#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:04:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179466 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/63/4336307.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_4336307
loop_
_publ_author_name
'Ahmad El-Hellani'
'Julien Monot'
'Shun Tang'
'Régis Guillot'
'Christophe Bour'
'Vincent Gandon'
_publ_contact_author_address
;Institut de Chimie Moléculaire et des Matériaux d'Orsay,
ICMMO,
Université Paris-sud 11,
Bâtiment 420,
91405 Orsay cedex,
France.
;
_publ_contact_author_email       vincent.gandon@u-psud.fr
_publ_contact_author_name        'Vincent Gandon'
_publ_section_title
;
 Relationship between Gallium Pyramidalization in L.GaCl3 Complexes and
 the Electronic Ligand Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11493
_journal_page_last               11502
_journal_paper_doi               10.1021/ic401817g
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C11 H24 Cl3 Ga N4'
_chemical_formula_sum            'C11 H24 Cl3 Ga N4'
_chemical_formula_weight         388.41
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.3185(7)
_cell_length_b                   8.0781(3)
_cell_length_c                   27.4363(13)
_cell_measurement_reflns_used    9807
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.14
_cell_measurement_theta_min      2.76
_cell_volume                     3395.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            50202
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_exptl_absorpt_coefficient_mu    2.086
_exptl_absorpt_correction_T_max  0.8560
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         10013
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0477P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                8417
_reflns_number_total             10013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401817g_si_001_4.cif
_cod_data_source_block           5-GaCl3
_cod_database_code               4336307
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'
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 -0.10527(15) 0.9960(3) 0.41014(10) 0.0105(5) Uani 1 1 d .
C2 C -0.13172(15) 1.1136(3) 0.44439(9) 0.0105(5) Uani 1 1 d .
C3 C -0.16299(16) 0.9514(3) 0.37099(10) 0.0120(5) Uani 1 1 d .
C4 C 0.00434(16) 1.2782(4) 0.45289(15) 0.0175(7) Uani 1 1 d .
H4A H 0.0068 1.2614 0.4183 0.026 Uiso 1 1 calc R
H4B H 0.0541 1.2271 0.4679 0.026 Uiso 1 1 calc R
H4C H 0.0045 1.3947 0.4598 0.026 Uiso 1 1 calc R
C5 C -0.08854(18) 1.2307(3) 0.52416(13) 0.0170(6) Uani 1 1 d .
H5A H -0.1345 1.1596 0.5355 0.026 Uiso 1 1 calc R
H5B H -0.1043 1.3441 0.5298 0.026 Uiso 1 1 calc R
H5C H -0.0357 1.2057 0.5414 0.026 Uiso 1 1 calc R
C6 C -0.24773(16) 1.3099(3) 0.46817(11) 0.0143(6) Uani 1 1 d .
H6A H -0.2002 1.3869 0.4656 0.021 Uiso 1 1 calc R
H6B H -0.2690 1.3085 0.5011 0.021 Uiso 1 1 calc R
H6C H -0.2939 1.3429 0.4466 0.021 Uiso 1 1 calc R
C7 C -0.28866(16) 1.0264(3) 0.44789(11) 0.0152(6) Uani 1 1 d .
H7A H -0.3206 1.0545 0.4189 0.023 Uiso 1 1 calc R
H7B H -0.3271 1.0304 0.4755 0.023 Uiso 1 1 calc R
H7C H -0.2652 0.9167 0.4447 0.023 Uiso 1 1 calc R
C8 C -0.18394(17) 0.6665(3) 0.40002(11) 0.0172(6) Uani 1 1 d .
H8A H -0.1655 0.7153 0.4302 0.026 Uiso 1 1 calc R
H8B H -0.1457 0.5766 0.3918 0.026 Uiso 1 1 calc R
H8C H -0.2425 0.6256 0.4034 0.026 Uiso 1 1 calc R
C9 C -0.1987(2) 0.7256(4) 0.31293(13) 0.0185(6) Uani 1 1 d .
H9A H -0.1849 0.8080 0.2889 0.028 Uiso 1 1 calc R
H9B H -0.2593 0.6965 0.3104 0.028 Uiso 1 1 calc R
H9C H -0.1635 0.6290 0.3075 0.028 Uiso 1 1 calc R
C10 C -0.28211(18) 1.0488(4) 0.31682(11) 0.0197(6) Uani 1 1 d .
H10A H -0.3095 0.9478 0.3272 0.030 Uiso 1 1 calc R
H10B H -0.2726 1.0451 0.2823 0.030 Uiso 1 1 calc R
H10C H -0.3192 1.1408 0.3246 0.030 Uiso 1 1 calc R
C11 C -0.1644(2) 1.2368(3) 0.33987(13) 0.0173(7) Uani 1 1 d .
H11A H -0.1968 1.3057 0.3619 0.026 Uiso 1 1 calc R
H11B H -0.1700 1.2790 0.3073 0.026 Uiso 1 1 calc R
H11C H -0.1040 1.2365 0.3492 0.026 Uiso 1 1 calc R
N1 N -0.07503(14) 1.2044(3) 0.47201(9) 0.0133(4) Uani 1 1 d .
N2 N -0.21738(14) 1.1443(3) 0.45480(9) 0.0120(5) Uani 1 1 d .
N3 N -0.18126(14) 0.7913(3) 0.36141(9) 0.0133(5) Uani 1 1 d .
N4 N -0.19855(13) 1.0679(3) 0.34180(8) 0.0124(4) Uani 1 1 d .
Cl1 Cl 0.09973(4) 1.04765(8) 0.35723(2) 0.01691(13) Uani 1 1 d .
Cl2 Cl 0.08272(4) 0.87614(8) 0.47676(2) 0.01841(14) Uani 1 1 d .
Cl3 Cl 0.02441(4) 0.65349(8) 0.37256(3) 0.01881(14) Uani 1 1 d .
Ga1 Ga 0.012561(16) 0.90052(3) 0.407011(10) 0.01125(6) Uani 1 1 d .
C12 C 0.13467(15) 0.9950(3) 0.15083(10) 0.0113(5) Uani 1 1 d .
C13 C 0.10708(16) 1.1141(3) 0.11687(9) 0.0105(5) Uani 1 1 d .
C14 C 0.07677(15) 0.9498(3) 0.19013(9) 0.0090(5) Uani 1 1 d .
C15 C 0.24342(17) 1.2789(4) 0.10833(14) 0.0179(7) Uani 1 1 d .
H15A H 0.2457 1.2648 0.1430 0.027 Uiso 1 1 calc R
H15B H 0.2440 1.3948 0.1006 0.027 Uiso 1 1 calc R
H15C H 0.2931 1.2263 0.0937 0.027 Uiso 1 1 calc R
C16 C 0.15093(19) 1.2317(4) 0.03785(13) 0.0184(7) Uani 1 1 d .
H16A H 0.0985 1.1766 0.0277 0.028 Uiso 1 1 calc R
H16B H 0.1997 1.1880 0.0200 0.028 Uiso 1 1 calc R
H16C H 0.1457 1.3482 0.0316 0.028 Uiso 1 1 calc R
C17 C -0.00885(17) 1.3096(4) 0.09377(12) 0.0173(6) Uani 1 1 d .
H17A H 0.0394 1.3855 0.0947 0.026 Uiso 1 1 calc R
H17B H -0.0526 1.3443 0.1167 0.026 Uiso 1 1 calc R
H17C H -0.0334 1.3080 0.0616 0.026 Uiso 1 1 calc R
C18 C -0.04882(15) 1.0252(3) 0.11335(10) 0.0132(5) Uani 1 1 d .
H18A H -0.0248 0.9162 0.1171 0.020 Uiso 1 1 calc R
H18B H -0.0866 1.0273 0.0854 0.020 Uiso 1 1 calc R
H18C H -0.0816 1.0539 0.1420 0.020 Uiso 1 1 calc R
C19 C 0.07459(19) 1.2327(3) 0.22337(15) 0.0192(7) Uani 1 1 d .
H19A H 0.1352 1.2333 0.2144 0.029 Uiso 1 1 calc R
H19B H 0.0686 1.2699 0.2564 0.029 Uiso 1 1 calc R
H19C H 0.0427 1.3053 0.2022 0.029 Uiso 1 1 calc R
C20 C -0.04430(17) 1.0411(3) 0.24349(10) 0.0158(6) Uani 1 1 d .
H20A H -0.0728 0.9448 0.2305 0.024 Uiso 1 1 calc R
H20B H -0.0803 1.1366 0.2381 0.024 Uiso 1 1 calc R
H20C H -0.0349 1.0267 0.2778 0.024 Uiso 1 1 calc R
C21 C 0.05574(17) 0.6635(3) 0.16191(10) 0.0154(6) Uani 1 1 d .
H21A H -0.0028 0.6220 0.1597 0.023 Uiso 1 1 calc R
H21B H 0.0948 0.5743 0.1696 0.023 Uiso 1 1 calc R
H21C H 0.0723 0.7119 0.1313 0.023 Uiso 1 1 calc R
C22 C 0.04502(19) 0.7249(4) 0.24919(13) 0.0178(6) Uani 1 1 d .
H22A H 0.0577 0.8097 0.2727 0.027 Uiso 1 1 calc R
H22B H 0.0823 0.6312 0.2549 0.027 Uiso 1 1 calc R
H22C H -0.0149 0.6916 0.2523 0.027 Uiso 1 1 calc R
N5 N 0.16441(13) 1.2049(3) 0.08965(9) 0.0126(4) Uani 1 1 d .
N6 N 0.02160(13) 1.1437(3) 0.10657(8) 0.0114(5) Uani 1 1 d .
N7 N 0.03997(14) 1.0642(2) 0.21900(8) 0.0130(5) Uani 1 1 d .
N8 N 0.06029(14) 0.7888(3) 0.20013(9) 0.0128(4) Uani 1 1 d .
Cl4 Cl 0.32313(4) 0.87942(8) 0.08454(2) 0.01806(14) Uani 1 1 d .
Cl5 Cl 0.33840(4) 1.04796(8) 0.20477(2) 0.01794(14) Uani 1 1 d .
Cl6 Cl 0.26453(4) 0.65207(8) 0.18716(3) 0.01799(14) Uani 1 1 d .
Ga2 Ga 0.252514(16) 0.90174(3) 0.154323(10) 0.01102(6) Uani 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 0.0031 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
C2 C1 C3 119.7(2)
C2 C1 Ga1 124.26(19)
C3 C1 Ga1 115.74(18)
N2 C2 N1 113.4(2)
N2 C2 C1 122.9(2)
N1 C2 C1 123.7(2)
N3 C3 N4 117.9(2)
N3 C3 C1 120.9(2)
N4 C3 C1 121.1(2)
C2 N1 C4 123.5(3)
C2 N1 C5 122.1(2)
C4 N1 C5 114.4(2)
C2 N2 C7 124.9(2)
C2 N2 C6 121.6(2)
C7 N2 C6 113.0(2)
C3 N3 C9 124.4(2)
C3 N3 C8 121.7(2)
C9 N3 C8 113.9(2)
C3 N4 C10 123.9(2)
C3 N4 C11 121.8(2)
C10 N4 C11 113.3(2)
C1 Ga1 Cl2 116.44(8)
C1 Ga1 Cl3 116.57(7)
Cl2 Ga1 Cl3 104.48(3)
C1 Ga1 Cl1 111.38(7)
Cl2 Ga1 Cl1 106.56(3)
Cl3 Ga1 Cl1 99.68(3)
C13 C12 C14 118.9(2)
C13 C12 Ga2 124.98(19)
C14 C12 Ga2 115.64(18)
N6 C13 N5 114.3(2)
N6 C13 C12 123.2(2)
N5 C13 C12 122.5(2)
N7 C14 N8 117.6(2)
N7 C14 C12 121.7(2)
N8 C14 C12 120.6(2)
C13 N5 C15 124.5(2)
C13 N5 C16 121.6(2)
C15 N5 C16 113.9(2)
C13 N6 C18 124.9(2)
C13 N6 C17 121.2(2)
C18 N6 C17 113.4(2)
C14 N7 C19 122.4(2)
C14 N7 C20 123.5(2)
C19 N7 C20 113.5(2)
C14 N8 C21 122.0(2)
C14 N8 C22 123.8(2)
C21 N8 C22 114.2(2)
C12 Ga2 Cl4 116.16(9)
C12 Ga2 Cl6 116.51(7)
Cl4 Ga2 Cl6 103.75(3)
C12 Ga2 Cl5 111.59(8)
Cl4 Ga2 Cl5 106.90(3)
Cl6 Ga2 Cl5 100.34(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.397(3)
C1 C3 1.437(4)
C1 Ga1 1.965(2)
C2 N2 1.366(3)
C2 N1 1.366(3)
C3 N3 1.349(3)
C3 N4 1.350(3)
C4 N1 1.452(3)
C5 N1 1.461(4)
C6 N2 1.463(3)
C7 N2 1.461(3)
C8 N3 1.463(3)
C9 N3 1.457(4)
C10 N4 1.460(3)
C11 N4 1.462(3)
Cl1 Ga1 2.2497(7)
Cl2 Ga1 2.2036(7)
Cl3 Ga1 2.2156(7)
C12 C13 1.405(3)
C12 C14 1.443(4)
C12 Ga2 1.958(2)
C13 N6 1.361(3)
C13 N5 1.366(3)
C14 N7 1.341(3)
C14 N8 1.353(3)
C15 N5 1.444(3)
C16 N5 1.452(4)
C17 N6 1.462(3)
C18 N6 1.454(3)
C19 N7 1.465(3)
C20 N7 1.467(3)
C21 N8 1.459(3)
C22 N8 1.461(4)
Cl4 Ga2 2.2064(7)
Cl5 Ga2 2.2454(7)
Cl6 Ga2 2.2166(7)
