#------------------------------------------------------------------------------
#$Date: 2016-02-19 15:29:56 +0100 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/65/2006518.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2006518
loop_
_publ_author_name
'Velichka Velikova'
'Rosica Petrova'
'Olyana Angelova'
_publ_section_title
;
 <i>N</i>-(2-Pyridinium)urea Perrhenate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1230
_journal_page_last               1232
_journal_paper_doi               10.1107/S0108270197004794
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C6 H8 N3 O+.Re O4-'
_chemical_formula_sum            'C6 H8 N3 O5 Re'
_chemical_formula_weight         400.35
_chemical_name_systematic        'N-(2-pyridinium)urea perrhenate'
_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_type_scat_source
'as coded in SDP/PDP User's Guide (Enraf-Nonius, 1985)'
_cell_angle_alpha                74.61(3)
_cell_angle_beta                 84.65(2)
_cell_angle_gamma                86.42(5)
_cell_formula_units_Z            2
_cell_length_a                   5.2150(10)
_cell_length_b                   9.167(3)
_cell_length_c                   10.597(4)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    292
_cell_measurement_theta_max      21.63
_cell_measurement_theta_min      19.99
_cell_volume                     485.9(3)
_computing_data_collection       'CAD4 Manual (Enraf-Nonius, 1988)'
_computing_data_reduction        'SDP/PDP User's Guide (Enraf-Nonius, 1985)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'KAPPA (Mac\'i\<cek, 1992; Unpublished)'
_computing_structure_refinement  'SDP/PDP User's Guide'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      292
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w/\q
_diffrn_radiation_monochromator  'graphite (perpendicular mode)'
_diffrn_radiation_source         '2kW fine focus Philips tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3110
_diffrn_reflns_reduction_process
'F~obs~ = ( I~raw~/LP )^1/2^, where LP = Lorentz-polarization correction'
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         0.0
_diffrn_standards_decay_%        6.8
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.68
_exptl_absorpt_correction_T_max  0.123
_exptl_absorpt_correction_T_min  0.104
_exptl_absorpt_correction_type
'empirical based on \y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.735
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.165
_exptl_crystal_size_rad          0.132
_refine_diff_density_max         2.3
_refine_diff_density_min         -2.3
_refine_ls_extinction_coef       0.17783E-5
_refine_ls_extinction_method     'Stout & Jensen (1968) formula 17.16'
_refine_ls_goodness_of_fit_all   1.658
_refine_ls_goodness_of_fit_obs   1.180
_refine_ls_hydrogen_treatment    'H atoms constrained'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2604
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.051
_refine_ls_R_factor_obs          .045
_refine_ls_shift/esd_max         0.036
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     '1/[\s^2^(F) + (0.065F)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.115
_refine_ls_wR_factor_obs         .081
_reflns_number_observed          2604
_reflns_number_total             2825
_reflns_observed_criterion       'I > 2.0\s(I)'
_cod_data_source_file            mu1281.cif
_cod_data_source_block           LRSA0234
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        486.0(7)
_cod_database_code               2006518
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Re1 .03670(10) .03410(10) .02990(10) -.00980(10) .00480(10) -.01500(10)
O11 .036(3) .101(5) .065(4) -.015(3) .014(3) -.040(3)
O12 .075(5) .101(6) .043(4) -.029(5) -.006(4) -.007(4)
O13 .053(3) .047(3) .054(3) -.011(3) .015(3) -.029(2)
O14 .091(6) .039(3) .055(4) -.010(4) .003(4) -.015(3)
O1 .049(3) .038(3) .051(3) -.018(2) .021(3) -.020(2)
N1 .045(3) .037(3) .030(3) -.011(3) .009(3) -.012(2)
N2 .051(5) .040(3) .033(3) .001(3) .000(3) -.016(2)
N3 .043(4) .080(5) .050(4) -.017(3) .003(3) -.033(3)
C1 .036(3) .050(4) .034(3) .008(3) -.009(3) -.018(3)
C2 .032(3) .038(3) .031(3) -.017(2) -.004(2) -.011(2)
C3 .039(3) .031(3) .044(4) -.010(3) -.016(3) -.004(3)
C4 .045(4) .048(4) .046(5) -.015(4) -.008(4) .003(4)
C5 .036(3) .062(5) .035(4) -.014(4) .001(3) -.002(4)
C6 .048(4) .059(5) .036(4) -.014(4) .012(3) -.018(3)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Re1 .36412(5) .20796(3) .22564(2) .03240(8) Uani ? ?
O11 .0284(15) .2080(11) .2342(9) .065(2) Uani ? ?
O12 .4599(19) .1363(12) .3751(8) .074(3) Uani ? ?
O13 .4826(15) .0999(8) .1228(7) .049(2) Uani ? ?
O14 .4573(19) .3896(9) .1687(8) .061(2) Uani ? ?
O1 .7225(13) .4544(7) .6135(7) .045(2) Uani ? ?
N1 .3287(15) .3624(8) .7757(7) .037(2) Uani ? ?
N2 .5012(16) .2495(9) .6095(7) .040(2) Uani ? ?
N3 .8387(17) .3383(12) .4542(9) .054(2) Uani ? ?
C1 .6963(16) .3502(10) .5609(8) .038(2) Uani ? ?
C2 .3267(14) .2487(9) .7110(7) .033(2) Uani ? ?
C3 .1350(15) .1472(9) .7506(9) .037(2) Uani ? ?
C4 -.0402(19) .1537(12) .8517(10) .048(2) Uani ? ?
C5 -.0422(17) .2696(12) .9140(9) .046(2) Uani ? ?
C6 .1530(19) .3673(12) .8783(9) .047(2) Uani ? ?
HN1 .4576 .4355 .7489 .0569 Uiso calc N1
HN2 .4943 .1700 .5680 .0569 Uiso calc N2
HN31 .8083 .2565 .4188 .0569 Uiso calc N3
HN32 .9740 .4046 .4157 .0569 Uiso calc N3
H3 .1265 .0698 .7067 .0569 Uiso calc C3
H4 -.1650 .0782 .8807 .0569 Uiso calc C4
H5 -.1720 .2773 .9812 .0569 Uiso calc C5
H6 .1617 .4452 .9214 .0569 Uiso calc C6
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
Re -1.598 7.232
O 0.008 0.006
N 0.004 0.003
C 0.002 0.002
H 0.000 0.000
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 3 0
1 3 2
2 -1 -2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O11 Re1 O12 1 1 108.8(4) yes
O11 Re1 O13 1 1 107.8(4) yes
O11 Re1 O14 1 1 108.6(5) yes
O12 Re1 O13 1 1 110.9(5) yes
O12 Re1 O14 1 1 109.2(5) yes
O13 Re1 O14 1 1 111.5(4) yes
C2 N1 C6 1 1 120.9(8) yes
C2 N1 HN1 1 1 119.07 no
C6 N1 HN1 1 1 120.03 no
C1 N2 C2 1 1 127.5(9) yes
C1 N2 HN2 1 1 116.08 no
C2 N2 HN2 1 1 116.43 no
C1 N3 HN32 1 1 122.34 no
C1 N3 HN31 1 1 117.57 no
HN31 N3 HN32 1 1 120.00 no
O1 C1 N2 1 1 119.6(8) yes
O1 C1 N3 1 1 121.8(9) yes
N2 C1 N3 1 1 118.4(9) yes
N1 C2 N2 1 1 118.8(7) yes
N1 C2 C3 1 1 117.4(7) yes
N2 C2 C3 1 1 123.7(9) yes
C2 C3 C4 1 1 121.3(9) yes
C2 C3 H3 1 1 119.17 no
C4 C3 H3 1 1 119.47 no
C3 C4 C5 1 1 121.2(9) yes
C3 C4 H4 1 1 119.73 no
C5 C4 H4 1 1 119.08 no
C4 C5 C6 1 1 117.5(9) yes
C4 C5 H5 1 1 120.95 no
C6 C5 H5 1 1 121.52 no
N1 C6 C5 1 1 121.3(1.1) yes
N1 C6 H6 1 1 118.78 no
C5 C6 H6 1 1 119.75 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Re1 O11 . 1 1.745(8) yes
Re1 O12 . 1 1.657(9) yes
Re1 O13 . 1 1.709(8) yes
Re1 O14 . 1 1.699(8) yes
O1 C1 . 1 1.247(13) yes
N1 C2 . 1 1.392(12) yes
N1 C6 . 1 1.364(12) yes
N1 HN1 . 1 .950 no
N2 C1 . 1 1.386(11) yes
N2 C2 . 1 1.341(11) yes
N2 HN2 . 1 .950 no
N3 C1 . 1 1.319(12) yes
N3 HN31 . 1 .950 no
N3 HN32 . 1 .950 no
C2 C3 . 1 1.368(11) yes
C3 C4 . 1 1.353(13) yes
C3 H3 . 1 .950 no
C4 C5 . 1 1.391(17) yes
C4 H4 . 1 .950 no
C5 C6 . 1 1.358(14) yes
C5 H5 . 1 .950 no
C6 H6 . 1 .950 no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
C6 N1 C2 N2 179.2(8) no
C6 N1 C2 C3 3.0(10) no
C2 N1 C6 C5 -6.0(10) no
C2 N2 C1 O1 .0(10) no
C2 N2 C1 N3 -175.6(9) no
C1 N2 C2 N1 2.0(10) no
C1 N2 C2 C3 178.1(8) no
N1 C2 C3 C4 -2.0(10) no
N2 C2 C3 C4 -178.3(9) no
C2 C3 C4 C5 4.0(10) no
C3 C4 C5 C6 -6.0(10) no
C4 C5 C6 N1 7.0(10) no