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#$Date: 2016-03-23 20:26:20 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179449 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/46/4334677.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_4334677
loop_
_publ_author_name
'Christian Hering'
'Axel Schulz'
'Alexander Villinger'
_publ_contact_author_address
;
Universität Rostock
Institut für Chemie
Abteilung für Anorganische Chemie
Albert-Einstein-Strasse 3a 
18059 Rostock
Bundesrepublik Deutschland
;
_publ_contact_author_email
;
axel.schulz@uni-rostock.de'
;
_publ_contact_author_fax         '+49 (0)381/498-6382'
_publ_contact_author_name        'Axel Schulz'
_publ_contact_author_phone       '+49 (0)381/498-6400'
_publ_section_title
;
 On the Synthesis and Reactivity of Highly Labile Pseudohalogen
 Phosphenium Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5214
_journal_page_last               5225
_journal_paper_doi               10.1021/ic4001285
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C4 H9 Cl3 Ga N Si'
_chemical_formula_sum            'C4 H9 Cl3 Ga N Si'
_chemical_formula_weight         275.28
_chemical_name_systematic
;
Trimethylsilylisonitrile/trimethylsilylnitrile galliumtrichloride adduct
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      146
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   9.9350(5)
_cell_length_b                   9.9350(5)
_cell_length_c                   9.5741(8)
_cell_measurement_reflns_used    1468
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      61.489
_cell_measurement_theta_min      6.368
_cell_volume                     818.40(9)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex Kappa-II-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2705
_diffrn_reflns_theta_full        30.36
_diffrn_reflns_theta_max         30.36
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    3.305
_exptl_absorpt_correction_T_max  0.8016
_exptl_absorpt_correction_T_min  0.4804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       block
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.019(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         902
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0069P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0350
_refine_ls_wR_factor_ref         0.0353
_reflns_number_gt                842
_reflns_number_total             902
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic4001285_si_002_04.cif
_cod_data_source_block           is_ch68_nc_gacl3
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4334677
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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
Si1 Si 0.3333 0.6667 0.89218(9) 0.0230(2) Uani 1 3 d S . .
C1A C 0.3333 0.6667 0.5789(4) 0.0289(8) Uani 0.770(4) 3 d SP A 1
N1A N 0.3333 0.6667 0.6981(3) 0.0282(7) Uani 0.770(4) 3 d SP A 1
N1B N 0.3333 0.6667 0.5789(4) 0.0289(8) Uani 0.230(4) 3 d SP A 2
C1B C 0.3333 0.6667 0.6981(3) 0.0282(7) Uani 0.230(4) 3 d SP A 2
C2 C 0.2896(3) 0.4693(3) 0.9377(3) 0.0330(5) Uani 1 1 d . A .
H2A H 0.2894 0.4591 1.0395 0.050 Uiso 1 1 calc R . .
H2B H 0.3688 0.4497 0.8972 0.050 Uiso 1 1 calc R . .
H2C H 0.1872 0.3937 0.9007 0.050 Uiso 1 1 calc R . .
Ga1 Ga 0.3333 0.6667 0.36701(2) 0.02397(11) Uani 1 3 d S . .
Cl1 Cl 0.39136(7) 0.89627(6) 0.30253(6) 0.03689(16) Uani 1 1 d . A .
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
Si1 0.0269(3) 0.0269(3) 0.0152(7) 0.000 0.000 0.01343(14)
C1A 0.0323(12) 0.0323(12) 0.0221(17) 0.000 0.000 0.0161(6)
N1A 0.0323(11) 0.0323(11) 0.0200(17) 0.000 0.000 0.0162(6)
N1B 0.0323(12) 0.0323(12) 0.0221(17) 0.000 0.000 0.0161(6)
C1B 0.0323(11) 0.0323(11) 0.0200(17) 0.000 0.000 0.0162(6)
C2 0.0404(13) 0.0337(11) 0.0274(11) -0.0008(10) -0.0018(9) 0.0204(11)
Ga1 0.02907(14) 0.02907(14) 0.0138(2) 0.000 0.000 0.01454(7)
Cl1 0.0474(4) 0.0303(3) 0.0333(4) 0.0025(2) -0.0010(3) 0.0197(3)
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'
Si Si 0.0817 0.0704 '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
C2 Si1 C2 114.55(7) 3_565 2_665
C2 Si1 C2 114.55(7) 3_565 .
C2 Si1 C2 114.55(7) 2_665 .
C2 Si1 N1A 103.73(9) 3_565 .
C2 Si1 N1A 103.73(9) 2_665 .
C2 Si1 N1A 103.73(9) . .
N1A C1A Ga1 180.000(1) . .
C1A N1A Si1 180.000(1) . .
Si1 C2 H2A 109.5 . .
Si1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Si1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1A Ga1 Cl1 106.725(17) . .
C1A Ga1 Cl1 106.725(17) . 2_665
Cl1 Ga1 Cl1 112.072(15) . 2_665
C1A Ga1 Cl1 106.725(17) . 3_565
Cl1 Ga1 Cl1 112.072(15) . 3_565
Cl1 Ga1 Cl1 112.072(15) 2_665 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C2 1.836(2) 3_565
Si1 C2 1.836(2) 2_665
Si1 C2 1.836(2) .
Si1 N1A 1.858(3) .
C1A N1A 1.141(4) .
C1A Ga1 2.029(4) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
Ga1 Cl1 2.1452(5) .
Ga1 Cl1 2.1452(5) 2_665
Ga1 Cl1 2.1452(5) 3_565
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_4
Ga1 C1A N1A Si1 0(100) . .
C2 Si1 N1A C1A -102(100) 3_565 .
C2 Si1 N1A C1A 138(100) 2_665 .
C2 Si1 N1A C1A 18(100) . .
N1A C1A Ga1 Cl1 -16(100) . .
N1A C1A Ga1 Cl1 -136(100) . 2_665
N1A C1A Ga1 Cl1 104(100) . 3_565
