#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:37:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179338 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/35/4323533.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_4323533
loop_
_publ_author_name
'Suzanne Bélanger'
'André L. Beauchamp'
_publ_section_title
;
 Oxo Ligand Reactivity in the [ReO2L4]+ Complex of 1-Methylimidazole.
 Preparation and Crystal Structures of Salts Containing the ReOL43+ Core
 and Apical CH3O-, BF3O2-, and (CH3O)2PO2- Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3640
_journal_page_last               3647
_journal_paper_doi               10.1021/ic970067w
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         'Re P2 F12 O2 N8 C17 H27'
_chemical_formula_sum            'C17 H27 F12 N8 O2 P2 Re'
_chemical_formula_weight         851.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-93 (Sheldrick,1995)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.022(3)
_cell_length_b                   13.022
_cell_length_c                   17.218(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      22.00
_cell_measurement_theta_min      20.00
_cell_volume                     2919.7(11)
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1995)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device       'Nonius CAD-4'
_diffrn_measurement_method       'Theta/2theta scan b/P/b'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           'Copper K\a'
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17948
_diffrn_reflns_theta_max         69.73
_diffrn_reflns_theta_min         4.80
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    9.93
_exptl_absorpt_correction_T_max  0.3355
_exptl_absorpt_correction_T_min  0.0666
_exptl_absorpt_correction_type   integration
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.00057(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-93 (Sheldrick,1995)'
_refine_ls_goodness_of_fit_all   0.916
_refine_ls_goodness_of_fit_obs   1.027
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_restrained_S_obs      1.027
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_obs          0.0271
_refine_ls_shift/esd_max         0.964
_refine_ls_shift/esd_mean        0.044
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0483P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0758
_refine_ls_wR_factor_obs         0.0698
_reflns_number_observed          979
_reflns_number_total             1396
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970067w_1.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4323533
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'-x+1/2, y, z+1/2'
'y, x, z+1/2'
'x, -y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'
'x-1/2, -y, -z-1/2'
'-y, -x, -z-1/2'
'-x, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re Re 0.2500 0.2500 0.03544(2) 0.0533(2) Uani 1 d S .
O1 O 0.2500 0.2500 -0.0633(4) 0.073(2) Uani 1 d S .
O2 O 0.2500 0.2500 0.1430(3) 0.0552(11) Uani 1 d S .
C2 C 0.2500 0.2500 0.2262(5) 0.077(3) Uani 1 d S .
N11 N 0.5563(3) 0.3506(3) 0.0765(2) 0.0702(9) Uani 1 d . .
C21 C 0.4668(3) 0.3098(4) 0.0967(2) 0.0721(12) Uani 1 d . .
H21 H 0.4511(3) 0.2872(4) 0.1465(2) 0.086 Uiso 1 calc R .
N31 N 0.4029(3) 0.3054(3) 0.0374(2) 0.0569(8) Uani 1 d . .
C41 C 0.4575(4) 0.3457(4) -0.0243(2) 0.0720(12) Uani 1 d . .
H41 H 0.4329(4) 0.3525(4) -0.0748(2) 0.086 Uiso 1 calc R .
C51 C 0.5503(4) 0.3730(4) -0.0004(3) 0.0789(13) Uani 1 d . .
H51 H 0.6017(4) 0.4021(4) -0.0307(3) 0.095 Uiso 1 calc R .
C61 C 0.6420(4) 0.3709(5) 0.1281(3) 0.106(2) Uani 1 d . .
H61A H 0.6168(5) 0.3965(35) 0.1768(11) 0.158 Uiso 1 calc R .
H61B H 0.6865(20) 0.4210(28) 0.1049(13) 0.158 Uiso 1 calc R .
H61C H 0.6796(22) 0.3085(9) 0.1368(22) 0.158 Uiso 1 calc R .
P1 P 0.42698(11) 0.57302(11) 0.2500 0.0834(5) Uani 1 d S .
F1 F 0.4509(5) 0.5924(5) 0.3352(2) 0.211(3) Uani 1 d . .
F2 F 0.5426(7) 0.5723(13) 0.2296(8) 0.222(7) Uani 0.70 d P 1
F3 F 0.4252(16) 0.6812(8) 0.2295(9) 0.304(11) Uani 0.70 d P 1
F4 F 0.3450(17) 0.6550(17) 0.2500 0.247(28) Uani 0.30 d SP 2
F5 F 0.4983(12) 0.5017(12) 0.2500 0.285(28) Uani 0.30 d SP 2
F6 F 0.3240(19) 0.5130(13) 0.2683(9) 0.108(7) Uani 0.30 d P 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Re Re -5.7900 5.8910 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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 O2 180.0 . . ?
O1 Re N31 90.89(8) . 3 ?
O2 Re N31 89.11(8) . 3 ?
O1 Re N31 90.89(8) . . ?
O2 Re N31 89.11(8) . . ?
N31 Re N31 178.21(15) 3 . ?
O1 Re N31 90.89(8) . 4 ?
O2 Re N31 89.11(8) . 4 ?
N31 Re N31 89.986(9) 3 4 ?
N31 Re N31 89.986(8) . 4 ?
O1 Re N31 90.89(8) . 2 ?
O2 Re N31 89.11(8) . 2 ?
N31 Re N31 89.986(8) 3 2 ?
N31 Re N31 89.986(8) . 2 ?
N31 Re N31 178.22(15) 4 2 ?
C2 O2 Re 180.0 . . ?
C21 N11 C51 106.9(4) . . ?
C21 N11 C61 126.0(4) . . ?
C51 N11 C61 127.0(4) . . ?
N31 C21 N11 111.7(4) . . ?
N31 C21 H21 124.2(2) . . ?
N11 C21 H21 124.2(2) . . ?
C21 N31 C41 104.7(4) . . ?
C21 N31 Re 128.3(3) . . ?
C41 N31 Re 126.9(3) . . ?
C51 C41 N31 109.4(4) . . ?
C51 C41 H41 125.3(3) . . ?
N31 C41 H41 125.3(3) . . ?
C41 C51 N11 107.3(4) . . ?
C41 C51 H51 126.3(3) . . ?
N11 C51 H51 126.4(3) . . ?
N11 C61 H61A 109.5(3) . . ?
N11 C61 H61B 109.5(3) . . ?
H61A C61 H61B 109.5 . . ?
N11 C61 H61C 109.4(3) . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
F3 P1 F3 91.6(16) 14_666 . ?
F5 P1 F4 179.900(4) . . ?
F5 P1 F1 88.4(3) . 14_666 ?
F3 P1 F1 94.4(7) 14_666 14_666 ?
F3 P1 F1 87.8(7) . 14_666 ?
F4 P1 F1 91.6(3) . 14_666 ?
F5 P1 F1 88.4(3) . . ?
F3 P1 F1 87.8(7) 14_666 . ?
F3 P1 F1 94.4(7) . . ?
F4 P1 F1 91.6(3) . . ?
F1 P1 F1 176.8(6) 14_666 . ?
F3 P1 F2 88.1(8) 14_666 14_666 ?
F3 P1 F2 178.9(10) . 14_666 ?
F1 P1 F2 91.2(6) 14_666 14_666 ?
F1 P1 F2 86.6(6) . 14_666 ?
F3 P1 F2 178.9(11) 14_666 . ?
F3 P1 F2 88.1(8) . . ?
F1 P1 F2 86.6(6) 14_666 . ?
F1 P1 F2 91.2(6) . . ?
F2 P1 F2 92.3(13) 14_666 . ?
F5 P1 F6 104.4(9) . 14_666 ?
F4 P1 F6 75.5(9) . 14_666 ?
F1 P1 F6 93.7(6) 14_666 14_666 ?
F1 P1 F6 87.1(6) . 14_666 ?
F5 P1 F6 104.5(9) . . ?
F4 P1 F6 75.6(9) . . ?
F1 P1 F6 87.1(6) 14_666 . ?
F1 P1 F6 93.7(6) . . ?
F6 P1 F6 151.1(18) 14_666 . ?
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 1.701(6) . ?
Re O2 1.852(6) . ?
Re N31 2.118(3) 3 ?
Re N31 2.118(3) . ?
Re N31 2.118(3) 4 ?
Re N31 2.118(3) 2 ?
O2 C2 1.433(8) . ?
N11 C21 1.326(5) . ?
N11 C51 1.359(6) . ?
N11 C61 1.451(6) . ?
C21 N31 1.319(5) . ?
C21 H21 0.93 . ?
N31 C41 1.381(5) . ?
C41 C51 1.325(7) . ?
C41 H41 0.93 . ?
C51 H51 0.93 . ?
C61 H61A 0.96 . ?
C61 H61B 0.96 . ?
C61 H61C 0.96 . ?
P1 F5 1.31(2) . ?
P1 F3 1.452(10) 14_666 ?
P1 F3 1.452(10) . ?
P1 F4 1.51(3) . ?
P1 F1 1.521(4) 14_666 ?
P1 F1 1.521(4) . ?
P1 F2 1.546(9) 14_666 ?
P1 F2 1.546(9) . ?
P1 F6 1.58(2) 14_666 ?
P1 F6 1.58(2) . ?
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
O1 Re O2 C2 0.0 . . . . ?
N31 Re O2 C2 25.1(1000) 3 . . . ?
N31 Re O2 C2 -154.9(1000) . . . . ?
N31 Re O2 C2 -64.9(1000) 4 . . . ?
N31 Re O2 C2 115.1(1000) 2 . . . ?
C51 N11 C21 N31 -0.5(6) . . . . ?
C61 N11 C21 N31 177.2(5) . . . . ?
N11 C21 N31 C41 0.5(6) . . . . ?
N11 C21 N31 Re -179.1(3) . . . . ?
O1 Re N31 C21 -167.2(4) . . . . ?
O2 Re N31 C21 12.8(4) . . . . ?
N31 Re N31 C21 12.8(4) 3 . . . ?
N31 Re N31 C21 -76.3(4) 4 . . . ?
N31 Re N31 C21 101.9(4) 2 . . . ?
O1 Re N31 C41 13.2(4) . . . . ?
O2 Re N31 C41 -166.8(4) . . . . ?
N31 Re N31 C41 -166.8(4) 3 . . . ?
N31 Re N31 C41 104.0(4) 4 . . . ?
N31 Re N31 C41 -77.7(4) 2 . . . ?
C21 N31 C41 C51 -0.3(5) . . . . ?
Re N31 C41 C51 179.3(3) . . . . ?
N31 C41 C51 N11 0.0(6) . . . . ?
C21 N11 C51 C41 0.3(5) . . . . ?
C61 N11 C51 C41 -177.4(5) . . . . ?
