#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:30:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179114 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/76/4307687.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_4307687
loop_
_publ_author_name
'Luciano Cuesta'
'Miguel A. Huertos'
'Dolores Morales'
'Julio Pérez'
'Lucía Riera'
'Víctor Riera'
'Daniel Miguel'
'Amador Menéndez-Velázquez'
'Santiago García-Granda'
_publ_contact_author
;    JULIO PEREZ
     Departamento de Quimica Organica e Inorganica 
     IUQOEM - Facultad de Quimica
     Universidad de Oviedo-CSIC
     C/ Julian Claveria s/n
     33006 Oviedo  (ASTURIAS)
     SPAIN
;
_publ_contact_author_email       japm@sauron.quimica.uniovi.es
_publ_contact_author_fax         +34-85-103446
_publ_contact_author_phone       +34-85-102985
_publ_section_title
;
Synthesis, Structure, and Reactivity of Mononuclear Re(I) Oximato Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2836
_journal_page_last               2845
_journal_paper_doi               10.1021/ic062168c
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C24 H21 N4 O4 Re S'
_chemical_formula_weight         647.71
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.758(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.559(5)
_cell_length_b                   18.448(14)
_cell_length_c                   22.006(17)
_cell_measurement_temperature    296(2)
_cell_volume                     2663(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11795
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    4.677
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.650268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.846
_refine_diff_density_min         -3.889
_refine_diff_density_rms         0.181
_refine_ls_extinction_coef       0.00020(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0722P)²+35.8451P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1706
_refine_ls_wR_factor_ref         0.1791
_reflns_number_gt                3045
_reflns_number_total             3800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062168csi20070112_023228_3.cif
_cod_data_source_block           Compound_4_(lc38am)
_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.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-scan' 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               4307687
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
Re1 Re 0.08481(10) 0.77411(3) 0.10105(3) 0.0418(3) Uani 1 1 d . . .
S1 S 0.2940(6) 0.8258(2) 0.1858(2) 0.0497(11) Uani 1 1 d . . .
N1 N -0.0594(18) 0.7164(6) 0.1768(6) 0.039(3) Uani 1 1 d . . .
N2 N 0.283(2) 0.6814(7) 0.1193(6) 0.050(3) Uani 1 1 d . . .
N3 N 0.168(3) 1.0299(7) 0.1549(8) 0.066(5) Uani 1 1 d . . .
N4 N 0.406(2) 0.9560(8) 0.2260(7) 0.061(4) Uani 1 1 d . . .
C1 C -0.062(2) 0.7253(10) 0.0317(11) 0.056(5) Uani 1 1 d . . .
O1 O -0.149(2) 0.7023(10) -0.0004(6) 0.083(5) Uani 1 1 d . . .
C2 C 0.245(3) 0.8195(9) 0.0387(8) 0.048(4) Uani 1 1 d . . .
O2 O 0.342(2) 0.8450(8) 0.0036(7) 0.086(5) Uani 1 1 d . . .
C3 C -0.100(3) 0.8499(10) 0.0954(7) 0.050(4) Uani 1 1 d . . .
O3 O -0.229(2) 0.8967(9) 0.0927(7) 0.086(4) Uani 1 1 d . . .
C4 C 0.304(2) 0.9198(8) 0.1889(7) 0.036(4) Uani 1 1 d . . .
O4 O 0.1808(19) 0.9504(6) 0.1458(6) 0.063(3) Uani 1 1 d . . .
C5 C 0.207(3) 1.0606(10) 0.1080(9) 0.067(5) Uani 1 1 d . . .
C6 C 0.282(8) 1.0281(19) 0.0534(15) 0.22(3) Uani 1 1 d . . .
H6A H 0.3645 0.9866 0.0638 0.337 Uiso 1 1 calc R . .
H6B H 0.3635 1.0626 0.0319 0.337 Uiso 1 1 calc R . .
H6C H 0.1697 1.0131 0.0282 0.337 Uiso 1 1 calc R . .
C7 C 0.181(4) 1.1412(11) 0.1095(11) 0.095(8) Uani 1 1 d . . .
H7A H 0.2134 1.1588 0.1495 0.142 Uiso 1 1 calc R . .
H7B H 0.0421 1.1532 0.0994 0.142 Uiso 1 1 calc R . .
H7C H 0.2701 1.1632 0.0806 0.142 Uiso 1 1 calc R . .
C11 C -0.230(3) 0.7376(9) 0.2027(8) 0.054(5) Uani 1 1 d . . .
H11 H -0.2995 0.7773 0.1868 0.065 Uiso 1 1 calc R . .
C12 C -0.307(3) 0.7026(10) 0.2525(9) 0.063(5) Uani 1 1 d . . .
H12 H -0.4279 0.7184 0.2696 0.075 Uiso 1 1 calc R . .
C13 C -0.206(3) 0.6451(11) 0.2766(9) 0.070(6) Uani 1 1 d . . .
H13 H -0.2540 0.6214 0.3109 0.084 Uiso 1 1 calc R . .
C14 C -0.032(3) 0.6230(10) 0.2485(8) 0.060(5) Uani 1 1 d . . .
H14 H 0.0388 0.5829 0.2635 0.072 Uiso 1 1 calc R . .
C15 C 0.042(2) 0.6593(8) 0.1985(7) 0.036(4) Uani 1 1 d . . .
C16 C 0.228(2) 0.6381(8) 0.1670(8) 0.046(4) Uani 1 1 d . . .
C17 C 0.349(3) 0.5805(9) 0.1824(9) 0.055(5) Uani 1 1 d . . .
H17 H 0.3149 0.5524 0.2159 0.067 Uiso 1 1 calc R . .
C18 C 0.515(3) 0.5634(10) 0.1507(10) 0.070(6) Uani 1 1 d . . .
H18 H 0.5935 0.5235 0.1617 0.084 Uiso 1 1 calc R . .
C19 C 0.567(3) 0.6051(11) 0.1020(10) 0.069(5) Uani 1 1 d . . .
H19 H 0.6798 0.5937 0.0787 0.082 Uiso 1 1 calc R . .
C20 C 0.450(3) 0.6635(11) 0.0890(9) 0.065(5) Uani 1 1 d . . .
H20 H 0.4877 0.6929 0.0568 0.078 Uiso 1 1 calc R . .
C21 C 0.536(3) 0.9224(9) 0.2694(7) 0.049(4) Uani 1 1 d . . .
C22 C 0.735(3) 0.9108(10) 0.2576(9) 0.062(5) Uani 1 1 d . . .
H22 H 0.7873 0.9240 0.2202 0.074 Uiso 1 1 calc R . .
C23 C 0.861(3) 0.8794(12) 0.3013(10) 0.078(6) Uani 1 1 d . . .
H23 H 0.9971 0.8712 0.2916 0.093 Uiso 1 1 calc R . .
C24 C 0.800(4) 0.8605(12) 0.3556(11) 0.080(6) Uani 1 1 d . . .
C25 C 0.597(4) 0.8748(15) 0.3681(10) 0.102(9) Uani 1 1 d . . .
H25 H 0.5469 0.8630 0.4062 0.122 Uiso 1 1 calc R . .
C26 C 0.471(4) 0.9058(14) 0.3261(11) 0.093(8) Uani 1 1 d . . .
H26 H 0.3367 0.9159 0.3364 0.112 Uiso 1 1 calc R . .
C27 C 0.939(4) 0.827(2) 0.4030(14) 0.145(13) Uani 1 1 d . . .
H27A H 1.0755 0.8446 0.3977 0.218 Uiso 1 1 calc R . .
H27B H 0.9379 0.7752 0.3986 0.218 Uiso 1 1 calc R . .
H27C H 0.8929 0.8397 0.4428 0.218 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 0.0033 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
C3 Re1 C2 89.2(7) . . ?
C3 Re1 C1 89.0(7) . . ?
C2 Re1 C1 85.0(8) . . ?
C3 Re1 N2 172.3(6) . . ?
C2 Re1 N2 98.1(6) . . ?
C1 Re1 N2 93.9(6) . . ?
C3 Re1 N1 97.4(6) . . ?
C2 Re1 N1 172.3(6) . . ?
C1 Re1 N1 98.8(7) . . ?
N2 Re1 N1 75.1(5) . . ?
C3 Re1 S1 96.6(5) . . ?
C2 Re1 S1 93.8(5) . . ?
C1 Re1 S1 174.4(5) . . ?
N2 Re1 S1 80.8(4) . . ?
N1 Re1 S1 81.7(3) . . ?
C4 S1 Re1 115.5(5) . . ?
C11 N1 C15 120.0(14) . . ?
C11 N1 Re1 123.9(10) . . ?
C15 N1 Re1 115.9(10) . . ?
C20 N2 C16 117.9(15) . . ?
C20 N2 Re1 126.4(12) . . ?
C16 N2 Re1 115.7(10) . . ?
C5 N3 O4 109.6(15) . . ?
C4 N4 C21 121.6(14) . . ?
O1 C1 Re1 173.7(18) . . ?
O2 C2 Re1 178.2(17) . . ?
O3 C3 Re1 176.2(16) . . ?
N4 C4 O4 123.0(14) . . ?
N4 C4 S1 125.4(12) . . ?
O4 C4 S1 111.5(11) . . ?
C4 O4 N3 110.5(12) . . ?
N3 C5 C6 127(2) . . ?
N3 C5 C7 114.9(18) . . ?
C6 C5 C7 118(2) . . ?
N1 C11 C12 121.9(16) . . ?
C13 C12 C11 119.8(18) . . ?
C12 C13 C14 117.6(17) . . ?
C13 C14 C15 121.1(16) . . ?
N1 C15 C14 119.5(14) . . ?
N1 C15 C16 117.1(13) . . ?
C14 C15 C16 123.4(14) . . ?
C17 C16 N2 118.9(16) . . ?
C17 C16 C15 125.1(15) . . ?
N2 C16 C15 116.1(13) . . ?
C18 C17 C16 121.9(18) . . ?
C17 C18 C19 119.4(18) . . ?
C20 C19 C18 117.8(18) . . ?
N2 C20 C19 124.1(18) . . ?
C22 C21 C26 117.1(18) . . ?
C22 C21 N4 121.0(17) . . ?
C26 C21 N4 121.7(18) . . ?
C21 C22 C23 120.3(19) . . ?
C24 C23 C22 123(2) . . ?
C23 C24 C25 116(2) . . ?
C23 C24 C27 123(2) . . ?
C25 C24 C27 121(2) . . ?
C26 C25 C24 121(2) . . ?
C21 C26 C25 122(2) . . ?
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 C3 1.852(19) . ?
Re1 C2 1.931(18) . ?
Re1 C1 2.01(2) . ?
Re1 N2 2.183(13) . ?
Re1 N1 2.202(13) . ?
Re1 S1 2.490(5) . ?
S1 C4 1.736(14) . ?
N1 C11 1.32(2) . ?
N1 C15 1.331(18) . ?
N2 C20 1.33(2) . ?
N2 C16 1.37(2) . ?
N3 C5 1.21(2) . ?
N3 O4 1.482(17) . ?
N4 C4 1.24(2) . ?
N4 C21 1.41(2) . ?
C1 O1 1.00(2) . ?
C2 O2 1.109(19) . ?
C3 O3 1.21(2) . ?
C4 O4 1.359(18) . ?
C5 C6 1.44(4) . ?
C5 C7 1.50(3) . ?
C11 C12 1.37(2) . ?
C12 C13 1.35(2) . ?
C13 C14 1.37(2) . ?
C14 C15 1.38(2) . ?
C15 C16 1.46(2) . ?
C16 C17 1.37(2) . ?
C17 C18 1.34(2) . ?
C18 C19 1.37(3) . ?
C19 C20 1.35(3) . ?
C21 C22 1.35(2) . ?
C21 C26 1.36(3) . ?
C22 C23 1.39(3) . ?
C23 C24 1.31(3) . ?
C24 C25 1.38(3) . ?
C24 C27 1.51(3) . ?
C25 C26 1.36(3) . ?
