Synthesis, characterization and reactivity studies of electrophilic ruthenium(ii) complexes: a study of H2 activation and labilization.
Naidu, K. S.; Patil, Yogesh P.; Nethaji, Munirathinam; Jagirdar, Balaji R.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 13410–13423; doi:10.1039/c4dt00295d

data_7031576
_publ_section_title
;
 Synthesis, characterization and reactivity studies of electrophilic
 ruthenium(ii) complexes: a study of H2 activation and labilization.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13410
_journal_page_last               13423
_journal_paper_doi               10.1039/c4dt00295d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'C40 H21 Cl F20 N2 P3 Ru, SO3CF3,0.5(C7H18O2),H2O'
_chemical_formula_sum            'C43.5 H32 Cl F23 N2 O5 P3 Ru S'
_chemical_formula_weight         1361.20
_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                109.4870(10)
_cell_angle_beta                 94.6870(10)
_cell_angle_gamma                113.2980(10)
_cell_formula_units_Z            4
_cell_length_a                   16.2162(6)
_cell_length_b                   18.2514(7)
_cell_length_c                   20.5416(7)
_cell_measurement_reflns_used    569
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      1.4
_cell_volume                     5101.3(3)
_computing_cell_refinement       'bruker smart apex ccd'
_computing_data_collection       'bruker smart apex ccd'
_computing_data_reduction        'bruker saint'
_computing_molecular_graphics    ortep-iii
_computing_publication_material  WinGXv1.80.05
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    shelxs-97
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.3
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'bruker smart apex ccd'
_diffrn_measurement_method       omega
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            87871
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.9010
_exptl_absorpt_correction_T_min  0.8491
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
PLATON SQUEEZE was used to remove the disordered solvents as per the reviewer
suggestion.
 
The electron count of 185 electrons per unit cell could correspond to the
possible combinations of solvents, likely to be propanol, 2-butanol 
and water. This could not be assigned unambiguously; hence propanol, 
2-butanol and two water molecules were accounted [that is two propanol, 
two 2-butanol and four water molecules in the unit cell] and the molecular
formula was corrected accordingly in the ins file and completed the refinement. 
One of the triflate ion was not modelled properly and attempts were made to 
model triflate ion but were not sucessful.

As the squeeze command was used to remove the disordered solvents
a void is created.
;
_refine_diff_density_max         2.247
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1319
_refine_ls_number_reflns         19796
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+12.2962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                16753
_reflns_number_total             19796
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4dt00295d2.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7031571--7031581.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C43.50 H32 Cl F23 N2 O5 P3 Ru S'
_cod_database_code               7031576