#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:04:38 +0100 (Fri, 25 Mar 2016) $
#$Revision: 179739 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/7/00/35/7003518.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_7003518
loop_
_publ_author_name
'Davis, Martin F.'
'Levason, William'
'Reid, Gillian'
'Webster, Michael'
_publ_section_title
;
 Complexes of germanium(iv) fluoride with phosphane ligands: structural
 and spectroscopic authentication of germanium(iv) phosphane complexes
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              2261
_journal_page_last               2269
_journal_paper_doi               10.1039/b716765b
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C6 H15 As Cl2'
_chemical_formula_sum            'C6 H15 As Cl2'
_chemical_formula_weight         233.00
_chemical_name_common            Dichloridotriethylarsenic(V)
_chemical_name_systematic
;
Dichloridotriethylarsenic(V)
;
_space_group_IT_number           174
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      174
_symmetry_space_group_name_Hall  'P -6'
_symmetry_space_group_name_H-M   'P -6'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2007-07-17
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   8.354(2)
_cell_length_b                   8.354(2)
_cell_length_c                   8.629(2)
_cell_measurement_reflns_used    1250
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.0
_cell_volume                     521.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'area detector, Nonius Kappa ccd'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7342
_diffrn_reflns_theta_full        27.66
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.702
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             236
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         861
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.9648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                723
_reflns_number_total             861
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b716765b.txt
_cod_data_source_block           06mfd018w_[C6H15AsCl2]
_cod_database_code               7003518
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
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
As1 As 0.6667 0.3333 0.0000 0.0295(6) Uani 1 6 d S . .
Cl1 Cl 0.6667 0.3333 0.2760(5) 0.0521(13) Uani 1 3 d S . .
C1 C 0.4038(9) 0.1645(9) 0.0000 0.0322(14) Uani 1 2 d SD . .
H1A H 0.3459 0.1830 0.0933 0.039 Uiso 0.50 1 calc PR . .
H1B H 0.3459 0.1830 -0.0933 0.039 Uiso 0.50 1 calc PR . .
C2 C 0.3801(15) -0.0382(16) 0.0000 0.085(6) Uani 1 2 d SD . .
H2A H 0.2483 -0.1312 0.0000 0.127 Uiso 1 2 calc SR . .
H2B H 0.4388 -0.0536 0.0927 0.127 Uiso 0.50 1 calc PR . .
H2C H 0.4388 -0.0536 -0.0927 0.127 Uiso 0.50 1 calc PR . .
As2 As 0.0000 0.0000 0.5000 0.0266(5) Uani 1 6 d S . .
Cl2 Cl 0.0000 0.0000 0.7738(5) 0.0541(13) Uani 1 3 d S . .
C3 C 0.1918(10) -0.0627(11) 0.5000 0.047(2) Uani 1 2 d SD . .
H3A H 0.2705 -0.0122 0.4068 0.056 Uiso 0.50 1 calc PR . .
H3B H 0.2705 -0.0122 0.5932 0.056 Uiso 0.50 1 calc PR . .
C4 C 0.0865(18) -0.2887(18) 0.5000 0.098(7) Uani 1 2 d SD . .
H4A H 0.1785 -0.3288 0.5000 0.147 Uiso 1 2 calc SR . .
H4B H 0.0090 -0.3364 0.4073 0.147 Uiso 0.50 1 calc PR . .
H4C H 0.0090 -0.3364 0.5927 0.147 Uiso 0.50 1 calc PR . .
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
As1 0.0278(7) 0.0278(7) 0.0329(14) 0.000 0.000 0.0139(4)
Cl1 0.064(2) 0.064(2) 0.028(2) 0.000 0.000 0.0321(10)
C1 0.027(3) 0.031(4) 0.035(4) 0.000 0.000 0.012(3)
C2 0.031(6) 0.043(9) 0.141(14) 0.000 0.000 -0.011(6)
As2 0.0247(7) 0.0247(7) 0.0304(12) 0.000 0.000 0.0124(3)
Cl2 0.067(2) 0.067(2) 0.027(2) 0.000 0.000 0.0337(10)
C3 0.029(4) 0.044(4) 0.071(6) 0.000 0.000 0.020(3)
C4 0.091(13) 0.096(13) 0.161(17) 0.000 0.000 0.087(12)
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'
As As 0.0499 2.0058 '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
C1 As1 C1 120.0 2_655 . ?
C1 As1 C1 120.0 2_655 3_665 ?
C1 As1 C1 120.0 . 3_665 ?
C1 As1 Cl1 90.0 2_655 4 ?
C1 As1 Cl1 90.0 . 4 ?
C1 As1 Cl1 90.0 3_665 4 ?
C1 As1 Cl1 90.0 2_655 . ?
C1 As1 Cl1 90.0 . . ?
C1 As1 Cl1 90.0 3_665 . ?
Cl1 As1 Cl1 180.0 4 . ?
C2 C1 As1 105.4(5) . . ?
C2 C1 H1A 110.7 . . ?
As1 C1 H1A 110.7 . . ?
C2 C1 H1B 110.7 . . ?
As1 C1 H1B 110.7 . . ?
H1A C1 H1B 108.8 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 As2 C3 120.0 3 . ?
C3 As2 C3 120.0 3 2 ?
C3 As2 C3 120.0 . 2 ?
C3 As2 Cl2 90.0 3 . ?
C3 As2 Cl2 90.0 . . ?
C3 As2 Cl2 90.0 2 . ?
C3 As2 Cl2 90.0 3 4_556 ?
C3 As2 Cl2 90.0 . 4_556 ?
C3 As2 Cl2 90.0 2 4_556 ?
Cl2 As2 Cl2 180.0 . 4_556 ?
C4 C3 As2 105.9(6) . . ?
C4 C3 H3A 110.5 . . ?
As2 C3 H3A 110.5 . . ?
C4 C3 H3B 110.5 . . ?
As2 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
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
As1 C1 1.927(6) 2_655 ?
As1 C1 1.927(6) . ?
As1 C1 1.927(6) 3_665 ?
As1 Cl1 2.382(4) 4 ?
As1 Cl1 2.382(4) . ?
C1 C2 1.604(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
As2 C3 1.918(7) 3 ?
As2 C3 1.918(7) . ?
As2 C3 1.918(7) 2 ?
As2 Cl2 2.362(4) . ?
As2 Cl2 2.362(4) 4_556 ?
C3 C4 1.637(12) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
