#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:30:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179114 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/76/4307692.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_4307692
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            'C19 H16 N3 O8 Re'
_chemical_formula_weight         600.55
_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                103.459(7)
_cell_angle_beta                 106.804(7)
_cell_angle_gamma                105.346(7)
_cell_formula_units_Z            2
_cell_length_a                   8.374(3)
_cell_length_b                   10.639(4)
_cell_length_c                   13.446(5)
_cell_measurement_temperature    296(2)
_cell_volume                     1042.0(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'phi and omega scans'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       CCD
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4738
_diffrn_reflns_theta_full        23.41
_diffrn_reflns_theta_max         23.41
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    5.883
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.793896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         2998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0361
_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)+(0.0094P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0546
_reflns_number_gt                2435
_reflns_number_total             2998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062168csi20070112_023228_8.cif
_cod_data_source_block           Compound_10_(lc32am)
_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        1041.9(7)
_cod_database_code               4307692
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 0.51606(5) -0.16589(4) 0.71278(3) 0.03616(12) Uani 1 1 d . . .
N1 N 0.6793(8) -0.1789(7) 0.6113(6) 0.0368(17) Uani 1 1 d . . .
N2 N 0.7809(8) -0.0206(6) 0.8201(6) 0.0371(17) Uani 1 1 d . . .
C1 C 0.5516(11) -0.3108(11) 0.7610(8) 0.063(3) Uani 1 1 d . . .
O1 O 0.5661(9) -0.4051(7) 0.7897(6) 0.092(3) Uani 1 1 d . . .
C2 C 0.3908(10) -0.1382(8) 0.8109(7) 0.046(2) Uani 1 1 d . . .
O2 O 0.3161(8) -0.1263(7) 0.8696(6) 0.081(2) Uani 1 1 d . . .
C3 C 0.2932(12) -0.2929(9) 0.6025(7) 0.046(2) Uani 1 1 d . . .
N3 N 0.4798(7) 0.0105(6) 0.6552(5) 0.0361(16) Uani 1 1 d . . .
H3A H 0.4663 -0.0140 0.5837 0.043 Uiso 1 1 calc R . .
H3B H 0.3755 0.0159 0.6577 0.043 Uiso 1 1 calc R . .
O3 O 0.1604(8) -0.3727(7) 0.5380(5) 0.074(2) Uani 1 1 d . . .
C4 C 0.6132(9) 0.1510(8) 0.7096(6) 0.0334(19) Uani 1 1 d . . .
O4 O 0.7300(6) 0.1230(6) 0.5728(5) 0.0479(15) Uani 1 1 d . . .
C5 C 0.7312(9) 0.1942(8) 0.6610(7) 0.035(2) Uani 1 1 d . . .
C6 C 0.5997(11) 0.2271(9) 0.8094(7) 0.043(2) Uani 1 1 d . . .
O6 O 0.4746(7) 0.1810(6) 0.8379(5) 0.0656(18) Uani 1 1 d . . .
C7 C 0.7234(13) 0.4243(10) 0.9687(9) 0.088(3) Uani 1 1 d . . .
H7A H 0.6124 0.4401 0.9516 0.133 Uiso 1 1 calc R . .
H7B H 0.8209 0.5115 1.0028 0.133 Uiso 1 1 calc R . .
H7C H 0.7298 0.3724 1.0184 0.133 Uiso 1 1 calc R . .
O7 O 0.7342(8) 0.3480(6) 0.8690(5) 0.0578(16) Uani 1 1 d . . .
C8 C 0.8762(11) 0.3384(9) 0.7112(7) 0.044(2) Uani 1 1 d . . .
O8 O 1.0307(8) 0.3588(7) 0.7560(5) 0.074(2) Uani 1 1 d . . .
C9 C 0.9390(12) 0.5710(8) 0.7221(8) 0.090(4) Uani 1 1 d . . .
H9A H 1.0333 0.5876 0.7900 0.135 Uiso 1 1 calc R . .
H9B H 0.8826 0.6380 0.7329 0.135 Uiso 1 1 calc R . .
H9C H 0.9877 0.5788 0.6664 0.135 Uiso 1 1 calc R . .
O9 O 0.8079(7) 0.4326(6) 0.6873(5) 0.0549(16) Uani 1 1 d . . .
C11 C 0.6197(11) -0.2598(9) 0.5083(7) 0.051(2) Uani 1 1 d . . .
H11 H 0.5000 -0.3168 0.4743 0.061 Uiso 1 1 calc R . .
C12 C 0.7311(13) -0.2630(10) 0.4477(8) 0.067(3) Uani 1 1 d . . .
H12 H 0.6859 -0.3208 0.3747 0.081 Uiso 1 1 calc R . .
C13 C 0.9055(13) -0.1804(11) 0.4976(9) 0.071(3) Uani 1 1 d . . .
H13 H 0.9814 -0.1805 0.4589 0.085 Uiso 1 1 calc R . .
C14 C 0.9686(11) -0.0978(10) 0.6037(9) 0.062(3) Uani 1 1 d . . .
H14 H 1.0890 -0.0427 0.6382 0.075 Uiso 1 1 calc R . .
C15 C 0.8553(10) -0.0937(9) 0.6635(8) 0.044(2) Uani 1 1 d . . .
C16 C 0.9089(10) -0.0047(9) 0.7763(8) 0.042(2) Uani 1 1 d . . .
C17 C 1.0787(11) 0.0902(10) 0.8387(9) 0.060(3) Uani 1 1 d . . .
H17 H 1.1668 0.0971 0.8090 0.072 Uiso 1 1 calc R . .
C18 C 1.1203(13) 0.1748(10) 0.9439(10) 0.071(3) Uani 1 1 d . . .
H18 H 1.2343 0.2403 0.9848 0.085 Uiso 1 1 calc R . .
C19 C 0.9900(13) 0.1602(9) 0.9867(8) 0.065(3) Uani 1 1 d . . .
H19 H 1.0130 0.2161 1.0574 0.078 Uiso 1 1 calc R . .
C20 C 0.8258(11) 0.0622(9) 0.9241(7) 0.049(2) Uani 1 1 d . . .
H20 H 0.7391 0.0516 0.9549 0.059 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'
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
C1 Re1 C3 89.0(4) . . ?
C1 Re1 C2 87.6(4) . . ?
C3 Re1 C2 87.6(3) . . ?
C1 Re1 N2 93.7(3) . . ?
C3 Re1 N2 172.4(3) . . ?
C2 Re1 N2 99.6(3) . . ?
C1 Re1 N1 94.2(3) . . ?
C3 Re1 N1 97.5(3) . . ?
C2 Re1 N1 174.6(3) . . ?
N2 Re1 N1 75.3(3) . . ?
C1 Re1 N3 178.7(3) . . ?
C3 Re1 N3 92.0(3) . . ?
C2 Re1 N3 93.3(3) . . ?
N2 Re1 N3 85.2(2) . . ?
N1 Re1 N3 84.8(2) . . ?
C11 N1 C15 120.2(7) . . ?
C11 N1 Re1 124.9(6) . . ?
C15 N1 Re1 114.9(5) . . ?
C20 N2 C16 117.4(7) . . ?
C20 N2 Re1 125.4(6) . . ?
C16 N2 Re1 117.0(6) . . ?
O1 C1 Re1 177.1(8) . . ?
O2 C2 Re1 177.6(8) . . ?
O3 C3 Re1 177.5(8) . . ?
C4 N3 Re1 121.6(4) . . ?
C5 C4 C6 128.5(8) . . ?
C5 C4 N3 117.7(7) . . ?
C6 C4 N3 113.8(6) . . ?
O4 C5 C4 124.3(8) . . ?
O4 C5 C8 113.8(7) . . ?
C4 C5 C8 121.9(8) . . ?
O6 C6 O7 123.1(8) . . ?
O6 C6 C4 121.8(9) . . ?
O7 C6 C4 115.1(7) . . ?
C6 O7 C7 115.7(7) . . ?
O8 C8 O9 125.8(8) . . ?
O8 C8 C5 123.3(8) . . ?
O9 C8 C5 110.6(7) . . ?
C8 O9 C9 114.6(7) . . ?
N1 C11 C12 122.1(9) . . ?
C13 C12 C11 118.8(9) . . ?
C14 C13 C12 119.6(9) . . ?
C13 C14 C15 121.2(9) . . ?
N1 C15 C14 118.0(8) . . ?
N1 C15 C16 116.6(7) . . ?
C14 C15 C16 125.3(8) . . ?
N2 C16 C17 120.1(9) . . ?
N2 C16 C15 116.0(7) . . ?
C17 C16 C15 123.8(8) . . ?
C18 C17 C16 121.3(9) . . ?
C19 C18 C17 118.2(9) . . ?
C20 C19 C18 118.8(10) . . ?
N2 C20 C19 124.1(8) . . ?
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 C1 1.866(10) . ?
Re1 C3 1.908(10) . ?
Re1 C2 1.926(8) . ?
Re1 N2 2.165(6) . ?
Re1 N1 2.200(6) . ?
Re1 N3 2.248(5) . ?
N1 C11 1.314(10) . ?
N1 C15 1.373(9) . ?
N2 C20 1.348(10) . ?
N2 C16 1.356(9) . ?
C1 O1 1.179(9) . ?
C2 O2 1.145(8) . ?
C3 O3 1.144(9) . ?
N3 C4 1.467(8) . ?
C4 C5 1.374(9) . ?
C4 C6 1.449(10) . ?
O4 C5 1.244(9) . ?
C5 C8 1.530(10) . ?
C6 O6 1.238(8) . ?
C6 O7 1.340(9) . ?
C7 O7 1.438(10) . ?
C8 O8 1.193(8) . ?
C8 O9 1.335(9) . ?
C9 O9 1.456(9) . ?
C11 C12 1.407(10) . ?
C12 C13 1.355(11) . ?
C13 C14 1.350(12) . ?
C14 C15 1.412(10) . ?
C15 C16 1.453(11) . ?
C16 C17 1.379(11) . ?
C17 C18 1.374(13) . ?
C18 C19 1.364(12) . ?
C19 C20 1.360(10) . ?
