#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/47/4304770.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_4304770
loop_
_publ_author_name
'Nguyen Hung Huy'
'Jacqueline Grewe'
'Jennifer Schroer'
'Bernd Kuhn'
'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 Tridentate
N-[(N",N"-Dialkylamino)(thiocarbonyl)]-N'-substituted Benzamidine 
Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5136
_journal_page_last               5144
_journal_paper_doi               10.1021/ic702344s
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C18 H17 Cl N3 O3 Re S'
_chemical_formula_sum            'C18 H17 Cl N3 O3 Re S'
_chemical_formula_weight         577.06
_chemical_name_common            '[ReOCl(MortcbPhOH)]'
_chemical_name_systematic
;
Chloro(N-(N"-morpholinylaminothiocarbonyl)-N'-(2-hydroxyphenyl)benzamidinato-
oxorhenium(V)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.248(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3104(10)
_cell_length_b                   12.3886(10)
_cell_length_c                   15.2945(10)
_cell_measurement_reflns_used    14609
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.14
_cell_volume                     1901.6(3)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0828
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16231
_diffrn_reflns_theta_full        29.32
_diffrn_reflns_theta_max         29.32
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    6.665
_exptl_absorpt_correction_T_max  0.7656
_exptl_absorpt_correction_T_min  0.3515
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-Red 32'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.941
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0475
_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)+(0.0865P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                3927
_reflns_number_total             5099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702344s-file010_2.cif
_cod_data_source_block           bkreanoh
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy atom' was changed to
'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4304770
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Re Re 0.64635(3) 0.35502(2) 0.87049(2) 0.02393(11) Uani 1 1 d . . .
O10 O 0.5868(8) 0.3926(6) 0.9583(4) 0.0384(15) Uani 1 1 d . . .
Cl Cl 0.6555(3) 0.16616(18) 0.87940(18) 0.0452(6) Uani 1 1 d . . .
S1 S 0.8739(2) 0.34916(17) 0.91380(15) 0.0298(4) Uani 1 1 d . . .
C2 C 0.9338(9) 0.4741(7) 0.8799(6) 0.0287(17) Uani 1 1 d . . .
N3 N 0.8603(7) 0.5635(6) 0.8700(5) 0.0261(13) Uani 1 1 d . . .
C4 C 0.7311(8) 0.5715(7) 0.8392(5) 0.0241(15) Uani 1 1 d . . .
N5 N 0.6520(6) 0.4887(5) 0.7983(4) 0.0210(12) Uani 1 1 d . . .
C31 C 0.6729(8) 0.6770(7) 0.8523(5) 0.0221(14) Uani 1 1 d . . .
C32 C 0.7432(10) 0.7723(7) 0.8494(6) 0.0291(17) Uani 1 1 d . . .
H32 H 0.8263 0.7704 0.8354 0.035 Uiso 1 1 calc R . .
C33 C 0.6889(10) 0.8713(7) 0.8675(6) 0.0322(18) Uani 1 1 d . . .
H33 H 0.7338 0.9353 0.8629 0.039 Uiso 1 1 calc R . .
C34 C 0.5691(12) 0.8730(7) 0.8921(7) 0.038(2) Uani 1 1 d . . .
H34 H 0.5337 0.9385 0.9050 0.046 Uiso 1 1 calc R . .
C35 C 0.4997(12) 0.7777(8) 0.8979(7) 0.040(2) Uani 1 1 d . . .
H35 H 0.4211 0.7796 0.9179 0.048 Uiso 1 1 calc R . .
C36 C 0.5475(10) 0.6805(8) 0.8741(6) 0.0329(19) Uani 1 1 d . . .
H36 H 0.4973 0.6179 0.8724 0.040 Uiso 1 1 calc R . .
N6 N 1.0593(9) 0.4791(7) 0.8709(6) 0.041(2) Uani 1 1 d . . .
O43 O 1.3061(8) 0.4837(8) 0.8270(7) 0.059(2) Uani 1 1 d . . .
C41 C 1.1106(10) 0.5816(9) 0.8444(8) 0.042(2) Uani 1 1 d . . .
H41A H 1.1586 0.6202 0.8971 0.050 Uiso 1 1 calc R . .
H41B H 1.0375 0.6266 0.8132 0.050 Uiso 1 1 calc R . .
C42 C 1.2018(16) 0.5561(11) 0.7839(10) 0.063(3) Uani 1 1 d . . .
H42A H 1.1511 0.5233 0.7291 0.076 Uiso 1 1 calc R . .
H42B H 1.2409 0.6224 0.7680 0.076 Uiso 1 1 calc R . .
C44 C 1.2452(16) 0.3821(11) 0.8402(11) 0.063(4) Uani 1 1 d . . .
H44A H 1.3137 0.3291 0.8633 0.075 Uiso 1 1 calc R . .
H44B H 1.1925 0.3560 0.7832 0.075 Uiso 1 1 calc R . .
C45 C 1.1571(12) 0.3968(11) 0.9058(9) 0.051(3) Uani 1 1 d . . .
H45A H 1.1128 0.3294 0.9130 0.061 Uiso 1 1 calc R . .
H45B H 1.2103 0.4185 0.9639 0.061 Uiso 1 1 calc R . .
C51 C 0.5440(10) 0.5000(6) 0.7221(5) 0.0284(17) Uani 1 1 d . . .
C52 C 0.5187(12) 0.5880(7) 0.6629(6) 0.036(2) Uani 1 1 d . . .
H52 H 0.5717 0.6496 0.6724 0.044 Uiso 1 1 calc R . .
C53 C 0.4107(12) 0.5792(8) 0.5891(7) 0.043(2) Uani 1 1 d . . .
H53 H 0.3858 0.6385 0.5516 0.051 Uiso 1 1 calc R . .
C54 C 0.3412(12) 0.4852(8) 0.5711(7) 0.047(3) Uani 1 1 d . . .
H54 H 0.2710 0.4809 0.5207 0.056 Uiso 1 1 calc R . .
C55 C 0.3732(10) 0.3960(9) 0.6263(7) 0.038(2) Uani 1 1 d . . .
H55 H 0.3291 0.3308 0.6112 0.045 Uiso 1 1 calc R . .
C56 C 0.4712(9) 0.4053(7) 0.7039(6) 0.0280(17) Uani 1 1 d . . .
O57 O 0.5105(6) 0.3226(5) 0.7616(4) 0.0273(12) Uani 1 1 d . . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
_geom_angle_publ_flag
O10 Re O57 114.8(3) . . ?
O10 Re N5 106.1(3) . . ?
O57 Re N5 78.8(3) . . ?
O10 Re S1 108.6(3) . . ?
O57 Re S1 136.6(2) . . ?
N5 Re S1 91.62(19) . . ?
O10 Re Cl 104.4(3) . . ?
O57 Re Cl 81.71(18) . . ?
N5 Re Cl 148.6(2) . . ?
S1 Re Cl 85.78(9) . . ?
C2 S1 Re 106.7(3) . . ?
N3 C2 N6 119.3(8) . . ?
N3 C2 S1 121.9(7) . . ?
N6 C2 S1 118.6(7) . . ?
C4 N3 C2 127.5(8) . . ?
N3 C4 N5 123.8(8) . . ?
N3 C4 C31 115.6(7) . . ?
N5 C4 C31 120.6(7) . . ?
C4 N5 C51 125.0(7) . . ?
C4 N5 Re 117.3(5) . . ?
C51 N5 Re 114.6(5) . . ?
C32 C31 C36 119.6(8) . . ?
C32 C31 C4 121.2(8) . . ?
C36 C31 C4 119.0(8) . . ?
C31 C32 C33 120.1(9) . . ?
C34 C33 C32 119.6(9) . . ?
C33 C34 C35 120.8(9) . . ?
C36 C35 C34 120.1(11) . . ?
C35 C36 C31 119.5(9) . . ?
C2 N6 C45 122.7(9) . . ?
C2 N6 C41 119.2(8) . . ?
C45 N6 C41 116.5(9) . . ?
C42 O43 C44 107.7(10) . . ?
N6 C41 C42 107.8(10) . . ?
O43 C42 C41 111.0(11) . . ?
O43 C44 C45 109.6(11) . . ?
N6 C45 C44 108.3(11) . . ?
C56 C51 C52 121.0(8) . . ?
C56 C51 N5 111.6(7) . . ?
C52 C51 N5 126.8(8) . . ?
C53 C52 C51 117.2(9) . . ?
C54 C53 C52 121.0(9) . . ?
C53 C54 C55 121.2(9) . . ?
C56 C55 C54 119.0(9) . . ?
O57 C56 C55 123.4(8) . . ?
O57 C56 C51 116.2(7) . . ?
C55 C56 C51 120.1(8) . . ?
C56 O57 Re 116.7(5) . . ?
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
Re O10 1.665(7) . ?
Re O57 1.957(6) . ?
Re N5 1.999(7) . ?
Re S1 2.289(2) . ?
Re Cl 2.344(2) . ?
S1 C2 1.786(9) . ?
C2 N3 1.331(11) . ?
C2 N6 1.333(12) . ?
N3 C4 1.311(10) . ?
C4 N5 1.370(10) . ?
C4 C31 1.470(11) . ?
N5 C51 1.422(11) . ?
C31 C32 1.392(12) . ?
C31 C36 1.407(13) . ?
C32 C33 1.401(12) . ?
C33 C34 1.371(16) . ?
C34 C35 1.394(15) . ?
C35 C36 1.381(14) . ?
N6 C45 1.447(14) . ?
N6 C41 1.468(13) . ?
O43 C42 1.439(17) . ?
O43 C44 1.441(16) . ?
C41 C42 1.496(17) . ?
C44 C45 1.511(18) . ?
C51 C56 1.386(11) . ?
C51 C52 1.404(11) . ?
C52 C53 1.396(14) . ?
C53 C54 1.362(14) . ?
C54 C55 1.385(15) . ?
C55 C56 1.375(12) . ?
C56 O57 1.353(10) . ?
