#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:20:18 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/03/4350352.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_4350352
loop_
_publ_author_name
'Arroyo, Marta'
'Miguel, Daniel'
'Villafañe, Fernando'
'Nieto, Sonia'
'Pérez, Julio'
'Riera, Lucía'
_publ_section_title
;
 Rhenium-mediated coupling of acetonitrile and pyrazoles. New molecular
 clefts for anion binding.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7018
_journal_page_last               7026
_journal_paper_doi               10.1021/ic0607078
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C12 H14 Cl N4 O7 Re'
_chemical_formula_weight         547.92
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                84.399(4)
_cell_angle_beta                 87.253(4)
_cell_angle_gamma                77.109(4)
_cell_formula_units_Z            2
_cell_length_a                   8.2464(16)
_cell_length_b                   9.2149(18)
_cell_length_c                   12.074(2)
_cell_measurement_temperature    296(2)
_cell_volume                     889.8(3)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3981
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    7.020
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.444946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.994
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       0.0003(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0369
_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)+(0.0845P)²+0.0839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1007
_reflns_number_gt                2409
_reflns_number_total             2531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0607078si20060426_072212.cif
_cod_data_source_block           Compound_9_ma2091am
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4350352
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
Re1 Re 0.25883(3) 0.15141(2) 0.157719(17) 0.03489(19) Uani 1 1 d .
N1 N 0.0551(7) 0.3465(6) 0.1661(5) 0.0367(14) Uani 1 1 d .
N2 N -0.0910(6) 0.3168(6) 0.2132(4) 0.0347(12) Uani 1 1 d .
N3 N 0.0510(8) 0.0767(7) 0.2374(5) 0.0390(14) Uani 1 1 d .
H3 H 0.0609 -0.0160 0.2608 0.047 Uiso 1 1 calc R
N4 N 0.3000(8) 0.2092(8) 0.3199(6) 0.0451(16) Uani 1 1 d .
C1 C 0.2040(11) 0.0965(11) 0.0175(7) 0.050(2) Uani 1 1 d .
O1 O 0.1694(9) 0.0571(8) -0.0641(5) 0.0696(18) Uani 1 1 d .
C2 C 0.4310(12) 0.2434(10) 0.0828(7) 0.054(2) Uani 1 1 d .
O2 O 0.5311(8) 0.2909(8) 0.0340(6) 0.0756(19) Uani 1 1 d .
C3 C 0.4179(12) -0.0339(11) 0.1775(8) 0.049(2) Uani 1 1 d .
O3 O 0.5160(9) -0.1447(8) 0.1924(6) 0.0749(19) Uani 1 1 d .
C4 C -0.0880(8) 0.1693(7) 0.2504(5) 0.0326(14) Uani 1 1 d .
C5 C -0.2392(9) 0.1218(9) 0.2995(7) 0.0499(18) Uani 1 1 d .
H5A H -0.2157 0.0149 0.3138 0.075 Uiso 1 1 calc R
H5B H -0.3286 0.1531 0.2483 0.075 Uiso 1 1 calc R
H5C H -0.2709 0.1667 0.3680 0.075 Uiso 1 1 calc R
C6 C 0.3088(10) 0.2368(9) 0.4089(7) 0.0459(19) Uani 1 1 d .
C7 C 0.3241(12) 0.2695(13) 0.5234(7) 0.070(3) Uani 1 1 d .
H7A H 0.4341 0.2836 0.5334 0.106 Uiso 1 1 calc R
H7B H 0.3041 0.1876 0.5737 0.106 Uiso 1 1 calc R
H7C H 0.2440 0.3588 0.5384 0.106 Uiso 1 1 calc R
C11 C 0.0321(10) 0.4924(8) 0.1485(6) 0.0406(17) Uani 1 1 d .
C12 C -0.1298(9) 0.5597(7) 0.1844(6) 0.0443(17) Uani 1 1 d .
H12 H -0.1761 0.6617 0.1810 0.053 Uiso 1 1 calc R
C13 C -0.2065(9) 0.4480(8) 0.2250(6) 0.0409(16) Uani 1 1 d .
C14 C 0.1660(10) 0.5684(8) 0.1009(7) 0.0504(18) Uani 1 1 d .
H14A H 0.2244 0.5148 0.0414 0.076 Uiso 1 1 calc R
H14B H 0.2425 0.5701 0.1580 0.076 Uiso 1 1 calc R
H14C H 0.1169 0.6689 0.0728 0.076 Uiso 1 1 calc R
C15 C -0.3778(10) 0.4647(10) 0.2736(8) 0.057(2) Uani 1 1 d .
H15A H -0.3727 0.4259 0.3504 0.086 Uiso 1 1 calc R
H15B H -0.4391 0.4105 0.2336 0.086 Uiso 1 1 calc R
H15C H -0.4325 0.5686 0.2683 0.086 Uiso 1 1 calc R
Cl1 Cl 0.1637(3) 0.7203(3) 0.41560(17) 0.0642(6) Uani 1 1 d .
O11 O 0.0439(9) 0.7729(7) 0.3332(5) 0.0753(18) Uani 1 1 d .
O12 O 0.2706(15) 0.5901(13) 0.3829(10) 0.178(6) Uani 1 1 d .
O13 O 0.2585(12) 0.8319(14) 0.4221(7) 0.132(4) Uani 1 1 d .
O14 O 0.0860(11) 0.6919(12) 0.5186(6) 0.096(3) 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'
Cl Cl 0.1484 0.1585 '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
C3 Re1 C1 89.2(4)
C3 Re1 C2 89.5(4)
C1 Re1 C2 89.6(4)
C3 Re1 N3 97.4(3)
C1 Re1 N3 90.8(3)
C2 Re1 N3 173.1(3)
C3 Re1 N4 92.2(3)
C1 Re1 N4 175.1(3)
C2 Re1 N4 95.1(3)
N3 Re1 N4 84.3(2)
C3 Re1 N1 168.5(3)
C1 Re1 N1 96.6(3)
C2 Re1 N1 100.4(3)
N3 Re1 N1 72.7(2)
N4 Re1 N1 81.2(2)
C11 N1 N2 106.8(6)
C11 N1 Re1 138.1(5)
N2 N1 Re1 114.7(4)
C13 N2 N1 110.3(5)
C13 N2 C4 132.7(6)
N1 N2 C4 116.4(5)
C4 N3 Re1 120.3(5)
C6 N4 Re1 173.9(7)
O1 C1 Re1 176.6(8)
O2 C2 Re1 175.6(8)
O3 C3 Re1 177.9(9)
N3 C4 N2 115.9(6)
N3 C4 C5 122.5(6)
N2 C4 C5 121.7(6)
N4 C6 C7 178.6(10)
N1 C11 C12 109.7(7)
N1 C11 C14 122.6(7)
C12 C11 C14 127.7(7)
C13 C12 C11 107.6(6)
C12 C13 N2 105.6(6)
C12 C13 C15 127.1(7)
N2 C13 C15 127.2(7)
O12 Cl1 O14 110.7(6)
O12 Cl1 O11 108.5(7)
O14 Cl1 O11 110.4(5)
O12 Cl1 O13 108.7(8)
O14 Cl1 O13 110.3(6)
O11 Cl1 O13 108.2(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 C3 1.909(10)
Re1 C1 1.916(9)
Re1 C2 1.954(10)
Re1 N3 2.139(6)
Re1 N4 2.141(7)
Re1 N1 2.176(6)
N1 C11 1.312(10)
N1 N2 1.379(8)
N2 C13 1.377(9)
N2 C4 1.384(8)
N3 C4 1.280(9)
N4 C6 1.137(11)
C1 O1 1.152(11)
C2 O2 1.133(11)
C3 O3 1.157(12)
C4 C5 1.490(9)
C6 C7 1.460(12)
C11 C12 1.408(11)
C11 C14 1.498(11)
C12 C13 1.364(11)
C13 C15 1.485(10)
Cl1 O12 1.400(10)
Cl1 O14 1.401(8)
Cl1 O11 1.410(6)
Cl1 O13 1.433(10)
