#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:45:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179261 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/81/4318181.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_4318181
loop_
_publ_author_name
'Nadia C. Mösch-Zanetti'
'Sinje Köpke'
'Regine Herbst-Irmer'
'Manuel Hewitt'
_publ_section_title
;
 Unsymmetrical Tren-Based Ligands: Synthesis and Reactivity of Rhenium
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3513
_journal_page_last               3520
_journal_paper_doi               10.1021/ic025572u
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C25 H14 F15 N6 Re'
_chemical_formula_weight         869.62
_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                91.66(3)
_cell_angle_beta                 93.04(3)
_cell_angle_gamma                109.18(3)
_cell_formula_units_Z            2
_cell_length_a                   9.409(2)
_cell_length_b                   11.554(2)
_cell_length_c                   13.180(3)
_cell_measurement_reflns_used    975
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.87
_cell_volume                     1349.7(5)
_computing_cell_refinement       'Siemens SAINT (V. 6.08b, BRUKER 1999)'
_computing_data_collection       'Siemens SMART (V.5.050, Siemens 1998)'
_computing_data_reduction        'Siemens SAINT (V. 6.08b, BRUKER 1999)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type
'STOE-Siemens-Huber four circle diffractometer'
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22326
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    4.636
_exptl_absorpt_correction_T_max  0.6543
_exptl_absorpt_correction_T_min  0.4574
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.336
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.0022(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   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0261
_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)+(0.0322P)²+1.4681P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0619
_reflns_number_gt                6063
_reflns_number_total             6343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025572u_s1_4.cif
_cod_data_source_block           ekzem
_cod_database_code               4318181
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
N100 N 0.5320(3) 0.2058(3) 0.2679(2) 0.0260(6) Uani 1 1 d . . .
N101 N 0.4360(3) 0.2372(3) 0.2543(2) 0.0200(6) Uani 1 1 d . . .
Re1 Re 0.270122(12) 0.299845(11) 0.228445(9) 0.01388(5) Uani 1 1 d . . .
N1 N 0.2530(3) 0.2645(3) 0.0835(2) 0.0192(5) Uani 1 1 d . . .
N2 N 0.3859(3) 0.4684(2) 0.2708(2) 0.0174(5) Uani 1 1 d . . .
N3 N 0.1423(3) 0.1836(2) 0.3166(2) 0.0185(5) Uani 1 1 d . . .
N4 N 0.1006(3) 0.3850(3) 0.1899(2) 0.0200(6) Uani 1 1 d . . .
C1 C 0.1226(4) 0.2848(4) 0.0255(3) 0.0264(7) Uani 1 1 d . . .
H1A H 0.0302 0.2129 0.0286 0.032 Uiso 1 1 calc R . .
H1B H 0.1442 0.2986 -0.0467 0.032 Uiso 1 1 calc R . .
C2 C 0.1029(4) 0.3984(3) 0.0766(3) 0.0260(7) Uani 1 1 d . . .
H2A H 0.1870 0.4724 0.0614 0.031 Uiso 1 1 calc R . .
H2B H 0.0073 0.4081 0.0499 0.031 Uiso 1 1 calc R . .
C3 C 0.3199(4) 0.5660(3) 0.2486(3) 0.0262(8) Uani 1 1 d . . .
H3A H 0.3531 0.6017 0.1830 0.031 Uiso 1 1 calc R . .
H3B H 0.3543 0.6322 0.3027 0.031 Uiso 1 1 calc R . .
C4 C 0.1499(4) 0.5103(3) 0.2434(3) 0.0253(7) Uani 1 1 d . . .
H4A H 0.1145 0.5034 0.3131 0.030 Uiso 1 1 calc R . .
H4B H 0.1044 0.5641 0.2062 0.030 Uiso 1 1 calc R . .
C5 C -0.0169(4) 0.1643(4) 0.3389(3) 0.0267(8) Uani 1 1 d . . .
H5A H -0.0299 0.1423 0.4106 0.032 Uiso 1 1 calc R . .
H5B H -0.0832 0.0938 0.2955 0.032 Uiso 1 1 calc R . .
C6 C -0.0679(4) 0.2736(4) 0.3218(3) 0.0288(8) Uani 1 1 d . . .
H6A H -0.0064 0.3424 0.3686 0.035 Uiso 1 1 calc R . .
H6B H -0.1741 0.2524 0.3396 0.035 Uiso 1 1 calc R . .
C7 C -0.0565(4) 0.3160(3) 0.2143(3) 0.0251(7) Uani 1 1 d . . .
H7A H -0.0976 0.2435 0.1664 0.030 Uiso 1 1 calc R . .
H7B H -0.1195 0.3690 0.2041 0.030 Uiso 1 1 calc R . .
C10 C 0.3430(4) 0.2129(3) 0.0266(2) 0.0195(6) Uani 1 1 d . . .
C11 C 0.4980(4) 0.2684(3) 0.0270(2) 0.0216(7) Uani 1 1 d . . .
C12 C 0.5882(4) 0.2174(3) -0.0263(3) 0.0226(7) Uani 1 1 d . . .
C13 C 0.5241(4) 0.1091(3) -0.0844(3) 0.0246(7) Uani 1 1 d . . .
C14 C 0.3699(4) 0.0541(3) -0.0884(3) 0.0242(7) Uani 1 1 d . . .
C15 C 0.2825(4) 0.1047(3) -0.0331(3) 0.0215(7) Uani 1 1 d . . .
C20 C 0.5392(3) 0.5117(3) 0.3062(2) 0.0169(6) Uani 1 1 d . . .
C21 C 0.5906(4) 0.4662(3) 0.3925(2) 0.0183(6) Uani 1 1 d . . .
C22 C 0.7391(4) 0.5061(3) 0.4290(2) 0.0204(6) Uani 1 1 d . . .
C23 C 0.8450(4) 0.5961(3) 0.3802(3) 0.0234(7) Uani 1 1 d . . .
C24 C 0.7990(4) 0.6428(3) 0.2946(3) 0.0244(7) Uani 1 1 d . . .
C25 C 0.6502(4) 0.5993(3) 0.2580(3) 0.0222(7) Uani 1 1 d . . .
C30 C 0.1896(3) 0.0897(3) 0.3605(2) 0.0163(6) Uani 1 1 d . . .
C31 C 0.1840(4) -0.0152(3) 0.3033(3) 0.0220(7) Uani 1 1 d . . .
C32 C 0.2354(4) -0.1040(3) 0.3437(3) 0.0260(7) Uani 1 1 d . . .
C33 C 0.2938(4) -0.0911(4) 0.4437(3) 0.0310(8) Uani 1 1 d . . .
C34 C 0.2986(4) 0.0102(4) 0.5020(3) 0.0289(8) Uani 1 1 d . . .
C35 C 0.2462(4) 0.0984(3) 0.4614(3) 0.0242(7) Uani 1 1 d . . .
F11 F 0.5665(2) 0.37665(19) 0.07774(17) 0.0288(5) Uani 1 1 d . . .
F12 F 0.7380(2) 0.2740(2) -0.02333(17) 0.0323(5) Uani 1 1 d . . .
F13 F 0.6102(3) 0.0587(2) -0.13444(18) 0.0350(5) Uani 1 1 d . . .
F14 F 0.3064(3) -0.0519(2) -0.14363(19) 0.0375(6) Uani 1 1 d . . .
F15 F 0.1331(2) 0.0448(2) -0.03736(18) 0.0327(5) Uani 1 1 d . . .
F21 F 0.4918(2) 0.38289(18) 0.44603(15) 0.0232(4) Uani 1 1 d . . .
F22 F 0.7816(3) 0.4603(2) 0.51389(17) 0.0338(5) Uani 1 1 d . . .
F23 F 0.9887(2) 0.6393(2) 0.41828(17) 0.0325(5) Uani 1 1 d . . .
F24 F 0.8998(2) 0.7297(2) 0.24560(18) 0.0400(6) Uani 1 1 d . . .
F25 F 0.6137(2) 0.6449(2) 0.17074(17) 0.0349(5) Uani 1 1 d . . .
F31 F 0.1283(2) -0.03057(19) 0.20597(16) 0.0277(4) Uani 1 1 d . . .
F32 F 0.2301(3) -0.2042(2) 0.2865(2) 0.0378(6) Uani 1 1 d . . .
F33 F 0.3442(3) -0.1782(2) 0.4814(2) 0.0465(7) Uani 1 1 d . . .
F34 F 0.3545(3) 0.0224(3) 0.59949(19) 0.0436(6) Uani 1 1 d . . .
F35 F 0.2501(3) 0.1958(2) 0.52148(16) 0.0330(5) 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'
N N 0.0061 0.0033 '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'
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
N100 N101 Re1 177.7(3) . . y
N1 Re1 N2 114.60(12) . . y
N1 Re1 N3 120.12(12) . . y
N2 Re1 N3 123.87(12) . . y
N1 Re1 N101 94.73(11) . . y
N2 Re1 N101 95.06(11) . . y
N3 Re1 N101 92.18(12) . . y
N1 Re1 N4 82.55(11) . . y
N2 Re1 N4 81.11(11) . . y
N3 Re1 N4 94.00(11) . . y
N101 Re1 N4 173.81(11) . . y
C10 N1 C1 116.1(3) . . ?
C10 N1 Re1 127.4(2) . . ?
C1 N1 Re1 116.4(2) . . ?
C20 N2 C3 114.6(3) . . ?
C20 N2 Re1 125.8(2) . . ?
C3 N2 Re1 118.7(2) . . ?
C30 N3 C5 109.4(3) . . ?
C30 N3 Re1 121.1(2) . . ?
C5 N3 Re1 129.1(2) . . ?
C7 N4 C2 108.4(3) . . ?
C7 N4 C4 109.2(3) . . ?
C2 N4 C4 109.5(3) . . ?
C7 N4 Re1 116.3(2) . . ?
C2 N4 Re1 105.4(2) . . ?
C4 N4 Re1 107.89(19) . . ?
N1 C1 C2 105.8(3) . . ?
N4 C2 C1 109.6(3) . . ?
N2 C3 C4 108.6(3) . . ?
N4 C4 C3 110.1(3) . . ?
N3 C5 C6 114.7(3) . . ?
C5 C6 C7 114.3(3) . . ?
N4 C7 C6 113.3(3) . . ?
C11 C10 C15 115.8(3) . . ?
C11 C10 N1 121.6(3) . . ?
C15 C10 N1 122.6(3) . . ?
F11 C11 C10 120.5(3) . . ?
F11 C11 C12 117.2(3) . . ?
C10 C11 C12 122.3(3) . . ?
F12 C12 C13 119.5(3) . . ?
F12 C12 C11 120.2(3) . . ?
C13 C12 C11 120.3(3) . . ?
F13 C13 C14 120.8(3) . . ?
F13 C13 C12 120.6(3) . . ?
C14 C13 C12 118.6(3) . . ?
F14 C14 C13 119.2(3) . . ?
F14 C14 C15 120.5(3) . . ?
C13 C14 C15 120.2(3) . . ?
F15 C15 C14 117.6(3) . . ?
F15 C15 C10 119.7(3) . . ?
C14 C15 C10 122.7(3) . . ?
C25 C20 C21 115.0(3) . . ?
C25 C20 N2 123.6(3) . . ?
C21 C20 N2 121.4(3) . . ?
F21 C21 C22 117.2(3) . . ?
F21 C21 C20 119.8(3) . . ?
C22 C21 C20 123.0(3) . . ?
F22 C22 C21 120.3(3) . . ?
F22 C22 C23 119.7(3) . . ?
C21 C22 C23 119.9(3) . . ?
F23 C23 C24 121.0(3) . . ?
F23 C23 C22 120.1(3) . . ?
C24 C23 C22 118.9(3) . . ?
F24 C24 C23 119.9(3) . . ?
F24 C24 C25 119.9(3) . . ?
C23 C24 C25 120.2(3) . . ?
F25 C25 C24 117.2(3) . . ?
F25 C25 C20 119.7(3) . . ?
C24 C25 C20 123.0(3) . . ?
C31 C30 C35 116.5(3) . . ?
C31 C30 N3 121.2(3) . . ?
C35 C30 N3 122.3(3) . . ?
F31 C31 C32 118.7(3) . . ?
F31 C31 C30 119.6(3) . . ?
C32 C31 C30 121.6(3) . . ?
F32 C32 C31 120.5(4) . . ?
F32 C32 C33 119.1(3) . . ?
C31 C32 C33 120.4(3) . . ?
F33 C33 C34 121.4(4) . . ?
F33 C33 C32 119.4(4) . . ?
C34 C33 C32 119.2(3) . . ?
F34 C34 C33 119.2(4) . . ?
F34 C34 C35 120.6(4) . . ?
C33 C34 C35 120.2(4) . . ?
F35 C35 C34 118.6(3) . . ?
F35 C35 C30 119.3(3) . . ?
C34 C35 C30 122.1(3) . . ?
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
N100 N101 1.087(4) . y
N101 Re1 1.943(3) . y
Re1 N1 1.929(3) . y
Re1 N2 1.941(3) . y
Re1 N3 1.943(3) . y
Re1 N4 2.178(3) . y
N1 C10 1.416(4) . ?
N1 C1 1.498(4) . ?
N2 C20 1.411(4) . ?
N2 C3 1.484(4) . ?
N3 C30 1.427(4) . ?
N3 C5 1.487(4) . ?
N4 C7 1.488(4) . ?
N4 C2 1.506(4) . ?
N4 C4 1.507(4) . ?
C1 C2 1.527(5) . ?
C3 C4 1.513(5) . ?
C5 C6 1.509(5) . ?
C6 C7 1.510(5) . ?
C10 C11 1.387(5) . ?
C10 C15 1.391(5) . ?
C11 F11 1.343(4) . ?
C11 C12 1.388(5) . ?
C12 F12 1.343(4) . ?
C12 C13 1.384(5) . ?
C13 F13 1.332(4) . ?
C13 C14 1.377(5) . ?
C14 F14 1.344(4) . ?
C14 C15 1.381(5) . ?
C15 F15 1.344(4) . ?
C20 C25 1.389(5) . ?
C20 C21 1.396(4) . ?
C21 F21 1.345(4) . ?
C21 C22 1.375(4) . ?
C22 F22 1.348(4) . ?
C22 C23 1.383(5) . ?
C23 F23 1.342(4) . ?
C23 C24 1.373(5) . ?
C24 F24 1.342(4) . ?
C24 C25 1.378(5) . ?
C25 F25 1.353(4) . ?
C30 C31 1.392(5) . ?
C30 C35 1.394(5) . ?
C31 F31 1.344(4) . ?
C31 C32 1.379(5) . ?
C32 F32 1.349(4) . ?
C32 C33 1.385(6) . ?
C33 F33 1.342(4) . ?
C33 C34 1.368(6) . ?
C34 F34 1.347(4) . ?
C34 C35 1.379(5) . ?
C35 F35 1.347(4) . ?
