#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:06:34 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178549 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/56/4065602.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_4065602
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            'C66 H72 Mg2 O4 P4 S4'
_chemical_formula_weight         1229.98
_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                 96.986(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.420(4)
_cell_length_b                   13.181(5)
_cell_length_c                   23.464(9)
_cell_measurement_reflns_used    1002
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.28
_cell_measurement_theta_min      2.33
_cell_volume                     3199(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0936
_diffrn_reflns_av_sigmaI/netI    0.1336
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21358
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8845
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7736
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1906
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0969P)²+1.6247P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.2355
_reflns_number_gt                3215
_reflns_number_total             7736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100019c_si_001.cif
_cod_data_source_block           2
_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               4065602
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
Mg1 Mg 0.15503(15) 0.55022(11) 0.02705(7) 0.0434(4) Uani 1 1 d .
P1 P 0.01467(12) 0.35445(9) 0.08712(5) 0.0402(3) Uani 1 1 d .
P2 P 0.10575(12) 0.31195(9) -0.02415(5) 0.0419(3) Uani 1 1 d .
S1 S 0.11226(14) 0.47867(10) 0.11947(5) 0.0567(4) Uani 1 1 d .
S2 S 0.24981(13) 0.41577(10) -0.02725(6) 0.0569(4) Uani 1 1 d .
O1 O 0.3299(3) 0.6141(3) 0.05854(17) 0.0651(10) Uani 1 1 d D
C2 C 0.4254(6) 0.5613(5) 0.0958(4) 0.107(3) Uani 1 1 d D
H2A H 0.4843 0.5255 0.0738 0.128 Uiso 1 1 calc R
H2B H 0.3852 0.5126 0.1191 0.128 Uiso 1 1 calc R
C3 C 0.4940(8) 0.6392(7) 0.1319(3) 0.112(3) Uani 1 1 d D
H3A H 0.5847 0.6219 0.1409 0.134 Uiso 1 1 calc R
H3B H 0.4564 0.6473 0.1674 0.134 Uiso 1 1 calc R
C4 C 0.4786(8) 0.7323(6) 0.0973(4) 0.117(3) Uani 1 1 d D
H4A H 0.4403 0.7858 0.1180 0.141 Uiso 1 1 calc R
H4B H 0.5615 0.7555 0.0875 0.141 Uiso 1 1 calc R
C5 C 0.3927(7) 0.7040(5) 0.0455(3) 0.091(2) Uani 1 1 d D
H5A H 0.3301 0.7573 0.0350 0.109 Uiso 1 1 calc R
H5B H 0.4423 0.6929 0.0136 0.109 Uiso 1 1 calc R
O2 O 0.5852(13) -0.0305(17) 0.2296(6) 0.338(10) Uani 1 1 d D
C6 C 0.5829(19) -0.0359(15) 0.1697(8) 0.363(17) Uani 1 1 d D
H6A H 0.5747 0.0295 0.1506 0.435 Uiso 1 1 calc R
H6B H 0.5211 -0.0843 0.1513 0.435 Uiso 1 1 calc R
C7 C 0.713(2) -0.0732(17) 0.1794(13) 0.373(17) Uani 1 1 d D
H7A H 0.7221 -0.1282 0.2070 0.447 Uiso 1 1 calc R
H7B H 0.7449 -0.0940 0.1441 0.447 Uiso 1 1 calc R
C8 C 0.7690(14) 0.0165(18) 0.2014(9) 0.264(9) Uani 1 1 d D
H8A H 0.7935 0.0604 0.1714 0.317 Uiso 1 1 calc R
H8B H 0.8436 0.0038 0.2295 0.317 Uiso 1 1 calc R
C9 C 0.661(2) 0.0574(9) 0.2277(7) 0.261(10) Uani 1 1 d D
H9A H 0.6885 0.0839 0.2658 0.313 Uiso 1 1 calc R
H9B H 0.6162 0.1099 0.2042 0.313 Uiso 1 1 calc R
C1 C -0.0170(4) 0.3430(3) 0.01427(19) 0.0420(11) Uani 1 1 d .
C11 C -0.1401(5) 0.3557(4) 0.1161(2) 0.0476(12) Uani 1 1 d .
C12 C -0.2382(6) 0.2931(5) 0.0943(3) 0.0723(17) Uani 1 1 d .
H12A H -0.2264 0.2501 0.0639 0.087 Uiso 1 1 calc R
C13 C -0.3560(7) 0.2928(6) 0.1167(4) 0.098(2) Uani 1 1 d .
H13A H -0.4217 0.2493 0.1016 0.118 Uiso 1 1 calc R
C14 C -0.3751(8) 0.3557(7) 0.1607(3) 0.096(2) Uani 1 1 d .
H14A H -0.4543 0.3567 0.1752 0.115 Uiso 1 1 calc R
C15 C -0.2792(8) 0.4160(6) 0.1828(3) 0.088(2) Uani 1 1 d .
H15A H -0.2921 0.4583 0.2133 0.106 Uiso 1 1 calc R
C16 C -0.1612(6) 0.4174(4) 0.1617(2) 0.0654(15) Uani 1 1 d .
H16A H -0.0957 0.4599 0.1782 0.078 Uiso 1 1 calc R
C21 C 0.0979(5) 0.2453(4) 0.1234(2) 0.0515(13) Uani 1 1 d .
C22 C 0.0427(7) 0.1520(5) 0.1206(3) 0.097(2) Uani 1 1 d .
H22A H -0.0405 0.1445 0.1016 0.117 Uiso 1 1 calc R
C23 C 0.1061(10) 0.0674(5) 0.1452(4) 0.118(3) Uani 1 1 d .
H23A H 0.0661 0.0043 0.1421 0.141 Uiso 1 1 calc R
C24 C 0.2243(10) 0.0767(7) 0.1733(3) 0.109(3) Uani 1 1 d .
H24A H 0.2673 0.0203 0.1900 0.131 Uiso 1 1 calc R
C25 C 0.2811(9) 0.1686(8) 0.1773(4) 0.134(3) Uani 1 1 d .
H25A H 0.3643 0.1754 0.1963 0.161 Uiso 1 1 calc R
C26 C 0.2163(7) 0.2535(5) 0.1533(3) 0.093(2) Uani 1 1 d .
H26A H 0.2552 0.3169 0.1580 0.111 Uiso 1 1 calc R
C31 C 0.0355(5) 0.2860(4) -0.0978(2) 0.0520(13) Uani 1 1 d .
C32 C -0.0831(6) 0.2420(4) -0.1093(2) 0.0645(15) Uani 1 1 d .
H32A H -0.1293 0.2253 -0.0791 0.077 Uiso 1 1 calc R
C33 C -0.1367(8) 0.2214(5) -0.1656(3) 0.095(2) Uani 1 1 d .
H33A H -0.2181 0.1920 -0.1731 0.114 Uiso 1 1 calc R
C34 C -0.0660(10) 0.2457(6) -0.2099(3) 0.107(3) Uani 1 1 d .
H34A H -0.1002 0.2321 -0.2476 0.129 Uiso 1 1 calc R
C35 C 0.0506(10) 0.2883(6) -0.1994(3) 0.105(3) Uani 1 1 d .
H35A H 0.0962 0.3049 -0.2297 0.126 Uiso 1 1 calc R
C36 C 0.1044(7) 0.3082(5) -0.1432(3) 0.0778(18) Uani 1 1 d .
H36A H 0.1866 0.3363 -0.1361 0.093 Uiso 1 1 calc R
C41 C 0.1907(5) 0.1918(3) -0.0051(2) 0.0462(12) Uani 1 1 d .
C42 C 0.3107(6) 0.1886(4) 0.0236(3) 0.0792(19) Uani 1 1 d .
H42A H 0.3523 0.2489 0.0350 0.095 Uiso 1 1 calc R
C43 C 0.3729(7) 0.0978(5) 0.0363(4) 0.102(3) Uani 1 1 d .
H43A H 0.4564 0.0983 0.0555 0.122 Uiso 1 1 calc R
C44 C 0.3168(7) 0.0097(5) 0.0219(3) 0.088(2) Uani 1 1 d .
H44A H 0.3607 -0.0509 0.0303 0.106 Uiso 1 1 calc R
C45 C 0.1964(9) 0.0095(5) -0.0049(4) 0.123(3) Uani 1 1 d .
H45A H 0.1541 -0.0516 -0.0139 0.148 Uiso 1 1 calc R
C46 C 0.1344(7) 0.1004(4) -0.0192(4) 0.113(3) Uani 1 1 d .
H46A H 0.0516 0.0991 -0.0391 0.136 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'
Mg Mg 0.0486 0.0363 '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'
O O 0.0106 0.0060 '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
O1 Mg1 C1 114.00(17) . 3_565
O1 Mg1 S1 95.04(13) . .
C1 Mg1 S1 117.71(14) 3_565 .
O1 Mg1 S2 95.00(13) . .
C1 Mg1 S2 121.69(14) 3_565 .
S1 Mg1 S2 107.96(8) . .
O1 Mg1 Mg1 177.51(13) . 3_565
C1 Mg1 Mg1 63.75(13) 3_565 3_565
S1 Mg1 Mg1 85.30(7) . 3_565
S2 Mg1 Mg1 87.23(7) . 3_565
C1 P1 C11 107.6(2) . .
C1 P1 C21 114.7(2) . .
C11 P1 C21 102.9(2) . .
C1 P1 S1 118.26(16) . .
C11 P1 S1 106.21(17) . .
C21 P1 S1 105.81(19) . .
C1 P2 C31 107.8(2) . .
C1 P2 C41 116.7(2) . .
C31 P2 C41 101.2(2) . .
C1 P2 S2 117.47(17) . .
C31 P2 S2 107.72(19) . .
C41 P2 S2 104.55(17) . .
P1 S1 Mg1 96.68(7) . .
P2 S2 Mg1 96.97(7) . .
C5 O1 C2 103.7(4) . .
C5 O1 Mg1 133.0(4) . .
C2 O1 Mg1 122.8(3) . .
O1 C2 C3 105.5(6) . .
C2 C3 C4 104.7(6) . .
C5 C4 C3 105.1(6) . .
O1 C5 C4 106.7(6) . .
C6 O2 C9 87.2(12) . .
O2 C6 C7 87.6(14) . .
C8 C7 C6 96.6(14) . .
C7 C8 C9 99.2(12) . .
O2 C9 C8 100.1(12) . .
P2 C1 P1 119.0(3) . .
P2 C1 Mg1 115.0(2) . 3_565
P1 C1 Mg1 115.4(2) . 3_565
C12 C11 C16 117.6(5) . .
C12 C11 P1 120.7(4) . .
C16 C11 P1 121.6(4) . .
C11 C12 C13 121.0(6) . .
C14 C13 C12 120.2(7) . .
C15 C14 C13 119.3(7) . .
C14 C15 C16 121.8(7) . .
C15 C16 C11 120.2(6) . .
C26 C21 C22 116.9(6) . .
C26 C21 P1 122.0(5) . .
C22 C21 P1 121.0(5) . .
C21 C22 C23 122.1(7) . .
C24 C23 C22 119.9(8) . .
C23 C24 C25 119.4(8) . .
C24 C25 C26 120.5(9) . .
C21 C26 C25 121.0(8) . .
C32 C31 C36 118.6(5) . .
C32 C31 P2 121.2(4) . .
C36 C31 P2 120.2(5) . .
C31 C32 C33 121.2(6) . .
C34 C33 C32 118.6(7) . .
C35 C34 C33 121.0(7) . .
C34 C35 C36 120.4(8) . .
C31 C36 C35 120.1(7) . .
C42 C41 C46 116.1(5) . .
C42 C41 P2 122.5(4) . .
C46 C41 P2 121.4(4) . .
C41 C42 C43 121.3(6) . .
C44 C43 C42 121.7(7) . .
C43 C44 C45 118.8(6) . .
C44 C45 C46 119.9(7) . .
C41 C46 C45 122.2(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 O1 2.061(4) .
Mg1 C1 2.156(5) 3_565
Mg1 S1 2.455(2) .
Mg1 S2 2.459(2) .
Mg1 Mg1 3.579(3) 3_565
P1 C1 1.708(5) .
P1 C11 1.825(5) .
P1 C21 1.835(5) .
P1 S1 2.0258(19) .
P2 C1 1.702(5) .
P2 C31 1.824(5) .
P2 C41 1.842(5) .
P2 S2 2.0391(19) .
O1 C5 1.405(6) .
O1 C2 1.424(7) .
C2 C3 1.462(9) .
C3 C4 1.468(10) .
C4 C5 1.467(9) .
O2 C6 1.405(16) .
O2 C9 1.407(14) .
C6 C7 1.430(16) .
C7 C8 1.392(15) .
C8 C9 1.449(14) .
C1 Mg1 2.156(5) 3_565
C11 C12 1.364(7) .
C11 C16 1.382(7) .
C12 C13 1.394(8) .
C13 C14 1.356(10) .
C14 C15 1.332(10) .
C15 C16 1.381(8) .
C21 C26 1.348(8) .
C21 C22 1.357(8) .
C22 C23 1.385(9) .
C23 C24 1.329(11) .
C24 C25 1.347(12) .
C25 C26 1.389(10) .
C31 C32 1.363(7) .
C31 C36 1.386(7) .
C32 C33 1.397(8) .
C33 C34 1.382(10) .
C34 C35 1.334(11) .
C35 C36 1.393(9) .
C41 C42 1.346(7) .
C41 C46 1.364(8) .
C42 C43 1.377(8) .
C43 C44 1.325(9) .
C44 C45 1.334(9) .
C45 C46 1.382(9) .
