#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:51:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179158 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/19/4311960.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_4311960
loop_
_publ_author_name
'Theresa I. Kückmann'
'Ulrich Abram'
_publ_section_title
;
 Rhenium(V) Oxo Complexes with N-Heterocyclic Carbenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7068
_journal_page_last               7074
_journal_paper_doi               10.1021/ic0497578
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '[ReOCl(Etcarbene)4][PF6]x 2KPF6'
_chemical_formula_sum            'C36 H64 Cl F24 K2 N8 O P4 Re'
_chemical_formula_weight         1504.68
_chemical_name_systematic
;
Chlorotetrakis(3,4-dimethyl-2,5-diethylimidazolylidene)oxorhenium(V)-
bis(hexafluorophosphate) x 2 KPF6
;
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.098(2)
_cell_length_b                   17.098(2)
_cell_length_c                   9.673(2)
_cell_measurement_temperature    193(2)
_cell_volume                     2827.8(7)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       'omega and phi 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  0.0804
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17381
_diffrn_reflns_theta_full        30.72
_diffrn_reflns_theta_max         30.72
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  .923
_exptl_absorpt_correction_T_min  .885
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4303
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0582P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                3643
_reflns_number_total             4303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0497578rom20040224_091421_2.cif
_cod_data_source_block           reocletcarb
_cod_database_code               4311960
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+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
Re Re 0.0000 0.0000 0.44125(2) 0.02894(11) Uani 1 4 d SD . .
Cl1 Cl 0.0000 0.0000 0.2055(12) 0.0360(9) Uani 0.343(16) 4 d SPD . .
Cl1A Cl 0.0000 0.0000 0.6779(6) 0.0360(9) Uani 0.657(16) 4 d SPD . .
O1 O 0.0000 0.0000 0.611(4) 0.031(3) Uani 0.343(16) 4 d SP . .
O1A O 0.0000 0.0000 0.250(2) 0.031(3) Uani 0.657(16) 4 d SP . .
C1 C 0.0716(2) 0.1065(2) 0.4434(10) 0.0287(8) Uani 1 1 d . . .
N2 N 0.1352(3) 0.1227(2) 0.5217(5) 0.0305(9) Uani 1 1 d . . .
C3 C 0.1634(3) 0.1981(3) 0.4935(6) 0.0321(11) Uani 1 1 d . . .
C4 C 0.1160(3) 0.2287(3) 0.3977(5) 0.0337(12) Uani 1 1 d . . .
N5 N 0.0599(3) 0.1730(3) 0.3675(5) 0.0310(9) Uani 1 1 d . . .
C6 C 0.2329(4) 0.2329(4) 0.5585(7) 0.0453(14) Uani 1 1 d . . .
H6A H 0.2544 0.1968 0.6245 0.068 Uiso 1 1 calc R . .
H6B H 0.2185 0.2804 0.6046 0.068 Uiso 1 1 calc R . .
H6C H 0.2713 0.2440 0.4888 0.068 Uiso 1 1 calc R . .
C7 C 0.1155(4) 0.3085(4) 0.3349(7) 0.0461(15) Uani 1 1 d . . .
H7A H 0.0739 0.3120 0.2685 0.069 Uiso 1 1 calc R . .
H7B H 0.1646 0.3179 0.2898 0.069 Uiso 1 1 calc R . .
H7C H 0.1077 0.3468 0.4060 0.069 Uiso 1 1 calc R . .
C8 C 0.1727(3) 0.0731(3) 0.6258(6) 0.0366(12) Uani 1 1 d . . .
H8A H 0.2288 0.0736 0.6103 0.044 Uiso 1 1 calc R . .
H8B H 0.1547 0.0198 0.6137 0.044 Uiso 1 1 calc R . .
C9 C 0.0020(4) 0.1843(4) 0.2568(6) 0.0441(14) Uani 1 1 d . . .
H9A H -0.0202 0.2363 0.2644 0.053 Uiso 1 1 calc R . .
H9B H -0.0400 0.1468 0.2682 0.053 Uiso 1 1 calc R . .
C10 C 0.1568(5) 0.0980(5) 0.7722(7) 0.0581(18) Uani 1 1 d . . .
H10A H 0.1826 0.0628 0.8347 0.087 Uiso 1 1 calc R . .
H10B H 0.1015 0.0970 0.7891 0.087 Uiso 1 1 calc R . .
H10C H 0.1762 0.1501 0.7863 0.087 Uiso 1 1 calc R . .
C11 C 0.0378(5) 0.1745(6) 0.1144(8) 0.074(2) Uani 1 1 d . . .
H11A H -0.0018 0.1818 0.0453 0.111 Uiso 1 1 calc R . .
H11B H 0.0595 0.1229 0.1060 0.111 Uiso 1 1 calc R . .
H11C H 0.0785 0.2126 0.1017 0.111 Uiso 1 1 calc R . .
P P 0.07831(10) 0.36489(9) 0.80682(18) 0.0411(4) Uani 1 1 d . . .
F1 F 0.0790(4) 0.2738(3) 0.8044(7) 0.0927(18) Uani 1 1 d . . .
F5 F 0.0754(3) 0.4589(3) 0.8085(5) 0.0755(14) Uani 1 1 d . . .
F2 F 0.0853(6) 0.3680(4) 0.6490(7) 0.155(4) Uani 1 1 d . . .
F6 F 0.0744(8) 0.3653(4) 0.9645(7) 0.212(6) Uani 1 1 d . . .
F3 F 0.1693(4) 0.3601(5) 0.8125(10) 0.136(3) Uani 1 1 d . . .
F4 F -0.0091(4) 0.3696(4) 0.8001(15) 0.205(6) Uani 1 1 d . . .
K K 0.0000 0.5000 0.5581(2) 0.0426(4) Uani 1 2 d S . .
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'
Cl Cl 0.1484 0.1585 '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'
Re Re -1.0185 7.2310 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
H H 0.0000 0.0000 '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 Re O1A 180.000(7) . . ?
O1 Re C1 89.5(3) . . ?
O1A Re C1 90.5(3) . . ?
O1 Re C1 89.5(3) . 4 ?
O1A Re C1 90.5(3) . 4 ?
C1 Re C1 89.995(6) . 4 ?
O1 Re C1 89.5(3) . 3 ?
O1A Re C1 90.5(3) . 3 ?
C1 Re C1 178.9(5) . 3 ?
C1 Re C1 89.995(6) 4 3 ?
O1 Re C1 89.5(3) . 2 ?
O1A Re C1 90.5(3) . 2 ?
C1 Re C1 89.995(6) . 2 ?
C1 Re C1 178.9(5) 4 2 ?
C1 Re C1 89.995(6) 3 2 ?
O1 Re Cl1 180.000(5) . . ?
O1A Re Cl1 0.000(1) . . ?
C1 Re Cl1 90.5(3) . . ?
C1 Re Cl1 90.5(3) 4 . ?
C1 Re Cl1 90.5(3) 3 . ?
C1 Re Cl1 90.5(3) 2 . ?
O1 Re Cl1A 0.000(4) . . ?
O1A Re Cl1A 180.000(1) . . ?
C1 Re Cl1A 89.5(3) . . ?
C1 Re Cl1A 89.5(3) 4 . ?
C1 Re Cl1A 89.5(3) 3 . ?
C1 Re Cl1A 89.5(3) 2 . ?
Cl1 Re Cl1A 180.000(1) . . ?
O1 Cl1A Re 0.000(11) . . ?
Cl1A O1 Re 180.000(2) . . ?
N2 C1 N5 104.3(4) . . ?
N2 C1 Re 128.6(4) . . ?
N5 C1 Re 127.1(4) . . ?
C1 N2 C3 110.9(4) . . ?
C1 N2 C8 128.2(5) . . ?
C3 N2 C8 120.9(5) . . ?
C4 C3 N2 106.6(5) . . ?
C4 C3 C6 128.9(5) . . ?
N2 C3 C6 124.5(5) . . ?
C3 C4 N5 107.3(5) . . ?
C3 C4 C7 129.9(5) . . ?
N5 C4 C7 122.6(5) . . ?
C1 N5 C4 110.9(4) . . ?
C1 N5 C9 126.8(5) . . ?
C4 N5 C9 122.0(4) . . ?
N2 C8 C10 113.9(5) . . ?
N5 C9 C11 112.1(6) . . ?
F4 P F6 90.0(7) . . ?
F4 P F2 91.8(7) . . ?
F6 P F2 177.1(7) . . ?
F4 P F1 93.4(4) . . ?
F6 P F1 91.1(4) . . ?
F2 P F1 91.1(4) . . ?
F4 P F3 179.5(7) . . ?
F6 P F3 90.5(6) . . ?
F2 P F3 87.7(5) . . ?
F1 P F3 86.6(4) . . ?
F4 P F5 85.2(4) . . ?
F6 P F5 89.1(3) . . ?
F2 P F5 88.7(3) . . ?
F1 P F5 178.6(3) . . ?
F3 P F5 94.8(4) . . ?
F4 P K 64.2(5) . . ?
F6 P K 130.5(3) . . ?
F2 P K 48.7(2) . . ?
F1 P K 129.4(3) . . ?
F3 P K 115.4(4) . . ?
F5 P K 49.66(19) . . ?
F4 P K 68.0(4) . 6 ?
F6 P K 46.3(2) . 6 ?
F2 P K 132.6(2) . 6 ?
F1 P K 130.7(2) . 6 ?
F3 P K 112.4(3) . 6 ?
F5 P K 48.86(19) . 6 ?
K P K 84.33(4) . 6 ?
P F5 K 105.8(2) . 6 ?
P F5 K 104.7(2) . . ?
K F5 K 117.48(19) 6 . ?
P F2 K 107.3(3) . . ?
P F6 K 110.4(3) . 6 ?
P F4 K 91.2(4) . . ?
P F4 K 87.5(5) . 6 ?
K F4 K 94.46(19) . 6 ?
F6 K F6 142.0(3) 8_454 6_554 ?
F6 K F5 46.17(18) 8_454 8_454 ?
F6 K F5 97.8(2) 6_554 8_454 ?
F6 K F5 97.8(2) 8_454 6_554 ?
F6 K F5 46.17(18) 6_554 6_554 ?
F5 K F5 62.6(2) 8_454 6_554 ?
F6 K F2 99.4(4) 8_454 . ?
F6 K F2 92.2(4) 6_554 . ?
F5 K F2 91.73(19) 8_454 . ?
F5 K F2 120.1(2) 6_554 . ?
F6 K F2 92.2(4) 8_454 3_565 ?
F6 K F2 99.4(4) 6_554 3_565 ?
F5 K F2 120.1(2) 8_454 3_565 ?
F5 K F2 91.73(19) 6_554 3_565 ?
F2 K F2 143.8(3) . 3_565 ?
F6 K F5 122.8(2) 8_454 . ?
F6 K F5 90.9(2) 6_554 . ?
F5 K F5 136.95(13) 8_454 . ?
F5 K F5 136.95(13) 6_554 . ?
F2 K F5 45.66(17) . . ?
F2 K F5 99.61(17) 3_565 . ?
F6 K F5 90.9(2) 8_454 3_565 ?
F6 K F5 122.8(2) 6_554 3_565 ?
F5 K F5 136.95(13) 8_454 3_565 ?
F5 K F5 136.95(13) 6_554 3_565 ?
F2 K F5 99.61(17) . 3_565 ?
F2 K F5 45.66(17) 3_565 3_565 ?
F5 K F5 62.4(2) . 3_565 ?
F6 K F4 126.2(2) 8_454 3_565 ?
F6 K F4 83.2(3) 6_554 3_565 ?
F5 K F4 160.73(19) 8_454 3_565 ?
F5 K F4 107.0(2) 6_554 3_565 ?
F2 K F4 107.5(2) . 3_565 ?
F2 K F4 41.4(2) 3_565 3_565 ?
F5 K F4 62.03(19) . 3_565 ?
F5 K F4 39.85(19) 3_565 3_565 ?
F6 K F4 83.2(3) 8_454 . ?
F6 K F4 126.2(2) 6_554 . ?
F5 K F4 107.0(2) 8_454 . ?
F5 K F4 160.73(19) 6_554 . ?
F2 K F4 41.4(2) . . ?
F2 K F4 107.5(2) 3_565 . ?
F5 K F4 39.85(19) . . ?
F5 K F4 62.03(19) 3_565 . ?
F4 K F4 87.4(4) 3_565 . ?
F6 K F4 39.4(3) 8_454 8_454 ?
F6 K F4 106.7(2) 6_554 8_454 ?
F5 K F4 38.64(16) 8_454 8_454 ?
F5 K F4 60.5(2) 6_554 8_454 ?
F2 K F4 127.7(2) . 8_454 ?
F2 K F4 81.5(2) 3_565 8_454 ?
F5 K F4 162.1(2) . 8_454 ?
F5 K F4 108.8(2) 3_565 8_454 ?
F4 K F4 122.59(11) 3_565 8_454 ?
F4 K F4 122.59(11) . 8_454 ?
F6 K F4 106.7(2) 8_454 6_554 ?
F6 K F4 39.4(3) 6_554 6_554 ?
F5 K F4 60.5(2) 8_454 6_554 ?
F5 K F4 38.64(16) 6_554 6_554 ?
F2 K F4 81.5(2) . 6_554 ?
F2 K F4 127.7(2) 3_565 6_554 ?
F5 K F4 108.8(2) . 6_554 ?
F5 K F4 162.1(2) 3_565 6_554 ?
F4 K F4 122.59(11) 3_565 6_554 ?
F4 K F4 122.59(11) . 6_554 ?
F4 K F4 83.7(4) 8_454 6_554 ?
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
Re O1 1.64(4) . ?
Re O1A 1.85(2) . ?
Re C1 2.195(4) . ?
Re C1 2.195(4) 4 ?
Re C1 2.195(4) 3 ?
Re C1 2.195(4) 2 ?
Re Cl1 2.280(12) . ?
Re Cl1A 2.289(6) . ?
Cl1A O1 0.65(4) . ?
C1 N2 1.353(8) . ?
C1 N5 1.368(7) . ?
N2 C3 1.402(7) . ?
N2 C8 1.465(7) . ?
C3 C4 1.338(8) . ?
C3 C6 1.470(8) . ?
C4 N5 1.382(7) . ?
C4 C7 1.493(8) . ?
N5 C9 1.470(7) . ?
C8 C10 1.503(10) . ?
C9 C11 1.517(11) . ?
P F4 1.498(6) . ?
P F6 1.527(7) . ?
P F2 1.532(7) . ?
P F1 1.557(5) . ?
P F3 1.559(7) . ?
P F5 1.607(5) . ?
P K 3.594(2) . ?
P K 3.611(2) 6 ?
F5 K 2.826(5) 6 ?
F5 K 2.832(5) . ?
F2 K 2.827(6) . ?
F6 K 2.783(6) 6 ?
F4 K 3.236(12) . ?
F4 K 3.351(11) 6 ?
K F6 2.783(6) 8_454 ?
K F6 2.783(6) 6_554 ?
K F5 2.826(5) 8_454 ?
K F5 2.826(5) 6_554 ?
K F2 2.827(6) 3_565 ?
K F5 2.832(5) 3_565 ?
K F4 3.236(12) 3_565 ?
K F4 3.351(11) 8_454 ?
K F4 3.351(12) 6_554 ?
