#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/96/2219666.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_2219666
loop_
_publ_author_name
'Schutte, Marietjie'
'Visser, Hendrik G.'
_publ_section_title
Aquatricarbonyl(4-carboxypyridine-2-carboxylato-κ²N,O²)rhenium(I)
_journal_coeditor_code           NG2479
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1226
_journal_page_last               m1227
_journal_paper_doi               10.1107/S160053680802761X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Re (C7 H4 N O4) (C O)3 (H2 O)]'
_chemical_formula_moiety         'C10 H6 N O8 Re'
_chemical_formula_sum            'C10 H6 N O8 Re'
_chemical_formula_weight         454.37
_chemical_name_systematic
;
Aquatricarbonyl(4-carboxypyridine-2-carboxylato-
κ²N,O²)rhenium(I)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.799(4)
_cell_angle_beta                 107.943(4)
_cell_angle_gamma                111.346(4)
_cell_formula_units_Z            4
_cell_length_a                   9.5024(11)
_cell_length_b                   12.4254(16)
_cell_length_c                   12.4889(16)
_cell_measurement_reflns_used    7140
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.745
_cell_volume                     1220.4(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_computing_molecular_graphics
'DIAMOND (Brandenberg & Putz, 2005) and ORTEP-3 (Farrugia, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_measured_fraction_theta_full 0.96
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15096
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.996
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_correction_T_min  0.140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             848.0
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.208
_refine_diff_density_min         -1.796
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5848
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0251P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.065
_reflns_number_gt                4869
_reflns_number_total             5048
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2479.cif
_cod_data_source_block           I
_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.

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (3 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (3
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2219666
_cod_database_fobs_code          2219666
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
N N1 0.3078(4) 0.2654(3) 0.5400(3) 0.0095(8) Uani d . 1
O O5 0.1030(4) 0.1933(3) 0.3130(2) 0.0113(7) Uani d . 1
O O6 0.2391(4) 0.1072(3) 0.2433(3) 0.0152(7) Uani d . 1
C C4 0.2193(6) 0.1635(4) 0.3289(4) 0.0116(9) Uani d . 1
O O15 0.0841(4) 0.2152(3) -0.1450(3) 0.0112(7) Uani d . 1
C C5 0.3392(6) 0.1998(4) 0.4572(4) 0.0102(9) Uani d . 1
O O16 0.0735(4) 0.0827(3) -0.3002(3) 0.0160(7) Uani d . 1
C C15 0.3019(5) 0.1585(4) -0.1099(4) 0.0097(9) Uani d . 1
C C14 0.1407(6) 0.1487(4) -0.1934(4) 0.0118(10) Uani d . 1
C C18 0.5968(5) 0.1949(4) 0.0518(4) 0.0116(9) Uani d . 1
H H18 0.6981 0.2089 0.1084 0.014 Uiso calc R 1
C C17 0.5336(6) 0.1168(4) -0.0662(4) 0.0115(9) Uani d . 1
C C16 0.3816(5) 0.0981(4) -0.1491(4) 0.0106(9) Uani d . 1
H H16 0.3358 0.0459 -0.2288 0.013 Uiso calc R 1
C C8 0.5409(6) 0.2756(4) 0.6944(4) 0.0127(10) Uani d . 1
H H8 0.6081 0.3019 0.7761 0.015 Uiso calc R 1
C C6 0.4696(6) 0.1716(4) 0.4875(4) 0.0129(10) Uani d . 1
H H6 0.4884 0.1278 0.4282 0.015 Uiso calc R 1
C C9 0.4082(5) 0.3013(4) 0.6568(4) 0.0122(10) Uani d . 1
H H9 0.3874 0.3453 0.7146 0.015 Uiso calc R 1
C C7 0.5727(5) 0.2098(4) 0.6085(4) 0.0105(9) Uani d . 1
C C20 0.6310(6) 0.0551(4) -0.0994(4) 0.0131(10) Uani d . 1
C C19 0.5084(5) 0.2516(4) 0.0845(4) 0.0118(10) Uani d . 1
H H19 0.5507 0.3031 0.1641 0.014 Uiso calc R 1
N N2 0.3633(4) 0.2346(3) 0.0051(3) 0.0092(8) Uani d . 1
O O8 0.7441(4) 0.1233(3) 0.5666(3) 0.0200(8) Uani d . 1
O O7 0.8100(4) 0.2290(3) 0.7589(3) 0.0190(8) Uani d . 1
H H7 0.8878 0.2118 0.773 0.029 Uiso calc R 1
C C10 0.7178(5) 0.1827(4) 0.6423(4) 0.0134(10) Uani d . 1
O O18 0.7570(4) 0.0669(3) -0.0231(3) 0.0174(8) Uani d . 1
O O17 0.5674(4) -0.0113(3) -0.2139(3) 0.0176(8) Uani d . 1
H H17 0.6264 -0.0424 -0.2258 0.026 Uiso calc R 1
O O11 0.4169(4) 0.4220(3) 0.3181(3) 0.0206(8) Uani d . 1
O O12 -0.0486(5) 0.3985(3) 0.0753(3) 0.0290(9) Uani d . 1
C C11 0.3339(6) 0.3833(4) 0.2154(4) 0.0129(10) Uani d . 1
C C12 0.0473(6) 0.3683(4) 0.0652(4) 0.0165(10) Uani d . 1
O O2 -0.2361(5) 0.3030(4) 0.3410(3) 0.0296(10) Uani d . 1
C C2 -0.1119(6) 0.3005(4) 0.3895(4) 0.0178(11) Uani d . 1
C C3 0.2069(6) 0.4532(5) 0.4629(4) 0.0211(12) Uani d . 1
O O3 0.2698(5) 0.5484(3) 0.4535(3) 0.0283(9) Uani d . 1
C C13 0.3283(6) 0.4712(5) 0.0407(4) 0.0162(10) Uani d . 1
O O13 0.4026(4) 0.5690(3) 0.0395(3) 0.0209(8) Uani d . 1
O O14 0.0791(4) 0.1290(3) 0.0380(3) 0.0128(7) Uani d D 1
O O4 -0.0362(4) 0.1106(3) 0.4661(3) 0.0191(8) Uani d D 1
H H4A -0.070(6) 0.046(3) 0.408(3) 0.029 Uiso d D 1
H H4B -0.092(6) 0.097(4) 0.508(4) 0.029 Uiso d D 1
H H14B 0.123(5) 0.112(5) 0.098(3) 0.029 Uiso d D 1
H H14A -0.025(2) 0.093(4) 0.010(4) 0.029 Uiso d D 1
Re Re2 0.20999(2) 0.315032(16) 0.046124(15) 0.00973(6) Uani d . 1
Re Re1 0.09158(2) 0.296297(16) 0.468442(15) 0.01020(6) Uani d . 1
C C1 0.1002(6) 0.3789(5) 0.6194(4) 0.0165(10) Uani d . 1
O O1 0.1138(5) 0.4303(3) 0.7126(3) 0.0272(9) Uani d . 1
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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.231 '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_site_symmetry_1
_geom_angle
_geom_angle_publ_flag
C9 N1 C5 . 117.6(4) ?
C9 N1 Re1 . 126.4(3) ?
C5 N1 Re1 . 115.9(3) ?
C4 O5 Re1 . 118.5(3) ?
O6 C4 O5 1 122.9(4) ?
O6 C4 O5 . 122.9(4) ?
O6 C4 C5 1 119.9(4) ?
O6 C4 C5 . 119.9(4) ?
O5 C4 C5 . 117.2(4) ?
C14 O15 Re2 . 118.6(3) ?
N1 C5 C6 . 123.1(4) ?
N1 C5 C4 . 113.5(4) ?
C6 C5 C4 . 123.3(4) ?
N2 C15 C16 . 122.9(4) ?
N2 C15 C14 . 114.7(4) ?
C16 C15 C14 . 122.3(4) ?
O16 C14 O15 . 124.0(4) ?
O16 C14 C15 . 120.6(4) ?
O15 C14 C15 . 115.4(4) ?
C19 C18 C17 . 119.4(4) ?
C19 C18 H18 . 120.3 ?
C17 C18 H18 . 120.3 ?
C18 C17 C16 . 118.9(4) ?
C18 C17 C20 . 118.5(4) ?
C16 C17 C20 . 122.6(4) ?
C15 C16 C17 . 118.2(4) ?
C15 C16 H16 . 120.9 ?
C17 C16 H16 . 120.9 ?
C9 C8 C7 . 119.0(4) ?
C9 C8 H8 . 120.5 ?
C7 C8 H8 . 120.5 ?
C5 C6 C7 . 118.6(4) ?
C5 C6 H6 . 120.7 ?
C7 C6 H6 . 120.7 ?
N1 C9 C8 . 122.7(4) ?
N1 C9 H9 . 118.7 ?
C8 C9 H9 . 118.7 ?
C6 C7 C8 . 119.0(4) ?
C6 C7 C10 . 119.0(4) ?
C8 C7 C10 . 122.0(4) ?
O18 C20 O17 . 124.8(4) ?
O18 C20 C17 . 120.7(4) ?
O17 C20 C17 . 114.5(4) ?
N2 C19 C18 . 121.8(4) ?
N2 C19 H19 . 119.1 ?
C18 C19 H19 . 119.1 ?
C19 N2 C15 . 118.7(4) ?
C19 N2 Re2 . 125.3(3) ?
C15 N2 Re2 . 115.9(3) ?
C10 O7 H7 . 109.5 ?
O8 C10 O7 . 125.2(4) ?
O8 C10 C7 . 121.8(4) ?
O7 C10 C7 . 113.0(4) ?
C20 O17 H17 . 109.5 ?
O11 C11 Re2 . 175.5(4) ?
O12 C12 Re2 . 179.4(5) ?
O2 C2 Re1 . 179.9(5) ?
O3 C3 Re1 . 176.0(5) ?
O13 C13 Re2 . 178.8(4) ?
Re2 O14 H14B . 116(3) ?
Re2 O14 H14A . 121(3) ?
H14B O14 H14A . 112(3) ?
Re1 O4 H4A . 124(3) ?
Re1 O4 H4B . 121(3) ?
H4A O4 H4B . 110(3) ?
C13 Re2 C11 . 88.2(2) ?
C13 Re2 C12 . 87.6(2) ?
C11 Re2 C12 . 89.52(19) y
C13 Re2 O15 . 97.19(16) ?
C11 Re2 O15 . 170.52(16) y
C12 Re2 O15 . 98.45(16) y
C13 Re2 O14 . 174.48(16) ?
C11 Re2 O14 . 95.63(16) y
C12 Re2 O14 . 96.35(17) y
O15 Re2 O14 . 78.48(12) y
C13 Re2 N2 . 96.92(17) ?
C11 Re2 N2 . 96.70(16) ?
C12 Re2 N2 . 172.39(16) ?
O15 Re2 N2 . 74.98(12) y
O14 Re2 N2 . 78.73(13) ?
C3 Re1 C2 . 88.6(2) ?
C3 Re1 C1 . 88.1(2) ?
C2 Re1 C1 . 88.6(2) ?
C3 Re1 O5 . 95.56(17) ?
C2 Re1 O5 . 98.77(15) y
C1 Re1 O5 . 171.85(16) ?
C3 Re1 O4 . 176.21(16) ?
C2 Re1 O4 . 92.71(18) ?
C1 Re1 O4 . 95.49(17) y
O5 Re1 O4 . 80.73(12) y
C3 Re1 N1 . 96.75(18) ?
C2 Re1 N1 . 171.93(16) ?
C1 Re1 N1 . 97.60(17) ?
O5 Re1 N1 . 74.77(12) y
O4 Re1 N1 . 81.58(14) ?
O1 C1 Re1 . 176.6(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
N1 C9 1.343(5) ?
N1 C5 1.357(5) ?
N1 Re1 2.180(4) y
O5 C4 1.261(5) ?
O5 Re1 2.153(3) y
O6 C4 1.258(5) ?
C4 O6 1.258(5) ?
C4 C5 1.508(6) ?
O15 C14 1.287(5) ?
O15 Re2 2.148(3) y
C5 C6 1.372(6) ?
O16 C14 1.227(5) ?
C15 N2 1.351(5) ?
C15 C16 1.368(6) ?
C15 C14 1.508(6) ?
C18 C19 1.376(6) ?
C18 C17 1.385(6) ?
C18 H18 0.93 ?
C17 C16 1.395(6) ?
C17 C20 1.496(6) ?
C16 H16 0.93 ?
C8 C9 1.379(6) ?
C8 C7 1.390(6) ?
C8 H8 0.93 ?
C6 C7 1.388(6) ?
C6 H6 0.93 ?
C9 H9 0.93 ?
C7 C10 1.493(6) ?
C20 O18 1.215(5) ?
C20 O17 1.309(5) ?
C19 N2 1.337(5) ?
C19 H19 0.93 ?
N2 Re2 2.166(4) y
O8 C10 1.223(5) ?
O7 C10 1.313(5) ?
O11 C11 1.161(5) ?
O12 C12 1.135(6) ?
C11 Re2 1.892(5) y
C12 Re2 1.947(5) y
O2 C2 1.164(6) ?
C2 Re1 1.906(5) y
C3 O3 1.165(6) ?
C3 Re1 1.885(6) y
C13 O13 1.169(6) ?
C13 Re2 1.883(5) y
O14 Re2 2.153(3) y
O14 H14B 0.85(4) ?
O14 H14A 0.85(4) ?
O4 Re1 2.170(3) y
O4 H4A 0.85(5) ?
O4 H4B 0.85(5) ?
Re1 C1 1.915(5) y
C1 O1 1.151(5) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O7 H7 O15 1_656 0.82 1.81 2.595(4) 159.7 yes
O4 H4B O16 1_556 0.85(5) 2.51(5) 2.920(5) 111(4) yes
O4 H4B O8 1_455 0.85(5) 2.01(3) 2.780(5) 150(5) yes
O4 H4B O16 1_556 0.85(5) 2.51(5) 2.920(5) 111(4) yes
O14 H14B O6 1 0.85(5) 1.84(2) 2.671(5) 169(5) yes
O14 H14A O18 1_455 0.840(18) 1.87(2) 2.674(4) 161(5) yes
O17 H17 O6 2_655 0.82 1.78 2.602(4) 176.9 no
C8 H8 O13 2_666 0.93 2.58 3.253(5) 129.9 no
C6 H6 O17 2_655 0.93 2.55 3.426(5) 156.3 no
C19 H19 O2 1_655 0.93 2.5 3.131(5) 125.7 no
