#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:18:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180071 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/17/7051729.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_7051729
loop_
_publ_author_name
'Vălean, Ana-Maria'
'Gómez-Ruiz, Santiago'
'Lönnecke, Peter'
'Silaghi-Dumitrescu, Ioan'
'Silaghi-Dumitrescu, Luminita'
'Hey-Hawkins, Evamarie'
_publ_section_title
;
 Stabilisation of an inorganic digallane by the phosphinobisthiolato
 P,S,S pincer ligand PPh(2-SC6H4)2
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1771
_journal_paper_doi               10.1039/b907668a
_journal_volume                  33
_journal_year                    2009
_chemical_formula_sum            'C42 H32 Ga2 P2 S5'
_chemical_formula_weight         898.36
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 95.722(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.4599(8)
_cell_length_b                   10.1678(4)
_cell_length_c                   18.2790(7)
_cell_measurement_reflns_used    11357
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.4683
_cell_measurement_theta_min      2.7545
_cell_volume                     3968.6(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
_computing_publication_material  'WINGX (L.J. Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ccd xcalibur s'
_diffrn_measurement_method       'ω scans and φ 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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50091
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    1.732
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.80778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.339
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         4922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0377
_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)+(0.0454P)²+0.9381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                3578
_reflns_number_total             4922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907668a.txt
_cod_data_source_block           c2c
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7051729
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'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.5000 0.12680(10) 0.2500 0.0334(3) Uani 1 2 d S . .
C20 C 0.4384(2) -0.0136(7) 0.0127(2) 0.0872(19) Uani 1 1 d . . .
H20 H 0.3961 -0.0189 0.0234 0.105 Uiso 1 1 calc R . .
C21 C 0.4695(2) 0.1042(7) 0.0265(2) 0.0815(18) Uani 1 1 d . . .
H21 H 0.4461 0.1750 0.0439 0.098 Uiso 1 1 calc R . .
C22 C 0.5340(2) 0.1292(7) 0.0168(2) 0.105(2) Uani 1 1 d . . .
H22 H 0.5554 0.2096 0.0280 0.127 Uiso 1 1 calc R . .
Ga1 Ga 0.428146(13) 0.26761(3) 0.207792(17) 0.02195(10) Uani 1 1 d . . .
P1 P 0.36174(3) 0.42362(7) 0.25698(4) 0.02004(16) Uani 1 1 d . . .
S2 S 0.46834(3) 0.43256(7) 0.14267(4) 0.02462(16) Uani 1 1 d . . .
S3 S 0.34586(3) 0.15760(8) 0.15141(5) 0.03207(19) Uani 1 1 d . . .
C1 C 0.43800(12) 0.5763(3) 0.18008(15) 0.0214(6) Uani 1 1 d . . .
C2 C 0.39382(12) 0.5782(3) 0.23177(15) 0.0209(6) Uani 1 1 d . . .
C3 C 0.37335(13) 0.6978(3) 0.25747(16) 0.0279(7) Uani 1 1 d . . .
H3 H 0.3434 0.6987 0.2924 0.033 Uiso 1 1 calc R . .
C4 C 0.39591(14) 0.8151(3) 0.23306(17) 0.0328(7) Uani 1 1 d . . .
H4 H 0.3820 0.8963 0.2513 0.039 Uiso 1 1 calc R . .
C5 C 0.43908(14) 0.8130(3) 0.18161(17) 0.0313(7) Uani 1 1 d . . .
H5 H 0.4544 0.8934 0.1639 0.038 Uiso 1 1 calc R . .
C6 C 0.45997(13) 0.6956(3) 0.15593(15) 0.0264(6) Uani 1 1 d . . .
H6 H 0.4900 0.6959 0.1210 0.032 Uiso 1 1 calc R . .
C7 C 0.28954(12) 0.2845(3) 0.14763(15) 0.0230(6) Uani 1 1 d . . .
C8 C 0.29335(11) 0.3970(3) 0.19264(15) 0.0213(6) Uani 1 1 d . . .
C9 C 0.24545(13) 0.4897(3) 0.18588(15) 0.0283(7) Uani 1 1 d . . .
H9 H 0.2484 0.5657 0.2162 0.034 Uiso 1 1 calc R . .
C10 C 0.19376(14) 0.4725(3) 0.13566(18) 0.0369(8) Uani 1 1 d . . .
H10 H 0.1610 0.5358 0.1315 0.044 Uiso 1 1 calc R . .
C11 C 0.19028(14) 0.3618(3) 0.09138(17) 0.0370(8) Uani 1 1 d . . .
H11 H 0.1549 0.3494 0.0565 0.044 Uiso 1 1 calc R . .
C12 C 0.23731(13) 0.2696(3) 0.09713(16) 0.0314(7) Uani 1 1 d . . .
H12 H 0.2340 0.1945 0.0661 0.038 Uiso 1 1 calc R . .
C13 C 0.33519(13) 0.4340(3) 0.34723(15) 0.0240(6) Uani 1 1 d . . .
C14 C 0.37388(14) 0.4886(3) 0.40519(16) 0.0336(7) Uani 1 1 d . . .
H14 H 0.4128 0.5267 0.3962 0.040 Uiso 1 1 calc R . .
C15 C 0.35571(17) 0.4875(4) 0.47550(18) 0.0422(8) Uani 1 1 d . . .
H15 H 0.3825 0.5241 0.5148 0.051 Uiso 1 1 calc R . .
C16 C 0.29929(17) 0.4339(3) 0.48909(18) 0.0443(9) Uani 1 1 d . . .
H16 H 0.2870 0.4338 0.5376 0.053 Uiso 1 1 calc R . .
C17 C 0.26063(16) 0.3803(3) 0.43224(18) 0.0387(8) Uani 1 1 d . . .
H17 H 0.2215 0.3433 0.4415 0.046 Uiso 1 1 calc R . .
C18 C 0.27848(14) 0.3800(3) 0.36172(16) 0.0295(7) Uani 1 1 d . . .
H18 H 0.2516 0.3425 0.3228 0.035 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ga Ga 0.2307 1.6083 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
Ga1 S1 Ga1 98.24(4) 2_655 . ?
C21 C20 C22 124.4(5) . 5_655 ?
C20 C21 C22 125.8(5) . . ?
C21 C22 C20 109.8(6) . 5_655 ?
S1 Ga1 S3 109.23(3) . . ?
S1 Ga1 S2 112.10(3) . . ?
S3 Ga1 S2 116.59(3) . . ?
S1 Ga1 P1 137.22(2) . . ?
S3 Ga1 P1 91.86(3) . . ?
S2 Ga1 P1 88.78(3) . . ?
C2 P1 C13 110.39(13) . . ?
C2 P1 C8 105.74(12) . . ?
C13 P1 C8 107.11(12) . . ?
C2 P1 Ga1 103.20(9) . . ?
C13 P1 Ga1 130.09(9) . . ?
C8 P1 Ga1 97.65(9) . . ?
C1 S2 Ga1 103.53(9) . . ?
C7 S3 Ga1 99.06(9) . . ?
C6 C1 C2 118.4(2) . . ?
C6 C1 S2 116.7(2) . . ?
C2 C1 S2 124.9(2) . . ?
C3 C2 C1 119.8(3) . . ?
C3 C2 P1 122.5(2) . . ?
C1 C2 P1 117.6(2) . . ?
C4 C3 C2 121.0(3) . . ?
C3 C4 C5 119.2(3) . . ?
C6 C5 C4 120.5(3) . . ?
C5 C6 C1 121.2(3) . . ?
C12 C7 C8 118.3(3) . . ?
C12 C7 S3 116.8(2) . . ?
C8 C7 S3 124.9(2) . . ?
C9 C8 C7 120.0(3) . . ?
C9 C8 P1 120.1(2) . . ?
C7 C8 P1 119.9(2) . . ?
C10 C9 C8 120.8(3) . . ?
C9 C10 C11 119.0(3) . . ?
C12 C11 C10 120.9(3) . . ?
C11 C12 C7 121.0(3) . . ?
C18 C13 C14 118.7(3) . . ?
C18 C13 P1 121.1(2) . . ?
C14 C13 P1 120.0(2) . . ?
C15 C14 C13 120.1(3) . . ?
C16 C15 C14 120.5(3) . . ?
C15 C16 C17 119.8(3) . . ?
C16 C17 C18 120.2(3) . . ?
C17 C18 C13 120.6(3) . . ?
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
S1 Ga1 2.1876(7) 2_655 ?
S1 Ga1 2.1876(7) . ?
C20 C21 1.382(8) . ?
C20 C22 1.444(8) 5_655 ?
C21 C22 1.436(7) . ?
C22 C20 1.444(8) 5_655 ?
Ga1 S3 2.2513(8) . ?
Ga1 S2 2.2757(8) . ?
Ga1 P1 2.3688(7) . ?
P1 C2 1.795(3) . ?
P1 C13 1.801(3) . ?
P1 C8 1.807(3) . ?
S2 C1 1.766(3) . ?
S3 C7 1.765(3) . ?
C1 C6 1.388(4) . ?
C1 C2 1.404(4) . ?
C2 C3 1.391(4) . ?
C3 C4 1.377(4) . ?
C4 C5 1.385(4) . ?
C5 C6 1.375(4) . ?
C7 C12 1.387(4) . ?
C7 C8 1.407(4) . ?
C8 C9 1.391(4) . ?
C9 C10 1.379(4) . ?
C10 C11 1.385(5) . ?
C11 C12 1.374(4) . ?
C13 C18 1.384(4) . ?
C13 C14 1.395(4) . ?
C14 C15 1.380(4) . ?
C15 C16 1.373(5) . ?
C16 C17 1.376(5) . ?
C17 C18 1.381(4) . ?
