#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/83/4318341.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_4318341
loop_
_publ_author_name
'Heidi Rohwer'
'Jan Dillen'
_publ_contact_author_address
;
 Department of Chemistry
 University of Stellenbosch
 Private Bag X1
 Matieland 7602
 South Africa
;
_publ_contact_author_email       jlmd@sun.ac.za
_publ_contact_author_fax         27(21)8083360
_publ_contact_author_name
;
 Prof Jan Dillen
;
_publ_contact_author_phone       27(21)8083346
_publ_section_title
;
 Deviation from Tetrahedral Geometry in Me2GeCl2: Crystal Structure of a
 Model Compound and Insight from ab Initio Calculations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4167
_journal_page_last               4172
_journal_paper_doi               10.1021/ic0256011
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C16 H18 Cl2 Ge'
_chemical_formula_weight         353.79
_chemical_name_systematic
;
 dichlorodi(2-phenethyl)germane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 114.2190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2079(2)
_cell_length_b                   19.5396(4)
_cell_length_c                   9.7845(2)
_cell_measurement_reflns_used    3049
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      1.02
_cell_volume                     1605.47(6)
_computing_data_collection       'Collect (Nonius-BV)'
_computing_data_reduction        'Denzo-SMN (Otwninoski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius Kappa CCD'
_diffrn_measurement_method       'A 181 π scan and 4 ο 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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8596
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    2.225
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0318P)²+2.7994P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                2437
_reflns_number_total             3056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0256011_s1.cif
_cod_data_source_block           r2gecl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4318341
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
C4 C 0.3548(4) 0.76679(16) 0.5791(4) 0.0455(8) Uani 1 1 d . . .
H4A H 0.3810 0.7457 0.6784 0.079(3) Uiso 1 1 calc R . .
H4B H 0.2382 0.7742 0.5322 0.079(3) Uiso 1 1 calc R . .
C5 C 0.3934(7) 0.7188(2) 0.4898(6) 0.0991(19) Uani 1 1 d . . .
H5A H 0.5099 0.7113 0.5363 0.079(3) Uiso 1 1 calc R . .
H5B H 0.3666 0.7395 0.3900 0.079(3) Uiso 1 1 calc R . .
C6 C 0.3125(4) 0.64987(16) 0.4671(4) 0.0460(8) Uani 1 1 d . . .
C7 C 0.1530(4) 0.64196(18) 0.3774(4) 0.0509(9) Uani 1 1 d . . .
H7 H 0.0916 0.6807 0.3276 0.079(3) Uiso 1 1 calc R . .
C8 C 0.0809(4) 0.5786(2) 0.3586(4) 0.0535(9) Uani 1 1 d . . .
H8 H -0.0293 0.5739 0.2962 0.079(3) Uiso 1 1 calc R . .
C9 C 0.1684(4) 0.52254(17) 0.4299(4) 0.0497(9) Uani 1 1 d . . .
H9 H 0.1190 0.4789 0.4178 0.079(3) Uiso 1 1 calc R . .
C10 C 0.3267(4) 0.52959(17) 0.5185(4) 0.0467(8) Uani 1 1 d . . .
H10 H 0.3878 0.4907 0.5673 0.079(3) Uiso 1 1 calc R . .
C11 C 0.3984(4) 0.59272(18) 0.5375(4) 0.0458(8) Uani 1 1 d . . .
H11 H 0.5086 0.5970 0.6001 0.079(3) Uiso 1 1 calc R . .
C12 C 0.3424(4) 0.93857(16) 0.6117(3) 0.0437(8) Uani 1 1 d . . .
H12A H 0.2851 0.9316 0.6769 0.079(3) Uiso 1 1 calc R . .
H12B H 0.4196 0.9763 0.6550 0.079(3) Uiso 1 1 calc R . .
C13 C 0.2220(4) 0.95958(18) 0.4543(4) 0.0526(9) Uani 1 1 d . . .
H13A H 0.1615 0.9999 0.4636 0.079(3) Uiso 1 1 calc R . .
H13B H 0.2811 0.9735 0.3942 0.079(3) Uiso 1 1 calc R . .
C14 C 0.1062(4) 0.90401(16) 0.3718(3) 0.0420(8) Uani 1 1 d . . .
C15 C 0.1054(4) 0.87587(17) 0.2413(3) 0.0399(7) Uani 1 1 d . . .
H15 H 0.1786 0.8922 0.2031 0.079(3) Uiso 1 1 calc R . .
C16 C 0.0000(4) 0.82442(18) 0.1662(4) 0.0452(8) Uani 1 1 d . . .
H16 H 0.0008 0.8062 0.0765 0.079(3) Uiso 1 1 calc R . .
C17 C -0.1065(4) 0.7992(2) 0.2198(4) 0.0517(9) Uani 1 1 d . . .
H17 H -0.1780 0.7635 0.1681 0.079(3) Uiso 1 1 calc R . .
C18 C -0.1080(4) 0.8261(2) 0.3480(4) 0.0574(10) Uani 1 1 d . . .
H18 H -0.1815 0.8090 0.3852 0.079(3) Uiso 1 1 calc R . .
C19 C -0.0038(4) 0.8778(2) 0.4245(4) 0.0543(9) Uani 1 1 d . . .
H19 H -0.0065 0.8959 0.5135 0.079(3) Uiso 1 1 calc R . .
Cl2 Cl 0.66527(9) 0.85094(4) 0.82089(9) 0.0475(2) Uani 1 1 d . . .
Cl3 Cl 0.55744(11) 0.86986(4) 0.44732(10) 0.0523(2) Uani 1 1 d . . .
Ge1 Ge 0.45747(4) 0.855802(15) 0.61101(3) 0.03177(10) 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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
_geom_angle_publ_flag
C5 C4 Ge1 117.5(2) . . ?
C4 C5 C6 116.5(3) . . ?
C7 C6 C11 118.1(3) . . ?
C7 C6 C5 121.8(4) . . ?
C11 C6 C5 120.1(4) . . ?
C6 C7 C8 121.0(3) . . ?
C9 C8 C7 119.9(3) . . ?
C10 C9 C8 119.7(3) . . ?
C9 C10 C11 120.4(3) . . ?
C10 C11 C6 120.9(3) . . ?
C13 C12 Ge1 113.0(2) . . ?
C14 C13 C12 113.9(3) . . ?
C15 C14 C19 117.4(3) . . ?
C15 C14 C13 121.0(3) . . ?
C19 C14 C13 121.6(3) . . ?
C16 C15 C14 121.0(3) . . ?
C17 C16 C15 120.7(3) . . ?
C18 C17 C16 119.3(4) . . ?
C17 C18 C19 120.7(3) . . ?
C18 C19 C14 120.8(3) . . ?
C12 Ge1 C4 121.20(14) . . ?
C12 Ge1 Cl2 107.83(10) . . ?
C4 Ge1 Cl2 107.24(11) . . ?
C12 Ge1 Cl3 107.22(10) . . ?
C4 Ge1 Cl3 108.70(9) . . ?
Cl2 Ge1 Cl3 103.24(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C4 C5 1.422(5) . ?
C4 Ge1 1.943(3) . ?
C5 C6 1.510(5) . ?
C6 C7 1.376(5) . ?
C6 C11 1.378(5) . ?
C7 C8 1.381(5) . ?
C8 C9 1.369(5) . ?
C9 C10 1.363(5) . ?
C10 C11 1.375(5) . ?
C12 C13 1.539(4) . ?
C12 Ge1 1.935(3) . ?
C13 C14 1.504(5) . ?
C14 C15 1.387(4) . ?
C14 C19 1.408(5) . ?
C15 C16 1.381(5) . ?
C16 C17 1.379(5) . ?
C17 C18 1.365(5) . ?
C18 C19 1.384(5) . ?
Cl2 Ge1 2.1595(8) . ?
Cl3 Ge1 2.1673(8) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30661063
