#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:04:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179466 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/63/4336306.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_4336306
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_formula_moiety         'C28 H26 Cl3 Ga P2, C H2 Cl2 '
_chemical_formula_sum            'C29 H28 Cl5 Ga P2'
_chemical_formula_weight         685.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.6300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8128(4)
_cell_length_b                   15.2735(6)
_cell_length_c                   16.6469(5)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      36.34
_cell_measurement_theta_min      2.19
_cell_volume                     2983.39(18)
_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 0.953
_diffrn_measured_fraction_theta_max 0.677
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            40867
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.39
_diffrn_reflns_theta_min         1.82
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.686
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         9839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0396P)²+2.4004P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                8385
_reflns_number_total             9839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401817g_si_001_3.cif
_cod_data_source_block           4-GaCl3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4336306
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.12279(12) 0.14413(8) 0.25097(8) 0.0120(2) Uani 1 1 d .
C2 C 0.08431(13) -0.02901(9) 0.31526(9) 0.0155(3) Uani 1 1 d .
H2A H 0.1526 -0.0562 0.2995 0.019 Uiso 1 1 calc R
H2B H 0.0658 -0.0581 0.3639 0.019 Uiso 1 1 calc R
C3 C -0.01420(13) -0.04283(9) 0.24748(9) 0.0170(3) Uani 1 1 d .
H3A H -0.0304 -0.1049 0.2417 0.020 Uiso 1 1 calc R
H3B H -0.0821 -0.0140 0.2621 0.020 Uiso 1 1 calc R
C4 C 0.01482(13) -0.00628(9) 0.16659(9) 0.0155(3) Uani 1 1 d .
H4A H -0.0465 -0.0209 0.1249 0.019 Uiso 1 1 calc R
H4B H 0.0834 -0.0348 0.1528 0.019 Uiso 1 1 calc R
C5 C 0.24879(13) 0.09164(9) 0.39965(8) 0.0137(3) Uani 1 1 d .
C6 C 0.34556(13) 0.07654(9) 0.36100(9) 0.0166(3) Uani 1 1 d .
H6 H 0.3379 0.0626 0.3063 0.020 Uiso 1 1 calc R
C7 C 0.45337(14) 0.08216(10) 0.40388(10) 0.0194(3) Uani 1 1 d .
H7 H 0.5178 0.0721 0.3779 0.023 Uiso 1 1 calc R
C8 C 0.46458(14) 0.10289(10) 0.48569(9) 0.0199(3) Uani 1 1 d .
H8 H 0.5368 0.1071 0.5143 0.024 Uiso 1 1 calc R
C9 C 0.36907(14) 0.11727(10) 0.52490(9) 0.0197(3) Uani 1 1 d .
H9 H 0.3772 0.1306 0.5798 0.024 Uiso 1 1 calc R
C10 C 0.26067(14) 0.11182(9) 0.48214(9) 0.0165(3) Uani 1 1 d .
H10 H 0.1965 0.1216 0.5084 0.020 Uiso 1 1 calc R
C11 C 0.00697(13) 0.12147(9) 0.40070(8) 0.0141(3) Uani 1 1 d .
C12 C 0.01203(13) 0.20834(10) 0.42862(9) 0.0169(3) Uani 1 1 d .
H12 H 0.0680 0.2458 0.4137 0.020 Uiso 1 1 calc R
C13 C -0.06605(14) 0.23838(10) 0.47822(10) 0.0197(3) Uani 1 1 d .
H13 H -0.0605 0.2954 0.4979 0.024 Uiso 1 1 calc R
C14 C -0.15273(14) 0.18409(11) 0.49879(9) 0.0196(3) Uani 1 1 d .
H14 H -0.2052 0.2047 0.5318 0.024 Uiso 1 1 calc R
C15 C -0.16035(15) 0.09893(11) 0.46969(10) 0.0219(3) Uani 1 1 d .
H15 H -0.2193 0.0629 0.4821 0.026 Uiso 1 1 calc R
C16 C -0.07993(14) 0.06708(10) 0.42179(10) 0.0194(3) Uani 1 1 d .
H16 H -0.0843 0.0094 0.4038 0.023 Uiso 1 1 calc R
C17 C 0.09817(13) 0.12986(9) 0.07349(8) 0.0140(3) Uani 1 1 d .
C18 C 0.19829(14) 0.08443(10) 0.06216(10) 0.0189(3) Uani 1 1 d .
H18 H 0.2339 0.0496 0.1034 0.023 Uiso 1 1 calc R
C19 C 0.24399(15) 0.09143(11) -0.01048(10) 0.0218(3) Uani 1 1 d .
H19 H 0.3095 0.0604 -0.0184 0.026 Uiso 1 1 calc R
C20 C 0.19201(15) 0.14477(11) -0.07171(10) 0.0223(3) Uani 1 1 d .
H20 H 0.2232 0.1495 -0.1203 0.027 Uiso 1 1 calc R
C21 C 0.09401(15) 0.19095(10) -0.06074(9) 0.0208(3) Uani 1 1 d .
H21 H 0.0601 0.2270 -0.1017 0.025 Uiso 1 1 calc R
C22 C 0.04646(14) 0.18338(10) 0.01154(8) 0.0165(3) Uani 1 1 d .
H22 H -0.0197 0.2139 0.0187 0.020 Uiso 1 1 calc R
C23 C -0.10525(12) 0.15799(9) 0.15403(8) 0.0131(2) Uani 1 1 d .
C24 C -0.18546(13) 0.13158(10) 0.08948(9) 0.0172(3) Uani 1 1 d .
H24 H -0.1649 0.0914 0.0518 0.021 Uiso 1 1 calc R
C25 C -0.29509(14) 0.16542(11) 0.08200(10) 0.0207(3) Uani 1 1 d .
H25 H -0.3477 0.1483 0.0389 0.025 Uiso 1 1 calc R
C26 C -0.32659(14) 0.22466(12) 0.13851(11) 0.0237(3) Uani 1 1 d .
H26 H -0.4004 0.2467 0.1337 0.028 Uiso 1 1 calc R
C27 C -0.24757(16) 0.25103(12) 0.20237(11) 0.0244(3) Uani 1 1 d .
H27 H -0.2687 0.2910 0.2401 0.029 Uiso 1 1 calc R
C28 C -0.13687(14) 0.21791(10) 0.21019(9) 0.0184(3) Uani 1 1 d .
H28 H -0.0843 0.2359 0.2529 0.022 Uiso 1 1 calc R
C29 C 0.51568(18) 1.00049(13) 0.20413(13) 0.0329(4) Uani 1 1 d .
H29A H 0.4932 1.0608 0.2115 0.039 Uiso 1 1 calc R
H29B H 0.4680 0.9634 0.2336 0.039 Uiso 1 1 calc R
P1 P 0.11357(3) 0.08549(2) 0.33784(2) 0.01174(7) Uani 1 1 d .
P2 P 0.03671(3) 0.11118(2) 0.16649(2) 0.01117(7) Uani 1 1 d .
Cl1 Cl 0.26314(3) 0.31957(2) 0.36297(2) 0.01952(8) Uani 1 1 d .
Cl2 Cl 0.38403(3) 0.22567(2) 0.20232(2) 0.01979(8) Uani 1 1 d .
Cl3 Cl 0.13100(3) 0.34810(2) 0.16645(2) 0.01805(7) Uani 1 1 d .
Cl4 Cl 0.49267(5) 0.97385(4) 0.09988(4) 0.04184(13) Uani 1 1 d .
Cl5 Cl 0.65862(6) 0.98700(5) 0.24426(4) 0.05682(18) Uani 1 1 d .
Ga Ga 0.217311(13) 0.248310(9) 0.248407(9) 0.01121(4) 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'
P P 0.1026 0.0946 '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
P2 C1 P1 116.70(8)
P2 C1 Ga 120.64(7)
P1 C1 Ga 122.52(7)
C3 C2 P1 113.21(9)
C4 C3 C2 111.55(13)
C3 C4 P2 114.06(10)
C6 C5 C10 119.66(13)
C6 C5 P1 116.64(10)
C10 C5 P1 123.69(12)
C7 C6 C5 120.31(14)
C6 C7 C8 119.72(16)
C9 C8 C7 120.50(14)
C8 C9 C10 120.02(14)
C9 C10 C5 119.78(16)
C16 C11 C12 118.89(15)
C16 C11 P1 122.99(12)
C12 C11 P1 118.12(12)
C13 C12 C11 120.28(15)
C12 C13 C14 120.61(15)
C15 C14 C13 119.53(16)
C14 C15 C16 120.34(16)
C15 C16 C11 120.30(15)
C22 C17 C18 119.52(14)
C22 C17 P2 122.62(12)
C18 C17 P2 117.75(11)
C19 C18 C17 119.95(15)
C18 C19 C20 120.11(16)
C21 C20 C19 120.42(16)
C20 C21 C22 119.93(15)
C21 C22 C17 120.05(15)
C28 C23 C24 119.53(14)
C28 C23 P2 119.98(10)
C24 C23 P2 120.45(11)
C25 C24 C23 120.09(14)
C24 C25 C26 120.22(14)
C25 C26 C27 119.90(15)
C26 C27 C28 120.38(16)
C23 C28 C27 119.88(14)
Cl5 C29 Cl4 112.20(11)
C1 P1 C5 108.43(7)
C1 P1 C11 116.38(7)
C5 P1 C11 106.50(7)
C1 P1 C2 110.97(7)
C5 P1 C2 107.70(6)
C11 P1 C2 106.47(7)
C1 P2 C17 113.44(7)
C1 P2 C4 111.18(6)
C17 P2 C4 103.21(7)
C1 P2 C23 115.57(7)
C17 P2 C23 107.31(7)
C4 P2 C23 105.09(7)
C1 Ga Cl1 117.90(4)
C1 Ga Cl3 110.59(4)
Cl1 Ga Cl3 104.028(15)
C1 Ga Cl2 114.45(5)
Cl1 Ga Cl2 103.665(16)
Cl3 Ga Cl2 104.943(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 P2 1.7131(12)
C1 P1 1.7152(14)
C1 Ga 1.9471(13)
C2 C3 1.5390(19)
C2 P1 1.8136(14)
C3 C4 1.533(2)
C4 P2 1.8126(14)
C5 C6 1.394(2)
C5 C10 1.399(2)
C5 P1 1.7999(13)
C6 C7 1.389(2)
C7 C8 1.389(2)
C8 C9 1.385(3)
C9 C10 1.394(2)
C11 C16 1.397(2)
C11 C12 1.405(2)
C11 P1 1.8130(16)
C12 C13 1.385(2)
C13 C14 1.391(2)
C14 C15 1.387(2)
C15 C16 1.396(3)
C17 C22 1.400(2)
C17 C18 1.403(2)
C17 P2 1.8069(15)
C18 C19 1.384(3)
C19 C20 1.391(2)
C20 C21 1.386(3)
C21 C22 1.390(2)
C23 C28 1.390(2)
C23 C24 1.4071(18)
C23 P2 1.8127(15)
C24 C25 1.387(2)
C25 C26 1.387(3)
C26 C27 1.391(2)
C27 C28 1.394(2)
C29 Cl5 1.755(2)
C29 Cl4 1.773(2)
Cl1 Ga 2.2082(4)
Cl2 Ga 2.2216(4)
Cl3 Ga 2.2142(3)
