#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/07/52/4075231.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_4075231
loop_
_publ_author_name
'Gaderbauer, Walter'
'Zirngast, Michaela'
'Baumgartner, Judith'
'Marschner, Christoph'
'Tilley, T. Don'
_publ_section_title
;
 Synthesis of Polysilanylmagnesium Compounds
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2599
_journal_page_last               2606
_journal_paper_doi               10.1021/om060147k
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C22 H58 Br2 Mg2 O2 Si6'
_chemical_formula_weight         731.66
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0433(16)
_cell_length_b                   24.718(5)
_cell_length_c                   10.042(2)
_cell_measurement_temperature    100(2)
_cell_volume                     1981.6(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '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  0.0922
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14101
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    2.275
_exptl_absorpt_correction_T_max  0.6589
_exptl_absorpt_correction_T_min  0.4483
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0442P)²+5.0882P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                2600
_reflns_number_total             3495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060147ksi20060307_052954.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4075231
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Si1 Si 0.4534(2) 0.14443(7) 0.80626(17) 0.0222(4) Uani 1 1 d .
Si2 Si 0.1819(2) 0.17047(7) 0.83893(18) 0.0266(4) Uani 1 1 d .
Si3 Si 0.4498(2) 0.11434(8) 0.58596(18) 0.0308(5) Uani 1 1 d .
Mg1 Mg 0.5582(2) 0.06692(8) 0.9651(2) 0.0235(5) Uani 1 1 d .
Br1 Br 0.36484(8) 0.02553(2) 1.12674(6) 0.0261(2) Uani 1 1 d .
O1 O 0.7579(5) 0.08282(18) 1.1003(4) 0.0319(11) Uani 1 1 d .
C1 C 0.5804(8) 0.2100(3) 0.8229(7) 0.0331(16) Uani 1 1 d .
H1A H 0.6951 0.2028 0.8041 0.050 Uiso 1 1 calc R
H1B H 0.5829 0.2242 0.9143 0.050 Uiso 1 1 calc R
H1C H 0.5284 0.2368 0.7587 0.050 Uiso 1 1 calc R
C2 C 0.1900(9) 0.2063(3) 1.0032(7) 0.053(2) Uani 1 1 d .
H2A H 0.0768 0.2177 1.0175 0.079 Uiso 1 1 calc R
H2B H 0.2626 0.2381 1.0028 0.079 Uiso 1 1 calc R
H2C H 0.2348 0.1818 1.0756 0.079 Uiso 1 1 calc R
C3 C 0.0400(8) 0.1108(3) 0.8449(7) 0.0371(17) Uani 1 1 d .
H3A H 0.0849 0.0867 0.9181 0.056 Uiso 1 1 calc R
H3B H 0.0326 0.0912 0.7595 0.056 Uiso 1 1 calc R
H3C H -0.0718 0.1232 0.8603 0.056 Uiso 1 1 calc R
C4 C 0.0819(9) 0.2185(3) 0.7081(8) 0.052(2) Uani 1 1 d .
H4A H -0.0200 0.2337 0.7376 0.077 Uiso 1 1 calc R
H4B H 0.0531 0.1990 0.6234 0.077 Uiso 1 1 calc R
H4C H 0.1604 0.2478 0.6949 0.077 Uiso 1 1 calc R
C5 C 0.3271(8) 0.0499(3) 0.5593(7) 0.0352(17) Uani 1 1 d .
H5A H 0.2101 0.0566 0.5723 0.053 Uiso 1 1 calc R
H5B H 0.3747 0.0226 0.6238 0.053 Uiso 1 1 calc R
H5C H 0.3323 0.0367 0.4678 0.053 Uiso 1 1 calc R
C6 C 0.3637(10) 0.1643(3) 0.4541(7) 0.053(2) Uani 1 1 d .
H6A H 0.3638 0.1481 0.3650 0.080 Uiso 1 1 calc R
H6B H 0.4336 0.1969 0.4607 0.080 Uiso 1 1 calc R
H6C H 0.2488 0.1739 0.4678 0.080 Uiso 1 1 calc R
C7 C 0.6701(9) 0.0990(4) 0.5536(8) 0.060(2) Uani 1 1 d .
H7A H 0.7165 0.0703 0.6144 0.090 Uiso 1 1 calc R
H7B H 0.7389 0.1317 0.5689 0.090 Uiso 1 1 calc R
H7C H 0.6698 0.0871 0.4605 0.090 Uiso 1 1 calc R
C8 C 0.8746(9) 0.0426(3) 1.1645(7) 0.050(2) Uani 1 1 d .
H8A H 0.9564 0.0316 1.1035 0.060 Uiso 1 1 calc R
H8B H 0.8136 0.0101 1.1896 0.060 Uiso 1 1 calc R
C9 C 0.9612(10) 0.0701(5) 1.2868(8) 0.074(3) Uani 1 1 d .
H9A H 0.9063 0.0610 1.3670 0.089 Uiso 1 1 calc R
H9B H 1.0803 0.0591 1.3030 0.089 Uiso 1 1 calc R
C10 C 0.9462(14) 0.1268(5) 1.2572(9) 0.093(4) Uani 1 1 d .
H10A H 1.0420 0.1392 1.2119 0.112 Uiso 1 1 calc R
H10B H 0.9444 0.1479 1.3408 0.112 Uiso 1 1 calc R
C11 C 0.7809(11) 0.1343(3) 1.1645(9) 0.065(3) Uani 1 1 d .
H11A H 0.6874 0.1428 1.2167 0.079 Uiso 1 1 calc R
H11B H 0.7905 0.1635 1.0983 0.079 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'
Mg Mg 0.0486 0.0363 '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'
Br Br -0.2901 2.4595 '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
C1 Si1 Si3 107.3(2) . .
C1 Si1 Si2 104.6(2) . .
Si3 Si1 Si2 108.50(10) . .
C1 Si1 Mg1 116.5(2) . .
Si3 Si1 Mg1 108.46(9) . .
Si2 Si1 Mg1 111.08(9) . .
C2 Si2 C3 107.5(3) . .
C2 Si2 C4 106.6(4) . .
C3 Si2 C4 108.1(3) . .
C2 Si2 Si1 108.8(2) . .
C3 Si2 Si1 111.8(2) . .
C4 Si2 Si1 113.8(2) . .
C5 Si3 C7 107.1(4) . .
C5 Si3 C6 108.4(3) . .
C7 Si3 C6 106.5(4) . .
C5 Si3 Si1 110.6(2) . .
C7 Si3 Si1 109.0(3) . .
C6 Si3 Si1 114.8(3) . .
O1 Mg1 Si1 116.62(16) . .
O1 Mg1 Br1 102.05(15) . 3_657
Si1 Mg1 Br1 121.06(9) . 3_657
O1 Mg1 Br1 98.35(15) . .
Si1 Mg1 Br1 120.45(8) . .
Br1 Mg1 Br1 93.61(7) 3_657 .
O1 Mg1 Mg1 104.97(16) . 3_657
Si1 Mg1 Mg1 138.33(11) . 3_657
Br1 Mg1 Mg1 47.08(5) 3_657 3_657
Br1 Mg1 Mg1 46.53(5) . 3_657
Mg1 Br1 Mg1 86.39(7) 3_657 .
C11 O1 C8 111.5(6) . .
C11 O1 Mg1 121.8(5) . .
C8 O1 Mg1 125.6(4) . .
O1 C8 C9 105.2(7) . .
C10 C9 C8 104.7(7) . .
C9 C10 C11 106.7(7) . .
O1 C11 C10 102.7(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C1 1.913(6) .
Si1 Si3 2.331(2) .
Si1 Si2 2.338(2) .
Si1 Mg1 2.568(3) .
Si2 C2 1.866(7) .
Si2 C3 1.871(7) .
Si2 C4 1.877(7) .
Si3 C5 1.876(7) .
Si3 C7 1.879(7) .
Si3 C6 1.880(7) .
Mg1 O1 2.011(4) .
Mg1 Br1 2.568(2) 3_657
Mg1 Br1 2.592(2) .
Mg1 Mg1 3.532(4) 3_657
Br1 Mg1 2.568(2) 3_657
O1 C11 1.429(9) .
O1 C8 1.461(8) .
C8 C9 1.499(11) .
C9 C10 1.435(13) .
C10 C11 1.539(12) .
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
C1 Si1 Si2 C2 -55.4(4) . .
Si3 Si1 Si2 C2 -169.7(3) . .
Mg1 Si1 Si2 C2 71.2(3) . .
C1 Si1 Si2 C3 -173.9(3) . .
Si3 Si1 Si2 C3 71.7(3) . .
Mg1 Si1 Si2 C3 -47.4(3) . .
C1 Si1 Si2 C4 63.3(4) . .
Si3 Si1 Si2 C4 -51.0(3) . .
Mg1 Si1 Si2 C4 -170.2(3) . .
C1 Si1 Si3 C5 -179.9(3) . .
Si2 Si1 Si3 C5 -67.3(2) . .
Mg1 Si1 Si3 C5 53.4(3) . .
C1 Si1 Si3 C7 62.6(4) . .
Si2 Si1 Si3 C7 175.1(3) . .
Mg1 Si1 Si3 C7 -64.1(3) . .
C1 Si1 Si3 C6 -56.9(4) . .
Si2 Si1 Si3 C6 55.7(3) . .
Mg1 Si1 Si3 C6 176.4(3) . .
C1 Si1 Mg1 O1 3.1(3) . .
Si3 Si1 Mg1 O1 124.29(17) . .
Si2 Si1 Mg1 O1 -116.56(17) . .
C1 Si1 Mg1 Br1 -122.0(2) . 3_657
Si3 Si1 Mg1 Br1 -0.77(13) . 3_657
Si2 Si1 Mg1 Br1 118.39(10) . 3_657
C1 Si1 Mg1 Br1 122.0(2) . .
Si3 Si1 Mg1 Br1 -116.83(10) . .
Si2 Si1 Mg1 Br1 2.33(13) . .
C1 Si1 Mg1 Mg1 179.3(3) . 3_657
Si3 Si1 Mg1 Mg1 -59.50(18) . 3_657
Si2 Si1 Mg1 Mg1 59.65(18) . 3_657
O1 Mg1 Br1 Mg1 -102.74(15) . 3_657
Si1 Mg1 Br1 Mg1 129.55(12) . 3_657
Br1 Mg1 Br1 Mg1 0.0 3_657 3_657
Si1 Mg1 O1 C11 37.1(6) . .
Br1 Mg1 O1 C11 171.3(5) 3_657 .
Br1 Mg1 O1 C11 -93.2(5) . .
Mg1 Mg1 O1 C11 -140.3(5) 3_657 .
Si1 Mg1 O1 C8 -156.1(5) . .
Br1 Mg1 O1 C8 -21.9(5) 3_657 .
Br1 Mg1 O1 C8 73.6(5) . .
Mg1 Mg1 O1 C8 26.5(5) 3_657 .
C11 O1 C8 C9 7.0(8) . .
Mg1 O1 C8 C9 -161.0(5) . .
O1 C8 C9 C10 -23.6(9) . .
C8 C9 C10 C11 30.9(10) . .
C8 O1 C11 C10 11.2(8) . .
Mg1 O1 C11 C10 179.7(5) . .
C9 C10 C11 O1 -26.3(10) . .
