#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:53:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179216 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/43/4314337.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_4314337
loop_
_publ_author_name
'Paul D. Benny'
'Charles L. Barnes'
'Pamela M. Piekarski'
'John D. Lydon'
'Silvia S. Jurisson'
_publ_contact_author
; Dr. Silvia Jurisson
    Department of Chemistry
    University of Missouri - Columbia
    Columbia, Missouri 65211 USA
;
_publ_contact_author_email       JurissonS@missouri.edu
_publ_contact_author_fax         (573)882-2754
_publ_contact_author_phone       (573)882-2107
_publ_section_title
;
 Synthesis and Characterization of Novel Rhenium(V) Tetradentate N2O2
 Schiff Base Monomer and Dimer Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6519
_journal_page_last               6527
_journal_paper_doi               10.1021/ic030240q
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C14 H23 N2 O4 Re'
_chemical_formula_weight         469.54
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 92.197(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7104(8)
_cell_length_b                   27.844(3)
_cell_length_c                   8.2292(9)
_cell_measurement_reflns_used    6754
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      1
_cell_volume                     1536.4(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       '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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9315
_diffrn_reflns_theta_full        27.17
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    7.926
_exptl_absorpt_correction_T_max  0.30
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
   Data were corrected for decay and absorption using the program SADABS
   based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.457
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       0.0004(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   0.964
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.079
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                3074
_reflns_number_total             3392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030240q_5.cif
_cod_data_source_block           (4)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314337
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.42521(3) 0.620498(8) 0.52074(3) 0.01711(13) Uani 1 1 d . . .
O2 O 0.2624(7) 0.61873(15) 0.7252(6) 0.0232(10) Uani 1 1 d . . .
N2 N 0.6211(8) 0.56605(19) 0.6142(6) 0.0219(10) Uani 1 1 d . . .
O4 O 0.6041(6) 0.66272(16) 0.6372(5) 0.0225(9) Uani 1 1 d . . .
O1 O 0.2501(6) 0.67863(17) 0.4736(5) 0.0231(9) Uani 1 1 d . . .
O3 O 0.2949(7) 0.57898(18) 0.4074(5) 0.0254(9) Uani 1 1 d . . .
N1 N 0.6013(7) 0.6372(2) 0.3196(6) 0.0210(10) Uani 1 1 d . . .
C13 C 0.1947(10) 0.6105(3) 1.0019(7) 0.0247(12) Uani 1 1 d . . .
H13A H 0.2364 0.6415 1.0478 0.037 Uiso 1 1 calc R . .
H13B H 0.2101 0.5856 1.0856 0.037 Uiso 1 1 calc R . .
H13C H 0.0547 0.6123 0.9641 0.037 Uiso 1 1 calc R . .
C2 C 0.4513(9) 0.7153(2) 0.2742(7) 0.0257(13) Uani 1 1 d . . .
H2 H 0.4682 0.7445 0.2167 0.031 Uiso 1 1 calc R . .
C9 C 0.3220(9) 0.5983(2) 0.8615(7) 0.0208(12) Uani 1 1 d . . .
C12 C 0.7879(10) 0.5210(3) 0.8341(8) 0.0311(14) Uani 1 1 d . . .
H12A H 0.7731 0.4893 0.7833 0.047 Uiso 1 1 calc R . .
H12B H 0.7773 0.5178 0.9521 0.047 Uiso 1 1 calc R . .
H12C H 0.9186 0.5344 0.8101 0.047 Uiso 1 1 calc R . .
C7 C 0.6261(9) 0.5538(2) 0.7680(8) 0.0241(12) Uani 1 1 d . . .
C8 C 0.4863(9) 0.5699(2) 0.8844(7) 0.0245(12) Uani 1 1 d . . .
H8 H 0.5122 0.5592 0.9928 0.029 Uiso 1 1 calc R . .
C3 C 0.5899(9) 0.6781(3) 0.2429(7) 0.0248(12) Uani 1 1 d . . .
C4 C 0.7610(10) 0.6035(3) 0.2707(8) 0.0296(13) Uani 1 1 d . . .
H4A H 0.8913 0.6154 0.3143 0.036 Uiso 1 1 calc R . .
H4B H 0.7654 0.6032 0.1506 0.036 Uiso 1 1 calc R . .
C5 C 0.7301(10) 0.5523(2) 0.3307(8) 0.0298(14) Uani 1 1 d . . .
H5A H 0.5904 0.5429 0.3040 0.036 Uiso 1 1 calc R . .
H5B H 0.8174 0.5306 0.2698 0.036 Uiso 1 1 calc R . .
C6 C 0.7712(10) 0.5442(3) 0.5096(8) 0.0296(14) Uani 1 1 d . . .
H6A H 0.7763 0.5092 0.5306 0.035 Uiso 1 1 calc R . .
H6B H 0.9040 0.5577 0.5402 0.035 Uiso 1 1 calc R . .
C1 C 0.2960(9) 0.7139(2) 0.3776(7) 0.0214(11) Uani 1 1 d . . .
C10 C 0.1578(10) 0.7562(3) 0.3855(9) 0.0328(14) Uani 1 1 d . . .
H10A H 0.0234 0.7465 0.3479 0.049 Uiso 1 1 calc R . .
H10B H 0.2055 0.7819 0.3158 0.049 Uiso 1 1 calc R . .
H10C H 0.1544 0.7676 0.4979 0.049 Uiso 1 1 calc R . .
C11 C 0.7317(12) 0.6902(3) 0.1069(9) 0.0381(17) Uani 1 1 d . . .
H11A H 0.8700 0.6868 0.1479 0.057 Uiso 1 1 calc R . .
H11B H 0.7085 0.7233 0.0705 0.057 Uiso 1 1 calc R . .
H11C H 0.7071 0.6681 0.0154 0.057 Uiso 1 1 calc R . .
C14 C 0.8093(10) 0.6710(3) 0.6549(9) 0.0353(15) Uani 1 1 d . . .
H14A H 0.8737 0.6434 0.7089 0.053 Uiso 1 1 calc R . .
H14B H 0.8333 0.6999 0.7207 0.053 Uiso 1 1 calc R . .
H14C H 0.8647 0.6755 0.5475 0.053 Uiso 1 1 calc R . .
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
O3 Re1 O4 172.0(2) . . ?
O3 Re1 O1 98.9(2) . . ?
O4 Re1 O1 87.31(18) . . ?
O3 Re1 O2 98.9(2) . . ?
O4 Re1 O2 86.97(19) . . ?
O1 Re1 O2 81.52(17) . . ?
O3 Re1 N1 90.7(2) . . ?
O4 Re1 N1 84.15(19) . . ?
O1 Re1 N1 90.65(19) . . ?
O2 Re1 N1 168.43(19) . . ?
O3 Re1 N2 90.7(2) . . ?
O4 Re1 N2 83.7(2) . . ?
O1 Re1 N2 168.92(19) . . ?
O2 Re1 N2 91.57(19) . . ?
N1 Re1 N2 94.8(2) . . ?
C9 O2 Re1 124.2(4) . . ?
C7 N2 C6 117.6(5) . . ?
C7 N2 Re1 121.8(4) . . ?
C6 N2 Re1 120.4(4) . . ?
C14 O4 Re1 138.6(4) . . ?
C1 O1 Re1 124.6(4) . . ?
C3 N1 C4 116.7(5) . . ?
C3 N1 Re1 123.1(4) . . ?
C4 N1 Re1 120.0(4) . . ?
C1 C2 C3 127.5(6) . . ?
O2 C9 C8 126.2(5) . . ?
O2 C9 C13 113.4(5) . . ?
C8 C9 C13 120.3(5) . . ?
N2 C7 C8 124.7(5) . . ?
N2 C7 C12 119.9(6) . . ?
C8 C7 C12 115.3(5) . . ?
C9 C8 C7 129.3(5) . . ?
N1 C3 C2 125.1(5) . . ?
N1 C3 C11 121.2(6) . . ?
C2 C3 C11 113.7(6) . . ?
N1 C4 C5 113.1(5) . . ?
C6 C5 C4 115.8(6) . . ?
N2 C6 C5 113.8(5) . . ?
O1 C1 C2 126.9(6) . . ?
O1 C1 C10 113.8(5) . . ?
C2 C1 C10 119.3(6) . . ?
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 O3 1.705(5) . ?
Re1 O4 1.911(5) . ?
Re1 O1 2.029(4) . ?
Re1 O2 2.042(5) . ?
Re1 N1 2.122(5) . ?
Re1 N2 2.131(5) . ?
O2 C9 1.306(7) . ?
N2 C7 1.309(8) . ?
N2 C6 1.481(7) . ?
O4 C14 1.398(7) . ?
O1 C1 1.304(7) . ?
N1 C3 1.302(9) . ?
N1 C4 1.492(8) . ?
C13 C9 1.502(8) . ?
C2 C1 1.371(8) . ?
C2 C3 1.422(9) . ?
C9 C8 1.364(9) . ?
C12 C7 1.506(8) . ?
C7 C8 1.437(8) . ?
C3 C11 1.533(9) . ?
C4 C5 1.526(10) . ?
C5 C6 1.504(9) . ?
C1 C10 1.502(8) . ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Re1 O2 C9 105.7(5) . . . . ?
O4 Re1 O2 C9 -68.8(5) . . . . ?
O1 Re1 O2 C9 -156.6(5) . . . . ?
N1 Re1 O2 C9 -108.7(9) . . . . ?
N2 Re1 O2 C9 14.7(5) . . . . ?
O3 Re1 N2 C7 -113.6(5) . . . . ?
O4 Re1 N2 C7 72.1(5) . . . . ?
O1 Re1 N2 C7 36.5(12) . . . . ?
O2 Re1 N2 C7 -14.6(5) . . . . ?
N1 Re1 N2 C7 155.7(5) . . . . ?
O3 Re1 N2 C6 72.7(5) . . . . ?
O4 Re1 N2 C6 -101.6(5) . . . . ?
O1 Re1 N2 C6 -137.2(9) . . . . ?
O2 Re1 N2 C6 171.7(5) . . . . ?
N1 Re1 N2 C6 -18.0(5) . . . . ?
O3 Re1 O4 C14 3.9(18) . . . . ?
O1 Re1 O4 C14 -137.2(7) . . . . ?
O2 Re1 O4 C14 141.1(7) . . . . ?
N1 Re1 O4 C14 -46.3(7) . . . . ?
N2 Re1 O4 C14 49.2(7) . . . . ?
O3 Re1 O1 C1 -105.6(5) . . . . ?
O4 Re1 O1 C1 69.3(5) . . . . ?
O2 Re1 O1 C1 156.6(5) . . . . ?
N1 Re1 O1 C1 -14.8(5) . . . . ?
N2 Re1 O1 C1 104.8(10) . . . . ?
O3 Re1 N1 C3 111.1(5) . . . . ?
O4 Re1 N1 C3 -75.1(5) . . . . ?
O1 Re1 N1 C3 12.2(5) . . . . ?
O2 Re1 N1 C3 -35.0(11) . . . . ?
N2 Re1 N1 C3 -158.2(5) . . . . ?
O3 Re1 N1 C4 -75.2(5) . . . . ?
O4 Re1 N1 C4 98.7(5) . . . . ?
O1 Re1 N1 C4 -174.1(5) . . . . ?
O2 Re1 N1 C4 138.7(8) . . . . ?
N2 Re1 N1 C4 15.5(5) . . . . ?
Re1 O2 C9 C8 -9.0(9) . . . . ?
Re1 O2 C9 C13 168.3(4) . . . . ?
C6 N2 C7 C8 -177.0(6) . . . . ?
Re1 N2 C7 C8 9.1(9) . . . . ?
C6 N2 C7 C12 3.4(9) . . . . ?
Re1 N2 C7 C12 -170.4(5) . . . . ?
O2 C9 C8 C7 -3.2(11) . . . . ?
C13 C9 C8 C7 179.6(6) . . . . ?
N2 C7 C8 C9 2.7(11) . . . . ?
C12 C7 C8 C9 -177.7(7) . . . . ?
C4 N1 C3 C2 -178.6(6) . . . . ?
Re1 N1 C3 C2 -4.7(9) . . . . ?
C4 N1 C3 C11 1.2(9) . . . . ?
Re1 N1 C3 C11 175.1(5) . . . . ?
C1 C2 C3 N1 -6.1(11) . . . . ?
C1 C2 C3 C11 174.1(7) . . . . ?
C3 N1 C4 C5 -164.3(6) . . . . ?
Re1 N1 C4 C5 21.6(7) . . . . ?
N1 C4 C5 C6 -73.6(7) . . . . ?
C7 N2 C6 C5 168.5(6) . . . . ?
Re1 N2 C6 C5 -17.6(8) . . . . ?
C4 C5 C6 N2 71.1(8) . . . . ?
Re1 O1 C1 C2 10.3(9) . . . . ?
Re1 O1 C1 C10 -170.2(4) . . . . ?
C3 C2 C1 O1 3.3(11) . . . . ?
C3 C2 C1 C10 -176.1(6) . . . . ?
