#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/76/4307688.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_4307688
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            'C26.25 H21.5 Cl0.5 N4 O5 Re'
_chemical_formula_weight         676.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.207(6)
_cell_angle_beta                 111.490(5)
_cell_angle_gamma                95.130(6)
_cell_formula_units_Z            2
_cell_length_a                   9.984(3)
_cell_length_b                   11.569(4)
_cell_length_c                   13.526(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1389.2(8)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6026
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    4.462
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.594345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             661
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.863
_refine_diff_density_min         -1.863
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.0115(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0288
_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)+(0.0641P)²+3.3236P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                3703
_reflns_number_total             3877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062168csi20070112_023228_4.cif
_cod_data_source_block           Compound_5_(lc34am)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_original_cell_volume        1389.3(8)
_cod_original_formula_sum        'C26.25 H21.50 Cl0.50 N4 O5 Re'
_cod_database_code               4307688
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.69624(2) 0.926318(16) 0.747230(16) 0.03000(14) Uani 1 1 d . . .
N1 N 0.5786(5) 0.7803(4) 0.5937(4) 0.0320(10) Uani 1 1 d . . .
N2 N 0.4855(5) 0.8703(4) 0.7528(4) 0.0317(10) Uani 1 1 d . . .
N3 N 0.7531(5) 0.7753(4) 0.8171(4) 0.0290(10) Uani 1 1 d . . .
N4 N 0.9650(7) 0.5474(6) 0.8086(5) 0.0590(16) Uani 1 1 d . . .
C1 C 0.6359(8) 1.0476(6) 0.6735(6) 0.0473(16) Uani 1 1 d . . .
O1 O 0.6019(8) 1.1214(5) 0.6302(6) 0.0884(19) Uani 1 1 d . . .
C2 C 0.8830(7) 0.9574(6) 0.7372(5) 0.0396(14) Uani 1 1 d . . .
O2 O 0.9966(5) 0.9789(5) 0.7354(5) 0.0666(14) Uani 1 1 d . . .
C3 C 0.7819(7) 1.0495(6) 0.8857(6) 0.0436(15) Uani 1 1 d . . .
O3 O 0.8317(7) 1.1263(5) 0.9674(4) 0.0670(15) Uani 1 1 d . . .
C4 C 0.8338(6) 0.7037(5) 0.7824(5) 0.0316(12) Uani 1 1 d . . .
O4 O 0.8784(4) 0.7088(4) 0.7097(4) 0.0409(9) Uani 1 1 d . . .
O5 O 0.8613(4) 0.6130(4) 0.8355(4) 0.0420(10) Uani 1 1 d . . .
C5 C 0.9566(10) 0.4470(7) 0.8301(7) 0.068(2) Uani 1 1 d . . .
C6 C 0.8532(12) 0.3965(8) 0.8710(9) 0.090(3) Uani 1 1 d . . .
H6A H 0.8392 0.4600 0.9238 0.135 Uiso 1 1 calc R . .
H6B H 0.8921 0.3362 0.9057 0.135 Uiso 1 1 calc R . .
H6C H 0.7608 0.3602 0.8100 0.135 Uiso 1 1 calc R . .
C7 C 1.0659(18) 0.3735(14) 0.8129(14) 0.155(6) Uani 1 1 d . . .
H7A H 1.1335 0.4195 0.7944 0.233 Uiso 1 1 calc R . .
H7B H 1.0160 0.3009 0.7536 0.233 Uiso 1 1 calc R . .
H7C H 1.1186 0.3528 0.8796 0.233 Uiso 1 1 calc R . .
C11 C 0.6249(7) 0.7371(6) 0.5146(5) 0.0413(14) Uani 1 1 d . . .
H11 H 0.7161 0.7733 0.5215 0.050 Uiso 1 1 calc R . .
C12 C 0.5431(8) 0.6402(6) 0.4220(5) 0.0483(16) Uani 1 1 d . . .
H12 H 0.5784 0.6144 0.3676 0.058 Uiso 1 1 calc R . .
C13 C 0.4115(8) 0.5834(6) 0.4117(5) 0.0517(17) Uani 1 1 d . . .
H13 H 0.3573 0.5174 0.3509 0.062 Uiso 1 1 calc R . .
C14 C 0.3577(7) 0.6252(6) 0.4936(5) 0.0446(15) Uani 1 1 d . . .
C15 C 0.2220(8) 0.5700(7) 0.4914(7) 0.067(2) Uani 1 1 d . . .
H15 H 0.1639 0.5030 0.4330 0.080 Uiso 1 1 calc R . .
C16 C 0.1777(8) 0.6138(7) 0.5728(7) 0.068(2) Uani 1 1 d . . .
H16 H 0.0893 0.5760 0.5695 0.081 Uiso 1 1 calc R . .
C17 C 0.2627(7) 0.7171(6) 0.6648(6) 0.0497(16) Uani 1 1 d . . .
C18 C 0.2194(7) 0.7660(7) 0.7503(7) 0.0583(19) Uani 1 1 d . . .
H18 H 0.1318 0.7318 0.7507 0.070 Uiso 1 1 calc R . .
C19 C 0.3087(7) 0.8649(7) 0.8329(6) 0.0542(17) Uani 1 1 d . . .
H19 H 0.2816 0.8993 0.8902 0.065 Uiso 1 1 calc R . .
C20 C 0.4399(7) 0.9146(6) 0.8320(5) 0.0419(14) Uani 1 1 d . . .
H20 H 0.4987 0.9820 0.8895 0.050 Uiso 1 1 calc R . .
C21 C 0.3963(6) 0.7718(5) 0.6682(5) 0.0364(13) Uani 1 1 d . . .
C22 C 0.4454(6) 0.7243(5) 0.5823(5) 0.0362(13) Uani 1 1 d . . .
C31 C 0.7041(6) 0.7532(5) 0.8993(5) 0.0310(12) Uani 1 1 d . . .
C32 C 0.5880(7) 0.6614(5) 0.8734(6) 0.0430(14) Uani 1 1 d . . .
H32 H 0.5469 0.6067 0.8031 0.052 Uiso 1 1 calc R . .
C33 C 0.5319(8) 0.6502(6) 0.9519(6) 0.0508(16) Uani 1 1 d . . .
H33 H 0.4536 0.5878 0.9327 0.061 Uiso 1 1 calc R . .
C34 C 0.5886(8) 0.7284(6) 1.0565(6) 0.0518(17) Uani 1 1 d . . .
C35 C 0.7066(8) 0.8196(6) 1.0840(5) 0.0460(15) Uani 1 1 d . . .
H35 H 0.7483 0.8730 1.1549 0.055 Uiso 1 1 calc R . .
C36 C 0.7638(6) 0.8321(5) 1.0053(5) 0.0369(13) Uani 1 1 d . . .
H36 H 0.8427 0.8941 1.0246 0.044 Uiso 1 1 calc R . .
C37 C 0.5277(13) 0.7176(9) 1.1421(8) 0.091(3) Uani 1 1 d . . .
H37A H 0.4265 0.6781 1.1054 0.137 Uiso 1 1 calc R . .
H37B H 0.5354 0.7969 1.1878 0.137 Uiso 1 1 calc R . .
H37C H 0.5824 0.6711 1.1874 0.137 Uiso 1 1 calc R . .
Cl91 Cl 0.7974(10) 0.9785(13) 0.4269(11) 0.120 Uiso 0.25 1 d PG . .
C90 C 0.9326(13) 0.8882(10) 0.454(4) 0.120 Uiso 0.25 1 d PG . .
H90A H 0.9047 0.8400 0.4954 0.120 Uiso 0.25 1 d PG . .
H90B H 0.9130 0.8463 0.3792 0.120 Uiso 0.25 1 d PG . .
Cl92 Cl 1.1035(10) 0.9882(13) 0.5277(11) 0.120 Uiso 0.25 1 d PG . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Re Re -1.0185 7.2310 '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'
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'
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 C1 89.4(3) . . ?
C3 Re1 C2 86.2(3) . . ?
C1 Re1 C2 88.8(3) . . ?
C3 Re1 N2 98.2(2) . . ?
C1 Re1 N2 95.6(2) . . ?
C2 Re1 N2 173.7(2) . . ?
C3 Re1 N1 173.8(2) . . ?
C1 Re1 N1 91.9(2) . . ?
C2 Re1 N1 99.8(2) . . ?
N2 Re1 N1 75.72(17) . . ?
C3 Re1 N3 95.7(2) . . ?
C1 Re1 N3 174.8(2) . . ?
C2 Re1 N3 92.3(2) . . ?
N2 Re1 N3 82.84(17) . . ?
N1 Re1 N3 82.83(17) . . ?
C11 N1 C22 117.3(5) . . ?
C11 N1 Re1 127.7(4) . . ?
C22 N1 Re1 115.0(4) . . ?
C20 N2 C21 117.4(5) . . ?
C20 N2 Re1 127.5(4) . . ?
C21 N2 Re1 114.8(4) . . ?
C4 N3 C31 120.0(5) . . ?
C4 N3 Re1 119.5(4) . . ?
C31 N3 Re1 120.5(3) . . ?
C5 N4 O5 110.1(6) . . ?
O1 C1 Re1 178.9(7) . . ?
O2 C2 Re1 177.3(6) . . ?
O3 C3 Re1 177.9(6) . . ?
O4 C4 N3 127.1(5) . . ?
O4 C4 O5 120.5(5) . . ?
N3 C4 O5 112.4(5) . . ?
C4 O5 N4 111.5(4) . . ?
N4 C5 C6 127.3(7) . . ?
N4 C5 C7 115.3(10) . . ?
C6 C5 C7 117.4(9) . . ?
N1 C11 C12 123.0(6) . . ?
C13 C12 C11 119.7(6) . . ?
C12 C13 C14 119.6(6) . . ?
C22 C14 C13 116.9(6) . . ?
C22 C14 C15 119.3(6) . . ?
C13 C14 C15 123.8(6) . . ?
C16 C15 C14 120.8(6) . . ?
C15 C16 C17 122.0(7) . . ?
C18 C17 C21 118.6(6) . . ?
C18 C17 C16 123.6(6) . . ?
C21 C17 C16 117.8(6) . . ?
C19 C18 C17 118.4(6) . . ?
C18 C19 C20 120.4(6) . . ?
N2 C20 C19 123.1(6) . . ?
N2 C21 C17 122.1(5) . . ?
N2 C21 C22 117.4(5) . . ?
C17 C21 C22 120.5(5) . . ?
N1 C22 C14 123.6(5) . . ?
N1 C22 C21 116.8(5) . . ?
C14 C22 C21 119.6(5) . . ?
C32 C31 C36 118.3(5) . . ?
C32 C31 N3 121.5(5) . . ?
C36 C31 N3 119.9(5) . . ?
C31 C32 C33 120.3(6) . . ?
C34 C33 C32 122.0(6) . . ?
C33 C34 C35 118.1(6) . . ?
C33 C34 C37 122.4(8) . . ?
C35 C34 C37 119.5(8) . . ?
C34 C35 C36 120.4(6) . . ?
C31 C36 C35 120.8(6) . . ?
Cl92 Cl91 C90 57.8(15) 2_776 . ?
Cl92 C90 Cl92 74.9(7) 2_776 . ?
Cl92 C90 Cl91 32.2(7) 2_776 . ?
Cl92 C90 Cl91 106.8 . . ?
Cl91 Cl92 C90 90.0(15) 2_776 2_776 ?
Cl91 Cl92 C90 163.3(16) 2_776 . ?
C90 Cl92 C90 105.1(9) 2_776 . ?
Cl91 Cl92 Cl92 148.0(19) 2_776 2_776 ?
C90 Cl92 Cl92 58.8(7) 2_776 2_776 ?
C90 Cl92 Cl92 46.4(7) . 2_776 ?
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 1.913(7) . ?
Re1 C1 1.917(7) . ?
Re1 C2 1.926(7) . ?
Re1 N2 2.179(5) . ?
Re1 N1 2.191(5) . ?
Re1 N3 2.192(5) . ?
N1 C11 1.329(8) . ?
N1 C22 1.364(8) . ?
N2 C20 1.329(8) . ?
N2 C21 1.370(8) . ?
N3 C4 1.333(7) . ?
N3 C31 1.432(7) . ?
N4 C5 1.263(10) . ?
N4 O5 1.438(6) . ?
C1 O1 1.150(9) . ?
C2 O2 1.150(8) . ?
C3 O3 1.153(8) . ?
C4 O4 1.228(7) . ?
C4 O5 1.395(7) . ?
C5 C6 1.474(14) . ?
C5 C7 1.494(13) . ?
C11 C12 1.392(9) . ?
C12 C13 1.359(10) . ?
C13 C14 1.410(10) . ?
C14 C22 1.394(9) . ?
C14 C15 1.433(10) . ?
C15 C16 1.345(11) . ?
C16 C17 1.437(10) . ?
C17 C18 1.398(10) . ?
C17 C21 1.404(9) . ?
C18 C19 1.363(10) . ?
C19 C20 1.388(9) . ?
C21 C22 1.437(8) . ?
C31 C32 1.381(8) . ?
C31 C36 1.386(8) . ?
C32 C33 1.394(9) . ?
C33 C34 1.371(10) . ?
C34 C35 1.384(10) . ?
C34 C37 1.515(9) . ?
C35 C36 1.408(9) . ?
Cl91 Cl92 0.940(19) 2_776 ?
Cl91 C90 1.7651 . ?
C90 Cl92 1.49(2) 2_776 ?
C90 Cl92 1.7651 . ?
Cl92 Cl91 0.940(17) 2_776 ?
Cl92 C90 1.49(3) 2_776 ?
Cl92 Cl92 1.993(19) 2_776 ?
