#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:54:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179134 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/96/4309602.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_4309602
loop_
_publ_author_name
'Neva Lazarova'
'John Babich'
'John Valliant'
'Paul Schaffer'
'Shelly James'
'Jon Zubieta'
_publ_section_title
;
Thiol- and Thioether-Based Bifunctional Chelates for the {M(CO)3}+ Core (M =
Tc, Re)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6763
_journal_page_last               6770
_journal_paper_doi               10.1021/ic050735a
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C17 H16 N3 O3 Re S'
_chemical_formula_weight         528.59
_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                 104.272(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.846(2)
_cell_length_b                   9.5722(12)
_cell_length_c                   11.6240(15)
_cell_measurement_reflns_used    5663
_cell_measurement_temperature    81(2)
_cell_measurement_theta_max      31.50
_cell_measurement_theta_min      2.51
_cell_volume                     1708.7(4)
_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      81(2)
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21517
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    7.255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXTL-97 (Sheldrick, 1997)'
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0181
_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)+(0.0242P)²+0.9103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0457
_reflns_number_gt                5314
_reflns_number_total             5663
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050735asi20050510_120128.cif
_cod_data_source_block           p21-c
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4309602
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 0.212724(4) 0.414686(7) 0.164208(6) 0.01198(3) Uani 1 1 d . . .
S1 S 0.17978(3) 0.64328(5) 0.06539(4) 0.01621(8) Uani 1 1 d . . .
O1 O 0.37541(11) 0.3941(2) 0.06566(16) 0.0303(4) Uani 1 1 d . . .
O2 O 0.10698(11) 0.25134(15) -0.04940(13) 0.0234(3) Uani 1 1 d . . .
O3 O 0.25949(11) 0.13422(17) 0.29471(15) 0.0265(3) Uani 1 1 d . . .
N1 N 0.09998(10) 0.46197(16) 0.23363(13) 0.0130(3) Uani 1 1 d . . .
N2 N 0.26885(10) 0.54917(17) 0.32585(13) 0.0134(3) Uani 1 1 d . . .
N3 N 0.44612(11) 0.6954(2) 0.48850(16) 0.0225(3) Uani 1 1 d . . .
C1 C 0.31528(14) 0.4006(2) 0.10377(18) 0.0194(4) Uani 1 1 d . . .
C2 C 0.14839(12) 0.31316(19) 0.03000(16) 0.0159(3) Uani 1 1 d . . .
C3 C 0.24141(13) 0.2408(2) 0.24875(16) 0.0178(3) Uani 1 1 d . . .
C4 C 0.01622(12) 0.44551(19) 0.17216(17) 0.0153(3) Uani 1 1 d . . .
C5 C -0.05296(12) 0.48974(19) 0.21559(17) 0.0161(3) Uani 1 1 d . . .
C6 C -0.03598(13) 0.5554(2) 0.32518(18) 0.0169(3) Uani 1 1 d . . .
C7 C 0.04964(13) 0.57459(18) 0.38827(17) 0.0151(3) Uani 1 1 d . . .
C8 C 0.11588(11) 0.52485(18) 0.34056(15) 0.0128(3) Uani 1 1 d . . .
C9 C 0.20988(12) 0.5312(2) 0.40730(16) 0.0146(3) Uani 1 1 d . . .
C10 C 0.35911(12) 0.5006(2) 0.38937(17) 0.0170(3) Uani 1 1 d . . .
C11 C 0.40092(13) 0.57974(19) 0.50136(18) 0.0171(3) Uani 1 1 d . . .
C12 C 0.39386(13) 0.5314(2) 0.61111(18) 0.0198(4) Uani 1 1 d . . .
C13 C 0.43426(15) 0.6067(2) 0.71231(19) 0.0233(4) Uani 1 1 d . . .
C14 C 0.47973(13) 0.7267(2) 0.70036(19) 0.0250(4) Uani 1 1 d . . .
C15 C 0.48417(14) 0.7667(2) 0.5875(2) 0.0252(4) Uani 1 1 d . . .
C16 C 0.27287(12) 0.7006(2) 0.29283(17) 0.0161(3) Uani 1 1 d . . .
C17 C 0.19412(13) 0.74837(19) 0.19900(17) 0.0159(3) Uani 1 1 d . . .
H4 H 0.0072(17) 0.400(2) 0.098(2) 0.012(6) Uiso 1 1 d . . .
H5 H -0.1086(18) 0.479(3) 0.173(2) 0.023(6) Uiso 1 1 d . . .
H6 H -0.0818(19) 0.587(2) 0.354(3) 0.017(7) Uiso 1 1 d . . .
H7 H 0.0633(18) 0.622(3) 0.463(3) 0.026(7) Uiso 1 1 d . . .
H9A H 0.2235(17) 0.449(3) 0.444(2) 0.018(6) Uiso 1 1 d . . .
H9B H 0.2199(18) 0.610(3) 0.461(2) 0.022(7) Uiso 1 1 d . . .
H10A H 0.3520(18) 0.401(3) 0.406(2) 0.018(6) Uiso 1 1 d . . .
H10B H 0.3934(16) 0.509(3) 0.339(2) 0.017(6) Uiso 1 1 d . . .
H12 H 0.3617(19) 0.449(3) 0.622(3) 0.025(7) Uiso 1 1 d . . .
H13 H 0.426(2) 0.577(3) 0.784(3) 0.039(9) Uiso 1 1 d . . .
H14 H 0.5062(19) 0.782(3) 0.770(3) 0.033(8) Uiso 1 1 d . . .
H15 H 0.5156(19) 0.844(3) 0.581(3) 0.033(8) Uiso 1 1 d . . .
H16A H 0.3263(17) 0.711(3) 0.261(2) 0.019(6) Uiso 1 1 d . . .
H16B H 0.2820(16) 0.756(3) 0.367(2) 0.022(6) Uiso 1 1 d . . .
H17A H 0.2036(17) 0.835(4) 0.176(2) 0.028(7) Uiso 1 1 d . . .
H17B H 0.1403(17) 0.748(3) 0.227(2) 0.019(6) Uiso 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'
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'
Re Re -1.0185 7.2310 '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
C2 Re1 C1 89.71(8) . . ?
C2 Re1 C3 89.34(8) . . ?
C1 Re1 C3 90.64(8) . . ?
C2 Re1 N1 94.99(7) . . ?
C1 Re1 N1 172.01(7) . . ?
C3 Re1 N1 95.86(7) . . ?
C2 Re1 N2 171.03(7) . . ?
C1 Re1 N2 98.50(7) . . ?
C3 Re1 N2 94.16(7) . . ?
N1 Re1 N2 76.45(6) . . ?
C2 Re1 S1 93.56(6) . . ?
C1 Re1 S1 89.60(6) . . ?
C3 Re1 S1 177.09(6) . . ?
N1 Re1 S1 83.66(4) . . ?
N2 Re1 S1 82.94(4) . . ?
C17 S1 Re1 97.21(6) . . ?
C8 N1 C4 118.37(16) . . ?
C8 N1 Re1 116.74(12) . . ?
C4 N1 Re1 124.54(12) . . ?
C9 N2 C16 110.17(14) . . ?
C9 N2 C10 108.60(14) . . ?
C16 N2 C10 109.05(15) . . ?
C9 N2 Re1 106.28(11) . . ?
C16 N2 Re1 111.57(11) . . ?
C10 N2 Re1 111.10(11) . . ?
C15 N3 C11 117.42(19) . . ?
O1 C1 Re1 178.4(2) . . ?
O2 C2 Re1 177.56(17) . . ?
O3 C3 Re1 176.82(17) . . ?
N1 C4 C5 122.35(17) . . ?
C4 C5 C6 118.88(17) . . ?
C5 C6 C7 119.28(18) . . ?
C6 C7 C8 118.79(17) . . ?
N1 C8 C7 122.30(17) . . ?
N1 C8 C9 115.51(15) . . ?
C7 C8 C9 122.12(16) . . ?
N2 C9 C8 111.88(15) . . ?
C11 C10 N2 115.31(15) . . ?
N3 C11 C12 122.83(19) . . ?
N3 C11 C10 116.67(18) . . ?
C12 C11 C10 120.48(18) . . ?
C11 C12 C13 118.6(2) . . ?
C14 C13 C12 119.2(2) . . ?
C13 C14 C15 118.36(19) . . ?
N3 C15 C14 123.6(2) . . ?
N2 C16 C17 113.33(15) . . ?
C16 C17 S1 110.88(13) . . ?
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 C2 1.9062(19) . ?
Re1 C1 1.928(2) . ?
Re1 C3 1.9291(19) . ?
Re1 N1 2.1814(15) . ?
Re1 N2 2.2704(16) . ?
Re1 S1 2.4666(5) . ?
S1 C17 1.8170(19) . ?
O1 C1 1.147(3) . ?
O2 C2 1.155(2) . ?
O3 C3 1.155(2) . ?
N1 C8 1.348(2) . ?
N1 C4 1.353(2) . ?
N2 C9 1.495(2) . ?
N2 C16 1.505(2) . ?
N2 C10 1.512(2) . ?
N3 C15 1.346(3) . ?
N3 C11 1.347(3) . ?
C4 C5 1.382(3) . ?
C5 C6 1.386(3) . ?
C6 C7 1.386(3) . ?
C7 C8 1.387(3) . ?
C8 C9 1.501(2) . ?
C10 C11 1.511(3) . ?
C11 C12 1.387(3) . ?
C12 C13 1.394(3) . ?
C13 C14 1.381(3) . ?
C14 C15 1.385(3) . ?
C16 C17 1.512(3) . ?
