#------------------------------------------------------------------------------
#$Date: 2016-04-05 18:43:53 +0300 (Tue, 05 Apr 2016) $
#$Revision: 181636 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/86/7038695.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_7038695
loop_
_publ_author_name
'Li, Yan'
'Blacque, Olivier'
'Fox, Thomas'
'Luber, Sandra'
'Polit, Walther'
'Winter, Rainer F.'
'Venkatesan, Koushik'
'Berke, Heinz'
_publ_section_title
;
 Electronic communication in phosphine substituted bridged dirhenium
 complexes - clarifying ambiguities raised by the redox non-innocence of
 the C4H2- and C4-bridges.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5783
_journal_page_last               5799
_journal_paper_doi               10.1039/c5dt04768d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C38 H90 P8 Re2 Si2, 2(F6 P), 2(C H2 Cl2)'
_chemical_formula_sum            'C40 H94 Cl4 F12 P10 Re2 Si2'
_chemical_formula_weight         1683.25
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-08-05 deposited with the CCDC.
2016-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.2406(2)
_cell_length_b                   15.7552(2)
_cell_length_c                   14.4581(2)
_cell_measurement_reflns_used    15757
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.7742
_cell_measurement_theta_min      2.5797
_cell_volume                     3699.45(8)
_computing_cell_refinement
;
CrysAlisPro, version 1.171.33.41
;
_computing_data_collection
;
CrysAlisPro, version 1.171.33.41 (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlisPro, version 1.171.33.41
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and/or Mercury (Macrae et
al.,
2006)
;
_computing_publication_material
; 
WinGX (Farrugia, 1999), PLATON for Windows (Spek, 2003) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement  ' SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    ' SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31036
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  40
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.718
_exptl_absorpt_correction_T_max  0.570
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.33.41 (Oxford diffraction, 2009).
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1676
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.678
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         5859
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0394P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                4500
_reflns_number_total             5859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04768d2.cif
_cod_data_source_block           7[PF6]2_ccdc859309
_cod_depositor_comments
'Adding full bibliography for 7038690--7038695.cif.'
_cod_database_code               7038695
_publcif_datablock.id            {f6213d1e-dee2-4ac8-90d7-fac0b5193909}
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x-1/2, y-1/2, z-1/2'
'x-1/2, -y-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
C1 C 0.3935(2) 0.0587(2) 0.5000 0.0325(8) Uani 1 2 d S
C2 C 0.4671(2) 0.0170(3) 0.5000 0.0401(9) Uani 1 2 d S
C3 C 0.1982(2) 0.2106(3) 0.5000 0.0318(8) Uani 1 2 d S
C4 C 0.1394(3) 0.2563(3) 0.5000 0.0436(10) Uani 1 2 d S
C5 C -0.0383(5) 0.2532(5) 0.5445(7) 0.135(3) Uani 0.50 1 d PD
H5A H -0.0409 0.2017 0.5091 0.202 Uiso 0.50 1 calc PR
H5B H -0.0896 0.2831 0.5392 0.202 Uiso 0.50 1 calc PR
H5C H -0.0281 0.2398 0.6082 0.202 Uiso 0.50 1 calc PR
C6A C 0.0514(10) 0.4073(6) 0.5862(7) 0.135(3) Uani 0.50 1 d PD
H6A1 H 0.0609 0.3838 0.6465 0.202 Uiso 0.50 1 calc PR
H6A2 H 0.0004 0.4381 0.5863 0.202 Uiso 0.50 1 calc PR
H6A3 H 0.0956 0.4451 0.5705 0.202 Uiso 0.50 1 calc PR
C6B C 0.0455(10) 0.3708(6) 0.3842(7) 0.135(3) Uani 0.50 1 d PD
H6B1 H 0.0962 0.4008 0.3749 0.202 Uiso 0.50 1 calc PR
H6B2 H 0.0002 0.4098 0.3800 0.202 Uiso 0.50 1 calc PR
H6B3 H 0.0397 0.3278 0.3375 0.202 Uiso 0.50 1 calc PR
C7 C 0.2439(2) -0.0778(2) 0.4054(2) 0.0564(9) Uani 1 1 d .
H7A H 0.2135 -0.1295 0.4139 0.085 Uiso 1 1 calc R
H7B H 0.3017 -0.0902 0.4046 0.085 Uiso 1 1 calc R
H7C H 0.2283 -0.0521 0.3478 0.085 Uiso 1 1 calc R
C8 C 0.1101(2) 0.0000(3) 0.5000 0.0435(10) Uani 1 2 d S
H8A H 0.0922 0.0424 0.5433 0.065 Uiso 0.50 1 calc PR
H8B H 0.0879 -0.0542 0.5175 0.065 Uiso 0.50 1 calc PR
H8C H 0.0910 0.0146 0.4392 0.065 Uiso 0.50 1 calc PR
C9 C 0.1737(2) 0.1169(2) 0.7047(2) 0.0476(8) Uani 1 1 d .
H9A H 0.1680 0.1326 0.7686 0.071 Uiso 1 1 calc R
H9B H 0.1657 0.0568 0.6984 0.071 Uiso 1 1 calc R
H9C H 0.1332 0.1463 0.6685 0.071 Uiso 1 1 calc R
C10 C 0.2801(2) 0.2526(2) 0.7083(2) 0.0570(9) Uani 1 1 d .
H10A H 0.2440 0.2880 0.6724 0.085 Uiso 1 1 calc R
H10B H 0.3354 0.2739 0.7040 0.085 Uiso 1 1 calc R
H10C H 0.2628 0.2531 0.7718 0.085 Uiso 1 1 calc R
C11 C 0.3448(2) 0.0874(2) 0.7420(2) 0.0575(9) Uani 1 1 d .
H11A H 0.4008 0.1038 0.7303 0.086 Uiso 1 1 calc R
H11B H 0.3389 0.0275 0.7316 0.086 Uiso 1 1 calc R
H11C H 0.3308 0.1004 0.8049 0.086 Uiso 1 1 calc R
C12 C 0.48024(17) 0.2307(2) 0.59554(18) 0.0442(7) Uani 1 1 d .
H12A H 0.5212 0.2742 0.5888 0.066 Uiso 1 1 calc R
H12B H 0.5063 0.1760 0.5944 0.066 Uiso 1 1 calc R
H12C H 0.4520 0.2381 0.6533 0.066 Uiso 1 1 calc R
C13 C 0.3762(3) 0.3488(3) 0.5000 0.0505(11) Uani 1 2 d S
H13A H 0.4246 0.3838 0.5007 0.076 Uiso 1 2 calc SR
H13B H 0.3435 0.3606 0.5538 0.076 Uiso 0.50 1 calc PR
H13C H 0.3446 0.3609 0.4454 0.076 Uiso 0.50 1 calc PR
Si1 Si 0.04594(10) 0.32051(10) 0.5000 0.0850(6) Uani 1 2 d SD
P1 P 0.22129(6) -0.00523(7) 0.5000 0.0343(2) Uani 1 2 d S
P2 P 0.27651(5) 0.14514(5) 0.66426(5) 0.03484(16) Uani 1 1 d .
P3 P 0.40598(6) 0.23815(6) 0.5000 0.0331(2) Uani 1 2 d S
Re1 Re 0.302490(8) 0.125464(9) 0.5000 0.02370(5) Uani 1 2 d S
P4 P 0.20021(7) 0.10806(8) 1.0000 0.0428(3) Uani 1 2 d S
F1 F 0.19724(18) 0.17923(17) 0.92382(14) 0.1015(10) Uani 1 1 d .
F2 F 0.2942(2) 0.1094(3) 1.0000 0.133(2) Uani 1 2 d S
F3 F 0.19951(14) 0.03661(15) 0.92214(14) 0.0790(7) Uani 1 1 d .
F4 F 0.1019(2) 0.1042(3) 1.0000 0.1049(13) Uani 1 2 d S
Cl1 Cl -0.04339(5) 0.07994(6) 0.74877(6) 0.0606(2) Uani 1 1 d .
C14 C 0.0000 0.0000 0.8174(3) 0.0539(12) Uani 1 2 d S
H14A H 0.0422 0.0243 0.8568 0.065 Uiso 0.50 1 calc PR
H14B H -0.0422 -0.0243 0.8568 0.065 Uiso 0.50 1 calc PR
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'
Si Si 0.0817 0.0704 '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'
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
C2 C1 Re1 173.3(3) . .
C2 C2 C1 177.8(6) 5_656 .
C4 C3 Re1 178.6(4) . .
C3 C4 Si1 176.7(4) . .
Si1 C5 H5A 109.5 . .
Si1 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
Si1 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
Si1 C6A H6A1 109.5 . .
Si1 C6A H6A2 109.5 . .
H6A1 C6A H6A2 109.5 . .
Si1 C6A H6A3 109.5 . .
H6A1 C6A H6A3 109.5 . .
H6A2 C6A H6A3 109.5 . .
Si1 C6B H6B1 109.5 . .
Si1 C6B H6B2 109.5 . .
H6B1 C6B H6B2 109.5 . .
Si1 C6B H6B3 109.5 . .
H6B1 C6B H6B3 109.5 . .
H6B2 C6B H6B3 109.5 . .
P1 C7 H7A 109.5 . .
P1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
P1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
P1 C8 H8A 109.5 . .
P1 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
P1 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
P2 C9 H9A 109.5 . .
P2 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
P2 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
P2 C10 H10A 109.5 . .
P2 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
P2 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
P2 C11 H11A 109.5 . .
P2 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
P2 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
P3 C12 H12A 109.5 . .
P3 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
P3 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
P3 C13 H13A 109.5 . .
P3 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
P3 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C4 Si1 C5 107.3(3) . 6_556
C4 Si1 C5 107.3(3) . .
C4 Si1 C6A 111.7(4) . .
C5 Si1 C6A 133.9(6) 6_556 .
C5 Si1 C6A 103.0(6) . .
C4 Si1 C6A 111.7(4) . 6_556
C5 Si1 C6A 103.0(6) 6_556 6_556
C5 Si1 C6A 133.9(6) . 6_556
C4 Si1 C6B 103.9(4) . 6_556
C6A Si1 C6B 107.0(5) 6_556 6_556
C4 Si1 C6B 103.9(4) . .
C5 Si1 C6B 123.9(6) . .
C6A Si1 C6B 107.0(5) . .
C6B Si1 C6B 129.3(7) 6_556 .
C8 P1 C7 103.28(15) . 6_556
C8 P1 C7 103.28(15) . .
C7 P1 C7 97.4(2) 6_556 .
C8 P1 Re1 120.02(15) . .
C7 P1 Re1 114.89(12) 6_556 .
C7 P1 Re1 114.89(12) . .
C10 P2 C11 103.35(17) . .
C10 P2 C9 98.34(15) . .
C11 P2 C9 103.74(15) . .
C10 P2 Re1 117.20(11) . .
C11 P2 Re1 115.63(12) . .
C9 P2 Re1 116.16(10) . .
C13 P3 C12 103.70(15) . .
C13 P3 C12 103.70(15) . 6_556
C12 P3 C12 97.49(18) . 6_556
C13 P3 Re1 121.06(17) . .
C12 P3 Re1 113.90(10) . .
C12 P3 Re1 113.90(10) 6_556 .
C1 Re1 C3 177.08(15) . .
C1 Re1 P2 102.432(19) . .
C3 Re1 P2 77.575(19) . .
C1 Re1 P2 102.432(19) . 6_556
C3 Re1 P2 77.575(19) . 6_556
P2 Re1 P2 155.13(4) . 6_556
C1 Re1 P3 82.02(12) . .
C3 Re1 P3 95.06(11) . .
P2 Re1 P3 91.531(19) . .
P2 Re1 P3 91.531(19) 6_556 .
C1 Re1 P1 87.18(12) . .
C3 Re1 P1 95.74(10) . .
P2 Re1 P1 90.789(19) . .
P2 Re1 P1 90.789(19) 6_556 .
P3 Re1 P1 169.20(3) . .
F2 P4 F1 91.21(18) . 6_557
F2 P4 F1 91.21(18) . .
F1 P4 F1 88.93(19) 6_557 .
F2 P4 F3 90.95(17) . 6_557
F1 P4 F3 90.50(13) 6_557 6_557
F1 P4 F3 177.77(16) . 6_557
F2 P4 F3 90.95(17) . .
F1 P4 F3 177.77(16) 6_557 .
F1 P4 F3 90.50(13) . .
F3 P4 F3 90.00(18) 6_557 .
F2 P4 F4 178.6(3) . .
F1 P4 F4 89.79(15) 6_557 .
F1 P4 F4 89.79(15) . .
F3 P4 F4 88.05(14) 6_557 .
F3 P4 F4 88.05(14) . .
Cl1 C14 Cl1 111.0(2) 2 .
Cl1 C14 H14A 109.4 2 .
Cl1 C14 H14A 109.4 . .
Cl1 C14 H14B 109.4 2 .
Cl1 C14 H14B 109.4 . .
H14A C14 H14B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.363(5) .
C1 Re1 1.814(4) .
C2 C2 1.197(8) 5_656
C3 C4 1.195(5) .
C3 Re1 2.161(4) .
C4 Si1 1.824(4) .
C5 Si1 1.846(8) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6A Si1 1.853(8) .
C6A H6A1 0.9600 .
C6A H6A2 0.9600 .
C6A H6A3 0.9600 .
C6B Si1 1.853(8) .
C6B H6B1 0.9600 .
C6B H6B2 0.9600 .
C6B H6B3 0.9600 .
C7 P1 1.820(3) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 P1 1.808(4) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 P2 1.825(3) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 P2 1.810(3) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 P2 1.823(3) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 P3 1.837(3) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 P3 1.810(4) .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
Si1 C5 1.846(8) 6_556
Si1 C6A 1.853(8) 6_556
Si1 C6B 1.853(8) 6_556
P1 C7 1.820(3) 6_556
P1 Re1 2.4452(10) .
P2 Re1 2.4319(7) .
P3 C12 1.837(3) 6_556
P3 Re1 2.4447(10) .
Re1 P2 2.4319(7) 6_556
P4 F2 1.527(4) .
P4 F1 1.573(2) 6_557
P4 F1 1.573(2) .
P4 F3 1.592(2) 6_557
P4 F3 1.592(2) .
P4 F4 1.598(4) .
Cl1 C14 1.752(2) .
C14 Cl1 1.752(2) 2
C14 H14A 0.9700 .
C14 H14B 0.9700 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C9 H9A F1 0.96 2.41 3.338(4) 162.8
