#------------------------------------------------------------------------------
#$Date: 2016-03-21 13:02:18 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178690 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/01/4080122.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_4080122
loop_
_publ_author_name
'Murugesapandian, Balasubramanian'
'Kuzdrowska, Magdalena'
'Gamer, Michael T.'
'Hartenstein, Larissa'
'Roesky, Peter W.'
_publ_section_title
;
 (Iminophosphoranyl)(thiophosphoranyl)methanide
 {CH(PPh2NSiMe3)(Ph2PS)}−as a Ligand in Rare-Earth-Element
 Chemistry
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1500
_journal_page_last               1506
_journal_paper_doi               10.1021/om400001e
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C32 H38 Cl2 Dy N O P2 S Si'
_chemical_formula_sum            'C32 H38 Cl2 Dy N O P2 S Si'
_chemical_formula_weight         808.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 111.6129(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.77838(24)
_cell_length_b                   33.7778(11)
_cell_length_c                   11.5709(3)
_cell_measurement_reflns_used    28701
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      1.89
_cell_volume                     3553.08(18)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20068
_diffrn_reflns_theta_full        25.54
_diffrn_reflns_theta_max         25.54
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    2.461
_exptl_absorpt_correction_T_max  0.9649
_exptl_absorpt_correction_T_min  0.7925
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.776
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6610
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0428P)²+0.9182P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                5892
_reflns_number_total             6610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400001e_si_001.cif
_cod_data_source_block           2a
_cod_original_cell_volume        3553.07(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4080122
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy Dy 0.719476(13) 0.160495(4) 0.852723(12) 0.03462(6) Uani 1 1 d . . .
Cl2 Cl 0.80279(13) 0.16987(3) 1.08692(9) 0.0678(3) Uani 1 1 d . . .
Cl1 Cl 0.95924(9) 0.15057(3) 0.81510(10) 0.0635(2) Uani 1 1 d . . .
S S 0.54894(8) 0.16358(2) 0.59347(7) 0.04287(18) Uani 1 1 d . . .
P2 P 0.48345(7) 0.10035(2) 0.85104(6) 0.03045(15) Uani 1 1 d . . .
P1 P 0.37981(8) 0.16646(2) 0.65208(7) 0.03330(16) Uani 1 1 d . . .
Si Si 0.75547(8) 0.05189(2) 0.87991(8) 0.03919(18) Uani 1 1 d . . .
O O 0.7141(3) 0.23005(7) 0.8445(2) 0.0547(6) Uani 1 1 d . B .
N N 0.6507(2) 0.09475(7) 0.8623(2) 0.0330(5) Uani 1 1 d . . .
C2 C 0.3163(3) 0.21704(9) 0.6534(3) 0.0401(6) Uani 1 1 d . . .
C11 C -0.0264(4) 0.10534(13) 0.3739(3) 0.0615(10) Uani 1 1 d . . .
H11 H -0.1106 0.0926 0.3164 0.074 Uiso 1 1 calc R . .
C12 C 0.0804(4) 0.11976(13) 0.3343(3) 0.0595(10) Uani 1 1 d . . .
H12 H 0.0685 0.1174 0.2493 0.071 Uiso 1 1 calc R . .
C10 C -0.0127(3) 0.10915(12) 0.4953(3) 0.0531(8) Uani 1 1 d . . .
H10 H -0.0876 0.0994 0.5217 0.064 Uiso 1 1 calc R . .
C8 C 0.2204(3) 0.14147(9) 0.5412(3) 0.0356(6) Uani 1 1 d . . .
C9 C 0.1110(3) 0.12738(10) 0.5801(3) 0.0418(7) Uani 1 1 d . . .
H9 H 0.1208 0.1302 0.6644 0.050 Uiso 1 1 calc R . .
C13 C 0.2054(3) 0.13770(11) 0.4178(3) 0.0467(7) Uani 1 1 d . . .
H13 H 0.2799 0.1473 0.3908 0.056 Uiso 1 1 calc R . .
C32 C 0.6649(5) 0.25840(12) 0.9152(5) 0.0695(11) Uani 1 1 d . . .
H32C H 0.7029 0.2517 1.0048 0.083 Uiso 0.40 1 calc PR A 2
H32D H 0.5562 0.2599 0.8843 0.083 Uiso 0.40 1 calc PR A 2
H32A H 0.6545 0.2455 0.9883 0.083 Uiso 0.60 1 calc PR A 1
H32B H 0.5689 0.2699 0.8630 0.083 Uiso 0.60 1 calc PR A 1
C6 C 0.3022(7) 0.28442(14) 0.5864(5) 0.0952(18) Uani 1 1 d . . .
H6 H 0.3321 0.3047 0.5440 0.114 Uiso 1 1 calc R . .
C1 C 0.4339(3) 0.14944(9) 0.8050(3) 0.0330(6) Uani 1 1 d . . .
H1 H 0.3934 0.1647 0.8593 0.040 Uiso 1 1 calc R . .
C26 C 0.6611(4) 0.00721(11) 0.9085(4) 0.0629(10) Uani 1 1 d . . .
H26A H 0.6297 0.0122 0.9784 0.094 Uiso 1 1 calc R . .
H26B H 0.7291 -0.0153 0.9283 0.094 Uiso 1 1 calc R . .
H26C H 0.5750 0.0012 0.8339 0.094 Uiso 1 1 calc R . .
C27 C 0.9306(3) 0.05896(12) 1.0158(4) 0.0597(10) Uani 1 1 d . . .
H27A H 0.9796 0.0831 1.0039 0.090 Uiso 1 1 calc R . .
H27B H 0.9951 0.0361 1.0230 0.090 Uiso 1 1 calc R . .
H27C H 0.9091 0.0614 1.0918 0.090 Uiso 1 1 calc R . .
C4 C 0.1635(5) 0.26416(12) 0.7058(4) 0.0664(10) Uani 1 1 d . . .
H4 H 0.0971 0.2703 0.7459 0.080 Uiso 1 1 calc R . .
C3 C 0.2190(4) 0.22586(10) 0.7122(4) 0.0524(8) Uani 1 1 d . . .
H3 H 0.1905 0.2059 0.7566 0.063 Uiso 1 1 calc R . .
C7 C 0.3579(6) 0.24650(12) 0.5914(4) 0.0716(12) Uani 1 1 d . . .
H7 H 0.4253 0.2408 0.5518 0.086 Uiso 1 1 calc R . .
C28 C 0.8001(5) 0.04356(14) 0.7389(4) 0.0695(11) Uani 1 1 d . . .
H28A H 0.7089 0.0424 0.6655 0.104 Uiso 1 1 calc R . .
H28B H 0.8537 0.0186 0.7473 0.104 Uiso 1 1 calc R . .
H28C H 0.8613 0.0654 0.7295 0.104 Uiso 1 1 calc R . .
C5 C 0.2039(6) 0.29271(13) 0.6425(5) 0.0782(13) Uani 1 1 d . . .
H5 H 0.1639 0.3186 0.6369 0.094 Uiso 1 1 calc R . .
C20 C 0.3684(3) 0.06305(8) 0.7463(3) 0.0357(6) Uani 1 1 d . . .
C25 C 0.2638(3) 0.04048(10) 0.7725(3) 0.0453(7) Uani 1 1 d . . .
H25 H 0.2477 0.0444 0.8478 0.054 Uiso 1 1 calc R . .
C29 C 0.8068(7) 0.25112(14) 0.7949(5) 0.0925(17) Uani 1 1 d U . .
H29A H 0.7478 0.2630 0.7135 0.111 Uiso 1 1 calc R B .
H29B H 0.8809 0.2332 0.7837 0.111 Uiso 1 1 calc R . .
C19 C 0.3232(3) 0.10564(9) 1.0077(3) 0.0401(6) Uani 1 1 d . . .
H19 H 0.2417 0.1130 0.9356 0.048 Uiso 1 1 calc R . .
C17 C 0.4260(4) 0.09406(12) 1.2274(3) 0.0534(8) Uani 1 1 d . . .
H17 H 0.4155 0.0936 1.3059 0.064 Uiso 1 1 calc R . .
C31B C 0.732(2) 0.2972(5) 0.8913(19) 0.091(5) Uani 0.40 1 d PU B 2
H31A H 0.7475 0.3164 0.9596 0.109 Uiso 0.40 1 calc PR B 2
H31B H 0.6694 0.3094 0.8115 0.109 Uiso 0.40 1 calc PR B 2
C16 C 0.5586(4) 0.08459(13) 1.2186(3) 0.0565(9) Uani 1 1 d . . .
H16 H 0.6392 0.0771 1.2911 0.068 Uiso 1 1 calc R . .
C15 C 0.5760(3) 0.08585(10) 1.1052(3) 0.0440(7) Uani 1 1 d . . .
H15 H 0.6685 0.0796 1.1005 0.053 Uiso 1 1 calc R . .
C21 C 0.3877(3) 0.05720(10) 0.6341(3) 0.0433(7) Uani 1 1 d . . .
H21 H 0.4575 0.0727 0.6149 0.052 Uiso 1 1 calc R . .
C24 C 0.1830(4) 0.01208(11) 0.6872(4) 0.0585(9) Uani 1 1 d . . .
H24 H 0.1126 -0.0035 0.7053 0.070 Uiso 1 1 calc R . .
C14 C 0.4578(3) 0.09623(8) 0.9982(3) 0.0341(6) Uani 1 1 d . . .
C30 C 0.8793(5) 0.28243(15) 0.8868(4) 0.0722(11) Uani 1 1 d . B .
H30C H 0.9299 0.3025 0.8547 0.087 Uiso 0.40 1 calc PR C 2
H30D H 0.9468 0.2718 0.9673 0.087 Uiso 0.40 1 calc PR C 2
H30A H 0.9771 0.2734 0.9440 0.087 Uiso 0.60 1 calc PR C 1
H30B H 0.8925 0.3067 0.8441 0.087 Uiso 0.60 1 calc PR C 1
C23 C 0.2039(4) 0.00643(11) 0.5780(4) 0.0595(10) Uani 1 1 d . . .
H23 H 0.1479 -0.0131 0.5209 0.071 Uiso 1 1 calc R . .
C22 C 0.3056(4) 0.02883(11) 0.5499(3) 0.0555(9) Uani 1 1 d . . .
H22 H 0.3195 0.0249 0.4736 0.067 Uiso 1 1 calc R . .
C18 C 0.3087(4) 0.10425(10) 1.1220(3) 0.0481(8) Uani 1 1 d . . .
H18 H 0.2166 0.1104 1.1278 0.058 Uiso 1 1 calc R . .
C31A C 0.7831(13) 0.2905(4) 0.9562(10) 0.082(3) Uani 0.60 1 d P B 1
H31C H 0.7384 0.3171 0.9359 0.098 Uiso 0.60 1 calc PR B 1
H31D H 0.8392 0.2890 1.0469 0.098 Uiso 0.60 1 calc PR B 1
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'
Dy Dy -0.1892 4.4098 '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'
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'
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
N Dy O 161.78(8)
N Dy Cl2 93.03(6)
O Dy Cl2 84.97(6)
N Dy Cl1 100.44(6)
O Dy Cl1 97.61(6)
Cl2 Dy Cl1 104.08(4)
N Dy C1 65.08(8)
O Dy C1 97.20(9)
Cl2 Dy C1 97.93(7)
Cl1 Dy C1 154.39(7)
N Dy S 91.01(6)
O Dy S 85.70(6)
Cl2 Dy S 161.92(3)
Cl1 Dy S 92.48(3)
C1 Dy S 67.95(6)
N Dy P2 30.88(5)
O Dy P2 130.95(6)
Cl2 Dy P2 91.96(3)
Cl1 Dy P2 130.24(3)
C1 Dy P2 34.73(6)
S Dy P2 82.55(2)
N Dy P1 81.84(5)
O Dy P1 84.73(6)
Cl2 Dy P1 126.07(3)
Cl1 Dy P1 129.73(3)
C1 Dy P1 32.06(6)
S Dy P1 37.38(2)
P2 Dy P1 58.247(18)
P1 S Dy 83.20(3)
N P2 C1 107.18(13)
N P2 C14 113.84(13)
C1 P2 C14 103.83(13)
N P2 C20 109.51(13)
C1 P2 C20 114.71(13)
C14 P2 C20 107.83(14)
N P2 Dy 48.35(9)
C1 P2 Dy 59.95(9)
C14 P2 Dy 114.08(9)
C20 P2 Dy 137.80(10)
C1 P1 C2 106.10(14)
C1 P1 C8 114.97(14)
C2 P1 C8 103.58(13)
C1 P1 S 110.26(10)
C2 P1 S 112.02(11)
C8 P1 S 109.73(10)
C1 P1 Dy 54.10(9)
C2 P1 Dy 108.13(10)
C8 P1 Dy 148.24(9)
S P1 Dy 59.42(3)
N Si C28 109.94(17)
N Si C26 112.74(14)
C28 Si C26 109.0(2)
N Si C27 108.07(14)
C28 Si C27 108.64(19)
C26 Si C27 108.38(19)
C29 O C32 106.8(3)
C29 O Dy 120.4(3)
C32 O Dy 130.1(2)
P2 N Si 130.23(15)
P2 N Dy 100.77(11)
Si N Dy 128.99(11)
C7 C2 C3 119.2(3)
C7 C2 P1 120.5(3)
C3 C2 P1 120.2(2)
C10 C11 C12 120.7(3)
C11 C12 C13 120.3(3)
C11 C10 C9 119.8(3)
C13 C8 C9 120.0(3)
C13 C8 P1 120.4(2)
C9 C8 P1 119.5(2)
C8 C9 C10 119.9(3)
C8 C13 C12 119.3(3)
O C32 C31A 105.9(6)
O C32 C31B 102.1(7)
C5 C6 C7 120.1(4)
P1 C1 P2 124.43(17)
P1 C1 Dy 93.84(11)
P2 C1 Dy 85.33(10)
C5 C4 C3 120.3(4)
C2 C3 C4 119.7(3)
C2 C7 C6 120.3(4)
C4 C5 C6 120.3(4)
C21 C20 C25 119.1(3)
C21 C20 P2 117.1(2)
C25 C20 P2 123.8(2)
C24 C25 C20 119.4(3)
O C29 C30 105.9(4)
C18 C19 C14 120.0(3)
C18 C17 C16 119.6(3)
C32 C31B C30 101.3(11)
C17 C16 C15 120.8(3)
C16 C15 C14 120.0(3)
C22 C21 C20 120.6(3)
C23 C24 C25 120.8(3)
C15 C14 C19 119.0(3)
C15 C14 P2 119.8(2)
C19 C14 P2 121.1(2)
C31A C30 C29 106.9(5)
C29 C30 C31B 92.8(7)
C24 C23 C22 120.5(3)
C23 C22 C21 119.5(4)
C17 C18 C19 120.7(3)
C30 C31A C32 105.2(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Dy N 2.335(2)
Dy O 2.351(2)
Dy Cl2 2.5457(9)
Dy Cl1 2.5594(8)
Dy C1 2.666(3)
Dy S 2.8469(8)
Dy P2 3.0694(7)
Dy P1 3.2835(7)
S P1 2.0076(11)
P2 N 1.604(2)
P2 C1 1.754(3)
P2 C14 1.815(3)
P2 C20 1.821(3)
P1 C1 1.747(3)
P1 C2 1.820(3)
P1 C8 1.821(3)
Si N 1.741(2)
Si C28 1.860(4)
Si C26 1.861(4)
Si C27 1.865(3)
O C29 1.429(5)
O C32 1.451(5)
C2 C7 1.374(5)
C2 C3 1.390(4)
C11 C10 1.367(5)
C11 C12 1.376(5)
C12 C13 1.388(5)
C10 C9 1.390(4)
C8 C13 1.387(4)
C8 C9 1.388(4)
C32 C31A 1.526(13)
C32 C31B 1.534(19)
C6 C5 1.373(7)
C6 C7 1.385(6)
C4 C5 1.354(6)
C4 C3 1.394(5)
C20 C21 1.393(4)
C20 C25 1.396(4)
C25 C24 1.394(5)
C29 C30 1.482(7)
C19 C18 1.382(5)
C19 C14 1.397(4)
C17 C18 1.376(5)
C17 C16 1.376(5)
C31B C30 1.54(2)
C16 C15 1.384(5)
C15 C14 1.392(4)
C21 C22 1.391(5)
C24 C23 1.366(6)
C30 C31A 1.470(13)
C23 C22 1.381(6)
