#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/02/2200235.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2200235
loop_
_publ_author_name
'Bolte, Michael'
'Faber, Alexander'
_publ_section_title
;
 Dihydridotetrakis(3-picoline)silicon dibromide chloroform tetrasolvate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o276
_journal_page_last               o278
_journal_paper_doi               10.1107/S1600536801003415
_journal_volume                  57
_journal_year                    2001
_chemical_formula_sum            'C28 H34 Br2 Cl12 N4 Si'
_chemical_formula_weight         1039.90
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.650(10)
_cell_angle_beta                 90.680(10)
_cell_angle_gamma                108.630(10)
_cell_formula_units_Z            1
_cell_length_a                   8.8400(10)
_cell_length_b                   10.0590(10)
_cell_length_c                   13.3300(10)
_cell_measurement_reflns_used    7621
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     1111.3(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Siemens CCD three-circle'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0869
_diffrn_reflns_av_sigmaI/netI    .0747
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22862
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  1200
_diffrn_standards_number         160
_exptl_absorpt_coefficient_mu    2.598
_exptl_absorpt_correction_T_max  .60
_exptl_absorpt_correction_T_min  .37
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             518
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .20
_refine_diff_density_max         2.386
_refine_diff_density_min         -.846
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         5095
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          .1339
_refine_ls_R_factor_gt           .0926
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0856P)²+12.6187P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .2682
_reflns_number_gt                3406
_reflns_number_total             5095
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wn6005.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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 
;
_cod_original_cell_volume        1111.35(19)
_cod_database_code               2200235
_cod_database_fobs_code          2200235
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Si1 .0000 .5000 .0000 .0181(6) Uani d SD 1 . . Si
H1 .095(8) .592(6) -.062(5) .022 Uiso d D 1 . . H
N11 .1233(8) .6138(7) .1258(5) .0245(13) Uani d . 1 . . N
C12 .0870(9) .5698(9) .2165(6) .0279(17) Uani d . 1 . . C
H12 .0024 .4839 .2190 .034 Uiso calc R 1 . . H
C13 .1699(10) .6467(10) .3067(7) .0346(19) Uani d . 1 . . C
C131 .1271(14) .5955(13) .4048(8) .059(3) Uani d . 1 . . C
H13A .0186 .5272 .3978 .088 Uiso calc R 1 . . H
H13B .1317 .6758 .4565 .088 Uiso calc R 1 . . H
H13C .2027 .5495 .4250 .088 Uiso calc R 1 . . H
C14 .2969(9) .7754(9) .2986(6) .0306(18) Uani d . 1 . . C
H14 .3556 .8321 .3581 .037 Uiso calc R 1 . . H
C15 .3335(10) .8167(9) .2068(6) .0318(18) Uani d . 1 . . C
H15 .4190 .9009 .2016 .038 Uiso calc R 1 . . H
C16 .2460(9) .7358(8) .1209(6) .0278(17) Uani d . 1 . . C
H16 .2718 .7657 .0568 .033 Uiso calc R 1 . . H
N21 .1444(8) .3859(7) -.0114(5) .0240(13) Uani d . 1 . . N
C22 .1176(10) .2725(8) .0383(6) .0278(17) Uani d . 1 . . C
H22 .0270 .2490 .0782 .033 Uiso calc R 1 . . H
C23 .2159(11) .1886(9) .0340(7) .0350(19) Uani d . 1 . . C
C231 .1800(14) .0644(11) .0918(8) .050(3) Uani d . 1 . . C
H23A .2541 .0888 .1517 .075 Uiso calc R 1 . . H
H23B .1925 -.0175 .0482 .075 Uiso calc R 1 . . H
H23C .0699 .0409 .1131 .075 Uiso calc R 1 . . H
C24 .3474(11) .2239(10) -.0254(8) .040(2) Uani d . 1 . . C
H24 .4175 .1690 -.0308 .048 Uiso calc R 1 . . H
C25 .3753(11) .3401(10) -.0768(7) .040(2) Uani d . 1 . . C
H25 .4643 .3645 -.1179 .048 Uiso calc R 1 . . H
C26 .2747(10) .4198(9) -.0683(6) .0303(18) Uani d . 1 . . C
H26 .2963 .5001 -.1028 .036 Uiso calc R 1 . . H
C1 .8545(14) .0240(12) .3371(9) .056(3) Uani d . 1 . . C
H11 .8022 .0465 .2776 .067 Uiso calc R 1 . . H
Cl11 .9042(8) -.1295(4) .2984(4) .1131(17) Uani d . 1 . . Cl
Cl12 .7192(5) -.0003(5) .4349(4) .1039(14) Uani d . 1 . . Cl
Cl13 1.0267(5) .1644(5) .3757(4) .0996(14) Uani d . 1 . . Cl
C2 .4663(12) -.3654(11) .6797(8) .048(2) Uani d . 1 . . C
H21 .4338 -.2974 .7295 .058 Uiso calc R 1 . . H
Cl21 .2981(4) -.5164(5) .6433(3) .0908(13) Uani d . 1 . . Cl
Cl22 .6144(4) -.4136(4) .7382(3) .0755(10) Uani d . 1 . . Cl
Cl23 .5386(4) -.2817(5) .5741(3) .0904(13) Uani d . 1 . . Cl
Br1 .32492(12) .85295(10) -.14354(7) .0387(3) Uani d . 1 . . Br
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si .0817 .0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
H1 Si1 N21 . . 90(3) ?
H1 Si1 N21 . 2_565 90(3) ?
N21 Si1 N21 . 2_565 179.9990(10) ?
H1 Si1 N11 . 2_565 88(3) ?
N21 Si1 N11 . 2_565 90.2(3) ?
N21 Si1 N11 2_565 2_565 89.8(3) ?
H1 Si1 N11 . . 92(3) ?
N21 Si1 N11 . . 89.8(3) y
N21 Si1 N11 2_565 . 90.2(3) ?
N11 Si1 N11 2_565 . 179.9990(10) ?
H1 Si1 H1 . . 0(3) ?
N21 Si1 H1 . . 90(3) ?
N21 Si1 H1 2_565 . 90(3) ?
N11 Si1 H1 2_565 . 88(3) ?
N11 Si1 H1 . . 92(3) ?
C12 N11 C16 . . 119.6(7) ?
C12 N11 Si1 . . 120.1(5) ?
C16 N11 Si1 . . 120.3(5) ?
N11 C12 C13 . . 122.0(8) ?
N11 C12 H12 . . 119.0 ?
C13 C12 H12 . . 119.0 ?
C12 C13 C14 . . 116.8(8) ?
C12 C13 C131 . . 120.6(8) ?
C14 C13 C131 . . 122.6(8) ?
C13 C131 H13A . . 109.5 ?
C13 C131 H13B . . 109.5 ?
H13A C131 H13B . . 109.5 ?
C13 C131 H13C . . 109.5 ?
H13A C131 H13C . . 109.5 ?
H13B C131 H13C . . 109.5 ?
C15 C14 C13 . . 120.4(8) ?
C15 C14 H14 . . 119.8 ?
C13 C14 H14 . . 119.8 ?
C14 C15 C16 . . 119.7(8) ?
C14 C15 H15 . . 120.2 ?
C16 C15 H15 . . 120.2 ?
N11 C16 C15 . . 121.6(7) ?
N11 C16 H16 . . 119.2 ?
C15 C16 H16 . . 119.2 ?
C22 N21 C26 . . 118.3(7) ?
C22 N21 Si1 . . 120.6(5) ?
C26 N21 Si1 . . 121.1(5) ?
N21 C22 C23 . . 123.3(7) ?
N21 C22 H22 . . 118.4 ?
C23 C22 H22 . . 118.4 ?
C22 C23 C24 . . 117.6(8) ?
C22 C23 C231 . . 120.6(8) ?
C24 C23 C231 . . 121.8(8) ?
C23 C231 H23A . . 109.5 ?
C23 C231 H23B . . 109.5 ?
H23A C231 H23B . . 109.5 ?
C23 C231 H23C . . 109.5 ?
H23A C231 H23C . . 109.5 ?
H23B C231 H23C . . 109.5 ?
C25 C24 C23 . . 119.4(8) ?
C25 C24 H24 . . 120.3 ?
C23 C24 H24 . . 120.3 ?
C26 C25 C24 . . 120.2(8) ?
C26 C25 H25 . . 119.9 ?
C24 C25 H25 . . 119.9 ?
N21 C26 C25 . . 121.2(8) ?
N21 C26 H26 . . 119.4 ?
C25 C26 H26 . . 119.4 ?
Cl13 C1 Cl11 . . 109.6(7) ?
Cl13 C1 Cl12 . . 110.7(7) ?
Cl11 C1 Cl12 . . 111.5(7) ?
Cl13 C1 H11 . . 108.3 ?
Cl11 C1 H11 . . 108.3 ?
Cl12 C1 H11 . . 108.3 ?
Cl22 C2 Cl23 . . 110.7(6) ?
Cl22 C2 Cl21 . . 109.7(6) ?
Cl23 C2 Cl21 . . 110.6(6) ?
Cl22 C2 H21 . . 108.6 ?
Cl23 C2 H21 . . 108.6 ?
Cl21 C2 H21 . . 108.6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Si1 H1 . 1.401(10) ?
Si1 N21 . 1.966(6) y
Si1 N21 2_565 1.966(6) ?
Si1 N11 2_565 1.990(7) ?
Si1 N11 . 1.990(7) ?
Si1 H1 . 1.401(10) ?
N11 C12 . 1.349(10) ?
N11 C16 . 1.363(10) ?
C12 C13 . 1.396(12) ?
C12 H12 . .9500 ?
C13 C14 . 1.435(12) ?
C13 C131 . 1.478(14) ?
C131 H13A . .9800 ?
C131 H13B . .9800 ?
C131 H13C . .9800 ?
C14 C15 . 1.354(12) ?
C14 H14 . .9500 ?
C15 C16 . 1.378(12) ?
C15 H15 . .9500 ?
C16 H16 . .9500 ?
N21 C22 . 1.353(10) ?
N21 C26 . 1.363(10) ?
C22 C23 . 1.388(11) ?
C22 H22 . .9500 ?
C23 C24 . 1.393(13) ?
C23 C231 . 1.505(12) ?
C231 H23A . .9800 ?
C231 H23B . .9800 ?
C231 H23C . .9800 ?
C24 C25 . 1.389(13) ?
C24 H24 . .9500 ?
C25 C26 . 1.371(12) ?
C25 H25 . .9500 ?
C26 H26 . .9500 ?
C1 Cl13 . 1.729(12) ?
C1 Cl11 . 1.752(12) ?
C1 Cl12 . 1.769(12) ?
C1 H11 . 1.0000 ?
C2 Cl22 . 1.743(11) ?
C2 Cl23 . 1.758(11) ?
C2 Cl21 . 1.760(11) ?
C2 H21 . 1.0000 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C1 H11 Br1 2_665 1.00 2.58 3.565(12) 169.9
C2 H21 Br1 1_546 1.00 2.52 3.519(11) 173.9
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_site_symmetry_1
_geom_torsion
H1 Si1 N11 C12 . -177(3)
N21 Si1 N11 C12 . -86.8(6)
N21 Si1 N11 C12 2_565 93.2(6)
H1 Si1 N11 C16 . 2(3)
N21 Si1 N11 C16 . 92.5(6)
N21 Si1 N11 C16 2_565 -87.5(6)
C16 N11 C12 C13 . 1.0(12)
Si1 N11 C12 C13 . -179.7(6)
N11 C12 C13 C14 . -.2(12)
N11 C12 C13 C131 . -180.0(9)
C12 C13 C14 C15 . -1.0(13)
C131 C13 C14 C15 . 178.8(9)
C13 C14 C15 C16 . 1.3(13)
C12 N11 C16 C15 . -.7(11)
Si1 N11 C16 C15 . -180.0(6)
C14 C15 C16 N11 . -.5(12)
H1 Si1 N21 C22 . 178(3)
N11 Si1 N21 C22 2_565 -94.4(6)
N11 Si1 N21 C22 . 85.6(6)
H1 Si1 N21 C26 . -1(3)
N11 Si1 N21 C26 2_565 86.5(6)
N11 Si1 N21 C26 . -93.5(6)
C26 N21 C22 C23 . -.2(12)
Si1 N21 C22 C23 . -179.4(7)
N21 C22 C23 C24 . -.5(13)
N21 C22 C23 C231 . 179.6(8)
C22 C23 C24 C25 . .4(14)
C231 C23 C24 C25 . -179.7(9)
C23 C24 C25 C26 . .5(15)
C22 N21 C26 C25 . 1.1(12)
Si1 N21 C26 C25 . -179.7(7)
C24 C25 C26 N21 . -1.3(14)
