#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:51:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179309 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/06/4320675.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_4320675
loop_
_publ_author_name
'Malcolm H. Chisholm'
'Diana Navarro-Llobet'
'Judith Gallucci'
_publ_section_title
;
 Siloxide and Triflate Gallium(III) Complexes Supported by the BDI Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6506
_journal_page_last               6508
_journal_paper_doi               10.1021/ic010771j
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C32 H50 Cl Ga N2 O Si'
_chemical_formula_weight         612.00
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-93 and manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 115.313(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1113(1)
_cell_length_b                   20.1484(2)
_cell_length_c                   10.1963(1)
_cell_measurement_reflns_used    4004
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.04
_cell_volume                     1692.10(3)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33256
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.953
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.406
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.038
_refine_ls_goodness_of_fit_obs   1.065
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_restrained_S_obs      1.065
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_obs          0.0295
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0367P)²+0.7227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0766
_refine_ls_wR_factor_obs         0.0730
_reflns_number_observed          3462
_reflns_number_total             3993
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010771j_2.cif
_cod_data_source_block           Chisholm909
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.7227P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.7227P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4320675
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ga Ga 0.03081(3) 0.2500 0.23335(2) 0.01859(8) Uani 1 d S .
Cl Cl -0.18331(7) 0.2500 0.02618(6) 0.03218(14) Uani 1 d S .
Si Si 0.25163(9) 0.2500 0.06470(8) 0.0426(2) Uani 1 d S .
O O 0.2106(2) 0.2500 0.2036(2) 0.0242(3) Uani 1 d S .
N N 0.02700(15) 0.32211(6) 0.35499(13) 0.0206(3) Uani 1 d . .
C1 C -0.0180(2) 0.31271(8) 0.4624(2) 0.0229(3) Uani 1 d . .
C2 C -0.0478(3) 0.2500 0.5049(2) 0.0263(5) Uani 1 d S .
H2 H -0.0949(3) 0.2500 0.5719(2) 0.032 Uiso 1 calc SR .
C3 C -0.0367(2) 0.37159(9) 0.5447(2) 0.0313(4) Uani 1 d . .
H3A H -0.0254(15) 0.35719(14) 0.6404(6) 0.047 Uiso 1 calc R .
H3B H -0.1441(6) 0.3915(4) 0.4908(7) 0.047 Uiso 1 calc R .
H3C H 0.0474(10) 0.4045(3) 0.5566(12) 0.047 Uiso 1 calc R .
C4 C 0.0758(2) 0.38712(8) 0.3273(2) 0.0252(3) Uani 1 d . .
C5 C 0.2431(2) 0.40085(9) 0.3846(2) 0.0349(4) Uani 1 d . .
C6 C 0.2886(3) 0.46247(10) 0.3494(3) 0.0487(6) Uani 1 d . .
H6 H 0.4006(3) 0.47314(10) 0.3857(3) 0.058 Uiso 1 calc R .
C7 C 0.1760(3) 0.50766(10) 0.2642(3) 0.0520(6) Uani 1 d . .
H7 H 0.2105(3) 0.54898(10) 0.2423(3) 0.062 Uiso 1 calc R .
C8 C 0.0134(3) 0.49346(9) 0.2104(2) 0.0441(5) Uani 1 d . .
H8 H -0.0635(3) 0.52532(9) 0.1517(2) 0.053 Uiso 1 calc R .
C9 C -0.0416(2) 0.43280(8) 0.2403(2) 0.0297(4) Uani 1 d . .
C10 C 0.3690(2) 0.35200(10) 0.4820(2) 0.0438(5) Uani 1 d . .
H10 H 0.3222(2) 0.30640(10) 0.4558(2) 0.053 Uiso 1 calc R .
C11 C 0.5263(3) 0.35399(14) 0.4614(3) 0.0725(8) Uani 1 d . .
H11A H 0.5965(11) 0.3170(6) 0.5143(19) 0.109 Uiso 1 calc R .
H11B H 0.5826(13) 0.3961(5) 0.4989(21) 0.109 Uiso 1 calc R .
H11C H 0.5001(3) 0.3502(11) 0.3579(4) 0.109 Uiso 1 calc R .
C12 C 0.4080(3) 0.36367(14) 0.6412(3) 0.0630(7) Uani 1 d . .
H12A H 0.3097(6) 0.3571(9) 0.6562(5) 0.095 Uiso 1 calc R .
H12B H 0.4475(21) 0.4092(3) 0.6681(6) 0.095 Uiso 1 calc R .
H12C H 0.4918(16) 0.3323(6) 0.7015(3) 0.095 Uiso 1 calc R .
C13 C -0.2223(2) 0.42039(9) 0.1796(2) 0.0354(4) Uani 1 d . .
H13 H -0.2394(2) 0.37573(9) 0.2135(2) 0.042 Uiso 1 calc R .
C14 C -0.3024(3) 0.42022(11) 0.0130(2) 0.0528(6) Uani 1 d . .
H14A H -0.4170(6) 0.4078(8) -0.0221(2) 0.079 Uiso 1 calc R .
H14B H -0.2470(13) 0.3881(6) -0.0224(2) 0.079 Uiso 1 calc R .
H14C H -0.2945(18) 0.4646(2) -0.0227(2) 0.079 Uiso 1 calc R .
C15 C -0.3069(3) 0.47229(11) 0.2340(2) 0.0497(5) Uani 1 d . .
H15A H -0.4217(5) 0.4605(4) 0.2003(14) 0.074 Uiso 1 calc R .
H15B H -0.2983(17) 0.5161(2) 0.1961(14) 0.074 Uiso 1 calc R .
H15C H -0.2548(13) 0.4734(6) 0.3403(3) 0.074 Uiso 1 calc R .
C16 C 0.4737(4) 0.2500 0.1240(4) 0.0800(13) Uani 1 d S .
H16A H 0.4980(5) 0.2655(17) 0.0443(14) 0.120 Uiso 0.50 calc PR .
H16B H 0.5158(7) 0.2049(3) 0.1516(37) 0.120 Uiso 0.50 calc PR .
H16C H 0.5250(6) 0.2797(14) 0.2075(25) 0.120 Uiso 0.50 calc PR .
C17 C 0.1674(5) 0.3261(3) -0.0434(5) 0.157(2) Uani 1 d . .
H17A H 0.0488(6) 0.3257(10) -0.0813(38) 0.235 Uiso 1 calc R .
H17B H 0.1983(43) 0.3278(11) -0.1243(26) 0.235 Uiso 1 calc R .
H17C H 0.2106(39) 0.3653(3) 0.0184(12) 0.235 Uiso 1 calc R .
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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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
_geom_angle_publ_flag
O Ga N 112.36(5) . . ?
O Ga N 112.35(5) . 4_565 ?
N Ga N 98.34(8) . 4_565 ?
O Ga Cl 109.92(5) . . ?
N Ga Cl 111.74(4) . . ?
N Ga Cl 111.74(4) 4_565 . ?
O Si C16 110.21(14) . . ?
O Si C17 109.26(14) . 4_565 ?
C16 Si C17 108.16(14) . 4_565 ?
O Si C17 109.26(14) . . ?
C16 Si C17 108.16(14) . . ?
C17 Si C17 111.8(4) 4_565 . ?
Si O Ga 136.25(10) . . ?
C1 N C4 120.99(13) . . ?
C1 N Ga 121.22(11) . . ?
C4 N Ga 117.78(9) . . ?
N C1 C2 123.34(15) . . ?
N C1 C3 119.52(14) . . ?
C2 C1 C3 117.13(14) . . ?
C1 C2 C1 129.1(2) . 4_565 ?
C1 C2 H2 115.46(10) . . ?
C1 C2 H2 115.46(10) 4_565 . ?
C1 C3 H3A 109.47(9) . . ?
C1 C3 H3B 109.47(9) . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.47(9) . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C9 C4 C5 122.1(2) . . ?
C9 C4 N 120.13(14) . . ?
C5 C4 N 117.69(15) . . ?
C6 C5 C4 116.9(2) . . ?
C6 C5 C10 121.3(2) . . ?
C4 C5 C10 121.8(2) . . ?
C7 C6 C5 121.9(2) . . ?
C7 C6 H6 119.06(12) . . ?
C5 C6 H6 119.06(12) . . ?
C6 C7 C8 120.2(2) . . ?
C6 C7 H7 119.90(12) . . ?
C8 C7 H7 119.90(13) . . ?
C7 C8 C9 121.3(2) . . ?
C7 C8 H8 119.35(13) . . ?
C9 C8 H8 119.35(12) . . ?
C4 C9 C8 117.6(2) . . ?
C4 C9 C13 123.58(15) . . ?
C8 C9 C13 118.9(2) . . ?
C5 C10 C12 111.3(2) . . ?
C5 C10 C11 112.5(2) . . ?
C12 C10 C11 109.6(2) . . ?
C5 C10 H10 107.73(9) . . ?
C12 C10 H10 107.73(14) . . ?
C11 C10 H10 107.73(12) . . ?
C10 C11 H11A 109.47(15) . . ?
C10 C11 H11B 109.47(12) . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.47(14) . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.47(11) . . ?
C10 C12 H12B 109.47(14) . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.47(12) . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 C14 111.9(2) . . ?
C9 C13 C15 111.5(2) . . ?
C14 C13 C15 109.0(2) . . ?
C9 C13 H13 108.10(9) . . ?
C14 C13 H13 108.10(11) . . ?
C15 C13 H13 108.10(11) . . ?
C13 C14 H14A 109.47(12) . . ?
C13 C14 H14B 109.47(11) . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.47(11) . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.47(12) . . ?
C13 C15 H15B 109.47(11) . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.47(11) . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si C16 H16A 109.47(11) . . ?
Si C16 H16B 109.47(2) . . ?
H16A C16 H16B 109.5 . . ?
Si C16 H16C 109.47(9) . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si C17 H17A 109.47(13) . . ?
Si C17 H17B 109.47(13) . . ?
H17A C17 H17B 109.5 . . ?
Si C17 H17C 109.5(2) . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ga O 1.7892(15) . ?
Ga N 1.9203(12) . ?
Ga N 1.9203(12) 4_565 ?
Ga Cl 2.1781(6) . ?
Si O 1.611(2) . ?
Si C16 1.847(3) . ?
Si C17 1.853(4) 4_565 ?
Si C17 1.853(4) . ?
N C1 1.337(2) . ?
N C4 1.449(2) . ?
C1 C2 1.399(2) . ?
C1 C3 1.504(2) . ?
C2 C1 1.399(2) 4_565 ?
C2 H2 0.95 . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 C9 1.402(2) . ?
C4 C5 1.407(2) . ?
C5 C6 1.403(3) . ?
C5 C10 1.515(3) . ?
C6 C7 1.369(3) . ?
C6 H6 0.95 . ?
C7 C8 1.372(3) . ?
C7 H7 0.95 . ?
C8 C9 1.403(2) . ?
C8 H8 0.95 . ?
C9 C13 1.512(3) . ?
C10 C12 1.524(3) . ?
C10 C11 1.535(3) . ?
C10 H10 1.00 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C14 1.535(3) . ?
C13 C15 1.537(3) . ?
C13 H13 1.00 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C15 H15C 0.98 . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 Si O Ga 180.0 . . . . ?
C17 Si O Ga -61.3(2) 4_565 . . . ?
C17 Si O Ga 61.3(2) . . . . ?
N Ga O Si -125.10(4) . . . . ?
N Ga O Si 125.10(4) 4_565 . . . ?
Cl Ga O Si 0.0 . . . . ?
O Ga N C1 -135.66(11) . . . . ?
N Ga N C1 -17.24(15) 4_565 . . . ?
Cl Ga N C1 100.24(11) . . . . ?
O Ga N C4 43.87(12) . . . . ?
N Ga N C4 162.29(8) 4_565 . . . ?
Cl Ga N C4 -80.22(11) . . . . ?
C4 N C1 C2 -172.2(2) . . . . ?
Ga N C1 C2 7.3(2) . . . . ?
C4 N C1 C3 7.0(2) . . . . ?
Ga N C1 C3 -173.44(11) . . . . ?
N C1 C2 C1 9.3(4) . . . 4_565 ?
C3 C1 C2 C1 -170.0(2) . . . 4_565 ?
C1 N C4 C9 -84.9(2) . . . . ?
Ga N C4 C9 95.54(15) . . . . ?
C1 N C4 C5 98.0(2) . . . . ?
Ga N C4 C5 -81.5(2) . . . . ?
C9 C4 C5 C6 -0.8(2) . . . . ?
N C4 C5 C6 176.23(15) . . . . ?
C9 C4 C5 C10 178.2(2) . . . . ?
N C4 C5 C10 -4.7(2) . . . . ?
C4 C5 C6 C7 0.5(3) . . . . ?
C10 C5 C6 C7 -178.5(2) . . . . ?
C5 C6 C7 C8 0.0(3) . . . . ?
C6 C7 C8 C9 -0.2(3) . . . . ?
C5 C4 C9 C8 0.6(2) . . . . ?
N C4 C9 C8 -176.38(14) . . . . ?
C5 C4 C9 C13 -178.6(2) . . . . ?
N C4 C9 C13 4.4(2) . . . . ?
C7 C8 C9 C4 -0.1(3) . . . . ?
C7 C8 C9 C13 179.2(2) . . . . ?
C6 C5 C10 C12 89.1(2) . . . . ?
C4 C5 C10 C12 -89.9(2) . . . . ?
C6 C5 C10 C11 -34.4(3) . . . . ?
C4 C5 C10 C11 146.6(2) . . . . ?
C4 C9 C13 C14 -118.2(2) . . . . ?
C8 C9 C13 C14 62.6(2) . . . . ?
C4 C9 C13 C15 119.4(2) . . . . ?
C8 C9 C13 C15 -59.8(2) . . . . ?
