 0.9585 0.2710 0.044 Uiso 1 1 calc R
H3C H 0.0972 0.8339 0.1483 0.044 Uiso 1 1 calc R
C4 C 0.7205(3) 0.8991(2) 0.36988(19) 0.0340(5) Uani 1 1 d .
H4A H 0.8393 0.8473 0.4043 0.051 Uiso 1 1 calc R
H4B H 0.6659 0.9624 0.4408 0.051 Uiso 1 1 calc R
H4C H 0.7929 0.9480 0.3205 0.051 Uiso 1 1 calc R
C5 C -0.0368(3) 0.60209(17) -0.10703(16) 0.0174(4) Uani 1 1 d .
H5B H -0.1080 0.6711 -0.0467 0.021 Uiso 1 1 d R
H5A H -0.1640 0.5297 -0.1552 0.021 Uiso 1 1 d R
C6 C -0.1687(4) 0.7251(2) -0.32923(19) 0.0316(5) Uani 1 1 d .
H6C H -0.2634 0.7856 -0.2767 0.047 Uiso 1 1 calc R
H6B H -0.2713 0.6451 -0.3833 0.047 Uiso 1 1 calc R
H6A H -0.1024 0.7700 -0.3837 0.047 Uiso 1 1 calc R
C7 C 0.2435(3) 0.5563(2) -0.33031(18) 0.0293(4) Uani 1 1 d .
H7C H 0.2793 0.5933 -0.3975 0.044 Uiso 1 1 calc R
H7B H 0.1427 0.4719 -0.3698 0.044 Uiso 1 1 calc R
H7A H 0.3932 0.5408 -0.2802 0.044 Uiso 1 1 calc R
C8 C 0.2891(4) 0.8313(2) -0.1367(2) 0.0357(5) Uani 1 1 d .
H8C H 0.3462 0.8672 -0.1998 0.054 Uiso 1 1 calc R
H8B H 0.4259 0.8097 -0.0816 0.054 Uiso 1 1 calc R
H8A H 0.2037 0.8978 -0.0841 0.054 Uiso 1 1 calc R
Si1 Si 0.45872(8) 0.78377(5) 0.26284(4) 0.01800(12) Uani 1 1 d .
Si2 Si 0.08184(8) 0.67686(5) -0.22214(4) 0.01884(12) 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'
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
Mn1 Mn1 Mn1 161.39(2) 2_665 2_565
C1 Mn1 C1 103.18(5) . 2_665
C1 Mn1 C5 120.31(7) . .
C1 Mn1 C5 114.33(6) . 2_565
C1 Mn1 C5 114.83(6) 2_665 .
C1 Mn1 C5 99.84(6) 2_665 2_565
C5 Mn1 C5 102.81(5) . 2_565
Mn1 C1 Mn1 76.82(5) . 2_665
Mn1 C1 H1A 109.6 . .
Mn1 C1 H1A 56.4 2_665 .
Mn1 C1 H1B 109.5 . .
Mn1 C1 H1B 77.8 2_665 .
Mn1 C1 Si1 110.51(8) . .
Mn1 C1 Si1 166.03(9) 2_665 .
H1A C1 H1B 108.1 . .
H1A C1 Si1 109.6 . .
H1B C1 Si1 109.5 . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2A C2 Si1 109.5 . .
H2B C2 H2C 109.5 . .
H2B C2 Si1 109.5 . .
H2C C2 Si1 109.5 . .
H3A C3 H3B 109.5 . .
H3A C3 H3C 109.5 . .
H3A C3 Si1 109.5 . .
H3B C3 H3C 109.5 . .
H3B C3 Si1 109.5 . .
H3C C3 Si1 109.5 . .
H4A C4 H4B 109.5 . .
H4A C4 H4C 109.5 . .
H4A C4 Si1 109.5 . .
H4B C4 H4C 109.5 . .
H4B C4 Si1 109.5 . .
H4C C4 Si1 109.5 . .
Mn1 C5 Mn1 77.19(5) . 2_565
Mn1 C5 H5B 109.5 . .
Mn1 C5 H5B 76.1 2_565 .
Mn1 C5 H5A 109.6 . .
Mn1 C5 H5A 57.7 2_565 .
Mn1 C5 Si2 110.64(8) . .
Mn1 C5 Si2 167.16(9) 2_565 .
H5B C5 H5A 108.1 . .
H5B C5 Si2 109.4 . .
H5A C5 Si2 109.5 . .
H6C C6 H6B 109.5 . .
H6C C6 H6A 109.5 . .
H6C C6 Si2 109.5 . .
H6B C6 H6A 109.5 . .
H6B C6 Si2 109.5 . .
H6A C6 Si2 109.5 . .
H7C C7 H7B 109.5 . .
H7C C7 H7A 109.5 . .
H7C C7 Si2 109.5 . .
H7B C7 H7A 109.5 . .
H7B C7 Si2 109.5 . .
H7A C7 Si2 109.5 . .
H8C C8 H8B 109.5 . .
H8C C8 H8A 109.5 . .
H8C C8 Si2 109.5 . .
H8B C8 H8A 109.5 . .
H8B C8 Si2 109.5 . .
H8A C8 Si2 109.5 . .
C1 Si1 C2 113.22(8) . .
C1 Si1 C3 111.35(8) . .
C1 Si1 C4 110.47(8) . .
C2 Si1 C3 107.84(9) . .
C2 Si1 C4 106.76(10) . .
C3 Si1 C4 106.89(10) . .
C5 Si2 C6 110.84(8) . .
C5 Si2 C7 111.96(8) . .
C5 Si2 C8 112.02(9) . .
C6 Si2 C7 106.39(9) . .
C6 Si2 C8 106.89(10) . .
C7 Si2 C8 108.45(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 Mn1 2.8874(5) 2_665
Mn1 Mn1 2.8897(5) 2_565
Mn1 C1 2.2023(17) .
Mn1 C1 2.4358(17) 2_665
Mn1 C5 2.2039(17) .
Mn1 C5 2.4203(17) 2_565
C1 Mn1 2.4358(17) 2_665
C1 H1A 0.9893 .
C1 H1B 0.9892 .
C1 Si1 1.8866(17) .
C2 H2A 0.980 .
C2 H2B 0.980 .
C2 H2C 0.980 .
C2 Si1 1.874(2) .
C3 H3A 0.980 .
C3 H3B 0.980 .
C3 H3C 0.980 .
C3 Si1 1.8729(19) .
C4 H4A 0.980 .
C4 H4B 0.980 .
C4 H4C 0.980 .
C4 Si1 1.876(2) .
C5 Mn1 2.4203(17) 2_565
C5 H5B 0.9898 .
C5 H5A 0.9897 .
C5 Si2 1.8826(17) .
C6 H6C 0.980 .
C6 H6B 0.980 .
C6 H6A 0.980 .
C6 Si2 1.8756(19) .
C7 H7C 0.980 .
C7 H7B 0.980 .
C7 H7A 0.980 .
C7 Si2 1.8725(19) .
C8 H8C 0.980 .
C8 H8B 0.980 .
C8 H8A 0.980 .
C8 Si2 1.873(2) .
