#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/15/2011552.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_2011552
loop_
_publ_author_name
'Bolte, Michael'
'Hensen, Karl'
'Faber, Alexander'
_publ_section_title
;
 trans-Tetrachlorobis(4-methylpyridine)germanium(IV)
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e497
_journal_page_last               e498
_journal_paper_doi               10.1107/S0108270100013482
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Ge Cl4 (C6 H7 N)2]'
_chemical_formula_sum            'C12 H14 Cl4 Ge N2'
_chemical_formula_weight         400.64
_chemical_name_systematic        ?
_space_group_IT_number           53
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2'
_symmetry_space_group_name_H-M   'P m n a'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.154(2)
_cell_length_b                   7.933(2)
_cell_length_c                   13.731(3)
_cell_measurement_reflns_used    2407
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     779.3(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full .991
_diffrn_measured_fraction_theta_max .991
_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  .031
_diffrn_reflns_av_sigmaI/netI    .0290
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3722
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  300
_diffrn_standards_number         10
_exptl_absorpt_coefficient_mu    2.638
_exptl_absorpt_correction_T_max  .621
_exptl_absorpt_correction_T_min  .301
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          .60
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .20
_refine_diff_density_max         .412
_refine_diff_density_min         -.511
_refine_ls_extinction_coef       .0063(14)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          .034
_refine_ls_R_factor_gt           .026
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0334P)²+0.1042P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .062
_reflns_number_gt                895
_reflns_number_total             1036
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qa0414.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 'Orthorhombic' changed to
'orthorhombic' 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_database_code               2011552
_cod_database_fobs_code          2011552
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x-1/2, -y, z-1/2'
'-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
Cl1 .72510(7) .16635(6) .43468(3) .02974(16) Uani d . 1 . . Cl
Ge1 .5000 .0000 .5000 .01699(14) Uani d S 1 . . Ge
N1 .5000 .1450(3) .62414(15) .0186(4) Uani d S 1 . . N
C2 .5000 .3149(3) .6175(2) .0230(6) Uani d S 1 . . C
H2 .5000 .3659 .5549 .028 Uiso calc SR 1 . . H
C3 .5000 .4162(3) .6989(2) .0240(6) Uani d S 1 . . C
H3 .5000 .5354 .6919 .029 Uiso calc SR 1 . . H
C4 .5000 .3445(3) .79128(19) .0205(5) Uani d S 1 . . C
C41 .5000 .4504(4) .8814(2) .0285(6) Uani d S 1 . . C
H41A .5000 .5623 .8628 .043 Uiso d SPR .50 A 1 H
H41B .3975 .4180 .9215 .043 Uiso d PR .50 A 1 H
H41C .5000 .3836 .9399 .043 Uiso d SPR .50 A 2 H
H41D .3929 .5179 .8789 .043 Uiso d PR .50 A 2 H
C5 .5000 .1696(3) .79704(19) .0230(5) Uani d S 1 . . C
H5 .5000 .1156 .8588 .028 Uiso calc SR 1 . . H
C6 .5000 .0748(3) .71332(19) .0220(5) Uani d S 1 . . C
H6 .5000 -.0446 .7186 .026 Uiso calc SR 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl1 .0322(3) .0279(3) .0291(3) -.01187(19) .0090(2) -.00667(19)
Ge1 .0192(2) .01502(19) .0167(2) .000 .000 -.00263(14)
N1 .0210(11) .0165(9) .0183(11) .000 .000 -.0028(8)
C2 .0272(14) .0195(12) .0224(14) .000 .000 .0010(10)
C3 .0272(14) .0158(12) .0288(14) .000 .000 -.0032(10)
C4 .0155(12) .0234(12) .0226(13) .000 .000 -.0064(11)
C41 .0313(15) .0290(13) .0251(15) .000 .000 -.0112(11)
C5 .0252(14) .0258(13) .0181(13) .000 .000 -.0006(11)
C6 .0261(13) .0178(12) .0221(13) .000 .000 .0018(10)
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'
Ge Ge .1547 1.8001 '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
N1 Ge1 N1 . 5_656 180.0
N1 Ge1 Cl1 . . 90.13(4)
N1 Ge1 Cl1 5_656 . 89.87(4)
N1 Ge1 Cl1 . 8_655 90.13(4)
N1 Ge1 Cl1 5_656 8_655 89.87(4)
Cl1 Ge1 Cl1 . 8_655 90.53(3)
N1 Ge1 Cl1 . 5_656 89.87(4)
N1 Ge1 Cl1 5_656 5_656 90.13(4)
Cl1 Ge1 Cl1 . 5_656 180.0
Cl1 Ge1 Cl1 8_655 5_656 89.47(3)
N1 Ge1 Cl1 . 4_556 89.87(4)
N1 Ge1 Cl1 5_656 4_556 90.13(4)
Cl1 Ge1 Cl1 . 4_556 89.47(3)
Cl1 Ge1 Cl1 8_655 4_556 180.0
Cl1 Ge1 Cl1 5_656 4_556 90.53(3)
C6 N1 C2 . . 118.3(2)
C6 N1 Ge1 . . 121.53(17)
C2 N1 Ge1 . . 120.14(17)
N1 C2 C3 . . 121.9(2)
N1 C2 H2 . . 119.1
C3 C2 H2 . . 119.1
C2 C3 C4 . . 120.1(2)
C2 C3 H3 . . 119.9
C4 C3 H3 . . 119.9
C3 C4 C5 . . 117.4(2)
C3 C4 C41 . . 121.7(2)
C5 C4 C41 . . 120.9(2)
C4 C41 H41A . . 108.2
C4 C41 H41B . . 109.1
H41A C41 H41B . . 114.8
C4 C41 H41C . . 112.4
H41A C41 H41C . . 139.4
H41B C41 H41C . . 50.8
C4 C41 H41D . . 107.0
H41A C41 H41D . . 55.9
H41B C41 H41D . . 62.9
H41C C41 H41D . . 110.2
C6 C5 C4 . . 119.9(2)
C6 C5 H5 . . 120.0
C4 C5 H5 . . 120.0
N1 C6 C5 . . 122.4(2)
N1 C6 H6 . . 118.8
C5 C6 H6 . . 118.8
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
Cl1 Ge1 . 2.2670(6) ?
Ge1 N1 . 2.057(2) ?
Ge1 N1 5_656 2.057(2) ?
Ge1 Cl1 8_655 2.2670(6) ?
Ge1 Cl1 5_656 2.2670(6) ?
Ge1 Cl1 4_556 2.2670(6) ?
N1 C6 . 1.345(3) ?
N1 C2 . 1.350(3) ?
C2 C3 . 1.377(4) ?
C2 H2 . .9500 ?
C3 C4 . 1.390(4) ?
C3 H3 . .9500 ?
C4 C5 . 1.390(4) ?
C4 C41 . 1.495(4) ?
C41 H41A . .9240 ?
C41 H41B . .9530 ?
C41 H41C . .9620 ?
C41 H41D . .9355 ?
C5 C6 . 1.373(4) ?
C5 H5 . .9500 ?
C6 H6 . .9500 ?
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
N1 Ge1 N1 C6 5_656 .0(3)
Cl1 Ge1 N1 C6 . -134.736(16)
Cl1 Ge1 N1 C6 8_655 134.736(16)
Cl1 Ge1 N1 C6 5_656 45.264(17)
Cl1 Ge1 N1 C6 4_556 -45.264(16)
N1 Ge1 N1 C2 5_656 180.0(3)
Cl1 Ge1 N1 C2 . 45.264(17)
Cl1 Ge1 N1 C2 8_655 -45.264(16)
Cl1 Ge1 N1 C2 5_656 -134.736(17)
Cl1 Ge1 N1 C2 4_556 134.736(17)
C6 N1 C2 C3 . .0
Ge1 N1 C2 C3 . 180.0
N1 C2 C3 C4 . .0
C2 C3 C4 C5 . .0
C2 C3 C4 C41 . 180.0
C3 C4 C5 C6 . .0
C41 C4 C5 C6 . 180.0
C2 N1 C6 C5 . .0
Ge1 N1 C6 C5 . 180.0
C4 C5 C6 N1 . .0
