#------------------------------------------------------------------------------
#$Date: 2016-04-05 18:43:53 +0300 (Tue, 05 Apr 2016) $
#$Revision: 181636 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/86/7038694.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_7038694
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 H92 P8 Re2 Si2, 2(F6 P), 2(C H2 Cl2)'
_chemical_formula_sum            'C40 H96 Cl4 F12 P10 Re2 Si2'
_chemical_formula_weight         1685.27
_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                   16.0272(4)
_cell_length_b                   15.8081(3)
_cell_length_c                   14.4694(3)
_cell_measurement_reflns_used    8995
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.7005
_cell_measurement_theta_min      2.5366
_cell_volume                     3665.96(14)
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18981
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  30
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.752
_exptl_absorpt_correction_T_max  0.487
_exptl_absorpt_correction_T_min  0.379
_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            red
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         5804
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0308
_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)+(0.0362P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                4285
_reflns_number_total             5804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04768d2.cif
_cod_data_source_block           6[PF6]2_ccdc859308
_cod_depositor_comments
'Adding full bibliography for 7038690--7038695.cif.'
_cod_database_code               7038694
_publcif_datablock.id            {b2f34fd2-f8a7-44fe-bf34-0ea6bb3599d5}
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 0.8988(3) 0.0577(3) 0.4817(5) 0.030(2) Uani 0.50 1 d P
C2 C 0.9721(3) 0.0097(4) 0.4676(4) 0.0371(15) Uani 0.50 1 d P
H2 H 1.0000 0.0000 0.402(4) 0.10(2) Uiso 1 2 d S
C3 C 0.7015(3) 0.2090(3) 0.5000 0.0309(9) Uani 1 2 d S
C4 C 0.6431(3) 0.2536(3) 0.5000 0.0434(11) Uani 1 2 d S
C5 C 0.5640(9) 0.4072(6) 0.4122(8) 0.129(3) Uani 0.50 1 d PD
H5A H 0.6049 0.4465 0.4345 0.193 Uiso 0.50 1 calc PR
H5B H 0.5120 0.4360 0.4027 0.193 Uiso 0.50 1 calc PR
H5C H 0.5826 0.3833 0.3548 0.193 Uiso 0.50 1 calc PR
C6 C 0.4604(5) 0.2525(5) 0.4535(8) 0.129(3) Uani 0.50 1 d PD
H6A H 0.4778 0.2254 0.3973 0.193 Uiso 0.50 1 calc PR
H6B H 0.4129 0.2877 0.4413 0.193 Uiso 0.50 1 calc PR
H6C H 0.4458 0.2103 0.4984 0.193 Uiso 1 2 calc SR
C7 C 0.5425(10) 0.3746(6) 0.6145(7) 0.129(3) Uani 0.50 1 d PD
H7A H 0.5228 0.3356 0.6604 0.193 Uiso 0.50 1 calc PR
H7B H 0.5047 0.4215 0.6101 0.193 Uiso 0.50 1 calc PR
H7C H 0.5968 0.3949 0.6317 0.193 Uiso 0.50 1 calc PR
C8 C 0.7478(3) -0.0794(2) 0.4054(3) 0.0646(11) Uani 1 1 d .
H8A H 0.7154 -0.1300 0.4132 0.097 Uiso 1 1 calc R
H8B H 0.8061 -0.0934 0.4056 0.097 Uiso 1 1 calc R
H8C H 0.7336 -0.0532 0.3476 0.097 Uiso 1 1 calc R
C9 C 0.6130(3) -0.0011(3) 0.5000 0.0466(12) Uani 1 2 d S
H9A H 0.5948 0.0380 0.4534 0.070 Uiso 0.50 1 calc PR
H9B H 0.5939 0.0176 0.5595 0.070 Uiso 0.50 1 calc PR
H9C H 0.5906 -0.0562 0.4871 0.070 Uiso 0.50 1 calc PR
C10 C 0.8500(3) 0.0859(3) 0.2573(3) 0.0690(12) Uani 1 1 d .
H10A H 0.8342 0.0979 0.1947 0.104 Uiso 1 1 calc R
H10B H 0.8452 0.0262 0.2686 0.104 Uiso 1 1 calc R
H10C H 0.9067 0.1033 0.2672 0.104 Uiso 1 1 calc R
C11 C 0.6773(2) 0.1144(2) 0.2959(2) 0.0514(10) Uani 1 1 d .
H11A H 0.6719 0.1282 0.2315 0.077 Uiso 1 1 calc R
H11B H 0.6363 0.1452 0.3308 0.077 Uiso 1 1 calc R
H11C H 0.6687 0.0548 0.3044 0.077 Uiso 1 1 calc R
C12 C 0.7845(2) 0.2501(2) 0.2914(2) 0.0571(10) Uani 1 1 d .
H12A H 0.8396 0.2730 0.2992 0.086 Uiso 1 1 calc R
H12B H 0.7451 0.2843 0.3245 0.086 Uiso 1 1 calc R
H12C H 0.7704 0.2496 0.2270 0.086 Uiso 1 1 calc R
C13 C 0.8796(3) 0.3470(3) 0.5000 0.0438(11) Uani 1 2 d S
H13A H 0.8395 0.3560 0.4517 0.066 Uiso 0.50 1 calc PR
H13B H 0.9274 0.3824 0.4897 0.066 Uiso 0.50 1 calc PR
H13C H 0.8550 0.3607 0.5586 0.066 Uiso 0.50 1 calc PR
C14 C 0.9875(2) 0.2313(2) 0.5955(2) 0.0469(8) Uani 1 1 d .
H14A H 1.0291 0.2743 0.5875 0.070 Uiso 1 1 calc R
H14B H 1.0138 0.1767 0.5955 0.070 Uiso 1 1 calc R
H14C H 0.9591 0.2398 0.6531 0.070 Uiso 1 1 calc R
C15 C 0.5000 0.0000 0.1839(3) 0.0549(13) Uani 1 2 d S
H15A H 0.5431 0.0236 0.1445 0.066 Uiso 0.50 1 calc PR
H15B H 0.4569 -0.0236 0.1445 0.066 Uiso 0.50 1 calc PR
F1 F 0.7027(2) 0.17357(17) -0.07619(15) 0.0949(10) Uani 1 1 d .
F2 F 0.70261(16) 0.03132(16) -0.07770(14) 0.0785(8) Uani 1 1 d .
F3 F 0.6040(2) 0.1009(3) 0.0000 0.0970(13) Uani 1 2 d S
F4 F 0.8001(2) 0.1029(4) 0.0000 0.131(2) Uani 1 2 d S
Si1 Si 0.54900(11) 0.31981(10) 0.5000 0.0849(6) Uani 1 2 d SD
P1 P 0.72557(8) -0.00633(7) 0.5000 0.0394(3) Uani 1 2 d S
P2 P 0.78181(6) 0.14310(6) 0.33593(6) 0.0394(2) Uani 1 1 d .
P3 P 0.91185(7) 0.23690(7) 0.5000 0.0334(2) Uani 1 2 d S
P4 P 0.70433(9) 0.10232(9) 0.0000 0.0453(3) Uani 1 2 d S
Re1 Re 0.808343(9) 0.123653(10) 0.5000 0.02690(5) Uani 1 2 d S
Cl1 Cl 0.45719(6) 0.08026(6) 0.25187(7) 0.0625(3) 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'
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 177.1(4) . .
C2 C2 C1 125.5(7) 5_756 .
C2 C2 H2 108.3(17) 5_756 .
C1 C2 H2 123.9(15) . .
C4 C3 Re1 178.7(4) . .
C3 C4 Si1 177.8(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 C6 H6A 109.5 . .
Si1 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
Si1 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
Si1 C7 H7A 109.5 . .
Si1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si1 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 . .
P1 C9 H9A 109.5 . .
P1 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
P1 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 . .
P2 C12 H12A 109.5 . .
P2 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
P2 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 . .
P3 C14 H14A 109.5 . .
P3 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
P3 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
Cl1 C15 Cl1 111.5(3) . 2_655
Cl1 C15 H15A 109.3 . .
Cl1 C15 H15A 109.3 2_655 .
Cl1 C15 H15B 109.3 . .
Cl1 C15 H15B 109.3 2_655 .
H15A C15 H15B 108.0 . .
C4 Si1 C7 108.0(4) . .
C4 Si1 C7 108.0(4) . 6_556
C7 Si1 C7 124.4(7) . 6_556
C4 Si1 C5 108.2(5) . 6_556
C7 Si1 C5 105.3(5) 6_556 6_556
C4 Si1 C5 108.2(5) . .
C7 Si1 C5 105.3(5) . .
C5 Si1 C5 84.4(8) 6_556 .
C4 Si1 C6 107.1(3) . .
C7 Si1 C6 122.1(6) . .
C7 Si1 C6 84.5(5) 6_556 .
C5 Si1 C6 137.9(6) 6_556 .
C5 Si1 C6 105.4(5) . .
C4 Si1 C6 107.1(3) . 6_556
C7 Si1 C6 84.5(5) . 6_556
C7 Si1 C6 122.1(6) 6_556 6_556
C5 Si1 C6 105.4(5) 6_556 6_556
C5 Si1 C6 137.9(6) . 6_556
C9 P1 C8 102.92(17) . .
C9 P1 C8 102.92(17) . 6_556
C8 P1 C8 97.1(3) . 6_556
C9 P1 Re1 120.24(16) . .
C8 P1 Re1 115.19(13) . .
C8 P1 Re1 115.19(13) 6_556 .
C12 P2 C10 103.17(19) . .
C12 P2 C11 98.10(17) . .
C10 P2 C11 103.25(17) . .
C12 P2 Re1 117.47(12) . .
C10 P2 Re1 116.27(15) . .
C11 P2 Re1 115.97(11) . .
C13 P3 C14 103.53(16) . .
C13 P3 C14 103.53(16) . 6_556
C14 P3 C14 97.3(2) . 6_556
C13 P3 Re1 120.66(17) . .
C14 P3 Re1 114.35(11) . .
C14 P3 Re1 114.35(11) 6_556 .
F4 P4 F1 90.70(19) . 6
F4 P4 F1 90.70(19) . .
F1 P4 F1 88.8(2) 6 .
F4 P4 F2 91.25(19) . .
F1 P4 F2 177.94(18) 6 .
F1 P4 F2 90.55(12) . .
F4 P4 F2 91.25(19) . 6
F1 P4 F2 90.55(12) 6 6
F1 P4 F2 177.94(18) . 6
F2 P4 F2 90.08(18) . 6
F4 P4 F3 179.6(3) . .
F1 P4 F3 89.61(17) 6 .
F1 P4 F3 89.61(17) . .
F2 P4 F3 88.44(15) . .
F2 P4 F3 88.44(15) 6 .
C1 Re1 C1 16.8(4) 6_556 .
C1 Re1 C3 171.2(2) 6_556 .
C1 Re1 C3 171.2(2) . .
C1 Re1 P2 94.0(2) 6_556 6_556
C1 Re1 P2 110.9(2) . 6_556
C3 Re1 P2 77.55(2) . 6_556
C1 Re1 P2 110.9(2) 6_556 .
C1 Re1 P2 94.0(2) . .
C3 Re1 P2 77.55(2) . .
P2 Re1 P2 155.07(4) 6_556 .
C1 Re1 P3 83.00(16) 6_556 .
C1 Re1 P3 83.00(16) . .
C3 Re1 P3 94.57(11) . .
P2 Re1 P3 91.50(2) 6_556 .
P2 Re1 P3 91.50(2) . .
C1 Re1 P1 87.13(16) 6_556 .
C1 Re1 P1 87.13(16) . .
C3 Re1 P1 95.40(11) . .
P2 Re1 P1 90.65(2) 6_556 .
P2 Re1 P1 90.65(2) . .
P3 Re1 P1 170.03(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.414(7) .
C1 Re1 1.805(5) .
C2 C2 1.331(10) 5_756
C2 H2 1.06(5) .
C3 C4 1.172(6) .
C3 Re1 2.179(4) .
C4 Si1 1.836(5) .
C5 Si1 1.892(8) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 Si1 1.898(7) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 Si1 1.873(8) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 P1 1.826(3) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 P1 1.806(4) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 P2 1.819(4) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 P2 1.830(3) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 P2 1.810(4) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 P3 1.815(4) .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 P3 1.840(3) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 Cl1 1.745(3) .
C15 Cl1 1.745(3) 2_655
C15 H15A 0.9700 .
C15 H15B 0.9700 .
F1 P4 1.576(2) .
F2 P4 1.589(2) .
F3 P4 1.608(4) .
F4 P4 1.534(4) .
Si1 C7 1.873(8) 6_556
Si1 C5 1.892(8) 6_556
Si1 C6 1.898(8) 6_556
P1 C8 1.826(3) 6_556
P1 Re1 2.4458(12) .
P2 Re1 2.4314(8) .
P3 C14 1.840(3) 6_556
P3 Re1 2.4407(11) .
P4 F1 1.576(2) 6
P4 F2 1.589(2) 6
Re1 C1 1.805(5) 6_556
Re1 P2 2.4314(8) 6_556
