#------------------------------------------------------------------------------
#$Date: 2025-08-20 15:06:16 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301830 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/78/4077811.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_4077811
loop_
_publ_author_name
'Toltl, Nicholas P.'
'Stradiotto, Mark'
'Morkin, Tracy L.'
'Leigh, William J.'
_publ_section_title
;
 Homo- and Cross-[2+2]-Cycloaddition of 1,1-Diphenylsilene and
 1,1-Diphenylgermene. Absolute Rate Constants for Dimerization and the
 Molecular Structures and Photochemistry of the Resulting
 1,3-Dimetallacyclobutanes
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5643
_journal_paper_doi               10.1021/om990447k
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C26 H24 Si2'
_chemical_formula_weight         392.63
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 97.2060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.5430(2)
_cell_length_b                   6.1256(2)
_cell_length_c                   17.8378(3)
_cell_measurement_reflns_used    64
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      22.49
_cell_measurement_theta_min      2.00
_cell_volume                     2226.95(8)
_computing_structure_refinement  'SHELXL-V.5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL-V.5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      300(2)
_diffrn_measurement_device_type  'Siemems Smart CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6265
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_obs          0.0396
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0486P)²+1.2468P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1012
_refine_ls_wR_factor_obs         0.0916
_reflns_number_observed          1144
_reflns_number_total             1461
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om990447k.cif
_cod_data_source_block           compound_3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+1.2468P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+1.2468P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4077811
loop_
_symmetry_equiv_pos_as_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Si1 Si 0.30667(3) 0.20061(11) 0.97800(4) 0.0381(3) Uani 1 d .
C1 C 0.23259(13) 0.0365(4) 0.9967(2) 0.0441(7) Uani 1 d .
C2 C 0.38379(12) 0.1316(4) 1.04143(13) 0.0411(6) Uani 1 d .
C3 C 0.41407(13) -0.0701(5) 1.0366(2) 0.0543(7) Uani 1 d .
H3A H 0.39514(13) -0.1726(5) 1.0021(2) 0.065 Uiso 1 calc R
C4 C 0.47164(15) -0.1220(6) 1.0819(2) 0.0693(9) Uani 1 d .
H4A H 0.49100(15) -0.2579(6) 1.0775(2) 0.083 Uiso 1 calc R
C5 C 0.5002(2) 0.0274(7) 1.1334(2) 0.0774(10) Uani 1 d .
H5A H 0.5386(2) -0.0079(7) 1.1645(2) 0.093 Uiso 1 calc R
C6 C 0.4723(2) 0.2260(7) 1.1385(2) 0.0850(11) Uani 1 d .
H6A H 0.4921(2) 0.3281(7) 1.1726(2) 0.102 Uiso 1 calc R
C7 C 0.41461(15) 0.2790(5) 1.0935(2) 0.0653(8) Uani 1 d .
H7A H 0.39610(15) 0.4161(5) 1.0982(2) 0.078 Uiso 1 calc R
C8 C 0.32196(11) 0.1915(4) 0.87683(14) 0.0411(6) Uani 1 d .
C9 C 0.35312(13) 0.3652(5) 0.8450(2) 0.0557(8) Uani 1 d .
H9A H 0.36509(13) 0.4876(5) 0.8744(2) 0.067 Uiso 1 calc R
C10 C 0.3666(2) 0.3597(6) 0.7709(2) 0.0704(9) Uani 1 d .
H10A H 0.3879(2) 0.4768(6) 0.7514(2) 0.085 Uiso 1 calc R
C11 C 0.3486(2) 0.1816(7) 0.7264(2) 0.0734(10) Uani 1 d .
H11A H 0.3574(2) 0.1784(7) 0.6765(2) 0.088 Uiso 1 calc R
C12 C 0.3179(2) 0.0094(6) 0.7554(2) 0.0712(9) Uani 1 d .
H12A H 0.3058(2) -0.1114(6) 0.7252(2) 0.085 Uiso 1 calc R
C13 C 0.30467(13) 0.0144(5) 0.8299(2) 0.0567(8) Uani 1 d .
H13A H 0.28365(13) -0.1042(5) 0.8488(2) 0.068 Uiso 1 calc R
H1A H 0.2407(13) -0.0604(44) 1.0354(15) 0.055(8) Uiso 1 d .
H1B H 0.2119(13) -0.0329(43) 0.9560(15) 0.053(8) Uiso 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'
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
C8 Si1 C2 110.11(10) . .
C8 Si1 C1 112.70(13) . 7_557
C2 Si1 C1 113.78(13) . 7_557
C8 Si1 C1 113.02(13) . .
C2 Si1 C1 114.33(13) . .
C1 Si1 C1 91.95(12) 7_557 .
C8 Si1 Si1 123.98(8) . 7_557
C2 Si1 Si1 125.91(8) . 7_557
C1 Si1 Si1 46.08(8) 7_557 7_557
C1 Si1 Si1 45.87(8) . 7_557
Si1 C1 Si1 88.05(12) 7_557 .
C7 C2 C3 116.6(2) . .
C7 C2 Si1 122.4(2) . .
C3 C2 Si1 120.9(2) . .
C4 C3 C2 121.6(3) . .
C5 C4 C3 120.0(3) . .
C6 C5 C4 119.6(3) . .
C5 C6 C7 120.7(3) . .
C6 C7 C2 121.4(3) . .
C13 C8 C9 116.4(2) . .
C13 C8 Si1 122.9(2) . .
C9 C8 Si1 120.6(2) . .
C10 C9 C8 121.7(3) . .
C11 C10 C9 120.0(3) . .
C12 C11 C10 119.9(3) . .
C11 C12 C13 120.1(3) . .
C8 C13 C12 121.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C8 1.871(3) .
Si1 C2 1.876(2) .
Si1 C1 1.881(3) 7_557
Si1 C1 1.888(3) .
Si1 Si1 2.6195(13) 7_557
C1 Si1 1.881(3) 7_557
C2 C7 1.389(4) .
C2 C3 1.391(4) .
C3 C4 1.383(4) .
C4 C5 1.375(4) .
C5 C6 1.353(5) .
C6 C7 1.385(4) .
C8 C13 1.389(4) .
C8 C9 1.398(4) .
C9 C10 1.384(4) .
C10 C11 1.373(4) .
C11 C12 1.364(4) .
C12 C13 1.390(4) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 12747011
