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_7031580
_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 H24 F23 N2 O7 P3 Ru S'
_chemical_formula_sum            'C40 H24 F23 N2 O7 P3 Ru S'
_chemical_formula_weight         1307.65
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.406(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.080(5)
_cell_length_b                   12.8866(18)
_cell_length_c                   24.761(4)
_cell_measurement_reflns_used    9227
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.46
_cell_measurement_theta_min      2.57
_cell_volume                     10126(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ortep-iii
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8401
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  0.9030
_exptl_absorpt_correction_T_min  0.8784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5168
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
PLATON SQUEEZE was used to remove the disordered solvents 
( As per reviewer?s suggestion we looked into the residual map and found 
that there was diffuse electron density associated with disordered solvent 
in the voids which could not be modelled appropriately.

SQUEEZE was applied and the electron count of 96 electrons per unit cell could
 correspond to a large number of possible combinations of solvent, likely to
 be CH2Cl2, MeOH and water. Hence corresponding to the electron counts in the
 squeeze eight water molecules could be accounted and the molecular formula 
in the INS file was modified. The H atom bond to the Ru atom included in the
 molecular formula and refined) 

whereas triflate ions could be located satisfactorily. 
;
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         8401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                5488
_reflns_number_total             8401
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4dt00295d2.cif
_cod_data_source_block           11c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        10127(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7031580