#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:38:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179120 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/82/4308259.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_4308259
loop_
_publ_author_name
'Nguyen Hung Huy'
'Ulrich Abram'
_publ_contact_author
;
      Ulrich Abram
      Free University of Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
Rhenium and Technetium Complexes with N,N-Dialkyl-N'-benzoylthioureas
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5310
_journal_page_last               5319
_journal_paper_doi               10.1021/ic070323x
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C30 H28 Cl2 N2 O3 P Re S'
_chemical_formula_sum            'C30 H28 Cl2 N2 O3 P Re S'
_chemical_formula_weight         784.47
_chemical_name_common            ReOCl2PPh3(PhCONCSMor)
_chemical_name_systematic
;
 TriphenylphosphineOxodichloro(N-benzoyl-N'-morpholinylthioreato-O,S)rhenium(V)
;
_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     'heavy tom'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 130.80(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.730(1)
_cell_length_b                   19.891(1)
_cell_length_c                   16.864(2)
_cell_measurement_reflns_used    28053
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      2.68
_cell_volume                     2978.6(6)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21879
_diffrn_reflns_theta_full        29.24
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        0.5
_exptl_absorpt_coefficient_mu    4.418
_exptl_absorpt_correction_T_max  0.6017
_exptl_absorpt_correction_T_min  0.2067
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.859
_refine_diff_density_min         -2.802
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0284
_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)+(0.0420P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                6862
_reflns_number_total             8007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070323x-file001_3.cif
_cod_data_source_block           ReOCl2PPh3(L-Mor)
_cod_original_cell_volume        2978.7(5)
_cod_database_code               4308259
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
Re1 Re 0.190304(11) -0.132052(5) 0.533771(9) 0.02042(4) Uani 1 1 d . . .
Cl2 Cl 0.03217(8) -0.17590(4) 0.35860(6) 0.02860(15) Uani 1 1 d . . .
Cl1 Cl 0.22679(9) -0.24456(3) 0.59419(7) 0.03283(16) Uani 1 1 d . . .
O10 O 0.0527(2) -0.10629(11) 0.53333(18) 0.0304(5) Uani 1 1 d . . .
S1 S 0.21123(9) -0.02733(3) 0.47351(6) 0.02801(15) Uani 1 1 d . . .
C2 C 0.2094(3) -0.05740(14) 0.3745(3) 0.0255(6) Uani 1 1 d . . .
N3 N 0.3203(3) -0.09688(13) 0.3974(2) 0.0271(5) Uani 1 1 d . . .
C4 C 0.3964(3) -0.13814(14) 0.4778(2) 0.0244(5) Uani 1 1 d . . .
O5 O 0.3598(2) -0.15669(10) 0.53185(17) 0.0244(4) Uani 1 1 d . . .
C31 C 0.5376(3) -0.16800(14) 0.5109(2) 0.0240(5) Uani 1 1 d . . .
C32 C 0.5943(3) -0.22581(15) 0.5717(3) 0.0294(6) Uani 1 1 d . . .
H32 H 0.5408 -0.2470 0.5877 0.035 Uiso 1 1 calc R . .
C33 C 0.7311(4) -0.25203(16) 0.6087(3) 0.0341(7) Uani 1 1 d . . .
H33 H 0.7674 -0.2918 0.6470 0.041 Uiso 1 1 calc R . .
C34 C 0.8131(4) -0.21902(17) 0.5883(3) 0.0355(7) Uani 1 1 d . . .
H34 H 0.9061 -0.2359 0.6150 0.043 Uiso 1 1 calc R . .
C35 C 0.7578(4) -0.16096(19) 0.5284(3) 0.0382(8) Uani 1 1 d . . .
H35 H 0.8143 -0.1386 0.5159 0.046 Uiso 1 1 calc R . .
C36 C 0.6180(4) -0.13615(16) 0.4871(3) 0.0324(7) Uani 1 1 d . . .
H36 H 0.5782 -0.0985 0.4439 0.039 Uiso 1 1 calc R . .
N6 N 0.1099(3) -0.03430(13) 0.2777(2) 0.0273(5) Uani 1 1 d . . .
C41 C -0.0248(4) 0.00507(16) 0.2379(3) 0.0345(7) Uani 1 1 d . . .
H41A H -0.0233 0.0480 0.2112 0.041 Uiso 1 1 calc R . .
H41B H -0.0253 0.0137 0.2943 0.041 Uiso 1 1 calc R . .
C42 C -0.1634(4) -0.0337(2) 0.1520(4) 0.0470(9) Uani 1 1 d . . .
H42A H -0.1685 -0.0747 0.1807 0.056 Uiso 1 1 calc R . .
H42B H -0.2520 -0.0071 0.1237 0.056 Uiso 1 1 calc R . .
O43 O -0.1631(3) -0.05020(17) 0.0700(2) 0.0576(8) Uani 1 1 d . . .
C44 C -0.0364(5) -0.0910(2) 0.1100(3) 0.0484(10) Uani 1 1 d . . .
H44A H -0.0387 -0.1033 0.0533 0.058 Uiso 1 1 calc R . .
H44B H -0.0417 -0.1320 0.1386 0.058 Uiso 1 1 calc R . .
C45 C 0.1092(4) -0.05533(17) 0.1940(3) 0.0339(7) Uani 1 1 d . . .
H45A H 0.1935 -0.0852 0.2223 0.041 Uiso 1 1 calc R . .
H45B H 0.1195 -0.0163 0.1646 0.041 Uiso 1 1 calc R . .
P P 0.38866(8) -0.09494(3) 0.71625(6) 0.02064(13) Uani 1 1 d . . .
C51 C 0.3585(3) -0.11889(14) 0.8055(2) 0.0231(5) Uani 1 1 d . . .
C52 C 0.2346(4) -0.15697(17) 0.7723(3) 0.0325(7) Uani 1 1 d . . .
H52 H 0.1655 -0.1718 0.7033 0.039 Uiso 1 1 calc R . .
C53 C 0.2145(4) -0.17278(18) 0.8430(3) 0.0384(8) Uani 1 1 d . . .
H53 H 0.1325 -0.1987 0.8212 0.046 Uiso 1 1 calc R . .
C54 C 0.3155(4) -0.15024(19) 0.9450(3) 0.0386(8) Uani 1 1 d . . .
H54 H 0.3015 -0.1609 0.9918 0.046 Uiso 1 1 calc R . .
C55 C 0.4380(4) -0.1117(2) 0.9778(3) 0.0389(7) Uani 1 1 d . . .
H55 H 0.5056 -0.0962 1.0465 0.047 Uiso 1 1 calc R . .
C56 C 0.4601(3) -0.09610(17) 0.9091(2) 0.0306(6) Uani 1 1 d . . .
H56 H 0.5428 -0.0704 0.9317 0.037 Uiso 1 1 calc R . .
C61 C 0.5714(3) -0.12728(13) 0.7705(2) 0.0236(5) Uani 1 1 d . . .
C62 C 0.6401(3) -0.10053(15) 0.7340(3) 0.0270(6) Uani 1 1 d . . .
H62 H 0.5926 -0.0665 0.6841 0.032 Uiso 1 1 calc R . .
C63 C 0.7779(4) -0.12449(16) 0.7718(3) 0.0345(7) Uani 1 1 d . . .
H63 H 0.8233 -0.1065 0.7475 0.041 Uiso 1 1 calc R . .
C64 C 0.8487(4) -0.17532(17) 0.8458(3) 0.0387(8) Uani 1 1 d . . .
H64 H 0.9425 -0.1909 0.8721 0.046 Uiso 1 1 calc R . .
C65 C 0.7805(4) -0.20281(17) 0.8805(3) 0.0398(8) Uani 1 1 d . . .
H65 H 0.8280 -0.2374 0.9294 0.048 Uiso 1 1 calc R . .
C66 C 0.6412(4) -0.17938(15) 0.8432(3) 0.0319(7) Uani 1 1 d . . .
H66 H 0.5955 -0.1983 0.8667 0.038 Uiso 1 1 calc R . .
C71 C 0.4135(3) -0.00404(13) 0.7341(2) 0.0224(5) Uani 1 1 d . . .
C72 C 0.5558(3) 0.02598(14) 0.7996(3) 0.0279(6) Uani 1 1 d . . .
H72 H 0.6417 -0.0006 0.8355 0.034 Uiso 1 1 calc R . .
C73 C 0.5696(4) 0.09549(15) 0.8113(3) 0.0315(7) Uani 1 1 d . . .
H73 H 0.6645 0.1152 0.8536 0.038 Uiso 1 1 calc R . .
C74 C 0.4429(4) 0.13521(15) 0.7605(3) 0.0330(7) Uani 1 1 d . . .
H74 H 0.4524 0.1817 0.7685 0.040 Uiso 1 1 calc R . .
C75 C 0.3018(4) 0.10591(16) 0.6978(3) 0.0325(7) Uani 1 1 d . . .
H75 H 0.2167 0.1327 0.6650 0.039 Uiso 1 1 calc R . .
C76 C 0.2861(3) 0.03654(15) 0.6833(3) 0.0274(6) Uani 1 1 d . . .
H76 H 0.1907 0.0173 0.6398 0.033 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 0.0030 0.0020 '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 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0180 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1250 0.1230 '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
O10 Re1 O5 175.95(9) . . ?
O10 Re1 Cl1 101.03(8) . . ?
O5 Re1 Cl1 83.00(6) . . ?
O10 Re1 S1 95.55(8) . . ?
O5 Re1 S1 80.43(6) . . ?
Cl1 Re1 S1 163.42(3) . . ?
O10 Re1 Cl2 97.87(8) . . ?
O5 Re1 Cl2 82.67(6) . . ?
Cl1 Re1 Cl2 87.90(3) . . ?
S1 Re1 Cl2 90.28(3) . . ?
O10 Re1 P 91.98(8) . . ?
O5 Re1 P 87.57(6) . . ?
Cl1 Re1 P 89.32(3) . . ?
S1 Re1 P 89.68(3) . . ?
Cl2 Re1 P 170.11(2) . . ?
C2 S1 Re1 99.53(9) . . ?
N6 C2 N3 117.8(3) . . ?
N6 C2 S1 120.4(2) . . ?
N3 C2 S1 121.2(2) . . ?
C4 N3 C2 122.6(3) . . ?
O5 C4 N3 126.4(3) . . ?
O5 C4 C31 115.2(3) . . ?
N3 C4 C31 118.4(3) . . ?
C4 O5 Re1 135.29(19) . . ?
C32 C31 C36 120.1(3) . . ?
C32 C31 C4 119.2(3) . . ?
C36 C31 C4 120.6(3) . . ?
C31 C32 C33 119.9(3) . . ?
C34 C33 C32 119.9(3) . . ?
C33 C34 C35 120.5(3) . . ?
C34 C35 C36 119.9(3) . . ?
C35 C36 C31 119.6(3) . . ?
C2 N6 C45 122.3(3) . . ?
C2 N6 C41 124.4(3) . . ?
C45 N6 C41 112.5(3) . . ?
N6 C41 C42 109.2(3) . . ?
O43 C42 C41 111.6(3) . . ?
C44 O43 C42 109.7(3) . . ?
O43 C44 C45 111.7(3) . . ?
N6 C45 C44 109.2(3) . . ?
C61 P C51 107.16(14) . . ?
C61 P C71 105.07(13) . . ?
C51 P C71 102.66(13) . . ?
C61 P Re1 111.36(10) . . ?
C51 P Re1 114.77(10) . . ?
C71 P Re1 114.93(10) . . ?
C52 C51 C56 119.5(3) . . ?
C52 C51 P 121.7(2) . . ?
C56 C51 P 118.7(2) . . ?
C51 C52 C53 119.6(3) . . ?
C54 C53 C52 120.4(3) . . ?
C53 C54 C55 120.0(3) . . ?
C56 C55 C54 120.3(3) . . ?
C55 C56 C51 120.2(3) . . ?
C66 C61 C62 119.6(3) . . ?
C66 C61 P 122.0(2) . . ?
C62 C61 P 118.3(2) . . ?
C63 C62 C61 120.3(3) . . ?
C62 C63 C64 120.0(3) . . ?
C65 C64 C63 120.0(3) . . ?
C64 C65 C66 120.8(3) . . ?
C61 C66 C65 119.2(3) . . ?
C76 C71 C72 119.0(3) . . ?
C76 C71 P 118.7(2) . . ?
C72 C71 P 122.2(2) . . ?
C73 C72 C71 120.3(3) . . ?
C74 C73 C72 120.2(3) . . ?
C73 C74 C75 119.9(3) . . ?
C74 C75 C76 120.5(3) . . ?
C75 C76 C71 120.0(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
Re1 O10 1.689(2) . ?
Re1 O5 2.069(2) . ?
Re1 Cl1 2.3790(7) . ?
Re1 S1 2.3996(7) . ?
Re1 Cl2 2.4015(8) . ?
Re1 P 2.4640(9) . ?
S1 C2 1.761(3) . ?
C2 N6 1.323(4) . ?
C2 N3 1.342(4) . ?
N3 C4 1.315(4) . ?
C4 O5 1.289(4) . ?
C4 C31 1.484(4) . ?
C31 C32 1.387(4) . ?
C31 C36 1.394(4) . ?
C32 C33 1.388(4) . ?
C33 C34 1.380(5) . ?
C34 C35 1.385(5) . ?
C35 C36 1.387(5) . ?
N6 C45 1.467(4) . ?
N6 C41 1.474(4) . ?
C41 C42 1.504(5) . ?
C42 O43 1.422(6) . ?
O43 C44 1.419(5) . ?
C44 C45 1.506(5) . ?
P C61 1.812(3) . ?
P C51 1.820(3) . ?
P C71 1.825(3) . ?
C51 C52 1.392(4) . ?
C51 C56 1.400(4) . ?
C52 C53 1.394(5) . ?
C53 C54 1.378(5) . ?
C54 C55 1.386(5) . ?
C55 C56 1.377(5) . ?
C61 C66 1.392(4) . ?
C61 C62 1.399(4) . ?
C62 C63 1.379(4) . ?
C63 C64 1.384(5) . ?
C64 C65 1.376(6) . ?
C65 C66 1.393(5) . ?
C71 C76 1.395(4) . ?
C71 C72 1.398(4) . ?
C72 C73 1.391(4) . ?
C73 C74 1.379(5) . ?
C74 C75 1.382(5) . ?
C75 C76 1.392(4) . ?
