#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:40:54 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178880 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/09/4110996.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_4110996
loop_
_publ_author_name
'Steven Y. Reece'
'Mohammad R. Seyedsayamdost'
'JoAnne Stubbe'
'Daniel G. Nocera'
_publ_contact_author             'Daniel G. Nocera'
_publ_contact_author_email       nocera@mit.edu
_publ_section_title
;
 Electron Transfer Reactions of Fluorotyrosyl Radicals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13654
_journal_page_last               13655
_journal_paper_doi               10.1021/ja0636688
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C17 H14 N3 O6 Re'
_chemical_formula_weight         542.51
_chemical_name_common            Re(bpy-COOH)(CO)3CN
_chemical_name_systematic
;
(4-methyl-2,2'-bipyridine-4'-carboxylic acid)(tricarbonyl)(cyano)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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                104.8670(10)
_cell_angle_beta                 96.5250(10)
_cell_angle_gamma                106.2030(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3707(5)
_cell_length_b                   10.4102(6)
_cell_length_c                   11.8772(7)
_cell_measurement_reflns_used    4580
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.35
_cell_volume                     941.28(10)
_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      373(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5964
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    6.493
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.928
_refine_diff_density_min         -1.457
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0297
_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)+(0.0445P)²+0.1679P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                4095
_reflns_number_total             4430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0636688rom20060525_015751.cif
_cod_data_source_block           1
_cod_database_code               4110996
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 0.524585(19) 0.814572(15) 0.681552(13) 0.02030(7) Uani 1 1 d . . .
C4 C 0.6088(6) 0.6650(5) 0.7435(4) 0.0258(9) Uani 1 1 d . . .
C2 C 0.3124(6) 0.6763(5) 0.5896(4) 0.0280(9) Uani 1 1 d . . .
C3 C 0.4127(6) 0.8491(5) 0.8129(4) 0.0271(9) Uani 1 1 d . . .
C1 C 0.4591(6) 0.9594(5) 0.6302(4) 0.0255(9) Uani 1 1 d . . .
C5 C 0.6185(6) 0.6846(5) 0.4395(4) 0.0239(9) Uani 1 1 d . . .
H5 H 0.5024 0.6373 0.4164 0.029 Uiso 1 1 calc R . .
C6 C 0.7226(6) 0.6561(4) 0.3605(4) 0.0254(9) Uani 1 1 d . . .
H6 H 0.6771 0.5911 0.2856 0.031 Uiso 1 1 calc R . .
C7 C 0.8951(6) 0.7256(4) 0.3944(4) 0.0237(8) Uani 1 1 d . . .
C8 C 0.9575(5) 0.8237(4) 0.5062(4) 0.0220(8) Uani 1 1 d . . .
H8 H 1.0728 0.8739 0.5298 0.026 Uiso 1 1 calc R . .
C9 C 0.8481(5) 0.8471(4) 0.5827(4) 0.0220(8) Uani 1 1 d . . .
C10 C 0.9043(5) 0.9455(4) 0.7040(4) 0.0209(8) Uani 1 1 d . . .
C11 C 1.0720(5) 1.0272(4) 0.7517(4) 0.0242(8) Uani 1 1 d . . .
H11 H 1.1549 1.0189 0.7070 0.029 Uiso 1 1 calc R . .
C14 C 0.8232(6) 1.0448(5) 0.8769(4) 0.0257(9) Uani 1 1 d . . .
H14 H 0.7386 1.0511 0.9204 0.031 Uiso 1 1 calc R . .
C15 C 1.2994(7) 1.2108(6) 0.9169(5) 0.0389(12) Uani 1 1 d . . .
H15A H 1.3483 1.1731 0.9726 0.058 Uiso 1 1 calc R . .
H15B H 1.3037 1.3048 0.9568 0.058 Uiso 1 1 calc R . .
H15C H 1.3622 1.2118 0.8541 0.058 Uiso 1 1 calc R . .
C16 C 1.0160(7) 0.6973(5) 0.3131(4) 0.0307(10) Uani 1 1 d . . .
C13 C 0.9871(6) 1.1280(5) 0.9283(4) 0.0286(9) Uani 1 1 d . . .
H13 H 1.0116 1.1891 1.0051 0.034 Uiso 1 1 calc R . .
C12 C 1.1173(5) 1.1210(5) 0.8653(4) 0.0260(9) Uani 1 1 d . . .
N1 N 0.6791(5) 0.7784(4) 0.5490(3) 0.0213(7) Uani 1 1 d . . .
N2 N 0.7791(5) 0.9540(4) 0.7656(3) 0.0225(7) Uani 1 1 d . . .
N3 N 0.6574(6) 0.5873(4) 0.7772(4) 0.0326(9) Uani 1 1 d . . .
O1 O 0.4119(4) 1.0437(4) 0.6045(3) 0.0351(8) Uani 1 1 d . . .
O2 O 0.1883(5) 0.5933(4) 0.5343(4) 0.0405(9) Uani 1 1 d . . .
O3 O 0.3449(5) 0.8702(4) 0.8918(3) 0.0382(8) Uani 1 1 d . . .
O4 O 0.9434(4) 0.5945(4) 0.2174(3) 0.0360(8) Uani 1 1 d . . .
H4 H 1.0150 0.5789 0.1790 0.054 Uiso 1 1 calc R . .
O5 O 1.1654(4) 0.7688(4) 0.3405(3) 0.0332(7) Uani 1 1 d . . .
C1S C 0.7422(7) 0.3828(6) 0.9454(5) 0.0380(11) Uani 0.286(8) 1 d P A 1
H1S1 H 0.8530 0.4513 0.9637 0.057 Uiso 0.286(8) 1 calc PR A 1
H1S2 H 0.7495 0.3034 0.9700 0.057 Uiso 0.286(8) 1 calc PR A 1
H1S3 H 0.6674 0.4234 0.9868 0.057 Uiso 0.286(8) 1 calc PR A 1
O1S O 0.6759(17) 0.3377(14) 0.8171(11) 0.037(3) Uani 0.286(8) 1 d P A 1
H1S H 0.6500 0.4010 0.7985 0.055 Uiso 0.286(8) 1 calc PR A 1
O2S O 0.8489(5) 0.4838(5) 0.9052(4) 0.0251(11) Uani 0.714(8) 1 d P A 2
H2S H 0.7941 0.4966 0.8497 0.038 Uiso 0.714(8) 1 calc PR A 2
C2S C 0.7422(7) 0.3828(6) 0.9454(5) 0.0380(11) Uani 0.714(8) 1 d P A 2
H2S1 H 0.7453 0.4216 1.0286 0.057 Uiso 0.714(8) 1 calc PR A 2
H2S2 H 0.7800 0.3023 0.9335 0.057 Uiso 0.714(8) 1 calc PR A 2
H2S3 H 0.6281 0.3555 0.9018 0.057 Uiso 0.714(8) 1 calc PR A 2
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
C3 Re1 C2 88.1(2)
C3 Re1 C1 89.42(19)
C2 Re1 C1 89.96(19)
C3 Re1 C4 90.57(18)
C2 Re1 C4 93.21(18)
C1 Re1 C4 176.82(17)
C3 Re1 N2 99.65(17)
C2 Re1 N2 171.72(16)
C1 Re1 N2 92.89(17)
C4 Re1 N2 83.98(15)
C3 Re1 N1 172.77(16)
C2 Re1 N1 97.49(17)
C1 Re1 N1 95.09(16)
C4 Re1 N1 84.62(15)
N2 Re1 N1 74.53(14)
N3 C4 Re1 178.5(4)
O2 C2 Re1 178.9(5)
O3 C3 Re1 179.7(4)
O1 C1 Re1 175.3(4)
N1 C5 C6 122.5(4)
C7 C6 C5 119.0(4)
C6 C7 C8 118.6(4)
C6 C7 C16 121.6(4)
C8 C7 C16 119.7(4)
C9 C8 C7 120.1(4)
N1 C9 C8 121.0(4)
N1 C9 C10 115.4(4)
C8 C9 C10 123.6(4)
N2 C10 C11 121.8(4)
N2 C10 C9 115.2(4)
C11 C10 C9 123.0(4)
C12 C11 C10 120.7(4)
N2 C14 C13 122.9(4)
O5 C16 O4 126.5(4)
O5 C16 C7 120.5(4)
O4 C16 C7 113.0(4)
C14 C13 C12 120.0(4)
C11 C12 C13 117.0(4)
C11 C12 C15 120.7(4)
C13 C12 C15 122.3(4)
C5 N1 C9 118.8(4)
C5 N1 Re1 123.9(3)
C9 N1 Re1 117.1(3)
C14 N2 C10 117.7(4)
C14 N2 Re1 124.7(3)
C10 N2 Re1 117.5(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 C3 1.916(5)
Re1 C2 1.935(5)
Re1 C1 1.950(4)
Re1 C4 2.132(5)
Re1 N2 2.166(4)
Re1 N1 2.174(4)
C4 N3 1.136(6)
C2 O2 1.144(6)
C3 O3 1.155(6)
C1 O1 1.150(6)
C5 N1 1.350(6)
C5 C6 1.384(6)
C6 C7 1.380(6)
C7 C8 1.389(6)
C7 C16 1.512(6)
C8 C9 1.387(6)
C9 N1 1.354(6)
C9 C10 1.471(6)
C10 N2 1.354(5)
C10 C11 1.386(6)
C11 C12 1.385(6)
C14 N2 1.353(6)
C14 C13 1.371(7)
C15 C12 1.508(7)
C16 O5 1.219(6)
C16 O4 1.290(6)
C13 C12 1.399(6)
C1S O1S 1.465(14)
