#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:48:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179264 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/84/4318452.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_4318452
loop_
_publ_author_name
'Stefan Nogai'
'Hubert Schmidbaur'
_publ_contact_author
;
    Prof. Dr. H. Schmidbaur
    Anorganisch-chemisches Institut
    der Technischen Universität München
    Lichtenbergstras̈e 4
    D-85747 Garching
    Germany
;
_publ_contact_author_email       H.Schmidbaur@lrz.tu-muenchen.de
_publ_contact_author_fax         '++49 89 2891-3125'
_publ_contact_author_phone       '++49 89 2891-3130'
_publ_section_title
;
 Dichlorogallane (HGaCl2)2: Its Molecular Structure and Synthetic
 Potential
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4770
_journal_page_last               4774
_journal_paper_doi               10.1021/ic0203015
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C6 H15 Cl3 Ga P'
_chemical_formula_weight         294.22
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.5461(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3043(2)
_cell_length_b                   12.8006(4)
_cell_length_c                   13.3458(4)
_cell_measurement_reflns_used    46636
_cell_measurement_temperature    143(2)
_cell_volume                     1247.37(6)
_computing_cell_refinement       DENZO
_computing_data_collection       XPRESS
_computing_data_reduction        SCALEPACK
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46636
_diffrn_reflns_theta_full        26.75
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    2.925
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_type   delabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0227
_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)+(0.0164P)²+0.3903P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0531
_reflns_number_gt                2520
_reflns_number_total             2657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0203015_4.cif
_cod_data_source_block           nog16
_cod_database_code               4318452
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 0.05221(2) 0.234681(15) 0.783840(14) 0.02655(7) Uani 1 1 d . . .
C12 C 0.1785(3) 0.45131(19) 0.61276(19) 0.0445(5) Uani 1 1 d . . .
P1 P -0.11512(6) 0.37981(3) 0.72364(3) 0.02415(10) Uani 1 1 d . . .
C21 C -0.2679(3) 0.43014(16) 0.81694(15) 0.0332(4) Uani 1 1 d . . .
Cl3 Cl -0.11859(6) 0.14568(3) 0.88501(3) 0.03574(12) Uani 1 1 d . . .
C31 C -0.2548(3) 0.34506(15) 0.61396(14) 0.0324(4) Uani 1 1 d . . .
Cl2 Cl 0.12516(7) 0.14064(4) 0.65513(4) 0.03828(12) Uani 1 1 d . . .
C11 C 0.0393(3) 0.48460(15) 0.68934(16) 0.0338(4) Uani 1 1 d . . .
Cl1 Cl 0.29420(6) 0.28845(4) 0.86718(4) 0.04227(13) Uani 1 1 d . . .
C22 C -0.1724(4) 0.45663(18) 0.91637(16) 0.0421(5) Uani 1 1 d . . .
C32 C -0.3786(3) 0.25162(17) 0.63225(18) 0.0374(4) Uani 1 1 d . . .
H22C H -0.255(3) 0.4877(18) 0.9621(17) 0.048(6) Uiso 1 1 d . . .
H12C H 0.253(3) 0.5076(19) 0.5966(17) 0.045(6) Uiso 1 1 d . . .
H21B H -0.360(3) 0.3791(18) 0.8217(17) 0.046(6) Uiso 1 1 d . . .
H32C H -0.448(3) 0.2401(16) 0.5753(19) 0.041(6) Uiso 1 1 d . . .
H12B H 0.251(3) 0.396(2) 0.6366(19) 0.055(7) Uiso 1 1 d . . .
H31B H -0.328(3) 0.4061(18) 0.5933(16) 0.043(6) Uiso 1 1 d . . .
H11B H 0.102(3) 0.5090(19) 0.7493(19) 0.052(7) Uiso 1 1 d . . .
H21A H -0.326(3) 0.4923(18) 0.7854(16) 0.039(6) Uiso 1 1 d . . .
H31A H -0.170(3) 0.3299(17) 0.5617(17) 0.042(6) Uiso 1 1 d . . .
H32B H -0.459(4) 0.261(2) 0.684(2) 0.066(8) Uiso 1 1 d . . .
H22B H -0.076(3) 0.505(2) 0.9087(18) 0.053(7) Uiso 1 1 d . . .
H11A H -0.037(3) 0.5424(18) 0.6667(17) 0.043(6) Uiso 1 1 d . . .
H12A H 0.116(4) 0.429(2) 0.549(2) 0.071(8) Uiso 1 1 d . . .
H32A H -0.310(4) 0.191(2) 0.646(2) 0.063(8) Uiso 1 1 d . . .
H22A H -0.122(3) 0.396(2) 0.9507(18) 0.053(7) Uiso 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'
P P 0.1023 0.0942 '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
Cl1 Ga1 Cl2 111.47(2) . . ?
Cl1 Ga1 Cl3 108.60(2) . . ?
Cl2 Ga1 Cl3 110.84(2) . . ?
Cl1 Ga1 P1 109.41(2) . . ?
Cl2 Ga1 P1 107.656(18) . . ?
Cl3 Ga1 P1 108.835(18) . . ?
C11 C12 H12C 110.1(14) . . ?
C11 C12 H12B 111.4(15) . . ?
H12C C12 H12B 110(2) . . ?
C11 C12 H12A 110.6(15) . . ?
H12C C12 H12A 106(2) . . ?
H12B C12 H12A 109(2) . . ?
C21 P1 C31 107.32(10) . . ?
C21 P1 C11 107.95(9) . . ?
C31 P1 C11 108.44(9) . . ?
C21 P1 Ga1 111.70(7) . . ?
C31 P1 Ga1 110.92(6) . . ?
C11 P1 Ga1 110.38(7) . . ?
C22 C21 P1 113.71(15) . . ?
C22 C21 H21B 114.0(14) . . ?
P1 C21 H21B 104.7(14) . . ?
C22 C21 H21A 111.9(12) . . ?
P1 C21 H21A 104.8(12) . . ?
H21B C21 H21A 107.0(18) . . ?
C32 C31 P1 112.70(14) . . ?
C32 C31 H31B 110.4(13) . . ?
P1 C31 H31B 108.7(13) . . ?
C32 C31 H31A 110.7(13) . . ?
P1 C31 H31A 106.0(13) . . ?
H31B C31 H31A 108.2(18) . . ?
C12 C11 P1 113.12(14) . . ?
C12 C11 H11B 109.8(14) . . ?
P1 C11 H11B 108.3(14) . . ?
C12 C11 H11A 113.0(13) . . ?
P1 C11 H11A 106.7(13) . . ?
H11B C11 H11A 105.5(19) . . ?
C21 C22 H22C 111.4(14) . . ?
C21 C22 H22B 112.1(15) . . ?
H22C C22 H22B 106(2) . . ?
C21 C22 H22A 113.4(14) . . ?
H22C C22 H22A 105.6(19) . . ?
H22B C22 H22A 107(2) . . ?
C31 C32 H32C 108.2(14) . . ?
C31 C32 H32B 114.1(16) . . ?
H32C C32 H32B 107(2) . . ?
C31 C32 H32A 111.3(16) . . ?
H32C C32 H32A 108(2) . . ?
H32B C32 H32A 108(2) . . ?
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 Cl1 2.1746(5) . ?
Ga1 Cl2 2.1756(5) . ?
Ga1 Cl3 2.1836(5) . ?
Ga1 P1 2.3531(5) . ?
C12 C11 1.522(3) . ?
C12 H12C 0.93(2) . ?
C12 H12B 0.93(3) . ?
C12 H12A 1.00(3) . ?
P1 C21 1.8126(19) . ?
P1 C31 1.8168(19) . ?
P1 C11 1.8191(19) . ?
C21 C22 1.521(3) . ?
C21 H21B 0.94(2) . ?
C21 H21A 0.99(2) . ?
C31 C32 1.523(3) . ?
C31 H31B 0.98(2) . ?
C31 H31A 0.96(2) . ?
C11 H11B 0.96(3) . ?
C11 H11A 0.97(2) . ?
C22 H22C 0.96(2) . ?
C22 H22B 0.94(3) . ?
C22 H22A 0.96(3) . ?
C32 H32C 0.92(3) . ?
C32 H32B 0.92(3) . ?
C32 H32A 0.94(3) . ?
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 P1 C21 -84.78(7) . . . . ?
Cl2 Ga1 P1 C21 153.93(7) . . . . ?
Cl3 Ga1 P1 C21 33.74(7) . . . . ?
Cl1 Ga1 P1 C31 155.54(7) . . . . ?
Cl2 Ga1 P1 C31 34.25(7) . . . . ?
Cl3 Ga1 P1 C31 -85.95(7) . . . . ?
Cl1 Ga1 P1 C11 35.33(7) . . . . ?
Cl2 Ga1 P1 C11 -85.95(7) . . . . ?
Cl3 Ga1 P1 C11 153.85(7) . . . . ?
C31 P1 C21 C22 176.41(15) . . . . ?
C11 P1 C21 C22 -66.89(17) . . . . ?
Ga1 P1 C21 C22 54.63(16) . . . . ?
C21 P1 C31 C32 -68.34(17) . . . . ?
C11 P1 C31 C32 175.28(15) . . . . ?
Ga1 P1 C31 C32 53.93(17) . . . . ?
C21 P1 C11 C12 178.61(16) . . . . ?
C31 P1 C11 C12 -65.42(18) . . . . ?
Ga1 P1 C11 C12 56.26(17) . . . . ?
