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#$Date: 2016-03-23 20:43:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179421 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/18/4331800.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_4331800
loop_
_publ_author_name
'Ahmad El-Hellani'
'Julien Monot'
'Régis Guillot'
'Christophe Bour'
'Vincent Gandon'
_publ_contact_author_address
;Université Paris-sud 11,
Institut de Chimie Moléculaire et des Matériaux d'Orsay (ICMMO),
UMR CNRS 8182,
Bâtiment 420,
91405 Orsay cedex,
France. 
;
_publ_contact_author_email       'vincent.gandon@u-psud.fr '
_publ_contact_author_name        'Vincent Gandon '
_publ_contact_author_phone       '01.69.15.39.31 '
_publ_section_title
;
 Molecular versus Ionic Structures in Adducts of GaX3 with Monodentate
 Carbon-Based Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              506
_journal_page_last               514
_journal_paper_doi               10.1021/ic302440g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C5 H8 Cl3 Ga N2'
_chemical_formula_sum            'C5 H8 Cl3 Ga N2'
_chemical_formula_weight         272.20
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.9690(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.4493(7)
_cell_length_b                   10.1648(4)
_cell_length_c                   14.2848(6)
_cell_measurement_reflns_used    7976
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      36.31
_cell_measurement_theta_min      3.02
_cell_volume                     1959.12(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.683
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10837
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         36.34
_diffrn_reflns_theta_min         2.51
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_exptl_absorpt_coefficient_mu    3.567
_exptl_absorpt_correction_T_max  0.9037
_exptl_absorpt_correction_T_min  0.5758
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.038
_refine_diff_density_min         -1.520
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         3243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0584P)²+5.0226P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                2969
_reflns_number_total             3243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302440g_si_001_2.cif
_cod_data_source_block           1rx1503GuillotICMMO
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4331800
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
C1 C 0.27924(15) 0.3414(2) 0.36089(14) 0.0136(4) Uani 1 1 d .
C2 C 0.38310(18) 0.3934(3) 0.51425(16) 0.0200(4) Uani 1 1 d .
H2 H 0.4413 0.4039 0.5694 0.024 Uiso 1 1 calc R
C3 C 0.29030(18) 0.4279(2) 0.50830(16) 0.0199(4) Uani 1 1 d .
H3 H 0.2727 0.4668 0.5585 0.024 Uiso 1 1 calc R
C4 C 0.11981(16) 0.4117(2) 0.37791(16) 0.0174(4) Uani 1 1 d .
H4A H 0.1009 0.4810 0.3291 0.026 Uiso 1 1 calc R
H4B H 0.1001 0.4341 0.4333 0.026 Uiso 1 1 calc R
H4C H 0.0879 0.3313 0.3479 0.026 Uiso 1 1 calc R
C5 C 0.45978(17) 0.2935(2) 0.39925(19) 0.0201(4) Uani 1 1 d .
H5A H 0.4453 0.2084 0.3683 0.030 Uiso 1 1 calc R
H5B H 0.5168 0.2875 0.4598 0.030 Uiso 1 1 calc R
H5C H 0.4730 0.3543 0.3541 0.030 Uiso 1 1 calc R
N1 N 0.37456(13) 0.33996(19) 0.42298(13) 0.0147(3) Uani 1 1 d .
N2 N 0.22747(14) 0.3941(2) 0.41363(13) 0.0151(3) Uani 1 1 d .
Cl1 Cl 0.32390(4) 0.24253(7) 0.14629(4) 0.02293(13) Uani 1 1 d .
Cl2 Cl 0.12556(4) 0.11313(6) 0.21557(4) 0.01969(12) Uani 1 1 d .
Cl3 Cl 0.11940(4) 0.43976(6) 0.12959(4) 0.02009(12) Uani 1 1 d .
Ga Ga 0.218436(16) 0.28505(2) 0.218180(16) 0.01306(8) Uani 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
C1 0.0147(9) 0.0132(11) 0.0147(7) -0.0012(6) 0.0076(7) -0.0022(7)
C2 0.0221(11) 0.0208(13) 0.0142(8) -0.0023(7) 0.0028(8) -0.0030(9)
C3 0.0250(11) 0.0206(13) 0.0138(8) -0.0045(7) 0.0066(8) -0.0024(9)
C4 0.0158(9) 0.0189(12) 0.0198(9) -0.0009(7) 0.0093(7) 0.0020(8)
C5 0.0131(10) 0.0197(13) 0.0272(10) -0.0008(8) 0.0067(8) 0.0013(8)
N1 0.0150(8) 0.0137(10) 0.0146(7) 0.0006(6) 0.0042(6) -0.0005(6)
N2 0.0157(8) 0.0164(10) 0.0154(7) -0.0007(6) 0.0079(6) -0.0003(7)
Cl1 0.0241(3) 0.0274(3) 0.0243(2) -0.0008(2) 0.0172(2) 0.0039(2)
Cl2 0.0181(2) 0.0194(3) 0.0205(2) -0.00311(18) 0.00558(19) -0.00497(19)
Cl3 0.0177(2) 0.0250(3) 0.0183(2) 0.00583(18) 0.00735(19) 0.0055(2)
Ga 0.01247(13) 0.01604(16) 0.01209(11) -0.00086(7) 0.00613(9) 0.00041(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0031 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 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2310 1.6080 '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
N1 C1 N2 106.12(17)
N1 C1 Ga 130.08(14)
N2 C1 Ga 123.78(16)
C3 C2 N1 106.9(2)
C2 C3 N2 106.64(18)
C1 N1 C2 110.12(18)
C1 N1 C5 126.65(18)
C2 N1 C5 123.20(19)
C1 N2 C3 110.23(18)
C1 N2 C4 125.89(18)
C3 N2 C4 123.87(17)
C1 Ga Cl1 114.53(6)
C1 Ga Cl2 106.80(6)
Cl1 Ga Cl2 111.28(3)
C1 Ga Cl3 109.96(7)
Cl1 Ga Cl3 107.08(2)
Cl2 Ga Cl3 106.96(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.345(3)
C1 N2 1.348(2)
C1 Ga 1.993(2)
C2 C3 1.359(3)
C2 N1 1.377(3)
C3 N2 1.376(3)
C4 N2 1.464(3)
C5 N1 1.467(3)
Cl1 Ga 2.1642(5)
Cl2 Ga 2.1956(6)
Cl3 Ga 2.1969(6)
