#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:33:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179116 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/78/4307833.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_4307833
loop_
_publ_author_name
'F. Albert Cotton'
'Naresh S. Dalal'
'Penglin Huang'
'Sergey A. Ibragimov'
'Carlos A. Murillo'
'Paula M. B. Piccoli'
'Chris M. Ramsey'
'Arthur J. Schultz'
'Xiaoping Wang'
'Qinliang Zhao'
_publ_section_title
;
Better Understanding of the Species with the Shortest Re26+ Bonds and
Related Re27+ Species with Tetraguanidinate Paddlewheel Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1718
_journal_page_last               1726
_journal_paper_doi               10.1021/ic062319b
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C32 H48 F6 N12 O4 Re2, 2(C H2 Cl2'
_chemical_formula_sum            'C34 H52 Cl4 F6 N12 O4 Re2'
_chemical_formula_weight         1321.08
_chemical_name_common            Re2(hpp)4(CF3CO2)2,4CH2Cl2
_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                93.392(6)
_cell_angle_beta                 103.510(5)
_cell_angle_gamma                95.500(6)
_cell_formula_units_Z            1
_cell_length_a                   9.459(3)
_cell_length_b                   10.728(4)
_cell_length_c                   11.194(4)
_cell_measurement_reflns_used    5659
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.0855
_cell_measurement_theta_min      2.2286
_cell_volume                     1095.5(7)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6557
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         1.88
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.843
_exptl_absorpt_correction_T_max  0.277
_exptl_absorpt_correction_T_min  0.176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.196
_refine_diff_density_min         -1.349
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0074(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4600
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0309P)²+0.3147P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                4386
_reflns_number_total             4600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062319bsi20061205_023430_2.cif
_cod_data_source_block           xl2
_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_cell_volume        1095.5(6)
_cod_database_code               4307833
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 -0.041444(11) 0.054635(10) -0.076579(9) 0.01686(6) Uani 1 1 d . . .
N1 N 0.0828(3) 0.2182(2) 0.0100(2) 0.0220(5) Uani 1 1 d . . .
N2 N 0.1657(3) 0.1056(2) 0.1763(2) 0.0200(5) Uani 1 1 d . . .
N3 N 0.2422(3) 0.3248(3) 0.1899(2) 0.0277(6) Uani 1 1 d . . .
N4 N 0.1252(3) 0.0215(3) -0.1619(2) 0.0223(5) Uani 1 1 d . . .
N5 N 0.2064(3) -0.1050(2) -0.0069(2) 0.0211(5) Uani 1 1 d . . .
N6 N 0.3243(3) -0.0931(3) -0.1705(3) 0.0333(7) Uani 1 1 d . . .
C1 C 0.0819(4) 0.3374(3) -0.0480(3) 0.0342(8) Uani 1 1 d . . .
H1A H 0.0068 0.3849 -0.0262 0.041 Uiso 1 1 calc R . .
H1B H 0.0575 0.3202 -0.1379 0.041 Uiso 1 1 calc R . .
C2 C 0.2289(4) 0.4146(3) -0.0065(3) 0.0344(8) Uani 1 1 d . . .
H2B H 0.2270 0.4939 -0.0458 0.041 Uiso 1 1 calc R . .
H2C H 0.3044 0.3687 -0.0298 0.041 Uiso 1 1 calc R . .
C3 C 0.2623(4) 0.4405(3) 0.1318(3) 0.0386(9) Uani 1 1 d . . .
H3A H 0.3635 0.4793 0.1624 0.046 Uiso 1 1 calc R . .
H3B H 0.1974 0.4995 0.1534 0.046 Uiso 1 1 calc R . .
C4 C 0.2999(5) 0.3355(4) 0.3232(3) 0.0418(9) Uani 1 1 d . . .
H4A H 0.2749 0.4137 0.3588 0.050 Uiso 1 1 calc R . .
H4B H 0.4068 0.3391 0.3421 0.050 Uiso 1 1 calc R . .
C5 C 0.2387(4) 0.2260(3) 0.3803(3) 0.0319(7) Uani 1 1 d . . .
H5B H 0.1368 0.2344 0.3816 0.038 Uiso 1 1 calc R . .
H5C H 0.2951 0.2238 0.4654 0.038 Uiso 1 1 calc R . .
C6 C 0.2465(4) 0.1065(3) 0.3057(3) 0.0293(7) Uani 1 1 d . . .
H6A H 0.3493 0.0967 0.3088 0.035 Uiso 1 1 calc R . .
H6B H 0.2061 0.0348 0.3423 0.035 Uiso 1 1 calc R . .
C7 C 0.1630(3) 0.2169(3) 0.1262(3) 0.0215(6) Uani 1 1 d . . .
C8 C 0.1554(4) 0.0838(4) -0.2676(3) 0.0357(8) Uani 1 1 d . . .
H8A H 0.2406 0.1471 -0.2401 0.043 Uiso 1 1 calc R . .
H8B H 0.0712 0.1261 -0.3064 0.043 Uiso 1 1 calc R . .
C9 C 0.1851(5) -0.0142(4) -0.3598(3) 0.0445(10) Uani 1 1 d . . .
H9A H 0.1015 -0.0794 -0.3849 0.053 Uiso 1 1 calc R . .
H9B H 0.1996 0.0253 -0.4335 0.053 Uiso 1 1 calc R . .
C10 C 0.3204(5) -0.0717(5) -0.2998(4) 0.0468(10) Uani 1 1 d . . .
H10A H 0.3228 -0.1519 -0.3456 0.056 Uiso 1 1 calc R . .
H10B H 0.4073 -0.0158 -0.3033 0.056 Uiso 1 1 calc R . .
C11 C 0.4445(4) -0.1634(4) -0.1136(4) 0.0436(10) Uani 1 1 d . . .
H11A H 0.5381 -0.1156 -0.1137 0.052 Uiso 1 1 calc R . .
H11B H 0.4372 -0.2437 -0.1624 0.052 Uiso 1 1 calc R . .
C12 C 0.4408(4) -0.1879(5) 0.0171(4) 0.0469(10) Uani 1 1 d . . .
H12A H 0.4949 -0.2592 0.0424 0.056 Uiso 1 1 calc R . .
H12B H 0.4869 -0.1139 0.0732 0.056 Uiso 1 1 calc R . .
C13 C 0.2836(4) -0.2164(3) 0.0229(3) 0.0343(8) Uani 1 1 d . . .
H13A H 0.2364 -0.2880 -0.0360 0.041 Uiso 1 1 calc R . .
H13B H 0.2791 -0.2386 0.1058 0.041 Uiso 1 1 calc R . .
C14 C 0.2190(3) -0.0593(3) -0.1136(3) 0.0214(6) Uani 1 1 d . . .
C15 C -0.1851(4) 0.2340(3) -0.3331(3) 0.0297(7) Uani 1 1 d D . .
O1 O -0.1588(3) 0.1682(2) -0.2443(2) 0.0289(5) Uani 1 1 d . A .
O2 O -0.1009(17) 0.2793(17) -0.3953(16) 0.047(3) Uani 0.58(3) 1 d PU A 1
O2A O -0.105(2) 0.313(2) -0.365(2) 0.047(3) Uani 0.42(3) 1 d P A 2
C16 C -0.3525(5) 0.2373(8) -0.3855(10) 0.0287(12) Uani 0.83(5) 1 d PD A 1
F1 F -0.4269(17) 0.2640(15) -0.3024(6) 0.065(3) Uani 0.83(5) 1 d PD A 1
F2 F -0.4113(13) 0.1261(9) -0.4423(9) 0.0500(14) Uani 0.83(5) 1 d PD A 1
F3 F -0.3789(11) 0.3193(9) -0.4697(11) 0.0627(14) Uani 0.83(5) 1 d PDU A 1
C16A C -0.3447(17) 0.247(3) -0.405(3) 0.0287(12) Uani 0.17(5) 1 d PD A 2
F1A F -0.390(5) 0.295(5) -0.311(3) 0.065(3) Uani 0.17(5) 1 d PD A 2
F2A F -0.435(4) 0.144(4) -0.452(4) 0.0500(14) Uani 0.17(5) 1 d PD A 2
F3A F -0.365(5) 0.329(4) -0.490(3) 0.0627(14) Uani 0.17(5) 1 d PD A 2
C1S C 0.160(3) 0.514(3) 0.623(2) 0.030(2) Uani 0.431(4) 1 d PD B 1
H1SA H 0.1642 0.5589 0.5500 0.036 Uiso 0.431(4) 1 calc PR B 1
H1SB H 0.0876 0.4404 0.5954 0.036 Uiso 0.431(4) 1 calc PR B 1
Cl1 Cl 0.089(2) 0.6126(19) 0.7201(15) 0.0627(13) Uani 0.431(4) 1 d PD B 1
Cl2 Cl 0.3332(18) 0.457(2) 0.674(3) 0.0512(12) Uani 0.431(4) 1 d PD B 1
C1SA C 0.151(2) 0.476(3) 0.619(3) 0.030(2) Uani 0.19(2) 1 d PD C 2
H1SC H 0.1435 0.5030 0.5359 0.036 Uiso 0.19(2) 1 calc PR C 2
H1SD H 0.1024 0.3903 0.6133 0.036 Uiso 0.19(2) 1 calc PR C 2
Cl1A Cl 0.080(3) 0.580(2) 0.710(2) 0.0627(13) Uani 0.19(2) 1 d PD C 2
Cl2A Cl 0.3375(16) 0.487(2) 0.7038(16) 0.0512(12) Uani 0.19(2) 1 d PD C 2
C1SB C 0.158(3) 0.494(3) 0.600(3) 0.030(2) Uani 0.38(2) 1 d PD D 3
H1SE H 0.1759 0.5306 0.5258 0.036 Uiso 0.38(2) 1 calc PR D 3
H1SF H 0.0803 0.4241 0.5749 0.036 Uiso 0.38(2) 1 calc PR D 3
Cl1B Cl 0.108(2) 0.6088(19) 0.6966(15) 0.0627(13) Uani 0.38(2) 1 d PD D 3
Cl2B Cl 0.321(2) 0.442(3) 0.687(3) 0.0512(12) Uani 0.38(2) 1 d PD D 3
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'
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'
Cl Cl 0.1484 0.1585 '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
N1 Re1 N4 88.63(11) . . ?
N1 Re1 N2 175.81(8) . 2 ?
N4 Re1 N2 89.04(10) . 2 ?
N1 Re1 N5 87.49(10) . 2 ?
N4 Re1 N5 174.90(9) . 2 ?
N2 Re1 N5 94.63(10) 2 2 ?
N1 Re1 Re1 92.97(7) . 2 ?
N4 Re1 Re1 93.42(7) . 2 ?
N2 Re1 Re1 90.64(7) 2 2 ?
N5 Re1 Re1 90.08(7) 2 2 ?
N1 Re1 O1 90.51(9) . . ?
N4 Re1 O1 91.58(9) . . ?
N2 Re1 O1 86.07(9) 2 . ?
N5 Re1 O1 85.15(9) 2 . ?
Re1 Re1 O1 173.97(6) 2 . ?
C7 N1 C1 118.5(3) . . ?
C7 N1 Re1 118.8(2) . . ?
C1 N1 Re1 122.6(2) . . ?
C7 N2 C6 117.0(3) . . ?
C7 N2 Re1 119.9(2) . 2 ?
C6 N2 Re1 122.7(2) . 2 ?
C7 N3 C3 122.7(3) . . ?
C7 N3 C4 122.5(3) . . ?
C3 N3 C4 114.6(3) . . ?
C14 N4 C8 116.3(3) . . ?
C14 N4 Re1 118.1(2) . . ?
C8 N4 Re1 125.5(2) . . ?
C14 N5 C13 114.4(3) . . ?
C14 N5 Re1 120.3(2) . 2 ?
C13 N5 Re1 122.8(2) . 2 ?
C14 N6 C11 123.9(3) . . ?
C14 N6 C10 122.8(3) . . ?
C11 N6 C10 113.1(3) . . ?
N1 C1 C2 110.8(3) . . ?
C1 C2 C3 108.1(3) . . ?
N3 C3 C2 110.5(3) . . ?
N3 C4 C5 111.1(3) . . ?
C4 C5 C6 108.9(3) . . ?
N2 C6 C5 112.2(3) . . ?
N1 C7 N2 117.5(3) . . ?
N1 C7 N3 121.0(3) . . ?
N2 C7 N3 121.5(3) . . ?
N4 C8 C9 109.0(3) . . ?
C10 C9 C8 108.6(3) . . ?
N6 C10 C9 111.6(3) . . ?
N6 C11 C12 111.4(3) . . ?
C13 C12 C11 108.6(3) . . ?
N5 C13 C12 109.2(3) . . ?
N5 C14 N4 117.8(3) . . ?
N5 C14 N6 121.1(3) . . ?
N4 C14 N6 121.1(3) . . ?
O2A C15 O1 129.4(11) . . ?
O1 C15 O2 129.6(8) . . ?
O2A C15 C16 116.1(12) . . ?
O1 C15 C16 112.2(5) . . ?
O2 C15 C16 117.2(9) . . ?
O2A C15 C16A 107.3(18) . . ?
O1 C15 C16A 121.9(14) . . ?
O2 C15 C16A 107.2(16) . . ?
C15 O1 Re1 164.6(2) . . ?
F2 C16 F1 107.1(3) . . ?
F2 C16 F3 106.1(3) . . ?
F1 C16 F3 107.1(4) . . ?
F2 C16 C15 109.2(7) . . ?
F1 C16 C15 115.3(10) . . ?
F3 C16 C15 111.7(6) . . ?
F1A C16A F2A 107.1(9) . . ?
F1A C16A F3A 106.5(9) . . ?
F2A C16A F3A 106.5(8) . . ?
F1A C16A C15 97(2) . . ?
F2A C16A C15 120(3) . . ?
F3A C16A C15 119(3) . . ?
Cl1 C1S Cl2 121.9(18) . . ?
Cl1A C1SA Cl2A 101.3(16) . . ?
Cl1B C1SB Cl2B 106.4(18) . . ?
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
Re1 N1 2.066(3) . ?
Re1 N4 2.073(3) . ?
Re1 N2 2.087(3) 2 ?
Re1 N5 2.093(3) 2 ?
Re1 Re1 2.1711(5) 2 ?
Re1 O1 2.408(2) . ?
N1 C7 1.346(4) . ?
N1 C1 1.468(4) . ?
N2 C7 1.349(4) . ?
N2 C6 1.470(4) . ?
N2 Re1 2.087(3) 2 ?
N3 C7 1.377(4) . ?
N3 C3 1.452(4) . ?
N3 C4 1.457(4) . ?
N4 C14 1.346(4) . ?
N4 C8 1.463(4) . ?
N5 C14 1.343(4) . ?
N5 C13 1.475(4) . ?
N5 Re1 2.093(3) 2 ?
N6 C14 1.367(4) . ?
N6 C11 1.466(5) . ?
N6 C10 1.472(5) . ?
C1 C2 1.505(5) . ?
C2 C3 1.510(5) . ?
C4 C5 1.502(5) . ?
C5 C6 1.506(5) . ?
C8 C9 1.521(6) . ?
C9 C10 1.506(6) . ?
C11 C12 1.510(6) . ?
C12 C13 1.507(5) . ?
C15 O2A 1.21(2) . ?
C15 O1 1.245(4) . ?
C15 O2 1.257(16) . ?
C15 C16 1.560(5) . ?
C15 C16A 1.560(10) . ?
C16 F2 1.325(4) . ?
C16 F1 1.325(4) . ?
C16 F3 1.325(4) . ?
C16A F1A 1.322(8) . ?
C16A F2A 1.324(8) . ?
C16A F3A 1.325(8) . ?
C1S Cl1 1.756(11) . ?
C1S Cl2 1.782(11) . ?
C1SA Cl1A 1.755(15) . ?
C1SA Cl2A 1.783(16) . ?
C1SB Cl1B 1.761(12) . ?
C1SB Cl2B 1.779(13) . ?
