#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/88/7008805.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_7008805
loop_
_publ_author_name
'Le Gal, Julien'
'Tisato, Francesco'
'Bandoli, Giuliano'
'Gressier, Marie'
'Jaud, Joël'
'Michaud, Sandra'
'Dartiguenave, Michèle'
'Benoist, Eric'
_publ_section_title
;
 Synthesis and structural characterization of new oxorhenium and
 oxotechnetium complexes with XN2S-tetradentate semi-rigid ligands (X =
 O, S, N)
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              3800
_journal_paper_doi               10.1039/b508661b
_journal_year                    2005
_chemical_formula_sum            'C26 H44 N3 O4 S Tc'
_chemical_formula_weight         592.70
_chemical_name_systematic
;
?
;
_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                 91.32(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.114(2)
_cell_length_b                   18.383(4)
_cell_length_c                   17.360(4)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      8.6
_cell_measurement_theta_min      6.1
_cell_volume                     2907.8(11)
_computing_cell_refinement       'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_data_collection       'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_data_reduction        'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_molecular_graphics    'SHELXTL NT vers.5.10 (Bruker, 1999)'
_computing_publication_material  'SHELXTL NT vers.5.10 (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL NT vers.5.10 (Bruker, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Nicolet R3m/V diffractometer'
_diffrn_measurement_method       omega-2theta
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7250
_diffrn_reflns_theta_full        29.55
_diffrn_reflns_theta_max         29.55
_diffrn_reflns_theta_min         3.53
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_type   'psi-scan method'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         7250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0454
_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)+(0.0613P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                3700
_reflns_number_total             7250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b508661b.txt
_cod_data_source_block           '[TcO(Ph-ON2S)]-'
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2908(1)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7008805
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
Tc1 Tc 0.14921(3) 0.790970(17) 0.096371(18) 0.05788(12) Uani 1 1 d . . .
S1 S 0.15719(11) 0.81190(6) -0.03270(6) 0.0657(3) Uani 1 1 d . . .
O1 O 0.1465(3) 1.01056(16) 0.05154(17) 0.0830(8) Uani 1 1 d . . .
O2 O -0.0971(4) 0.87390(19) 0.26816(17) 0.0936(10) Uani 1 1 d . . .
O3 O 0.0349(3) 0.70119(13) 0.07396(15) 0.0648(7) Uani 1 1 d . . .
O4 O 0.3140(3) 0.77087(15) 0.13203(17) 0.0783(8) Uani 1 1 d . . .
N1 N 0.1187(3) 0.89646(17) 0.10030(17) 0.0609(8) Uani 1 1 d . . .
N2 N -0.0052(3) 0.79815(17) 0.17471(17) 0.0583(7) Uani 1 1 d . . .
N3 N 0.1700(3) 0.75573(18) 0.43115(16) 0.0596(8) Uani 1 1 d . . .
C1 C 0.1856(4) 0.9100(2) -0.0321(2) 0.0705(11) Uani 1 1 d . . .
H1A H 0.2875 0.9201 -0.0431 0.085 Uiso 1 1 calc R . .
H1B H 0.1255 0.9317 -0.0728 0.085 Uiso 1 1 calc R . .
C2 C 0.1488(4) 0.9448(2) 0.0431(2) 0.0635(10) Uani 1 1 d . . .
C3 C 0.0570(5) 0.9241(2) 0.1711(2) 0.0751(12) Uani 1 1 d . . .
H3A H -0.0092 0.9641 0.1593 0.090 Uiso 1 1 calc R . .
H3B H 0.1350 0.9420 0.2049 0.090 Uiso 1 1 calc R . .
C4 C -0.0255(4) 0.8638(2) 0.2108(2) 0.0686(11) Uani 1 1 d . . .
C5 C -0.0870(4) 0.7340(2) 0.1871(2) 0.0612(10) Uani 1 1 d . . .
C6 C -0.1850(4) 0.7187(3) 0.2444(2) 0.0764(12) Uani 1 1 d . . .
H6A H -0.2056 0.7530 0.2820 0.092 Uiso 1 1 calc R . .
C7 C -0.2517(5) 0.6511(3) 0.2448(3) 0.0973(16) Uani 1 1 d . . .
H7A H -0.3174 0.6403 0.2833 0.117 Uiso 1 1 calc R . .
C8 C -0.2241(6) 0.5997(3) 0.1901(3) 0.0958(16) Uani 1 1 d . . .
H8A H -0.2708 0.5548 0.1917 0.115 Uiso 1 1 calc R . .
C9 C -0.1261(5) 0.6147(2) 0.1324(3) 0.0794(12) Uani 1 1 d . . .
H9A H -0.1068 0.5801 0.0948 0.095 Uiso 1 1 calc R . .
C10 C -0.0569(4) 0.6822(2) 0.1312(2) 0.0635(10) Uani 1 1 d . . .
C11 C 0.2057(4) 0.7102(2) 0.5024(2) 0.0647(10) Uani 1 1 d . . .
H11A H 0.3016 0.6884 0.4961 0.078 Uiso 1 1 calc R . .
H11B H 0.2131 0.7427 0.5464 0.078 Uiso 1 1 calc R . .
C12 C 0.0992(4) 0.6507(2) 0.5210(2) 0.0593(9) Uani 1 1 d . . .
H12A H 0.0942 0.6160 0.4790 0.071 Uiso 1 1 calc R . .
H12B H 0.0021 0.6712 0.5273 0.071 Uiso 1 1 calc R . .
C13 C 0.1487(4) 0.6126(2) 0.5948(2) 0.0699(11) Uani 1 1 d . . .
H13A H 0.2449 0.5915 0.5874 0.084 Uiso 1 1 calc R . .
H13B H 0.1579 0.6484 0.6357 0.084 Uiso 1 1 calc R . .
C14 C 0.0457(5) 0.5538(2) 0.6195(3) 0.0858(13) Uani 1 1 d . . .
H14A H 0.0837 0.5312 0.6656 0.129 Uiso 1 1 calc R . .
H14B H 0.0361 0.5181 0.5794 0.129 Uiso 1 1 calc R . .
H14C H -0.0488 0.5746 0.6292 0.129 Uiso 1 1 calc R . .
C15 C 0.0240(4) 0.7947(2) 0.4378(2) 0.0643(10) Uani 1 1 d . . .
H15A H 0.0057 0.8216 0.3905 0.077 Uiso 1 1 calc R . .
H15B H -0.0524 0.7581 0.4413 0.077 Uiso 1 1 calc R . .
C16 C 0.0086(5) 0.8456(3) 0.5032(3) 0.0914(14) Uani 1 1 d . . .
H16A H 0.0900 0.8796 0.5046 0.110 Uiso 1 1 calc R . .
H16B H 0.0095 0.8188 0.5514 0.110 Uiso 1 1 calc R . .
C17 C -0.1361(7) 0.8869(4) 0.4931(4) 0.137(2) Uani 1 1 d . . .
H17A H -0.1351 0.9121 0.4440 0.165 Uiso 1 1 calc R . .
H17B H -0.2152 0.8516 0.4904 0.165 Uiso 1 1 calc R . .
C18 C -0.1673(13) 0.9362(6) 0.5489(8) 0.291(7) Uani 1 1 d . . .
H18A H -0.2592 0.9594 0.5365 0.437 Uiso 1 1 calc R . .
H18B H -0.0910 0.9722 0.5518 0.437 Uiso 1 1 calc R . .
H18C H -0.1738 0.9118 0.5976 0.437 Uiso 1 1 calc R . .
C19 C 0.2947(4) 0.8093(3) 0.4238(2) 0.0752(12) Uani 1 1 d . . .
H19A H 0.3854 0.7821 0.4199 0.090 Uiso 1 1 calc R . .
H19B H 0.3015 0.8378 0.4707 0.090 Uiso 1 1 calc R . .
C20 C 0.2831(5) 0.8610(3) 0.3562(3) 0.0907(14) Uani 1 1 d . . .
H20A H 0.1996 0.8930 0.3625 0.109 Uiso 1 1 calc R . .
H20B H 0.2676 0.8336 0.3090 0.109 Uiso 1 1 calc R . .
C21 C 0.4218(7) 0.9058(4) 0.3508(4) 0.144(3) Uani 1 1 d . . .
H21A H 0.4040 0.9459 0.3156 0.173 Uiso 1 1 calc R . .
H21B H 0.4458 0.9261 0.4011 0.173 Uiso 1 1 calc R . .
C22 C 0.5405(8) 0.8658(5) 0.3257(5) 0.207(4) Uani 1 1 d . . .
H22A H 0.6248 0.8969 0.3227 0.311 Uiso 1 1 calc R . .
H22B H 0.5178 0.8459 0.2757 0.311 Uiso 1 1 calc R . .
H22C H 0.5609 0.8269 0.3613 0.311 Uiso 1 1 calc R . .
C23 C 0.1566(4) 0.7083(2) 0.3610(2) 0.0680(11) Uani 1 1 d . . .
H23A H 0.1266 0.7385 0.3176 0.082 Uiso 1 1 calc R . .
H23B H 0.0787 0.6734 0.3691 0.082 Uiso 1 1 calc R . .
C24 C 0.2939(5) 0.6665(3) 0.3388(3) 0.0892(14) Uani 1 1 d . . .
H24A H 0.3723 0.7007 0.3289 0.107 Uiso 1 1 calc R . .
H24B H 0.3254 0.6358 0.3815 0.107 Uiso 1 1 calc R . .
C25 C 0.2664(9) 0.6197(4) 0.2678(3) 0.127(2) Uani 1 1 d . . .
C26 C 0.1714(12) 0.5735(6) 0.2738(6) 0.088(3) Uiso 0.50 1 d P . .
C26' C 0.3724(12) 0.5846(6) 0.2263(6) 0.103(3) Uiso 0.50 1 d P . .
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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 '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
O4 Tc1 N1 109.66(13) . . ?
O4 Tc1 N2 114.26(13) . . ?
N1 Tc1 N2 78.86(13) . . ?
O4 Tc1 O3 110.84(12) . . ?
N1 Tc1 O3 139.01(11) . . ?
N2 Tc1 O3 79.19(12) . . ?
O4 Tc1 S1 110.91(11) . . ?
N1 Tc1 S1 82.81(9) . . ?
N2 Tc1 S1 134.66(9) . . ?
O3 Tc1 S1 88.64(8) . . ?
C1 S1 Tc1 99.74(13) . . ?
C10 O3 Tc1 113.5(2) . . ?
C2 N1 C3 118.4(3) . . ?
C2 N1 Tc1 125.9(3) . . ?
C3 N1 Tc1 115.6(3) . . ?
C4 N2 C5 125.9(3) . . ?
C4 N2 Tc1 118.5(3) . . ?
C5 N2 Tc1 115.7(3) . . ?
C23 N3 C19 110.9(3) . . ?
C23 N3 C15 106.3(3) . . ?
C19 N3 C15 111.2(3) . . ?
C23 N3 C11 110.6(3) . . ?
C19 N3 C11 106.2(3) . . ?
C15 N3 C11 111.6(3) . . ?
C2 C1 S1 113.1(3) . . ?
O1 C2 N1 123.6(4) . . ?
O1 C2 C1 122.2(4) . . ?
N1 C2 C1 114.2(3) . . ?
N1 C3 C4 109.6(3) . . ?
O2 C4 N2 126.0(4) . . ?
O2 C4 C3 122.9(4) . . ?
N2 C4 C3 111.1(4) . . ?
C6 C5 C10 120.2(4) . . ?
C6 C5 N2 129.1(4) . . ?
C10 C5 N2 110.6(3) . . ?
C5 C6 C7 118.5(5) . . ?
C8 C7 C6 122.0(5) . . ?
C7 C8 C9 119.8(5) . . ?
C8 C9 C10 119.2(5) . . ?
O3 C10 C5 117.9(3) . . ?
O3 C10 C9 121.8(4) . . ?
C5 C10 C9 120.2(4) . . ?
C12 C11 N3 116.6(3) . . ?
C11 C12 C13 109.7(3) . . ?
C14 C13 C12 113.4(3) . . ?
C16 C15 N3 117.1(3) . . ?
C15 C16 C17 108.8(4) . . ?
C18 C17 C16 116.3(8) . . ?
N3 C19 C20 115.9(3) . . ?
C19 C20 C21 110.2(4) . . ?
C22 C21 C20 113.0(7) . . ?
N3 C23 C24 116.4(3) . . ?
C25 C24 C23 111.6(4) . . ?
C26 C25 C26' 103.1(9) . . ?
C26 C25 C24 115.4(7) . . ?
C26' C25 C24 125.8(8) . . ?
C25 C26 C26' 41.2(5) . . ?
C25 C26' C26 35.6(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
Tc1 O4 1.653(2) . ?
Tc1 N1 1.960(3) . ?
Tc1 N2 1.984(3) . ?
Tc1 O3 1.986(2) . ?
Tc1 S1 2.2764(12) . ?
S1 C1 1.822(4) . ?
O1 C2 1.219(4) . ?
O2 C4 1.216(5) . ?
O3 C10 1.359(4) . ?
N1 C2 1.365(5) . ?
N1 C3 1.454(5) . ?
N2 C4 1.375(5) . ?
N2 C5 1.414(5) . ?
N3 C23 1.501(5) . ?
N3 C19 1.511(5) . ?
N3 C15 1.518(4) . ?
N3 C11 1.522(4) . ?
C1 C2 1.497(5) . ?
C3 C4 1.514(6) . ?
C5 C6 1.383(5) . ?
C5 C10 1.391(6) . ?
C6 C7 1.383(6) . ?
C7 C8 1.366(7) . ?
C8 C9 1.386(6) . ?
C9 C10 1.393(5) . ?
C11 C12 1.503(5) . ?
C12 C13 1.519(5) . ?
C13 C14 1.500(5) . ?
C15 C16 1.481(6) . ?
C16 C17 1.528(7) . ?
C17 C18 1.362(10) . ?
C19 C20 1.512(5) . ?
C20 C21 1.513(7) . ?
C21 C22 1.386(9) . ?
C23 C24 1.525(6) . ?
C24 C25 1.520(7) . ?
C25 C26 1.219(11) . ?
C25 C26' 1.378(12) . ?
C26 C26' 2.037(15) . ?
