#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/16/8101677.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_8101677
loop_
_publ_author_name
'B. Aechter'
'J. Knizek'
'H. Nöth'
'W. Beck'
_publ_contact_author
;
Beck, Wolfgang 
Department Chemie
Universität München
Butenandtstr. 5-13
81377  München
Germany
;
_publ_section_title
;
Crystal structure of μ-2,2'-bipyrimidine-hexacarbonyl-bis(triphenylphosphine)
dirhenium(I) bis(trifluormethanesulfonate) acetonitrile tetrasolvate, 
[Re₂(C₈H₆N₄)(CO)₆(C₁₈H₁₅P)₂](F₃CSO₃)₂ · 4CH₃CN
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              110
_journal_page_last               112
_journal_volume                  220
_journal_year                    2005
_chemical_formula_sum            'C60 H48 F6 N8 O12 P2 Re2 S2'
_chemical_formula_weight         1685.52
_chemical_name_systematic
; 
μ-2,2'-bipyrimidine-hexacarbonyl-bis(triphenyl-phosphine-dirhenium(I) 
bis(trifluormethanesulfonate) tetrakis(acetonitrile)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-CIF-file updated by CIFRTF'
_cell_angle_alpha                90.00
_cell_angle_beta                 109.41
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.980
_cell_length_b                   18.1165(2)
_cell_length_c                   14.437
_cell_measurement_reflns_used    133
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      14.72
_cell_measurement_theta_min      3.69
_cell_volume                     3201.94(4)
_computing_cell_refinement       'SMART (V4.C50)'
_computing_data_collection       'SMART (V4.C50)'
_computing_data_reduction        'SAINT (V4.D50)'
_computing_molecular_graphics    'XP (SHELXTL-Ver.5)'
_computing_publication_material  'SHELXL (Sheldrick 1993)'
_computing_structure_refinement  'SHELXL (Sheldrick 1993)'
_computing_structure_solution    'XS (SHELXTL-Ver.5)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens SMART Area-detector'
_diffrn_measurement_method       Hemisphere
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18799
_diffrn_reflns_theta_max         29.36
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.976
_exptl_absorpt_correction_T_max  0.458
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       prism
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.158
_refine_ls_goodness_of_fit_obs   1.164
_refine_ls_hydrogen_treatment    'Riding model, fixed isotropic U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_restrained_S_obs      1.164
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_obs          0.0259
_refine_ls_shift/esd_max         -0.012
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0165P)²+5.9285P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0578
_refine_ls_wR_factor_obs         0.0550
_reflns_number_observed          5948
_reflns_number_total             6604
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            1267-1345.cff
_cod_data_source_block           aech4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+5.9285P] 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^)+(0.0165P)^2^+5.9285P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy-atom-method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        3201.93(4)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               8101677
_publ_section_experimental_prep
;
To 115 mg (0.20 mmol) of (η³-C₃H₅)Re(CO)₃PPh₃ [1,2] in 10 ml of 
dichloromethane 17.9 µl (0.20 mmol) of trifluormethanesulfonic acid 
were added at 0 °C. After 15 min 16 mg (0.10 mmol) of 2,2'-bipyrimidine 
were added and the mixture was allowed to warm up to room temperature. The 
color of the solution changed from colorless to yellow and finally red. After 
1 h the red precipitate was centrifuged off, washed with n-pentane and dried in 
vacuo. Red powder was obtained. Red crystals were grown during cooling of a 
solution in acetonitrile (yield 100 mg, 66 %; m.p. 260 °C, 
decomposition). Elemental analysis: found - C, 40.70 %; H, 2.40 %; N, 3.69 %; 
calc. for C₅₂H₃₆F₆N₄O₁₂P₂Re₂S₂ - C, 
41.05 %; H, 2.39 %; N 3.68.
;
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re1 Re 0.570498(10) 0.871906(6) 0.130346(9) 0.01752(5) Uani 1 4 e d . .
P1 P 0.63773(7) 0.95405(5) 0.27678(6) 0.0190(2) Uani 1 4 e d . .
N1 N 0.6282(2) 0.95325(14) 0.0467(2) 0.0171(5) Uani 1 4 e d . .
N2 N 0.4286(2) 0.94293(14) 0.0603(2) 0.0179(5) Uani 1 4 e d . .
N3 N 0.3569(5) 1.1373(3) 0.1479(3) 0.074(2) Uani 1 4 e d . .
N4 N 0.7074(4) 1.2378(3) 0.4847(4) 0.0698(14) Uani 1 4 e d . .
O1 O 0.5122(2) 0.76142(15) -0.0438(2) 0.0364(6) Uani 1 4 e d . .
O2 O 0.4556(2) 0.7675(2) 0.2335(2) 0.0400(7) Uani 1 4 e d . .
O3 O 0.7846(2) 0.7851(2) 0.2088(2) 0.0403(7) Uani 1 4 e d . .
O4 O 0.9499(6) 1.4663(2) 0.3673(5) 0.135(3) Uani 1 4 e d . .
O5 O 0.8856(4) 1.3575(2) 0.4231(5) 0.110(2) Uani 1 4 e d . .
O6 O 1.0667(3) 1.3612(3) 0.4177(3) 0.0854(14) Uani 1 4 e d . .
S1 S 0.95836(11) 1.38943(7) 0.37907(12) 0.0600(4) Uani 1 4 e d . .
F1 F 0.8106(6) 1.3592(4) 0.2137(7) 0.252(5) Uani 1 4 e d . .
F2 F 0.9674(8) 1.3839(3) 0.2031(4) 0.190(4) Uani 1 4 e d . .
F3 F 0.9311(4) 1.2818(2) 0.2559(4) 0.128(2) Uani 1 4 e d . .
C1 C 0.5303(3) 0.8039(2) 0.0173(3) 0.0245(7) Uani 1 4 e d . .
C2 C 0.4997(3) 0.8059(2) 0.1960(2) 0.0259(7) Uani 1 4 e d . .
C3 C 0.7046(3) 0.8175(2) 0.1809(2) 0.0250(7) Uani 1 4 e d . .
C4 C 0.3255(3) 0.9363(2) 0.0628(2) 0.0228(7) Uani 1 4 e d . .
H4A H 0.3090(3) 0.8983(2) 0.0989(2) 0.027 Uiso 1 4 e calc R .
C5 C 0.2451(3) 0.9849(2) 0.0128(2) 0.0240(7) Uani 1 4 e d . .
H5A H 0.1747(3) 0.9802(2) 0.0153(2) 0.029 Uiso 1 4 e calc R .
C6 C 0.2702(3) 1.0411(2) -0.0414(2) 0.0215(7) Uani 1 4 e d . .
H6A H 0.2168(3) 1.0751(2) -0.0741(2) 0.026 Uiso 1 4 e calc R .
C7 C 0.4454(2) 0.9972(2) 0.0038(2) 0.0160(6) Uani 1 4 e d . .
C8 C 0.5404(3) 1.0006(2) 0.3235(2) 0.0242(7) Uani 1 4 e d . .
C9 C 0.5681(3) 1.0657(2) 0.3770(3) 0.0345(9) Uani 1 4 e d . .
H9A H 0.6349(3) 1.0881(2) 0.3849(3) 0.041 Uiso 1 4 e calc R .
C10 C 0.4969(4) 1.0975(2) 0.4187(3) 0.0423(10) Uani 1 4 e d . .
H10A H 0.5163(4) 1.1410(2) 0.4544(3) 0.051 Uiso 1 4 e calc R .
C11 C 0.3984(4) 1.0652(3) 0.4077(3) 0.0455(11) Uani 1 4 e d . .
H11A H 0.3507(4) 1.0869(3) 0.4356(3) 0.055 Uiso 1 4 e calc R .
C12 C 0.3697(4) 1.0003(3) 0.3551(3) 0.0444(11) Uani 1 4 e d . .
H12A H 0.3029(4) 0.9782(3) 0.3480(3) 0.053 Uiso 1 4 e calc R .
C13 C 0.4400(3) 0.9679(2) 0.3127(3) 0.0324(8) Uani 1 4 e d . .
H13A H 0.4200(3) 0.9244(2) 0.2771(3) 0.039 Uiso 1 4 e calc R .
C14 C 0.7308(3) 0.9116(2) 0.3888(2) 0.0239(7) Uani 1 4 e d . .
C15 C 0.7245(3) 0.8369(2) 0.4085(3) 0.0292(8) Uani 1 4 e d . .
H15A H 0.6745(3) 0.8070(2) 0.3628(3) 0.035 Uiso 1 4 e calc R .
C16 C 0.7926(4) 0.8066(2) 0.4962(3) 0.0362(9) Uani 1 4 e d . .
H16A H 0.7879(4) 0.7565(2) 0.5085(3) 0.043 Uiso 1 4 e calc R .
C17 C 0.8658(3) 0.8496(3) 0.5640(3) 0.0410(10) Uani 1 4 e d . .
H17A H 0.9110(3) 0.8288(3) 0.6223(3) 0.049 Uiso 1 4 e calc R .
C18 C 0.8733(4) 0.9250(3) 0.5464(3) 0.0445(11) Uani 1 4 e d . .
H18A H 0.9232(4) 0.9545(3) 0.5927(3) 0.053 Uiso 1 4 e calc R .
C19 C 0.8055(3) 0.9553(2) 0.4592(3) 0.0348(9) Uani 1 4 e d . .
H19A H 0.8100(3) 1.0055(2) 0.4475(3) 0.042 Uiso 1 4 e calc R .
C20 C 0.7192(3) 1.0276(2) 0.2493(2) 0.0229(7) Uani 1 4 e d . .
C21 C 0.8272(3) 1.0134(2) 0.2567(3) 0.0293(8) Uani 1 4 e d . .
H21A H 0.8598(3) 0.9692(2) 0.2842(3) 0.035 Uiso 1 4 e calc R .
C22 C 0.8866(3) 1.0646(2) 0.2235(3) 0.0364(9) Uani 1 4 e d . .
H22A H 0.9589(3) 1.0549(2) 0.2296(3) 0.044 Uiso 1 4 e calc R .
C23 C 0.8385(4) 1.1296(2) 0.1818(3) 0.0414(10) Uani 1 4 e d . .
H23A H 0.8781(4) 1.1635(2) 0.1587(3) 0.050 Uiso 1 4 e calc R .
C24 C 0.7313(4) 1.1449(2) 0.1741(3) 0.0377(9) Uani 1 4 e d . .
H24A H 0.6997(4) 1.1893(2) 0.1467(3) 0.045 Uiso 1 4 e calc R .
C25 C 0.6709(3) 1.0942(2) 0.2069(3) 0.0291(8) Uani 1 4 e d . .
H25A H 0.5987(3) 1.1044(2) 0.2009(3) 0.035 Uiso 1 4 e calc R .
C26 C 0.9153(7) 1.3532(4) 0.2555(7) 0.102(3) Uani 1 4 e d . .
C27 C 0.1685(5) 1.1293(3) 0.1704(4) 0.070(2) Uani 1 4 e d . .
H27A H 0.1184(10) 1.1620(18) 0.1248(22) 0.105 Uiso 1 4 e calc R .
H27B H 0.1746(8) 1.1430(23) 0.2363(10) 0.105 Uiso 1 4 e calc R .
H27C H 0.1422(16) 1.0795(6) 0.1581(31) 0.105 Uiso 1 4 e calc R .
C28 C 0.2746(6) 1.1345(3) 0.1584(3) 0.0571(15) Uani 1 4 e d . .
C29 C 0.8824(5) 1.1857(3) 0.4618(5) 0.066(2) Uani 1 4 e d . .
H29A H 0.8641(7) 1.1626(20) 0.3985(13) 0.099 Uiso 1 4 e calc R .
H29B H 0.9148(19) 1.1499(17) 0.5121(18) 0.099 Uiso 1 4 e calc R .
H29C H 0.9332(14) 1.2251(5) 0.4661(30) 0.099 Uiso 1 4 e calc R .
C30 C 0.7839(4) 1.2151(3) 0.4749(4) 0.0516(12) Uani 1 4 e 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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C3 Re1 C2 90.82(15) . . ?
C3 Re1 C1 87.21(14) . . ?
C2 Re1 C1 88.91(14) . . ?
C3 Re1 N1 97.02(12) . . ?
C2 Re1 N1 172.10(13) . . ?
C1 Re1 N1 90.54(11) . . ?
C3 Re1 N2 171.93(12) . . ?
C2 Re1 N2 97.20(13) . . ?
C1 Re1 N2 91.97(12) . . ?
N1 Re1 N2 74.95(9) . . ?
C3 Re1 P1 88.07(10) . . ?
C2 Re1 P1 92.46(10) . . ?
C1 Re1 P1 175.10(10) . . ?
N1 Re1 P1 88.76(7) . . ?
N2 Re1 P1 92.53(7) . . ?
C8 P1 C20 105.4(2) . . ?
C8 P1 C14 101.6(2) . . ?
C20 P1 C14 103.8(2) . . ?
C8 P1 Re1 119.93(12) . . ?
C20 P1 Re1 108.42(11) . . ?
C14 P1 Re1 116.09(12) . . ?
C7 N1 C6 116.9(3) 3_675 3_675 ?
C7 N1 Re1 116.1(2) 3_675 . ?
C6 N1 Re1 127.0(2) 3_675 . ?
C7 N2 C4 116.3(3) . . ?
C7 N2 Re1 115.3(2) . . ?
C4 N2 Re1 128.3(2) . . ?
O4 S1 O5 114.9(3) . . ?
O4 S1 O6 115.6(4) . . ?
O5 S1 O6 113.2(3) . . ?
O4 S1 C26 104.7(4) . . ?
O5 S1 C26 105.0(4) . . ?
O6 S1 C26 101.4(3) . . ?
O1 C1 Re1 175.3(3) . . ?
O2 C2 Re1 178.4(3) . . ?
O3 C3 Re1 178.4(3) . . ?
N2 C4 C5 120.9(3) . . ?
C4 C5 C6 119.2(3) . . ?
N1 C6 C5 120.3(3) 3_675 . ?
N1 C7 N2 126.4(3) 3_675 . ?
N1 C7 C7 116.5(3) 3_675 3_675 ?
N2 C7 C7 117.1(3) . 3_675 ?
C9 C8 C13 118.8(3) . . ?
C9 C8 P1 121.0(3) . . ?
C13 C8 P1 120.0(3) . . ?
C10 C9 C8 120.5(4) . . ?
C11 C10 C9 120.4(4) . . ?
C10 C11 C12 119.9(4) . . ?
C11 C12 C13 120.4(4) . . ?
C12 C13 C8 120.0(4) . . ?
C15 C14 C19 118.5(3) . . ?
C15 C14 P1 121.4(3) . . ?
C19 C14 P1 119.9(3) . . ?
C14 C15 C16 120.4(4) . . ?
C17 C16 C15 120.6(4) . . ?
C16 C17 C18 120.2(4) . . ?
C19 C18 C17 119.4(4) . . ?
C18 C19 C14 120.9(4) . . ?
C21 C20 C25 119.0(3) . . ?
C21 C20 P1 119.3(3) . . ?
C25 C20 P1 121.1(3) . . ?
C22 C21 C20 120.6(4) . . ?
C23 C22 C21 120.0(4) . . ?
C22 C23 C24 120.2(4) . . ?
C23 C24 C25 120.4(4) . . ?
C24 C25 C20 119.8(4) . . ?
F2 C26 F1 111.4(9) . . ?
F2 C26 F3 108.4(9) . . ?
F1 C26 F3 102.9(7) . . ?
F2 C26 S1 111.7(5) . . ?
F1 C26 S1 111.2(8) . . ?
F3 C26 S1 110.9(6) . . ?
N3 C28 C27 178.6(5) . . ?
N4 C30 C29 179.7(6) . . ?
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 C3 1.921(4) . ?
Re1 C2 1.937(4) . ?
Re1 C1 1.972(4) . ?
Re1 N1 2.188(3) . ?
Re1 N2 2.199(3) . ?
Re1 P1 2.4938(8) . ?
P1 C8 1.824(3) . ?
P1 C20 1.825(3) . ?
P1 C14 1.835(3) . ?
N1 C7 1.337(4) 3_675 ?
N1 C6 1.351(4) 3_675 ?
N2 C7 1.341(4) . ?
N2 C4 1.356(4) . ?
N3 C28 1.128(8) . ?
N4 C30 1.125(6) . ?
O1 C1 1.134(4) . ?
O2 C2 1.144(4) . ?
O3 C3 1.144(4) . ?
O4 S1 1.402(4) . ?
O5 S1 1.424(4) . ?
O6 S1 1.425(4) . ?
S1 C26 1.807(9) . ?
F1 C26 1.295(10) . ?
F2 C26 1.295(11) . ?
F3 C26 1.309(7) . ?
C4 C5 1.372(5) . ?
C5 C6 1.388(5) . ?
C6 N1 1.351(4) 3_675 ?
C7 N1 1.337(4) 3_675 ?
C7 C7 1.461(6) 3_675 ?
C8 C9 1.391(5) . ?
C8 C13 1.393(5) . ?
C9 C10 1.383(5) . ?
C10 C11 1.367(7) . ?
C11 C12 1.382(6) . ?
C12 C13 1.386(5) . ?
C14 C15 1.392(5) . ?
C14 C19 1.394(5) . ?
C15 C16 1.394(5) . ?
C16 C17 1.360(6) . ?
C17 C18 1.399(6) . ?
C18 C19 1.388(5) . ?
C20 C21 1.394(5) . ?
C20 C25 1.403(5) . ?
C21 C22 1.389(5) . ?
C22 C23 1.375(6) . ?
C23 C24 1.386(6) . ?
C24 C25 1.389(5) . ?
C27 C28 1.447(8) . ?
C29 C30 1.454(7) . ?
