#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:06:34 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178549 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/56/4065604.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_4065604
loop_
_publ_author_name
'Leung, Wing-Por'
'Wan, Chi-Ling'
'Mak, Thomas C. W.'
_publ_section_title
;
 Synthesis and Structure of Magnesium and Group 13 Metal
 Bis(thiophosphinoyl)methanediide Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1622
_journal_paper_doi               10.1021/om100019c
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C50 H40 Cl2 Ga2 P4 S4'
_chemical_formula_weight         1103.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 106.293(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.557(8)
_cell_length_b                   19.892(14)
_cell_length_c                   12.418(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2740(3)
_computing_cell_refinement       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_collection       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_reduction        'BRUKER SMART CCD DIFFRACTOMETER'
_computing_molecular_graphics    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKER SMART CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.0963
_diffrn_reflns_av_sigmaI/netI    0.1130
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14297
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5666
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0524
_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)+(0.0555P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1235
_reflns_number_gt                3021
_reflns_number_total             4819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100019c_si_001.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4065604
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ga1 Ga 0.58128(5) 0.99235(2) 0.88936(4) 0.02340(17) Uani 1 1 d .
Cl1 Cl 0.67452(12) 0.99412(6) 0.75563(11) 0.0395(3) Uani 1 1 d .
P1 P 0.37746(11) 1.09916(6) 0.87542(10) 0.0240(3) Uani 1 1 d .
P2 P 0.39005(11) 0.88142(6) 0.95502(10) 0.0226(3) Uani 1 1 d .
S1 S 0.27418(11) 1.05965(6) 0.97031(11) 0.0313(3) Uani 1 1 d .
S2 S 0.43488(12) 0.91350(6) 0.81492(10) 0.0306(3) Uani 1 1 d .
C1 C 0.5287(4) 1.0828(2) 0.9207(4) 0.0220(10) Uani 1 1 d .
C11 C 0.3179(4) 1.0676(2) 0.7355(4) 0.0288(12) Uani 1 1 d .
C12 C 0.2011(5) 1.0441(3) 0.7001(5) 0.0548(17) Uani 1 1 d .
H12A H 0.1523 1.0449 0.7482 0.066 Uiso 1 1 calc R
C13 C 0.1581(6) 1.0196(4) 0.5937(6) 0.085(2) Uani 1 1 d .
H13A H 0.0791 1.0041 0.5700 0.102 Uiso 1 1 calc R
C14 C 0.2272(7) 1.0173(3) 0.5208(5) 0.071(2) Uani 1 1 d .
H14A H 0.1956 1.0005 0.4486 0.086 Uiso 1 1 calc R
C15 C 0.3415(6) 1.0395(3) 0.5547(4) 0.0498(16) Uani 1 1 d .
H15A H 0.3895 1.0377 0.5059 0.060 Uiso 1 1 calc R
C16 C 0.3878(5) 1.0649(2) 0.6607(4) 0.0349(13) Uani 1 1 d .
H16A H 0.4668 1.0804 0.6830 0.042 Uiso 1 1 calc R
C21 C 0.3382(4) 1.1876(2) 0.8646(4) 0.0249(11) Uani 1 1 d .
C22 C 0.3519(5) 1.2239(2) 0.7733(5) 0.0434(15) Uani 1 1 d .
H22A H 0.3786 1.2026 0.7180 0.052 Uiso 1 1 calc R
C23 C 0.3256(5) 1.2920(3) 0.7654(5) 0.0487(16) Uani 1 1 d .
H23A H 0.3334 1.3163 0.7039 0.058 Uiso 1 1 calc R
C24 C 0.2883(5) 1.3234(3) 0.8468(5) 0.0478(16) Uani 1 1 d .
H24A H 0.2734 1.3694 0.8421 0.057 Uiso 1 1 calc R
C25 C 0.2725(6) 1.2880(3) 0.9352(5) 0.0534(17) Uani 1 1 d .
H25A H 0.2447 1.3094 0.9897 0.064 Uiso 1 1 calc R
C26 C 0.2985(5) 1.2193(2) 0.9437(5) 0.0440(15) Uani 1 1 d .
H26A H 0.2884 1.1951 1.0045 0.053 Uiso 1 1 calc R
C31 C 0.2306(4) 0.8957(2) 0.9303(4) 0.0274(11) Uani 1 1 d .
C32 C 0.1801(5) 0.8980(2) 1.0199(5) 0.0387(13) Uani 1 1 d .
H32A H 0.2288 0.8936 1.0932 0.046 Uiso 1 1 calc R
C33 C 0.0578(6) 0.9067(3) 0.9991(6) 0.0593(18) Uani 1 1 d .
H33A H 0.0246 0.9093 1.0590 0.071 Uiso 1 1 calc R
C34 C -0.0153(6) 0.9118(3) 0.8929(7) 0.068(2) Uani 1 1 d .
H34A H -0.0976 0.9187 0.8797 0.082 Uiso 1 1 calc R
C35 C 0.0341(6) 0.9067(3) 0.8063(6) 0.067(2) Uani 1 1 d .
H35A H -0.0162 0.9082 0.7333 0.080 Uiso 1 1 calc R
C36 C 0.1573(5) 0.8992(3) 0.8231(5) 0.0468(15) Uani 1 1 d .
H36A H 0.1893 0.8967 0.7624 0.056 Uiso 1 1 calc R
C41 C 0.3942(4) 0.7898(2) 0.9510(4) 0.0274(12) Uani 1 1 d .
C42 C 0.3948(5) 0.7566(2) 0.8552(4) 0.0384(14) Uani 1 1 d .
H42A H 0.4039 0.7805 0.7938 0.046 Uiso 1 1 calc R
C43 C 0.3821(6) 0.6882(2) 0.8489(5) 0.0500(16) Uani 1 1 d .
H43A H 0.3805 0.6659 0.7827 0.060 Uiso 1 1 calc R
C44 C 0.3719(5) 0.6529(3) 0.9396(5) 0.0449(15) Uani 1 1 d .
H44A H 0.3665 0.6063 0.9363 0.054 Uiso 1 1 calc R
C45 C 0.3697(6) 0.6857(3) 1.0349(5) 0.0524(17) Uani 1 1 d .
H45A H 0.3604 0.6618 1.0963 0.063 Uiso 1 1 calc R
C46 C 0.3812(5) 0.7542(2) 1.0398(4) 0.0384(14) Uani 1 1 d .
H46A H 0.3802 0.7766 1.1052 0.046 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
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'
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'
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
C1 Ga1 Cl1 111.98(14) . .
C1 Ga1 S1 117.42(13) . 3_677
Cl1 Ga1 S1 99.94(7) . 3_677
C1 Ga1 S2 117.92(14) . .
Cl1 Ga1 S2 99.60(6) . .
S1 Ga1 S2 107.12(6) 3_677 .
C1 P1 C11 109.3(2) . .
C1 P1 C21 114.9(2) . .
C11 P1 C21 104.3(2) . .
C1 P1 S1 116.33(17) . .
C11 P1 S1 107.15(19) . .
C21 P1 S1 103.92(18) . .
C1 P2 C31 111.2(2) 3_677 .
C1 P2 C41 115.2(2) 3_677 .
C31 P2 C41 100.7(2) . .
C1 P2 S2 115.36(17) 3_677 .
C31 P2 S2 107.20(17) . .
C41 P2 S2 105.81(18) . .
P1 S1 Ga1 101.05(8) . 3_677
P2 S2 Ga1 101.73(7) . .
P1 C1 P2 117.8(3) . 3_677
P1 C1 Ga1 116.9(2) . .
P2 C1 Ga1 115.7(2) 3_677 .
C12 C11 C16 118.3(5) . .
C12 C11 P1 120.2(4) . .
C16 C11 P1 121.5(4) . .
C13 C12 C11 119.2(6) . .
C12 C13 C14 122.2(7) . .
C15 C14 C13 119.2(6) . .
C14 C15 C16 120.4(6) . .
C15 C16 C11 120.8(5) . .
C26 C21 C22 119.4(4) . .
C26 C21 P1 121.8(4) . .
C22 C21 P1 118.8(4) . .
C23 C22 C21 119.5(5) . .
C24 C23 C22 120.4(6) . .
C23 C24 C25 120.4(5) . .
C24 C25 C26 119.5(6) . .
C21 C26 C25 120.7(5) . .
C36 C31 C32 119.5(5) . .
C36 C31 P2 120.0(4) . .
C32 C31 P2 120.3(4) . .
C33 C32 C31 119.5(5) . .
C34 C33 C32 121.3(6) . .
C33 C34 C35 118.7(6) . .
C34 C35 C36 122.1(6) . .
C31 C36 C35 118.8(6) . .
C46 C41 C42 119.1(4) . .
C46 C41 P2 119.4(4) . .
C42 C41 P2 121.0(4) . .
C41 C42 C43 120.3(5) . .
C44 C43 C42 119.9(5) . .
C45 C44 C43 120.1(5) . .
C44 C45 C46 119.3(5) . .
C41 C46 C45 121.1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga1 C1 1.972(4) .
Ga1 Cl1 2.2192(18) .
Ga1 S1 2.2944(16) 3_677
Ga1 S2 2.3023(16) .
P1 C1 1.710(5) .
P1 C11 1.794(5) .
P1 C21 1.813(4) .
P1 S1 2.054(2) .
P2 C1 1.720(5) 3_677
P2 C31 1.804(5) .
P2 C41 1.825(5) .
P2 S2 2.051(2) .
S1 Ga1 2.2943(16) 3_677
C1 P2 1.720(5) 3_677
C11 C12 1.378(7) .
C11 C16 1.392(7) .
C12 C13 1.365(8) .
C13 C14 1.366(10) .
C14 C15 1.344(9) .
C15 C16 1.371(7) .
C21 C26 1.351(7) .
C21 C22 1.389(7) .
C22 C23 1.386(7) .
C23 C24 1.357(8) .
C24 C25 1.358(8) .
C25 C26 1.398(7) .
C31 C36 1.364(7) .
C31 C32 1.395(7) .
C32 C33 1.375(8) .
C33 C34 1.355(8) .
C34 C35 1.355(9) .
C35 C36 1.388(8) .
C41 C46 1.354(7) .
C41 C42 1.362(6) .
C42 C43 1.368(7) .
C43 C44 1.359(7) .
C44 C45 1.358(7) .
C45 C46 1.368(7) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.039 0.250 -0.024 300.0 80.2
2 0.039 0.750 -0.001 300.1 77.9
