#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:04:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179091 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/53/4305388.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_4305388
loop_
_publ_author_name
'Brenton R. Franklin'
'Richard S. Herrick'
'Christopher J. Ziegler'
'Natalie Barone'
'Laura R. Condon'
_publ_section_title
;
Reactions of the Re(CO)3(H2O)3+ Synthon with Monodentate Ligands under
Aqueous Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5902
_journal_page_last               5909
_journal_paper_doi               10.1021/ic800363w
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C9 H13 N O4 Re'
_chemical_formula_weight         385.40
_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                77.992(2)
_cell_angle_beta                 78.810(2)
_cell_angle_gamma                83.014(2)
_cell_formula_units_Z            2
_cell_length_a                   7.1308(9)
_cell_length_b                   8.7059(11)
_cell_length_c                   9.6359(13)
_cell_measurement_reflns_used    3182
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.40
_cell_volume                     571.92(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4748
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    10.617
_exptl_absorpt_correction_T_max  0.346
_exptl_absorpt_correction_T_min  0.092
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.624
_refine_diff_density_min         -2.639
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0313
_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)+(0.0238P)²+1.0063P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                2336
_reflns_number_total             2440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800363w-file002_6.cif
_cod_data_source_block           7
_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_database_code               4305388
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 0.53222(3) -0.07729(2) 0.67558(2) 0.00926(9) Uani 1 1 d . . .
O4 O 0.3421(6) -0.0591(5) 0.5256(5) 0.0125(9) Uani 1 1 d . . .
O1 O 0.2914(7) -0.2577(5) 0.9465(5) 0.0204(10) Uani 1 1 d . . .
N1 N 0.3766(7) 0.1588(6) 0.7007(6) 0.0121(10) Uani 1 1 d . . .
O2 O 0.8251(7) -0.0653(6) 0.8658(5) 0.0257(11) Uani 1 1 d . . .
O3 O 0.7569(7) -0.3942(5) 0.6345(5) 0.0268(11) Uani 1 1 d . . .
C6 C 0.7139(9) -0.0680(7) 0.7937(7) 0.0153(12) Uani 1 1 d . . .
C8 C 0.6705(9) -0.2739(7) 0.6463(7) 0.0165(13) Uani 1 1 d . . .
C7 C 0.3816(9) -0.1887(7) 0.8428(7) 0.0149(12) Uani 1 1 d . . .
C9 C 0.2072(9) -0.1718(8) 0.5378(8) 0.0212(14) Uani 1 1 d . . .
H9A H 0.2756 -0.2701 0.5138 0.032 Uiso 1 1 calc R . .
H9B H 0.1173 -0.1304 0.4712 0.032 Uiso 1 1 calc R . .
H9C H 0.1363 -0.1923 0.6367 0.032 Uiso 1 1 calc R . .
C2 C 0.0595(9) 0.3163(7) 0.7475(7) 0.0180(13) Uani 1 1 d . . .
H2A H 0.0740 0.3743 0.6466 0.022 Uiso 1 1 calc R . .
H2B H -0.0790 0.3068 0.7846 0.022 Uiso 1 1 calc R . .
C1 C 0.1654(8) 0.1520(7) 0.7525(7) 0.0153(12) Uani 1 1 d . . .
H1A H 0.1430 0.0922 0.8527 0.018 Uiso 1 1 calc R . .
H1B H 0.1127 0.0949 0.6919 0.018 Uiso 1 1 calc R . .
C5 C 0.4549(9) 0.2461(7) 0.7922(8) 0.0196(14) Uani 1 1 d . . .
H5A H 0.5942 0.2526 0.7572 0.024 Uiso 1 1 calc R . .
H5B H 0.4374 0.1867 0.8926 0.024 Uiso 1 1 calc R . .
C4 C 0.3580(10) 0.4102(8) 0.7901(8) 0.0248(15) Uani 1 1 d . . .
H4A H 0.3852 0.4730 0.6913 0.030 Uiso 1 1 calc R . .
H4B H 0.4110 0.4619 0.8547 0.030 Uiso 1 1 calc R . .
C3 C 0.1411(10) 0.4072(8) 0.8388(8) 0.0232(15) Uani 1 1 d . . .
H3A H 0.0799 0.5164 0.8287 0.028 Uiso 1 1 calc R . .
H3B H 0.1127 0.3562 0.9416 0.028 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.00951(14) 0.01317(14) 0.00548(14) -0.00150(9) -0.00270(9) -0.00067(8)
O4 0.012(2) 0.015(2) 0.011(2) -0.0022(17) -0.0017(17) -0.0065(16)
O1 0.028(3) 0.021(2) 0.011(2) -0.0008(18) 0.0012(19) -0.0064(18)
N1 0.008(2) 0.018(2) 0.012(3) -0.006(2) -0.0006(19) -0.0018(18)
O2 0.022(3) 0.042(3) 0.013(3) 0.003(2) -0.010(2) -0.008(2)
O3 0.028(3) 0.023(2) 0.023(3) -0.002(2) 0.001(2) 0.010(2)
C6 0.012(3) 0.020(3) 0.014(3) 0.002(2) -0.005(2) -0.005(2)
C8 0.018(3) 0.024(3) 0.005(3) 0.000(2) 0.001(2) -0.002(2)
C7 0.019(3) 0.016(3) 0.011(3) -0.003(2) -0.007(2) 0.000(2)
C9 0.020(3) 0.025(3) 0.020(4) -0.004(3) -0.005(3) -0.009(3)
C2 0.017(3) 0.023(3) 0.012(3) -0.005(3) 0.000(3) 0.004(2)
C1 0.012(3) 0.019(3) 0.016(3) -0.006(2) -0.001(2) -0.005(2)
C5 0.018(3) 0.022(3) 0.022(4) -0.012(3) -0.002(3) -0.004(2)
C4 0.027(4) 0.020(3) 0.031(4) -0.015(3) -0.001(3) -0.003(3)
C3 0.029(4) 0.019(3) 0.021(4) -0.009(3) 0.000(3) 0.003(3)
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'
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
C6 Re1 C7 87.4(3) . . ?
C6 Re1 C8 85.4(3) . . ?
C7 Re1 C8 88.4(3) . . ?
C6 Re1 O4 172.3(2) . . ?
C7 Re1 O4 99.4(2) . . ?
C8 Re1 O4 98.4(2) . . ?
C6 Re1 O4 101.2(2) . 2_656 ?
C7 Re1 O4 170.5(2) . 2_656 ?
C8 Re1 O4 96.2(2) . 2_656 ?
O4 Re1 O4 71.78(18) . 2_656 ?
C6 Re1 N1 95.1(2) . . ?
C7 Re1 N1 94.1(2) . . ?
C8 Re1 N1 177.5(2) . . ?
O4 Re1 N1 80.92(17) . . ?
O4 Re1 N1 81.28(17) 2_656 . ?
C9 O4 Re1 123.0(4) . . ?
C9 O4 Re1 123.6(4) . 2_656 ?
Re1 O4 Re1 108.22(17) . 2_656 ?
C1 N1 C5 108.9(5) . . ?
C1 N1 Re1 113.4(3) . . ?
C5 N1 Re1 115.4(4) . . ?
O2 C6 Re1 178.7(6) . . ?
O3 C8 Re1 177.0(6) . . ?
O1 C7 Re1 179.0(6) . . ?
C3 C2 C1 109.9(5) . . ?
N1 C1 C2 112.1(5) . . ?
N1 C5 C4 112.3(5) . . ?
C5 C4 C3 111.3(5) . . ?
C4 C3 C2 109.9(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 C6 1.902(6) . ?
Re1 C7 1.903(7) . ?
Re1 C8 1.914(6) . ?
Re1 O4 2.137(4) . ?
Re1 O4 2.144(4) 2_656 ?
Re1 N1 2.250(5) . ?
O4 C9 1.428(7) . ?
O4 Re1 2.144(4) 2_656 ?
O1 C7 1.169(8) . ?
N1 C1 1.496(7) . ?
N1 C5 1.497(7) . ?
O2 C6 1.156(8) . ?
O3 C8 1.164(7) . ?
C2 C3 1.530(9) . ?
C2 C1 1.531(8) . ?
C5 C4 1.508(8) . ?
C4 C3 1.529(9) . ?
