#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/32/7013236.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_7013236
loop_
_publ_author_name
'Nogai, Stefan'
'Schriewer, Alexander'
'Schmidbaur, Hubert'
_publ_section_title
;
 Reactions of trichlorogermane HGeCl3 and dichlorogallane HGaCl2 with
 pyridine donors
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              3165
_journal_paper_doi               10.1039/b305792e
_journal_year                    2003
_chemical_formula_sum            'C7 H10 Cl2 Ga N'
_chemical_formula_weight         248.78
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.9204(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1301(2)
_cell_length_b                   9.1466(2)
_cell_length_c                   13.7748(4)
_cell_measurement_reflns_used    28989
_cell_measurement_temperature    143(2)
_cell_volume                     1002.24(4)
_computing_cell_refinement       DENZO
_computing_data_collection       XPRESS
_computing_data_reduction        SCALEPACK
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'NONIUS DIP 2020'
_diffrn_measurement_method       phi-rotation
_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  0.039
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28989
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    3.218
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[σ²(Fo²)+(0.0301P)²+0.5653P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                1791
_reflns_number_total             1830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305792e.txt
_cod_data_source_block           nog37
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7013236
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.22973(3) 0.83450(2) 0.897079(16) 0.03221(11) Uani 1 1 d . . .
Cl1 Cl 0.29594(7) 0.91723(6) 1.04858(4) 0.04072(15) Uani 1 1 d . . .
N1 N 0.0321(2) 0.70508(19) 0.90129(12) 0.0287(4) Uani 1 1 d . . .
Cl2 Cl 0.11675(8) 1.01044(7) 0.79818(4) 0.04702(17) Uani 1 1 d . . .
C2 C 0.0025(3) 0.5912(2) 0.83754(15) 0.0295(4) Uani 1 1 d . . .
H2 H 0.078(3) 0.583(2) 0.7965(16) 0.028(6) Uiso 1 1 d . . .
C3 C -0.1281(2) 0.4943(2) 0.83681(15) 0.0300(4) Uani 1 1 d . . .
C4 C -0.2307(3) 0.5196(2) 0.90429(16) 0.0314(4) Uani 1 1 d . . .
H4 H -0.314(3) 0.459(3) 0.9054(18) 0.038(6) Uiso 1 1 d . . .
C5 C -0.2033(3) 0.6364(2) 0.97053(15) 0.0310(4) Uani 1 1 d . . .
C6 C -0.0684(3) 0.7273(2) 0.96598(15) 0.0295(4) Uani 1 1 d . . .
H6 H -0.041(3) 0.809(3) 1.0086(17) 0.028(6) Uiso 1 1 d . . .
C7 C -0.1554(3) 0.3664(3) 0.76725(19) 0.0392(5) Uani 1 1 d . . .
H7C H -0.261(5) 0.376(4) 0.720(3) 0.070(9) Uiso 1 1 d . . .
H7B H -0.152(5) 0.288(5) 0.797(3) 0.084(12) Uiso 1 1 d . . .
H7A H -0.082(5) 0.363(4) 0.731(3) 0.068(10) Uiso 1 1 d . . .
C8 C -0.3112(3) 0.6646(3) 1.0446(2) 0.0409(6) Uani 1 1 d . . .
H8C H -0.244(5) 0.695(5) 1.102(3) 0.096(15) Uiso 1 1 d . . .
H8B H -0.360(6) 0.581(5) 1.065(3) 0.117(15) Uiso 1 1 d . . .
H8A H -0.391(6) 0.723(5) 1.022(3) 0.099(14) Uiso 1 1 d . . .
H1 H 0.360(3) 0.746(3) 0.8558(17) 0.034(6) Uiso 1 1 d . . .
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
Ga1 0.03164(17) 0.03385(17) 0.03323(17) -0.00201(9) 0.01154(11) -0.00322(8)
Cl1 0.0406(3) 0.0465(3) 0.0348(3) -0.0060(2) 0.0074(2) -0.0060(2)
N1 0.0295(8) 0.0282(8) 0.0285(8) 0.0030(7) 0.0059(7) 0.0023(7)
Cl2 0.0554(4) 0.0427(3) 0.0419(3) 0.0115(2) 0.0077(3) -0.0080(3)
C2 0.0307(10) 0.0315(10) 0.0265(9) 0.0039(8) 0.0065(8) 0.0040(8)
C3 0.0305(10) 0.0290(10) 0.0289(10) 0.0044(8) 0.0025(8) 0.0027(8)
C4 0.0271(10) 0.0316(11) 0.0339(11) 0.0063(8) 0.0024(8) -0.0005(9)
C5 0.0267(10) 0.0333(10) 0.0325(11) 0.0054(9) 0.0054(8) 0.0057(8)
C6 0.0302(10) 0.0288(10) 0.0293(10) 0.0011(8) 0.0056(8) 0.0035(8)
C7 0.0444(14) 0.0359(12) 0.0377(12) -0.0024(10) 0.0096(11) -0.0050(10)
C8 0.0334(12) 0.0467(15) 0.0455(14) -0.0017(11) 0.0151(11) 0.0008(10)
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'
N N 0.0061 0.0033 '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'
Ga Ga 0.2307 1.6083 '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
N1 Ga1 Cl1 102.59(5) . . ?
N1 Ga1 Cl2 102.51(5) . . ?
Cl1 Ga1 Cl2 109.28(3) . . ?
N1 Ga1 H1 108.6(9) . . ?
Cl1 Ga1 H1 119.0(9) . . ?
Cl2 Ga1 H1 113.0(9) . . ?
C6 N1 C2 119.76(18) . . ?
C6 N1 Ga1 122.05(14) . . ?
C2 N1 Ga1 118.18(14) . . ?
N1 C2 C3 122.19(19) . . ?
N1 C2 H2 114.3(14) . . ?
C3 C2 H2 123.5(14) . . ?
C2 C3 C4 117.04(19) . . ?
C2 C3 C7 121.2(2) . . ?
C4 C3 C7 121.8(2) . . ?
C3 C4 C5 121.9(2) . . ?
C3 C4 H4 118.6(16) . . ?
C5 C4 H4 119.5(16) . . ?
C6 C5 C4 116.80(19) . . ?
C6 C5 C8 120.4(2) . . ?
C4 C5 C8 122.8(2) . . ?
N1 C6 C5 122.30(19) . . ?
N1 C6 H6 115.5(14) . . ?
C5 C6 H6 122.2(14) . . ?
C3 C7 H7C 111(2) . . ?
C3 C7 H7B 112(3) . . ?
H7C C7 H7B 111(3) . . ?
C3 C7 H7A 112(2) . . ?
H7C C7 H7A 104(3) . . ?
H7B C7 H7A 107(3) . . ?
C5 C8 H8C 108(3) . . ?
C5 C8 H8B 114(3) . . ?
H8C C8 H8B 102(4) . . ?
C5 C8 H8A 112(3) . . ?
H8C C8 H8A 114(4) . . ?
H8B C8 H8A 107(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
Ga1 N1 2.0059(17) . ?
Ga1 Cl1 2.1803(6) . ?
Ga1 Cl2 2.1846(6) . ?
Ga1 H1 1.53(2) . ?
N1 C6 1.343(3) . ?
N1 C2 1.352(3) . ?
C2 C3 1.382(3) . ?
C2 H2 0.92(2) . ?
C3 C4 1.391(3) . ?
C3 C7 1.499(3) . ?
C4 C5 1.393(3) . ?
C4 H4 0.88(3) . ?
C5 C6 1.388(3) . ?
C5 C8 1.499(3) . ?
C6 H6 0.95(2) . ?
C7 H7C 0.96(4) . ?
C7 H7B 0.83(4) . ?
C7 H7A 0.86(4) . ?
C8 H8C 0.90(4) . ?
C8 H8B 0.93(5) . ?
C8 H8A 0.84(5) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl1 Ga1 N1 C6 26.63(16) . . . . ?
Cl2 Ga1 N1 C6 -86.71(15) . . . . ?
Cl1 Ga1 N1 C2 -152.35(13) . . . . ?
Cl2 Ga1 N1 C2 94.32(14) . . . . ?
C6 N1 C2 C3 -0.6(3) . . . . ?
Ga1 N1 C2 C3 178.37(15) . . . . ?
N1 C2 C3 C4 0.8(3) . . . . ?
N1 C2 C3 C7 -178.3(2) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
C7 C3 C4 C5 178.6(2) . . . . ?
C3 C4 C5 C6 0.2(3) . . . . ?
C3 C4 C5 C8 -179.3(2) . . . . ?
C2 N1 C6 C5 0.2(3) . . . . ?
Ga1 N1 C6 C5 -178.72(15) . . . . ?
C4 C5 C6 N1 0.0(3) . . . . ?
C8 C5 C6 N1 179.5(2) . . . . ?
