#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:30:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179114 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/76/4307689.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_4307689
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            'C22 H16 N3 O7 Re'
_chemical_formula_weight         620.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 129.629(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.471(14)
_cell_length_b                   10.101(5)
_cell_length_c                   20.223(10)
_cell_measurement_temperature    296(2)
_cell_volume                     4479(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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9651
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    5.474
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.617023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         3215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0240
_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)+(0.0274P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0542
_reflns_number_gt                2642
_reflns_number_total             3215
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062168csi20070112_023228_5.cif
_cod_data_source_block           Compound_6a_(lc36am)
_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_original_cell_volume        4480(4)
_cod_database_code               4307689
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.085687(8) 0.66878(2) 0.215125(11) 0.04181(9) Uani 1 1 d . . .
N1 N 0.10026(17) 0.5484(4) 0.3157(2) 0.0397(9) Uani 1 1 d . . .
N2 N 0.13959(17) 0.7934(4) 0.3294(2) 0.0404(10) Uani 1 1 d . . .
N3 N 0.1234(2) 0.2166(4) 0.2277(3) 0.0574(12) Uani 1 1 d . . .
C1 C 0.0120(2) 0.7527(6) 0.1754(3) 0.0525(14) Uani 1 1 d . . .
O1 O -0.03228(18) 0.8087(4) 0.1488(3) 0.0793(13) Uani 1 1 d . . .
C2 C 0.0841(2) 0.7815(6) 0.1374(3) 0.0534(14) Uani 1 1 d . . .
O2 O 0.08224(19) 0.8519(4) 0.0912(3) 0.0785(13) Uani 1 1 d . . .
C3 C 0.0363(3) 0.5413(6) 0.1251(3) 0.0573(15) Uani 1 1 d . . .
O3 O 0.0048(2) 0.4629(4) 0.0742(3) 0.0874(14) Uani 1 1 d . . .
C4 C 0.1941(2) 0.5700(4) 0.2318(3) 0.0412(12) Uani 1 1 d . . .
O4 O 0.17201(14) 0.5808(3) 0.27008(18) 0.0458(8) Uani 1 1 d . . .
C5 C 0.2542(2) 0.5012(6) 0.2823(3) 0.0491(12) Uani 1 1 d . . .
H5 H 0.2854 0.5423 0.2870 0.059 Uiso 1 1 calc R . .
O5 O 0.17181(19) 0.6122(4) 0.1607(2) 0.0688(11) Uani 1 1 d . . .
C6 C 0.2660(2) 0.3868(6) 0.3205(3) 0.0528(13) Uani 1 1 d . . .
H6 H 0.3048 0.3514 0.3501 0.063 Uiso 1 1 calc R . .
O6 O 0.2271(2) 0.2798(5) 0.3808(3) 0.0908(15) Uani 1 1 d . . .
C7 C 0.2212(3) 0.3112(5) 0.3192(4) 0.0565(15) Uani 1 1 d . . .
O7 O 0.17249(16) 0.2811(3) 0.2367(2) 0.0541(9) Uani 1 1 d . . .
C8 C 0.0807(3) 0.1874(5) 0.1493(4) 0.0556(14) Uani 1 1 d . . .
C9 C 0.0256(3) 0.1249(6) 0.1310(4) 0.0754(18) Uani 1 1 d . . .
H9A H 0.0331 0.1108 0.1839 0.113 Uiso 1 1 calc R . .
H9B H 0.0174 0.0417 0.1026 0.113 Uiso 1 1 calc R . .
H9C H -0.0089 0.1824 0.0947 0.113 Uiso 1 1 calc R . .
C10 C 0.0807(3) 0.2107(7) 0.0770(4) 0.084(2) Uani 1 1 d . . .
H10A H 0.0885 0.3026 0.0753 0.126 Uiso 1 1 calc R . .
H10B H 0.0417 0.1867 0.0240 0.126 Uiso 1 1 calc R . .
H10C H 0.1119 0.1578 0.0848 0.126 Uiso 1 1 calc R . .
C11 C 0.0823(2) 0.4241(5) 0.3088(3) 0.0538(14) Uani 1 1 d . . .
H11 H 0.0589 0.3834 0.2553 0.065 Uiso 1 1 calc R . .
C12 C 0.0972(3) 0.3520(5) 0.3793(4) 0.0631(16) Uani 1 1 d . . .
H12 H 0.0853 0.2640 0.3725 0.076 Uiso 1 1 calc R . .
C13 C 0.1291(3) 0.4108(6) 0.4573(4) 0.0609(15) Uani 1 1 d . . .
H13 H 0.1378 0.3647 0.5038 0.073 Uiso 1 1 calc R . .
C14 C 0.1487(2) 0.5412(5) 0.4670(3) 0.0471(13) Uani 1 1 d . . .
C15 C 0.1825(3) 0.6129(7) 0.5461(3) 0.0619(16) Uani 1 1 d . . .
H15 H 0.1923 0.5714 0.5946 0.074 Uiso 1 1 calc R . .
C16 C 0.2002(3) 0.7379(7) 0.5522(3) 0.0619(16) Uani 1 1 d . . .
H16 H 0.2223 0.7813 0.6048 0.074 Uiso 1 1 calc R . .
C17 C 0.1859(2) 0.8059(5) 0.4796(3) 0.0511(14) Uani 1 1 d . . .
C18 C 0.2017(3) 0.9384(6) 0.4813(4) 0.0637(16) Uani 1 1 d . . .
H18 H 0.2230 0.9870 0.5319 0.076 Uiso 1 1 calc R . .
C19 C 0.1858(3) 0.9953(6) 0.4086(4) 0.0668(16) Uani 1 1 d . . .
H19 H 0.1951 1.0836 0.4087 0.080 Uiso 1 1 calc R . .
C20 C 0.1556(2) 0.9202(5) 0.3344(4) 0.0537(14) Uani 1 1 d . . .
H20 H 0.1459 0.9599 0.2856 0.064 Uiso 1 1 calc R . .
C21 C 0.1540(2) 0.7385(5) 0.4012(3) 0.0393(11) Uani 1 1 d . . .
C22 C 0.1342(2) 0.6058(5) 0.3950(3) 0.0356(11) Uani 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'
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 C2 86.9(2) . . ?
C1 Re1 C3 87.5(2) . . ?
C2 Re1 C3 90.0(2) . . ?
C1 Re1 O4 175.27(16) . . ?
C2 Re1 O4 95.25(17) . . ?
C3 Re1 O4 96.74(19) . . ?
C1 Re1 N1 98.36(18) . . ?
C2 Re1 N1 172.35(18) . . ?
C3 Re1 N1 95.72(19) . . ?
O4 Re1 N1 79.10(13) . . ?
C1 Re1 N2 91.79(18) . . ?
C2 Re1 N2 99.1(2) . . ?
C3 Re1 N2 170.77(18) . . ?
O4 Re1 N2 83.72(13) . . ?
N1 Re1 N2 75.29(15) . . ?
C11 N1 C22 117.4(4) . . ?
C11 N1 Re1 126.9(3) . . ?
C22 N1 Re1 115.6(3) . . ?
C20 N2 C21 117.0(4) . . ?
C20 N2 Re1 127.4(3) . . ?
C21 N2 Re1 115.3(3) . . ?
C8 N3 O7 110.1(4) . . ?
O1 C1 Re1 176.1(5) . . ?
O2 C2 Re1 177.9(5) . . ?
O3 C3 Re1 174.6(5) . . ?
O5 C4 O4 126.7(5) . . ?
O5 C4 C5 118.6(5) . . ?
O4 C4 C5 114.7(4) . . ?
C4 O4 Re1 124.6(3) . . ?
C6 C5 C4 124.5(5) . . ?
C5 C6 C7 123.7(5) . . ?
O6 C7 O7 125.3(6) . . ?
O6 C7 C6 125.3(5) . . ?
O7 C7 C6 109.4(5) . . ?
C7 O7 N3 113.8(4) . . ?
N3 C8 C10 126.1(5) . . ?
N3 C8 C9 115.1(5) . . ?
C10 C8 C9 118.7(5) . . ?
N1 C11 C12 122.5(5) . . ?
C13 C12 C11 119.9(5) . . ?
C12 C13 C14 119.2(5) . . ?
C13 C14 C22 118.0(5) . . ?
C13 C14 C15 124.0(5) . . ?
C22 C14 C15 118.1(5) . . ?
C16 C15 C14 121.8(5) . . ?
C15 C16 C17 121.2(5) . . ?
C21 C17 C18 117.1(5) . . ?
C21 C17 C16 119.0(5) . . ?
C18 C17 C16 123.9(5) . . ?
C19 C18 C17 119.7(5) . . ?
C18 C19 C20 119.3(5) . . ?
N2 C20 C19 123.5(5) . . ?
N2 C21 C17 123.3(5) . . ?
N2 C21 C22 117.3(4) . . ?
C17 C21 C22 119.3(4) . . ?
N1 C22 C14 122.9(4) . . ?
N1 C22 C21 116.4(4) . . ?
C14 C22 C21 120.6(4) . . ?
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 1.901(6) . ?
Re1 C2 1.918(6) . ?
Re1 C3 1.919(6) . ?
Re1 O4 2.140(3) . ?
Re1 N1 2.170(4) . ?
Re1 N2 2.181(4) . ?
N1 C11 1.330(6) . ?
N1 C22 1.366(6) . ?
N2 C20 1.341(6) . ?
N2 C21 1.352(6) . ?
N3 C8 1.272(6) . ?
N3 O7 1.443(5) . ?
C1 O1 1.156(6) . ?
C2 O2 1.148(6) . ?
C3 O3 1.146(6) . ?
C4 O5 1.219(5) . ?
C4 O4 1.277(5) . ?
C4 C5 1.491(7) . ?
C5 C6 1.309(7) . ?
C6 C7 1.473(8) . ?
O6 C7 1.190(6) . ?
C7 O7 1.358(6) . ?
C8 C10 1.483(8) . ?
C8 C9 1.500(8) . ?
C11 C12 1.402(7) . ?
C12 C13 1.356(8) . ?
C13 C14 1.395(7) . ?
C14 C22 1.396(6) . ?
C14 C15 1.431(7) . ?
C15 C16 1.335(8) . ?
C16 C17 1.425(7) . ?
C17 C21 1.402(6) . ?
C17 C18 1.406(7) . ?
C18 C19 1.359(8) . ?
C19 C20 1.385(7) . ?
C21 C22 1.428(7) . ?
