Crystal structure of μ-2,2'-bipyrimidine-hexacarbonyl-bis(triphenylphosphine) dirhenium(I) bis(trifluormethanesulfonate) acetonitrile tetrasolvate, [Re~2~(C~8~H~6~N~4~)(CO)~6~(C~18~H~15~P)~2~](F~3~CSO~3~)~2~ · 4CH~3~CN
B. Aechter; J. Knizek; H. Nöth; W. Beck; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 110–112; doi:

data_8101677
_publ_contact_author
;
Beck, Wolfgang 
Department Chemie
Universit\"at M\"unchen
Butenandtstr. 5-13
81377  M\"unchen
Germany
;
_publ_section_title
;
Crystal structure of \m-2,2'-bipyrimidine-hexacarbonyl-bis(triphenylphosphine)
dirhenium(I) bis(trifluormethanesulfonate) acetonitrile tetrasolvate, 
[Re~2~(C~8~H~6~N~4~)(CO)~6~(C~18~H~15~P)~2~](F~3~CSO~3~)~2~ &#x00B7; 4CH~3~CN
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur 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
; 
\m-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/[\s^2^(Fo^2^)+(0.0165P)^2^+5.9285P] where P=(Fo^2^+2Fc^2^)/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 (\h^3^-C~3~H~5~)Re(CO)~3~PPh~3~ [1,2] in 10 ml of 
dichloromethane 17.9 &#x00B5;l (0.20 mmol) of trifluormethanesulfonic acid 
were added at 0 &#x00B0;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 &#x00B0;C, 
decomposition). Elemental analysis: found - C, 40.70 %; H, 2.40 %; N, 3.69 %; 
calc. for C~52~H~36~F~6~N~4~O~12~P~2~Re~2~S~2~ - C, 
41.05 %; H, 2.39 %; N 3.68.
;