#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:39:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179758 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/54/7005463.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_7005463
loop_
_publ_author_name
'Alvarez, Celedonio M.'
'García-Rodríguez, Raúl'
'Miguel, Daniel'
_publ_section_title
;
 Pyridine-2-carboxaldehyde as ligand: synthesis and derivatization of
 carbonyl complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3546
_journal_page_last               3554
_journal_paper_doi               10.1039/b702418e
_journal_year                    2007
_chemical_formula_sum            'C10 H5 F3 N O7 Re S'
_chemical_formula_weight         526.41
_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                70.449(14)
_cell_angle_beta                 72.368(15)
_cell_angle_gamma                74.795(16)
_cell_formula_units_Z            2
_cell_length_a                   8.547(7)
_cell_length_b                   8.892(7)
_cell_length_c                   10.399(9)
_cell_measurement_temperature    298(2)
_cell_volume                     698.3(10)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3158
_diffrn_reflns_theta_full        23.52
_diffrn_reflns_theta_max         23.52
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    8.923
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.453241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    2.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         7.012
_refine_diff_density_min         -5.296
_refine_diff_density_rms         0.636
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0905
_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)+(0.1794P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2266
_reflns_number_gt                1694
_reflns_number_total             2008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702418e.txt
_cod_data_source_block           Compound_3c_rg412am
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        698.2(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7005463
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 0.74210(9) 0.76032(10) 0.84825(7) 0.0307(5) Uani 1 1 d . . .
N1 N 0.662(2) 0.741(2) 0.6755(19) 0.034(4) Uani 1 1 d . . .
C1 C 0.697(3) 0.556(3) 0.965(2) 0.036(5) Uani 1 1 d . . .
O1 O 0.668(3) 0.432(2) 1.042(2) 0.063(6) Uani 1 1 d . . .
C2 C 0.780(3) 0.792(3) 1.005(3) 0.045(6) Uani 1 1 d . . .
O2 O 0.792(3) 0.803(2) 1.112(2) 0.065(6) Uani 1 1 d . . .
C3 C 0.975(3) 0.656(3) 0.808(2) 0.038(6) Uani 1 1 d . . .
O3 O 1.102(2) 0.593(2) 0.780(2) 0.057(5) Uani 1 1 d . . .
O4 O 0.4845(16) 0.8835(18) 0.8705(14) 0.031(3) Uani 1 1 d . . .
C11 C 0.750(3) 0.675(3) 0.574(2) 0.034(5) Uani 1 1 d . . .
H11 H 0.8614 0.6306 0.5727 0.041 Uiso 1 1 calc R . .
C12 C 0.690(4) 0.668(4) 0.473(3) 0.079(11) Uani 1 1 d . . .
H12 H 0.7602 0.6250 0.4017 0.095 Uiso 1 1 calc R . .
C13 C 0.520(3) 0.727(3) 0.475(2) 0.046(6) Uani 1 1 d . . .
H13 H 0.4732 0.7143 0.4100 0.055 Uiso 1 1 calc R . .
C14 C 0.428(3) 0.802(3) 0.575(2) 0.040(5) Uani 1 1 d . . .
H14 H 0.3166 0.8486 0.5768 0.048 Uiso 1 1 calc R . .
C15 C 0.500(3) 0.809(3) 0.672(2) 0.032(5) Uani 1 1 d . . .
C16 C 0.413(3) 0.885(3) 0.787(2) 0.036(5) Uani 1 1 d . . .
H16 H 0.3012 0.9348 0.7941 0.043 Uiso 1 1 calc R . .
C10 C 0.823(3) 1.221(3) 0.788(3) 0.050(6) Uani 1 1 d . . .
O11 O 0.7690(19) 1.0004(19) 0.7092(17) 0.040(4) Uani 1 1 d . . .
O12 O 1.0550(19) 1.016(2) 0.6851(16) 0.053(5) Uani 1 1 d . . .
O13 O 0.889(2) 1.219(2) 0.5330(17) 0.057(5) Uani 1 1 d . . .
S1 S 0.8969(7) 1.1027(7) 0.6638(5) 0.0339(13) Uani 1 1 d . . .
F1 F 0.669(2) 1.294(2) 0.796(2) 0.074(5) Uani 1 1 d . . .
F2 F 0.838(2) 1.1270(19) 0.9175(14) 0.058(4) Uani 1 1 d . . .
F3 F 0.9162(19) 1.3357(18) 0.7516(16) 0.059(4) 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'
F F 0.0171 0.0103 '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 86.7(10) . . ?
C2 Re1 C3 87.6(11) . . ?
C1 Re1 C3 86.7(9) . . ?
C2 Re1 O11 96.8(8) . . ?
C1 Re1 O11 174.0(7) . . ?
C3 Re1 O11 98.3(7) . . ?
C2 Re1 O4 97.6(9) . . ?
C1 Re1 O4 96.4(8) . . ?
C3 Re1 O4 174.1(7) . . ?
O11 Re1 O4 78.4(5) . . ?
C2 Re1 N1 171.9(9) . . ?
C1 Re1 N1 93.8(8) . . ?
C3 Re1 N1 100.5(9) . . ?
O11 Re1 N1 82.1(6) . . ?
O4 Re1 N1 74.3(6) . . ?
C11 N1 C15 116.4(19) . . ?
C11 N1 Re1 128.7(14) . . ?
C15 N1 Re1 114.9(14) . . ?
O1 C1 Re1 177(2) . . ?
O2 C2 Re1 174(2) . . ?
O3 C3 Re1 175(2) . . ?
C16 O4 Re1 117.4(14) . . ?
N1 C11 C12 124(2) . . ?
C11 C12 C13 120(3) . . ?
C14 C13 C12 117(2) . . ?
C13 C14 C15 119(2) . . ?
C14 C15 N1 123(2) . . ?
C14 C15 C16 124(2) . . ?
N1 C15 C16 113.1(18) . . ?
O4 C16 C15 120.3(19) . . ?
F1 C10 F3 108(2) . . ?
F1 C10 F2 109(2) . . ?
F3 C10 F2 107(2) . . ?
F1 C10 S1 113.2(18) . . ?
F3 C10 S1 109.7(17) . . ?
F2 C10 S1 110.5(17) . . ?
S1 O11 Re1 135.0(9) . . ?
O12 S1 O13 118.1(11) . . ?
O12 S1 O11 114.0(10) . . ?
O13 S1 O11 111.7(10) . . ?
O12 S1 C10 104.7(11) . . ?
O13 S1 C10 104.0(12) . . ?
O11 S1 C10 102.0(11) . . ?
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 1.88(2) . ?
Re1 C1 1.88(2) . ?
Re1 C3 1.95(2) . ?
Re1 O11 2.166(15) . ?
Re1 O4 2.167(13) . ?
Re1 N1 2.18(2) . ?
N1 C11 1.31(3) . ?
N1 C15 1.36(3) . ?
C1 O1 1.16(3) . ?
C2 O2 1.19(3) . ?
C3 O3 1.08(3) . ?
O4 C16 1.20(3) . ?
C11 C12 1.32(4) . ?
C12 C13 1.40(4) . ?
C13 C14 1.36(4) . ?
C14 C15 1.36(3) . ?
C15 C16 1.47(3) . ?
C10 F1 1.30(3) . ?
C10 F3 1.34(3) . ?
C10 F2 1.35(3) . ?
C10 S1 1.80(3) . ?
O11 S1 1.472(16) . ?
O12 S1 1.410(17) . ?
O13 S1 1.414(16) . ?
