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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/4/33/18/4331805.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_4331805
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_absolute_configuration ad
_chemical_formula_moiety         'C11 H16 Br3 Ga N2 O2'
_chemical_formula_sum            'C11 H16 Br3 Ga N2 O2'
_chemical_formula_weight         517.71
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            4
_cell_length_a                   9.4112(4)
_cell_length_b                   11.2663(4)
_cell_length_c                   15.2990(6)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      35.04
_cell_measurement_theta_min      2.54
_cell_volume                     1622.14(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.857
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23504
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         36.34
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_exptl_absorpt_coefficient_mu    9.084
_exptl_absorpt_correction_T_max  0.4132
_exptl_absorpt_correction_T_min  0.1812
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_description       bloc
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         6620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0108P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0381
_reflns_number_gt                5570
_reflns_number_total             6620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302440g_si_001_5.cif
_cod_data_source_block           6rx1519GuillotICMMO
_cod_database_code               4331805
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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
C1 C 1.0782(2) 0.38616(15) 0.25500(11) 0.0134(3) Uani 1 1 d .
C2 C 1.1657(2) 0.35933(17) 0.39125(12) 0.0182(4) Uani 1 1 d .
C3 C 1.2762(2) 0.35964(16) 0.33700(11) 0.0172(4) Uani 1 1 d .
C4 C 0.9208(2) 0.38365(16) 0.40184(11) 0.0157(4) Uani 1 1 d .
C5 C 0.9875(2) 0.31597(17) 0.47920(13) 0.0239(5) Uani 1 1 d .
H5A H 0.9451 0.3411 0.5339 0.029 Uiso 1 1 calc R
H5B H 0.9732 0.2312 0.4726 0.029 Uiso 1 1 calc R
C6 C 0.7909(2) 0.32211(19) 0.36737(13) 0.0273(5) Uani 1 1 d .
H6A H 0.7524 0.3668 0.3195 0.041 Uiso 1 1 calc R
H6B H 0.7212 0.3162 0.4130 0.041 Uiso 1 1 calc R
H6C H 0.8160 0.2440 0.3476 0.041 Uiso 1 1 calc R
C7 C 0.8944(2) 0.51300(16) 0.42583(13) 0.0223(4) Uani 1 1 d .
H7A H 0.9767 0.5445 0.4548 0.033 Uiso 1 1 calc R
H7B H 0.8139 0.5181 0.4641 0.033 Uiso 1 1 calc R
H7C H 0.8761 0.5579 0.3737 0.033 Uiso 1 1 calc R
C8 C 1.34135(19) 0.37595(16) 0.18960(12) 0.0167(4) Uani 1 1 d .
C9 C 1.4605(2) 0.3288(2) 0.24938(13) 0.0288(5) Uani 1 1 d .
H9A H 1.4745 0.2446 0.2394 0.035 Uiso 1 1 calc R
H9B H 1.5489 0.3696 0.2367 0.035 Uiso 1 1 calc R
C10 C 1.3223(2) 0.28961(18) 0.11430(13) 0.0246(4) Uani 1 1 d .
H10A H 1.2948 0.2134 0.1367 0.037 Uiso 1 1 calc R
H10B H 1.4102 0.2822 0.0829 0.037 Uiso 1 1 calc R
H10C H 1.2499 0.3186 0.0756 0.037 Uiso 1 1 calc R
C11 C 1.3687(2) 0.50275(16) 0.15999(13) 0.0224(4) Uani 1 1 d .
H11A H 1.2905 0.5296 0.1249 0.034 Uiso 1 1 calc R
H11B H 1.4546 0.5055 0.1262 0.034 Uiso 1 1 calc R
H11C H 1.3782 0.5532 0.2102 0.034 Uiso 1 1 calc R
N1 N 1.04592(17) 0.37593(12) 0.34167(9) 0.0136(3) Uani 1 1 d .
N2 N 1.22230(16) 0.37513(13) 0.25377(9) 0.0135(3) Uani 1 1 d .
O1 O 1.13907(16) 0.34455(13) 0.47769(8) 0.0244(3) Uani 1 1 d .
O2 O 1.41973(15) 0.34930(14) 0.33918(9) 0.0260(3) Uani 1 1 d .
Ga1 Ga 0.93890(2) 0.405684(18) 0.156496(12) 0.01372(4) Uani 1 1 d .
Br1 Br 1.03035(2) 0.462035(18) 0.021547(12) 0.02203(5) Uani 1 1 d .
Br2 Br 0.77999(2) 0.560451(17) 0.189094(12) 0.02171(5) Uani 1 1 d .
Br3 Br 0.80944(2) 0.231149(17) 0.137520(12) 0.02207(5) 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'
O O 0.0109 0.0061 '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'
Br Br -0.2910 2.4679 '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 103.15(15)
N1 C1 Ga1 126.32(14)
N2 C1 Ga1 130.49(13)
C3 C2 O1 138.82(19)
C3 C2 N1 107.29(16)
O1 C2 N1 113.86(17)
C2 C3 O2 139.73(17)
C2 C3 N2 106.73(16)
O2 C3 N2 113.54(16)
N1 C4 C6 113.43(15)
N1 C4 C7 109.39(15)
C6 C4 C7 113.18(18)
N1 C4 C5 97.07(15)
C6 C4 C5 111.89(16)
C7 C4 C5 110.77(16)
O1 C5 C4 106.03(15)
N2 C8 C10 114.04(15)
N2 C8 C11 109.23(15)
C10 C8 C11 113.31(16)
N2 C8 C9 98.87(14)
C10 C8 C9 108.37(17)
C11 C8 C9 112.17(17)
O2 C9 C8 108.40(16)
C1 N1 C2 111.46(16)
C1 N1 C4 140.12(16)
C2 N1 C4 108.30(14)
C1 N2 C3 111.38(15)
C1 N2 C8 139.24(15)
C3 N2 C8 109.38(15)
C2 O1 C5 102.85(15)
C3 O2 C9 104.77(14)
C1 Ga1 Br1 117.01(5)
C1 Ga1 Br3 110.00(5)
Br1 Ga1 Br3 108.250(11)
C1 Ga1 Br2 109.71(5)
Br1 Ga1 Br2 102.789(10)
Br3 Ga1 Br2 108.635(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.365(2)
C1 N2 1.362(2)
C1 Ga1 2.0096(18)
C2 C3 1.331(3)
C2 O1 1.356(2)
C2 N1 1.371(2)
C3 O2 1.356(2)
C3 N2 1.382(2)
C4 N1 1.497(2)
C4 C6 1.501(3)
C4 C7 1.523(3)
C4 C5 1.541(3)
C5 O1 1.462(3)
C8 N2 1.490(2)
C8 C10 1.518(3)
C8 C11 1.521(3)
C8 C9 1.542(3)
C9 O2 1.445(2)
Ga1 Br1 2.3251(3)
Ga1 Br3 2.3314(3)
Ga1 Br2 2.3507(3)
