#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/69/4086901.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_4086901
loop_
_publ_author_name
'Bayram, Melike'
'Naglav, Dominik'
'Wölper, Christoph'
'Schulz, Stephan'
_publ_contact_author
;
         Prof. Dr. Schulz, Stephan
         Fachbereich Chemie der
         Universität Duisburg-Essen
         Campus Essen, Universitätsstr. 7
         D-45141 Essen, Germany
;
_publ_section_title
;
 Syntheses and Structures of Homo- and Heteroleptic Beryllium Complexes
 Containing N,N′-Chelating Ligands
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00865
_journal_year                    2017
_chemical_formula_sum            'C16 H46 Be N4 S2 Si4'
_chemical_formula_weight         480.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 116.523(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0458(16)
_cell_length_b                   9.0862(7)
_cell_length_c                   17.6799(14)
_cell_measurement_reflns_used    9741
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.56
_cell_volume                     2881.3(4)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29875
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.572
_diffrn_reflns_theta_min         2.271
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         5197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0293P)²+1.6371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4659
_reflns_number_total             5197
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00865_si_002.cif
_cod_data_source_block           mb_177m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4086901
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.953
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
S1 S 0.00770(2) 0.37622(2) 0.38768(2) 0.01481(5) Uani 1 1 d . . .
Si1 Si 0.11360(2) 0.59776(3) 0.37307(2) 0.01636(5) Uani 1 1 d . . .
Si2 Si -0.12391(2) 0.18680(3) 0.28666(2) 0.01649(5) Uani 1 1 d . . .
N1 N 0.05662(4) 0.44495(8) 0.34427(4) 0.01515(12) Uani 1 1 d . . .
N2 N -0.04086(4) 0.27200(8) 0.30720(4) 0.01588(12) Uani 1 1 d . . .
C1 C 0.08799(6) 0.72851(11) 0.43749(6) 0.02731(18) Uani 1 1 d . . .
H1A H 0.1195 0.8165 0.4501 0.041 Uiso 1 1 calc R U .
H1B H 0.0956 0.6808 0.4904 0.041 Uiso 1 1 calc R U .
H1C H 0.0355 0.7568 0.4057 0.041 Uiso 1 1 calc R U .
C2 C 0.10363(5) 0.68670(11) 0.27349(6) 0.02477(17) Uani 1 1 d . . .
H2A H 0.1129 0.6138 0.2384 0.037 Uiso 1 1 calc R U .
H2B H 0.1397 0.7672 0.2872 0.037 Uiso 1 1 calc R U .
H2C H 0.0530 0.7259 0.2425 0.037 Uiso 1 1 calc R U .
C3 C 0.21465(5) 0.54908(13) 0.43389(6) 0.0294(2) Uani 1 1 d . . .
H3A H 0.2265 0.4672 0.4059 0.044 Uiso 1 1 calc R U .
H3B H 0.2250 0.5200 0.4915 0.044 Uiso 1 1 calc R U .
H3C H 0.2453 0.6346 0.4361 0.044 Uiso 1 1 calc R U .
C4 C -0.11037(6) 0.03387(11) 0.36260(6) 0.02542(17) Uani 1 1 d . . .
H4A H -0.1576 -0.0188 0.3456 0.038 Uiso 1 1 calc R U .
H4B H -0.0940 0.0744 0.4195 0.038 Uiso 1 1 calc R U .
H4C H -0.0725 -0.0342 0.3625 0.038 Uiso 1 1 calc R U .
C5 C -0.15989(6) 0.11083(11) 0.17776(6) 0.02638(18) Uani 1 1 d . . .
H5A H -0.1727 0.1919 0.1371 0.040 Uiso 1 1 calc R U .
H5B H -0.2044 0.0513 0.1651 0.040 Uiso 1 1 calc R U .
H5C H -0.1215 0.0492 0.1737 0.040 Uiso 1 1 calc R U .
C6 C -0.19357(5) 0.31735(12) 0.29238(7) 0.0303(2) Uani 1 1 d . . .
H6A H -0.2011 0.3998 0.2536 0.045 Uiso 1 1 calc R U .
H6B H -0.1751 0.3547 0.3502 0.045 Uiso 1 1 calc R U .
H6C H -0.2410 0.2660 0.2763 0.045 Uiso 1 1 calc R U .
C7 C 0.06819(5) 0.24935(10) 0.46785(5) 0.02160(16) Uani 1 1 d . . .
H7A H 0.0376 0.1800 0.4824 0.026 Uiso 1 1 calc R U .
H7B H 0.0972 0.1915 0.4454 0.026 Uiso 1 1 calc R U .
C8 C 0.12138(6) 0.33097(13) 0.54702(6) 0.0316(2) Uani 1 1 d . . .
H8A H 0.1512 0.4006 0.5326 0.047 Uiso 1 1 calc R U .
H8B H 0.1544 0.2602 0.5887 0.047 Uiso 1 1 calc R U .
H8C H 0.0927 0.3847 0.5708 0.047 Uiso 1 1 calc R U .
Be1 Be 0.0000 0.35278(16) 0.2500 0.0144(2) Uani 1 2 d S T P
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'
Be Be 0.0005 0.0002 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 S1 N2 93.59(3) . .
N1 S1 C7 106.36(4) . .
N2 S1 C7 104.18(4) . .
N1 S1 Be1 47.52(3) . .
N2 S1 Be1 46.44(4) . .
C7 S1 Be1 117.33(4) . .
N1 Si1 C2 107.01(4) . .
N1 Si1 C1 111.46(4) . .
C2 Si1 C1 110.91(5) . .
N1 Si1 C3 112.54(4) . .
C2 Si1 C3 106.06(5) . .
C1 Si1 C3 108.73(5) . .
N2 Si2 C5 106.05(4) . .
N2 Si2 C4 111.53(4) . .
C5 Si2 C4 109.44(5) . .
N2 Si2 C6 112.26(4) . .
C5 Si2 C6 109.74(5) . .
C4 Si2 C6 107.80(5) . .
S1 N1 Si1 129.29(4) . .
S1 N1 Be1 89.68(4) . .
Si1 N1 Be1 136.65(5) . .
S1 N2 Si2 126.33(4) . .
S1 N2 Be1 90.56(4) . .
Si2 N2 Be1 137.38(4) . .
C8 C7 S1 111.07(7) . .
N2 Be1 N2 129.60(10) . 2
N2 Be1 N1 119.03(3) . 2
N2 Be1 N1 85.48(3) 2 2
N2 Be1 N1 85.48(3) . .
N2 Be1 N1 119.03(3) 2 .
N1 Be1 N1 122.97(10) 2 .
N2 Be1 S1 43.00(2) . .
N2 Be1 S1 143.87(5) 2 .
N1 Be1 S1 130.41(5) 2 .
N1 Be1 S1 42.80(2) . .
N2 Be1 S1 143.86(5) . 2
N2 Be1 S1 43.00(2) 2 2
N1 Be1 S1 42.80(2) 2 2
N1 Be1 S1 130.41(5) . 2
S1 Be1 S1 169.73(7) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 N1 1.6165(7) .
S1 N2 1.6224(7) .
S1 C7 1.8092(9) .
S1 Be1 2.3789(3) .
Si1 N1 1.7241(7) .
Si1 C2 1.8650(9) .
Si1 C1 1.8693(10) .
Si1 C3 1.8735(10) .
Si2 N2 1.7212(7) .
Si2 C5 1.8609(10) .
Si2 C4 1.8660(9) .
Si2 C6 1.8692(10) .
N1 Be1 1.7544(10) .
N2 Be1 1.7240(9) .
C7 C8 1.5210(13) .
Be1 N2 1.7240(9) 2
Be1 N1 1.7544(10) 2
Be1 S1 2.3790(3) 2
