#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/83/7008352.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_7008352
loop_
_publ_author_name
'Saatchi, Katayoun'
'Patrick, Brian O.'
'Orvig, Chris'
_publ_section_title
;
 Coordination chemistry of P, O-bidentate phosphinophenolates with Ga3+
 and In3+.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2268
_journal_page_last               2274
_journal_paper_doi               10.1039/b501908g
_journal_year                    2005
_chemical_formula_sum            'C18.5 H16 Cl4 Ga O P'
_chemical_formula_weight         496.80
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.024(3)
_cell_angle_beta                 108.807(2)
_cell_angle_gamma                94.664(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2856(5)
_cell_length_b                   9.8663(7)
_cell_length_c                   12.5628(5)
_cell_measurement_reflns_used    6155
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.69
_cell_measurement_theta_min      2.91
_cell_volume                     1051.79(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.785
_diffrn_measured_fraction_theta_max 0.785
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4272
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    1.897
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4272
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0332
_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)+(0.0000P)²+0.7082P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                3703
_reflns_number_total             4272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b501908g.txt
_cod_data_source_block           copy
_cod_original_cell_volume        1051.79(10)
_cod_original_formula_sum        'C18.50 H16 Cl4 Ga O P'
_cod_database_code               7008352
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.76695(3) 0.86164(3) 0.79635(2) 0.01793(9) Uani 1 1 d . . .
Cl1 Cl 0.65019(8) 0.93793(8) 0.91619(6) 0.03073(16) Uani 1 1 d . . .
Cl2 Cl 0.60192(8) 0.72880(7) 0.63639(6) 0.03429(17) Uani 1 1 d . . .
Cl3 Cl 0.95388(8) 0.75629(7) 0.87466(6) 0.03204(16) Uani 1 1 d . . .
P1 P 1.10821(7) 1.22978(6) 0.82809(5) 0.01556(13) Uani 1 1 d . . .
O1 O 0.86429(19) 1.01244(18) 0.76793(16) 0.0213(4) Uani 1 1 d . . .
C1 C 1.1698(3) 1.1124(3) 0.7294(2) 0.0185(5) Uani 1 1 d . . .
C2 C 1.2258(3) 0.9939(3) 0.7588(2) 0.0285(6) Uani 1 1 d . . .
H2 H 1.2341 0.9770 0.8321 0.034 Uiso 1 1 calc R . .
C3 C 1.2698(3) 0.9003(3) 0.6807(3) 0.0371(7) Uani 1 1 d . . .
H3 H 1.3084 0.8192 0.7005 0.045 Uiso 1 1 calc R . .
C4 C 1.2574(3) 0.9253(3) 0.5740(3) 0.0328(6) Uani 1 1 d . . .
H4 H 1.2874 0.8608 0.5207 0.039 Uiso 1 1 calc R . .
C5 C 1.2021(3) 1.0423(3) 0.5445(2) 0.0304(6) Uani 1 1 d . . .
H5 H 1.1953 1.0591 0.4714 0.036 Uiso 1 1 calc R . .
C6 C 1.1563(3) 1.1362(3) 0.6214(2) 0.0259(5) Uani 1 1 d . . .
H6 H 1.1160 1.2162 0.6005 0.031 Uiso 1 1 calc R . .
C7 C 1.2238(3) 1.4002(3) 0.8793(2) 0.0190(5) Uani 1 1 d . . .
C8 C 1.3246(3) 1.4429(3) 0.8276(3) 0.0305(6) Uani 1 1 d . . .
H8 H 1.3393 1.3793 0.7654 0.037 Uiso 1 1 calc R . .
C9 C 1.4045(3) 1.5800(3) 0.8677(3) 0.0360(7) Uani 1 1 d . . .
H9 H 1.4736 1.6098 0.8324 0.043 Uiso 1 1 calc R . .
C10 C 1.3838(3) 1.6721(3) 0.9579(2) 0.0306(6) Uani 1 1 d . . .
H10 H 1.4373 1.7657 0.9839 0.037 Uiso 1 1 calc R . .
C11 C 1.2853(3) 1.6289(3) 1.0110(2) 0.0286(6) Uani 1 1 d . . .
H11 H 1.2728 1.6926 1.0742 0.034 Uiso 1 1 calc R . .
C12 C 1.2049(3) 1.4935(3) 0.9726(2) 0.0242(5) Uani 1 1 d . . .
H12 H 1.1374 1.4640 1.0092 0.029 Uiso 1 1 calc R . .
C13 C 0.9117(3) 1.2472(2) 0.7656(2) 0.0159(4) Uani 1 1 d . . .
C14 C 0.8627(3) 1.3706(3) 0.7386(2) 0.0214(5) Uani 1 1 d . . .
H14 H 0.9357 1.4522 0.7549 0.026 Uiso 1 1 calc R . .
C15 C 0.7066(3) 1.3722(3) 0.6878(2) 0.0258(5) Uani 1 1 d . . .
H15 H 0.6719 1.4549 0.6685 0.031 Uiso 1 1 calc R . .
C16 C 0.6011(3) 1.2527(3) 0.6652(2) 0.0224(5) Uani 1 1 d . . .
H16 H 0.4943 1.2549 0.6307 0.027 Uiso 1 1 calc R . .
C17 C 0.6481(3) 1.1297(3) 0.6919(2) 0.0198(5) Uani 1 1 d . . .
H17 H 0.5741 1.0491 0.6761 0.024 Uiso 1 1 calc R . .
C18 C 0.8045(3) 1.1258(2) 0.74190(19) 0.0156(4) Uani 1 1 d . . .
Cl4A Cl 0.1649(4) 0.4911(4) 0.5292(3) 0.1216(14) Uani 0.726(8) 1 d PD . 1
C19A C 0.0268(9) 0.5830(19) 0.5717(15) 0.107(6) Uiso 0.363(4) 1 d PD . 1
H19A H 0.0489 0.6834 0.5735 0.128 Uiso 0.363(4) 1 calc PR . 1
H19B H 0.0338 0.5762 0.6507 0.128 Uiso 0.363(4) 1 calc PR . 1
Cl4B Cl 0.0482(13) 0.3929(9) 0.4326(8) 0.075(3) Uiso 0.163(6) 1 d PD . 2
C19B C 0.1097(19) 0.510(2) 0.5755(14) 0.004(4) Uiso 0.082(3) 1 d PD . 2
H19C H 0.1245 0.4578 0.6362 0.005 Uiso 0.082(3) 1 calc PR . 2
H19D H 0.2067 0.5736 0.5916 0.005 Uiso 0.082(3) 1 calc PR . 2
Cl4C Cl 0.1272(15) 0.4179(15) 0.4750(12) 0.045(4) Uiso 0.099(7) 1 d PD . 3
C19C C 0.072(2) 0.570(3) 0.548(3) 0.004(4) Uiso 0.049(4) 1 d PD . 3
H19E H 0.1154 0.6520 0.5269 0.005 Uiso 0.049(4) 1 calc PR . 3
H19F H 0.1251 0.5828 0.6320 0.005 Uiso 0.049(4) 1 calc PR . 3
H1 H 1.125(3) 1.172(3) 0.919(3) 0.028(8) Uiso 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 0.0033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
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
O1 Ga1 Cl3 103.57(6) . . ?
O1 Ga1 Cl2 110.63(6) . . ?
Cl3 Ga1 Cl2 112.26(3) . . ?
O1 Ga1 Cl1 108.96(6) . . ?
Cl3 Ga1 Cl1 111.31(3) . . ?
Cl2 Ga1 Cl1 109.93(3) . . ?
C13 P1 C1 111.84(11) . . ?
C13 P1 C7 109.05(11) . . ?
C1 P1 C7 112.27(11) . . ?
C13 P1 H1 109.2(12) . . ?
C1 P1 H1 105.6(13) . . ?
C7 P1 H1 108.8(13) . . ?
C18 O1 Ga1 126.90(15) . . ?
C2 C1 C6 120.0(2) . . ?
C2 C1 P1 119.66(19) . . ?
C6 C1 P1 120.3(2) . . ?
C3 C2 C1 119.8(3) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 120.6(3) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.1(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 119.6(3) . . ?
C5 C6 H6 120.2 . . ?
C1 C6 H6 120.2 . . ?
C8 C7 C12 120.0(2) . . ?
C8 C7 P1 122.5(2) . . ?
C12 C7 P1 117.43(19) . . ?
C7 C8 C9 119.5(3) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 120.2(3) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C12 120.3(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 119.5(2) . . ?
C11 C12 H12 120.2 . . ?
C7 C12 H12 120.2 . . ?
C14 C13 C18 120.8(2) . . ?
C14 C13 P1 123.86(18) . . ?
C18 C13 P1 115.32(17) . . ?
C15 C14 C13 119.3(2) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 119.8(2) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C17 121.5(2) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C18 C17 C16 119.5(2) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
O1 C18 C17 125.0(2) . . ?
O1 C18 C13 115.8(2) . . ?
C17 C18 C13 119.1(2) . . ?
C19A Cl4A C19A 70.0(8) . 2_566 ?
Cl4A C19A Cl4A 110.0(8) . 2_566 ?
Cl4A C19A H19A 109.7 . . ?
Cl4A C19A H19A 109.7 2_566 . ?
Cl4A C19A H19B 109.7 . . ?
Cl4A C19A H19B 109.7 2_566 . ?
H19A C19A H19B 108.2 . . ?
C19B Cl4B C19B 77.3(10) 2_566 . ?
Cl4B C19B Cl4B 102.7(10) 2_566 . ?
Cl4B C19B H19C 111.2 2_566 . ?
Cl4B C19B H19C 111.2 . . ?
Cl4B C19B H19D 111.2 2_566 . ?
Cl4B C19B H19D 111.2 . . ?
H19C C19B H19D 109.1 . . ?
C19C Cl4C C19C 59.1(15) . 2_566 ?
Cl4C C19C Cl4C 120.9(15) . 2_566 ?
Cl4C C19C H19E 107.1 . . ?
Cl4C C19C H19E 107.1 2_566 . ?
Cl4C C19C H19F 107.1 . . ?
Cl4C C19C H19F 107.1 2_566 . ?
H19E C19C H19F 106.8 . . ?
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
Ga1 O1 1.8354(17) . ?
Ga1 Cl3 2.1633(7) . ?
Ga1 Cl2 2.1667(7) . ?
Ga1 Cl1 2.1730(7) . ?
P1 C13 1.777(2) . ?
P1 C1 1.781(2) . ?
P1 C7 1.790(2) . ?
P1 H1 1.35(3) . ?
O1 C18 1.343(3) . ?
C1 C2 1.389(4) . ?
C1 C6 1.393(4) . ?
C2 C3 1.387(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.384(3) . ?
C7 C12 1.400(4) . ?
C8 C9 1.395(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.374(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.403(3) . ?
C13 C18 1.407(3) . ?
C14 C15 1.386(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.392(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(3) . ?
C17 H17 0.9500 . ?
Cl4A C19A 1.784(10) . ?
Cl4A C19A 1.805(9) 2_566 ?
C19A Cl4A 1.805(9) 2_566 ?
C19A H19A 0.9900 . ?
C19A H19B 0.9900 . ?
Cl4B C19B 1.800(10) 2_566 ?
Cl4B C19B 1.805(10) . ?
C19B Cl4B 1.800(10) 2_566 ?
C19B H19C 0.9900 . ?
C19B H19D 0.9900 . ?
Cl4C C19C 1.791(10) . ?
Cl4C C19C 1.797(10) 2_566 ?
C19C Cl4C 1.797(10) 2_566 ?
C19C H19E 0.9900 . ?
C19C H19F 0.9900 . ?
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
Cl3 Ga1 O1 C18 -165.40(18) . . . . ?
Cl2 Ga1 O1 C18 74.12(19) . . . . ?
Cl1 Ga1 O1 C18 -46.8(2) . . . . ?
C13 P1 C1 C2 -120.9(2) . . . . ?
C7 P1 C1 C2 116.1(2) . . . . ?
C13 P1 C1 C6 56.6(2) . . . . ?
C7 P1 C1 C6 -66.3(2) . . . . ?
C6 C1 C2 C3 0.7(4) . . . . ?
P1 C1 C2 C3 178.2(2) . . . . ?
C1 C2 C3 C4 -0.1(5) . . . . ?
C2 C3 C4 C5 0.1(5) . . . . ?
C3 C4 C5 C6 -0.8(4) . . . . ?
C4 C5 C6 C1 1.3(4) . . . . ?
C2 C1 C6 C5 -1.3(4) . . . . ?
P1 C1 C6 C5 -178.8(2) . . . . ?
C13 P1 C7 C8 -110.9(2) . . . . ?
C1 P1 C7 C8 13.7(3) . . . . ?
C13 P1 C7 C12 66.8(2) . . . . ?
C1 P1 C7 C12 -168.72(19) . . . . ?
C12 C7 C8 C9 -1.3(4) . . . . ?
P1 C7 C8 C9 176.3(2) . . . . ?
C7 C8 C9 C10 0.2(5) . . . . ?
C8 C9 C10 C11 1.0(5) . . . . ?
C9 C10 C11 C12 -1.1(4) . . . . ?
C10 C11 C12 C7 -0.1(4) . . . . ?
C8 C7 C12 C11 1.3(4) . . . . ?
P1 C7 C12 C11 -176.4(2) . . . . ?
C1 P1 C13 C14 -111.9(2) . . . . ?
C7 P1 C13 C14 12.9(2) . . . . ?
C1 P1 C13 C18 67.0(2) . . . . ?
C7 P1 C13 C18 -168.25(17) . . . . ?
C18 C13 C14 C15 -0.1(4) . . . . ?
P1 C13 C14 C15 178.7(2) . . . . ?
C13 C14 C15 C16 0.5(4) . . . . ?
C14 C15 C16 C17 -0.3(4) . . . . ?
C15 C16 C17 C18 -0.3(4) . . . . ?
Ga1 O1 C18 C17 -24.3(3) . . . . ?
Ga1 O1 C18 C13 157.36(16) . . . . ?
C16 C17 C18 O1 -177.6(2) . . . . ?
C16 C17 C18 C13 0.7(3) . . . . ?
C14 C13 C18 O1 178.0(2) . . . . ?
P1 C13 C18 O1 -0.9(3) . . . . ?
C14 C13 C18 C17 -0.5(3) . . . . ?
P1 C13 C18 C17 -179.39(18) . . . . ?
C19A Cl4A C19A Cl4A 0.0 2_566 . . 2_566 ?
C19B Cl4B C19B Cl4B 0.0 2_566 . . 2_566 ?
C19C Cl4C C19C Cl4C 0.000(2) 2_566 . . 2_566 ?
