#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/53/4305384.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_4305384
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            'C18 H15 F6 N3 O3 P Re'
_chemical_formula_weight         652.50
_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                101.673(2)
_cell_angle_beta                 97.169(2)
_cell_angle_gamma                99.325(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1881(13)
_cell_length_b                   8.2792(13)
_cell_length_c                   16.024(2)
_cell_measurement_reflns_used    4439
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.56
_cell_volume                     1035.7(3)
_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 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8862
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    6.023
_exptl_absorpt_correction_T_max  0.5842
_exptl_absorpt_correction_T_min  0.2891
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.632
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0285P)²+0.6732P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                4211
_reflns_number_total             4586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800363w-file002_2.cif
_cod_data_source_block           3[PF6]
_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_original_formula_sum        'C18 H15 F6 N3 O3 P1 Re1'
_cod_database_code               4305384
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
C1 C 1.0241(6) -0.1643(7) 0.2172(3) 0.0282(11) Uani 1 1 d . . .
C2 C 1.2172(6) 0.1405(6) 0.2455(3) 0.0189(9) Uani 1 1 d . . .
C3 C 1.0776(5) 0.0342(5) 0.3748(3) 0.0173(9) Uani 1 1 d . . .
C4 C 0.8105(6) -0.0392(6) 0.0682(3) 0.0246(10) Uani 1 1 d . . .
H4 H 0.7837 -0.1461 0.0816 0.030 Uiso 1 1 calc R . .
C5 C 0.7537(6) -0.0235(7) -0.0143(3) 0.0289(12) Uani 1 1 d . . .
H5 H 0.6901 -0.1176 -0.0565 0.035 Uiso 1 1 calc R . .
C6 C 0.7911(6) 0.1309(7) -0.0340(3) 0.0299(12) Uani 1 1 d . . .
H6 H 0.7505 0.1467 -0.0894 0.036 Uiso 1 1 calc R . .
C7 C 0.8887(7) 0.2623(7) 0.0281(4) 0.0317(12) Uani 1 1 d . . .
H7 H 0.9198 0.3693 0.0155 0.038 Uiso 1 1 calc R . .
C8 C 0.9404(6) 0.2368(6) 0.1083(3) 0.0257(11) Uani 1 1 d . . .
H8 H 1.0075 0.3288 0.1505 0.031 Uiso 1 1 calc R . .
C9 C 0.6283(6) -0.1630(6) 0.2336(3) 0.0199(10) Uani 1 1 d . . .
H9 H 0.6610 -0.2178 0.1821 0.024 Uiso 1 1 calc R . .
C10 C 0.4754(6) -0.2262(6) 0.2527(3) 0.0227(10) Uani 1 1 d . . .
H10 H 0.4042 -0.3213 0.2144 0.027 Uiso 1 1 calc R . .
C11 C 0.4257(6) -0.1510(6) 0.3279(3) 0.0233(10) Uani 1 1 d . . .
H11 H 0.3220 -0.1952 0.3432 0.028 Uiso 1 1 calc R . .
C12 C 0.5312(6) -0.0092(6) 0.3805(3) 0.0206(10) Uani 1 1 d . . .
H12 H 0.4999 0.0474 0.4320 0.025 Uiso 1 1 calc R . .
C13 C 0.6817(6) 0.0479(6) 0.3568(3) 0.0203(10) Uani 1 1 d . . .
H13 H 0.7530 0.1452 0.3932 0.024 Uiso 1 1 calc R . .
C14 C 0.7889(6) 0.3462(6) 0.2731(3) 0.0198(9) Uani 1 1 d . . .
H14 H 0.7138 0.2643 0.2289 0.024 Uiso 1 1 calc R . .
C15 C 0.7441(6) 0.4976(6) 0.3024(3) 0.0215(10) Uani 1 1 d . . .
H15 H 0.6397 0.5193 0.2788 0.026 Uiso 1 1 calc R . .
C16 C 0.8522(6) 0.6186(6) 0.3665(3) 0.0246(11) Uani 1 1 d . . .
H16 H 0.8226 0.7233 0.3887 0.029 Uiso 1 1 calc R . .
C17 C 1.0031(6) 0.5834(6) 0.3972(3) 0.0223(10) Uani 1 1 d . . .
H17 H 1.0812 0.6656 0.4399 0.027 Uiso 1 1 calc R . .
C18 C 1.0417(6) 0.4286(6) 0.3660(3) 0.0190(9) Uani 1 1 d . . .
H18 H 1.1465 0.4064 0.3887 0.023 Uiso 1 1 calc R . .
F1 F 0.6441(3) 0.3957(4) 0.47677(19) 0.0275(6) Uani 1 1 d . . .
F2 F 0.4502(4) 0.5019(4) 0.40018(19) 0.0328(7) Uani 1 1 d . . .
F3 F 0.3685(4) 0.3289(4) 0.4864(2) 0.0320(7) Uani 1 1 d . . .
F4 F 0.4869(4) 0.6919(4) 0.0328(2) 0.0462(9) Uani 1 1 d . . .
F5 F 0.3577(9) 0.4530(6) 0.0503(5) 0.141(3) Uani 1 1 d . . .
F6 F 0.6346(8) 0.5188(7) 0.0799(4) 0.140(3) Uani 1 1 d . . .
N1 N 0.9017(4) 0.0892(5) 0.1305(2) 0.0179(8) Uani 1 1 d . . .
N2 N 0.7341(4) -0.0273(5) 0.2841(2) 0.0167(8) Uani 1 1 d . . .
N3 N 0.9375(4) 0.3083(4) 0.3052(2) 0.0147(7) Uani 1 1 d . . .
O1 O 1.0435(4) -0.3009(4) 0.1922(2) 0.0233(7) Uani 1 1 d . . .
O2 O 1.3520(4) 0.1876(4) 0.2353(2) 0.0271(8) Uani 1 1 d . . .
O3 O 1.1299(4) 0.0144(4) 0.4407(2) 0.0223(7) Uani 1 1 d . . .
P1 P 0.5000 0.5000 0.5000 0.0192(4) Uani 1 2 d S . .
P2 P 0.5000 0.5000 0.0000 0.0279(4) Uani 1 2 d S . .
Re1 Re 0.99319(2) 0.05792(2) 0.261227(11) 0.01362(7) Uani 1 1 d . . .
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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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
O1 C1 Re1 178.5(5) . . ?
O2 C2 Re1 178.9(4) . . ?
O3 C3 Re1 177.3(4) . . ?
N1 C4 C5 123.4(5) . . ?
N1 C4 H4 118.3 . . ?
C5 C4 H4 118.3 . . ?
C6 C5 C4 118.7(5) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
C5 C6 C7 118.7(5) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
C8 C7 C6 119.2(5) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
N1 C8 C7 123.6(5) . . ?
N1 C8 H8 118.2 . . ?
C7 C8 H8 118.2 . . ?
N2 C9 C10 123.4(4) . . ?
N2 C9 H9 118.3 . . ?
C10 C9 H9 118.3 . . ?
C9 C10 C11 119.6(4) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C10 C11 C12 118.2(4) . . ?
C10 C11 H11 120.9 . . ?
C12 C11 H11 120.9 . . ?
C13 C12 C11 118.9(4) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
N2 C13 C12 123.5(4) . . ?
N2 C13 H13 118.2 . . ?
C12 C13 H13 118.2 . . ?
N3 C14 C15 122.6(4) . . ?
N3 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C14 C15 C16 119.5(4) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C17 C16 C15 118.3(4) . . ?
C17 C16 H16 120.9 . . ?
C15 C16 H16 120.9 . . ?
C16 C17 C18 120.0(5) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
N3 C18 C17 122.7(4) . . ?
N3 C18 H18 118.6 . . ?
C17 C18 H18 118.6 . . ?
C8 N1 C4 116.4(4) . . ?
C8 N1 Re1 121.3(3) . . ?
C4 N1 Re1 122.2(3) . . ?
C9 N2 C13 116.4(4) . . ?
C9 N2 Re1 123.3(3) . . ?
C13 N2 Re1 120.0(3) . . ?
C18 N3 C14 116.9(4) . . ?
C18 N3 Re1 122.6(3) . . ?
C14 N3 Re1 120.5(3) . . ?
F3 P1 F3 180.0(2) 2_666 . ?
F3 P1 F2 90.19(16) 2_666 2_666 ?
F3 P1 F2 89.81(16) . 2_666 ?
F3 P1 F2 89.81(16) 2_666 . ?
F3 P1 F2 90.19(16) . . ?
F2 P1 F2 180.000(1) 2_666 . ?
F3 P1 F1 90.16(15) 2_666 2_666 ?
F3 P1 F1 89.84(15) . 2_666 ?
F2 P1 F1 90.47(15) 2_666 2_666 ?
F2 P1 F1 89.53(15) . 2_666 ?
F3 P1 F1 89.84(15) 2_666 . ?
F3 P1 F1 90.16(15) . . ?
F2 P1 F1 89.53(15) 2_666 . ?
F2 P1 F1 90.47(15) . . ?
F1 P1 F1 180.0(2) 2_666 . ?
F5 P2 F5 180.0(5) . 2_665 ?
F5 P2 F6 88.5(4) . 2_665 ?
F5 P2 F6 91.5(4) 2_665 2_665 ?
F5 P2 F6 91.5(4) . . ?
F5 P2 F6 88.5(4) 2_665 . ?
F6 P2 F6 180.0(6) 2_665 . ?
F5 P2 F4 87.8(2) . . ?
F5 P2 F4 92.2(2) 2_665 . ?
F6 P2 F4 90.9(2) 2_665 . ?
F6 P2 F4 89.1(2) . . ?
F5 P2 F4 92.2(2) . 2_665 ?
F5 P2 F4 87.8(2) 2_665 2_665 ?
F6 P2 F4 89.1(2) 2_665 2_665 ?
F6 P2 F4 90.9(2) . 2_665 ?
F4 P2 F4 180.0(3) . 2_665 ?
C1 Re1 C2 88.8(2) . . ?
C1 Re1 C3 88.1(2) . . ?
C2 Re1 C3 90.02(18) . . ?
C1 Re1 N3 175.33(18) . . ?
C2 Re1 N3 94.53(17) . . ?
C3 Re1 N3 95.16(16) . . ?
C1 Re1 N1 92.26(19) . . ?
C2 Re1 N1 88.69(16) . . ?
C3 Re1 N1 178.65(15) . . ?
N3 Re1 N1 84.55(14) . . ?
C1 Re1 N2 93.56(18) . . ?
C2 Re1 N2 177.42(16) . . ?
C3 Re1 N2 88.99(16) . . ?
N3 Re1 N2 83.18(13) . . ?
N1 Re1 N2 92.28(13) . . ?
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
C1 O1 1.164(6) . ?
C1 Re1 1.902(6) . ?
C2 O2 1.152(6) . ?
C2 Re1 1.917(5) . ?
C3 O3 1.142(6) . ?
C3 Re1 1.924(5) . ?
C4 N1 1.345(6) . ?
C4 C5 1.385(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.374(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.376(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.370(7) . ?
C7 H7 0.9500 . ?
C8 N1 1.341(6) . ?
C8 H8 0.9500 . ?
C9 N2 1.344(6) . ?
C9 C10 1.372(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.387(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.374(6) . ?
C12 H12 0.9500 . ?
C13 N2 1.359(6) . ?
C13 H13 0.9500 . ?
C14 N3 1.370(6) . ?
C14 C15 1.371(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.370(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.380(7) . ?
C17 H17 0.9500 . ?
C18 N3 1.339(6) . ?
C18 H18 0.9500 . ?
F1 P1 1.608(3) . ?
F2 P1 1.604(3) . ?
F3 P1 1.592(3) . ?
F4 P2 1.595(3) . ?
F5 P2 1.541(5) . ?
F6 P2 1.546(4) . ?
N1 Re1 2.216(4) . ?
N2 Re1 2.224(4) . ?
N3 Re1 2.190(4) . ?
P1 F3 1.592(3) 2_666 ?
P1 F2 1.604(3) 2_666 ?
P1 F1 1.608(3) 2_666 ?
P2 F5 1.541(5) 2_665 ?
P2 F6 1.546(4) 2_665 ?
P2 F4 1.595(3) 2_665 ?
