#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:36:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179508 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/05/4340585.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_4340585
loop_
_publ_author_name
'Swarnakar, Anindya K.'
'McDonald, Sean M.'
'Deutsch, Kelsey C.'
'Choi, Paul'
'Ferguson, Michael J.'
'McDonald, Robert'
'Rivard, Eric'
_publ_section_title
;
 Application of the Donor-Acceptor Concept to Intercept Low Oxidation
 State Group 14 Element Hydrides using a Wittig Reagent as a Lewis Base.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8662
_journal_page_last               8671
_journal_paper_doi               10.1021/ic501265k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C7 H10 Cl2 Ge N2'
_chemical_formula_sum            'C7 H10 Cl2 Ge N2'
_chemical_formula_weight         265.66
_chemical_name_common            1
_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                 90.1560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3784(2)
_cell_length_b                   10.6075(3)
_cell_length_c                   13.2845(3)
_cell_measurement_reflns_used    6486
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      67.56
_cell_measurement_theta_min      5.34
_cell_volume                     1039.73(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6480
_diffrn_reflns_theta_full        68.71
_diffrn_reflns_theta_max         68.71
_diffrn_reflns_theta_min         5.34
_exptl_absorpt_coefficient_mu    8.330
_exptl_absorpt_correction_T_max  0.7005
_exptl_absorpt_correction_T_min  0.1674
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0446P)²+0.7669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                1664
_reflns_number_total             1889
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic501265k_si_002.cif
_cod_data_source_block           riv1276
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4340585--4340595.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4340585
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
Ge Ge 0.20928(5) 0.02706(3) 0.44090(3) 0.03724(15) Uani 1 1 d .
Cl1 Cl 0.47797(12) 0.02773(9) 0.35531(6) 0.0546(2) Uani 1 1 d .
Cl2 Cl 0.03160(11) 0.05868(9) 0.30149(6) 0.0511(2) Uani 1 1 d .
N1 N 0.2227(3) 0.2142(2) 0.47096(17) 0.0328(5) Uani 1 1 d .
N2 N 0.2514(3) 0.5944(2) 0.54624(19) 0.0404(6) Uani 1 1 d .
C1 C 0.1956(4) 0.2534(3) 0.5669(2) 0.0333(6) Uani 1 1 d .
H1 H 0.1708 0.1918 0.6169 0.040 Uiso 1 1 calc R
C2 C 0.2022(4) 0.3774(3) 0.5949(2) 0.0336(6) Uani 1 1 d .
H2 H 0.1826 0.4001 0.6632 0.040 Uiso 1 1 calc R
C3 C 0.2380(4) 0.4719(3) 0.5228(2) 0.0334(6) Uani 1 1 d .
C4 C 0.2628(4) 0.4288(3) 0.4229(2) 0.0378(6) Uani 1 1 d .
H4 H 0.2860 0.4879 0.3707 0.045 Uiso 1 1 calc R
C5 C 0.2539(4) 0.3045(3) 0.4009(2) 0.0385(7) Uani 1 1 d .
H5 H 0.2704 0.2792 0.3330 0.046 Uiso 1 1 calc R
C6 C 0.2267(5) 0.6400(3) 0.6483(3) 0.0487(8) Uani 1 1 d .
H6A H 0.1119 0.6079 0.6750 0.058 Uiso 1 1 calc R
H6B H 0.2245 0.7324 0.6481 0.058 Uiso 1 1 calc R
H6C H 0.3270 0.6105 0.6907 0.058 Uiso 1 1 calc R
C7 C 0.2998(5) 0.6881(3) 0.4699(3) 0.0496(8) Uani 1 1 d .
H7A H 0.3261 0.7688 0.5027 0.059 Uiso 1 1 calc R
H7B H 0.1986 0.6986 0.4228 0.059 Uiso 1 1 calc R
H7C H 0.4072 0.6594 0.4332 0.074 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge 0.0404(2) 0.0333(2) 0.0381(2) -0.00381(14) 0.00871(15) 0.00205(14)
Cl1 0.0456(5) 0.0655(6) 0.0528(5) -0.0057(4) 0.0174(4) 0.0114(4)
Cl2 0.0514(5) 0.0604(5) 0.0414(4) -0.0151(4) -0.0024(3) 0.0028(4)
N1 0.0372(13) 0.0315(12) 0.0299(12) -0.0006(10) 0.0071(9) -0.0011(9)
N2 0.0396(14) 0.0327(13) 0.0489(15) -0.0001(11) 0.0018(11) 0.0009(10)
C1 0.0335(14) 0.0390(15) 0.0273(14) 0.0027(12) 0.0057(11) -0.0008(11)
C2 0.0351(14) 0.0389(15) 0.0269(13) -0.0012(12) 0.0046(11) 0.0004(12)
C3 0.0250(13) 0.0346(15) 0.0407(15) -0.0003(12) 0.0004(11) 0.0017(11)
C4 0.0397(16) 0.0396(16) 0.0343(15) 0.0086(13) 0.0055(12) -0.0027(13)
C5 0.0432(17) 0.0447(16) 0.0278(14) 0.0007(13) 0.0063(11) -0.0016(13)
C6 0.0500(19) 0.0387(16) 0.057(2) -0.0112(15) 0.0011(15) 0.0068(14)
C7 0.0475(19) 0.0328(16) 0.068(2) 0.0096(16) -0.0036(16) -0.0010(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 '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
N1 Ge Cl1 93.03(7)
N1 Ge Cl2 92.49(7)
Cl1 Ge Cl2 95.31(3)
C5 N1 C1 117.0(2)
C5 N1 Ge 124.40(19)
C1 N1 Ge 118.54(19)
C3 N2 C6 122.1(3)
C3 N2 C7 121.0(3)
C6 N2 C7 116.9(3)
N1 C1 C2 123.1(3)
C1 C2 C3 120.2(3)
N2 C3 C2 123.0(3)
N2 C3 C4 121.4(3)
C2 C3 C4 115.6(3)
C5 C4 C3 120.7(3)
C4 C5 N1 123.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ge N1 2.028(2)
Ge Cl1 2.2881(8)
Ge Cl2 2.2907(9)
N1 C5 1.355(4)
N1 C1 1.356(3)
N2 C3 1.340(4)
N2 C6 1.451(4)
N2 C7 1.464(4)
C1 C2 1.369(4)
C2 C3 1.412(4)
C3 C4 1.416(4)
C4 C5 1.352(4)
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
Cl1 Ge N1 C5 50.7(2)
Cl2 Ge N1 C5 -44.8(2)
Cl1 Ge N1 C1 -130.6(2)
Cl2 Ge N1 C1 133.9(2)
C5 N1 C1 C2 -1.4(4)
Ge N1 C1 C2 179.8(2)
N1 C1 C2 C3 0.2(4)
C6 N2 C3 C2 -1.1(4)
C7 N2 C3 C2 176.2(3)
C6 N2 C3 C4 -179.9(3)
C7 N2 C3 C4 -2.6(4)
C1 C2 C3 N2 -178.0(3)
C1 C2 C3 C4 0.8(4)
N2 C3 C4 C5 178.1(3)
C2 C3 C4 C5 -0.7(4)
C3 C4 C5 N1 -0.5(5)
C1 N1 C5 C4 1.5(4)
Ge N1 C5 C4 -179.8(2)
