#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:36:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179118 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/80/4308040.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_4308040
loop_
_publ_author_name
'Sonia Nieto'
'Julio Pérez'
'Lucía Riera'
'Víctor Riera'
'Daniel Miguel'
'James A. Golen'
'Arnold L. Rheingold'
_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@uniovi.es
_publ_contact_author_fax         +34-85-103446
_publ_contact_author_phone       +34-85-102985
_publ_section_title
;
Pyrazole Complexes as Anion Receptors: Effects of Changing the Metal, the
Pyrazole Substitution Pattern, and the Number of Pyrazole Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3407
_journal_page_last               3418
_journal_paper_doi               10.1021/ic0700046
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C11 H8 F3 N2 O8 Re S'
_chemical_formula_weight         571.45
_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                 92.686(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.407(5)
_cell_length_b                   18.291(10)
_cell_length_c                   10.210(6)
_cell_measurement_temperature    296(2)
_cell_volume                     1754.8(17)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7596
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    7.116
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.405029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.007
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0070(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0282
_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)+(0.0496P)²+0.3043P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0806
_reflns_number_gt                1958
_reflns_number_total             2518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0700046si20070102_075057_08.cif
_cod_data_source_block           Compound_9_(lr51bm)
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1754.9(17)
_cod_database_code               4308040
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 0.24772(2) 0.161044(12) 0.751260(18) 0.03711(16) Uani 1 1 d . . .
C1 C 0.2546(6) 0.2490(4) 0.8697(6) 0.0444(14) Uani 1 1 d . . .
O1 O 0.2608(5) 0.2999(3) 0.9298(4) 0.0628(12) Uani 1 1 d . . .
C2 C 0.3735(8) 0.1036(4) 0.8772(6) 0.0478(15) Uani 1 1 d . . .
O2 O 0.4506(6) 0.0717(3) 0.9397(5) 0.0802(16) Uani 1 1 d . . .
C3 C 0.4199(7) 0.1951(4) 0.6699(6) 0.0522(16) Uani 1 1 d . . .
O3 O 0.5222(6) 0.2138(3) 0.6266(5) 0.0851(17) Uani 1 1 d . . .
C4 C 0.1319(7) 0.2205(3) 0.6176(6) 0.0475(15) Uani 1 1 d . . .
O4 O 0.0771(5) 0.2565(3) 0.5422(4) 0.0714(14) Uani 1 1 d . . .
C5 C 0.2361(8) 0.0726(4) 0.6347(6) 0.0498(16) Uani 1 1 d . . .
O5 O 0.2295(6) 0.0219(3) 0.5742(4) 0.0771(15) Uani 1 1 d . . .
N1 N 0.0604(5) 0.1231(3) 0.8499(4) 0.0390(11) Uani 1 1 d . . .
N2 N 0.0624(5) 0.1194(3) 0.9827(4) 0.0385(11) Uani 1 1 d . . .
H2 H 0.129(5) 0.126(3) 1.032(5) 0.029(16) Uiso 1 1 d . . .
C11 C -0.0620(7) 0.0961(3) 1.0259(7) 0.0456(16) Uani 1 1 d . . .
C12 C -0.1470(7) 0.0843(3) 0.9177(7) 0.0587(19) Uani 1 1 d . . .
H12 H -0.2404 0.0674 0.9160 0.070 Uiso 1 1 calc R . .
C13 C -0.0706(7) 0.1018(3) 0.8108(6) 0.0504(16) Uani 1 1 d . . .
C14 C -0.0809(10) 0.0871(4) 1.1682(8) 0.080(3) Uani 1 1 d . . .
H14A H -0.0858 0.0360 1.1890 0.120 Uiso 1 1 calc R . .
H14B H -0.1674 0.1107 1.1913 0.120 Uiso 1 1 calc R . .
H14C H -0.0018 0.1089 1.2166 0.120 Uiso 1 1 calc R . .
C15 C -0.1191(8) 0.1000(5) 0.6698(7) 0.090(3) Uani 1 1 d . . .
H15A H -0.1338 0.1491 0.6387 0.136 Uiso 1 1 calc R . .
H15B H -0.2067 0.0732 0.6601 0.136 Uiso 1 1 calc R . .
H15C H -0.0480 0.0767 0.6199 0.136 Uiso 1 1 calc R . .
S1 S 0.32974(19) 0.16261(9) 1.28026(16) 0.0517(5) Uani 1 1 d . . .
O11 O 0.2948(6) 0.1610(3) 1.1426(5) 0.0695(16) Uani 1 1 d . . .
O12 O 0.4177(7) 0.2228(2) 1.3206(5) 0.0911(18) Uani 1 1 d . . .
O13 O 0.2166(7) 0.1448(4) 1.3619(6) 0.0909(19) Uani 1 1 d . . .
C21 C 0.4502(8) 0.0866(3) 1.3039(7) 0.0571(19) Uani 1 1 d . . .
F1 F 0.5635(5) 0.0933(2) 1.2334(5) 0.0902(15) Uani 1 1 d . . .
F2 F 0.3911(5) 0.0243(2) 1.2671(5) 0.1093(17) Uani 1 1 d . . .
F3 F 0.4934(6) 0.0796(2) 1.4277(5) 0.0899(16) 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
C3 Re1 C2 87.9(3) . . ?
C3 Re1 C5 91.6(3) . . ?
C2 Re1 C5 88.4(2) . . ?
C3 Re1 C1 89.8(3) . . ?
C2 Re1 C1 91.8(2) . . ?
C5 Re1 C1 178.5(2) . . ?
C3 Re1 C4 88.4(3) . . ?
C2 Re1 C4 176.3(2) . . ?
C5 Re1 C4 91.2(2) . . ?
C1 Re1 C4 88.7(2) . . ?
C3 Re1 N1 177.64(19) . . ?
C2 Re1 N1 90.1(2) . . ?
C5 Re1 N1 89.7(2) . . ?
C1 Re1 N1 88.9(2) . . ?
C4 Re1 N1 93.5(2) . . ?
O1 C1 Re1 176.2(5) . . ?
O2 C2 Re1 174.6(6) . . ?
O3 C3 Re1 177.5(6) . . ?
O4 C4 Re1 174.6(6) . . ?
O5 C5 Re1 177.3(5) . . ?
C13 N1 N2 104.7(5) . . ?
C13 N1 Re1 135.1(4) . . ?
N2 N1 Re1 120.2(3) . . ?
C11 N2 N1 111.9(5) . . ?
N2 C11 C12 106.0(6) . . ?
N2 C11 C14 120.3(6) . . ?
C12 C11 C14 133.7(7) . . ?
C11 C12 C13 107.5(6) . . ?
N1 C13 C12 109.9(5) . . ?
N1 C13 C15 122.1(6) . . ?
C12 C13 C15 128.0(6) . . ?
O13 S1 O12 116.6(4) . . ?
O13 S1 O11 115.4(3) . . ?
O12 S1 O11 113.8(3) . . ?
O13 S1 C21 103.2(4) . . ?
O12 S1 C21 101.8(3) . . ?
O11 S1 C21 103.3(3) . . ?
F2 C21 F3 107.3(6) . . ?
F2 C21 F1 105.4(6) . . ?
F3 C21 F1 108.2(6) . . ?
F2 C21 S1 112.0(5) . . ?
F3 C21 S1 111.6(5) . . ?
F1 C21 S1 112.0(5) . . ?
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 1.957(7) . ?
Re1 C2 2.005(7) . ?
Re1 C5 2.009(7) . ?
Re1 C1 2.011(7) . ?
Re1 C4 2.023(7) . ?
Re1 N1 2.183(4) . ?
C1 O1 1.116(6) . ?
C2 O2 1.108(7) . ?
C3 O3 1.131(8) . ?
C4 O4 1.121(7) . ?
C5 O5 1.114(7) . ?
N1 C13 1.336(7) . ?
N1 N2 1.357(6) . ?
N2 C11 1.340(8) . ?
C11 C12 1.350(9) . ?
C11 C14 1.482(10) . ?
C12 C13 1.373(9) . ?
C13 C15 1.489(9) . ?
S1 O13 1.420(6) . ?
S1 O12 1.426(5) . ?
S1 O11 1.429(6) . ?
S1 C21 1.802(7) . ?
C21 F2 1.315(7) . ?
C21 F3 1.316(8) . ?
C21 F1 1.319(9) . ?
