A binary catalyst system of a cationic Ru-CNC pincer complex with an alkali metal salt for selective hydroboration of carbon dioxide.
Ng, Chee Koon; Wu, Jie; Hor, T. S. Andy; Luo, He-Kuan; Chemical communications (Cambridge, England) 52 (2016) 11842–11845; doi:10.1039/c6cc06278d

data_7125036
_publ_section_title
;
 A binary catalyst system of a cationic Ru-CNC pincer complex with an
 alkali metal salt for selective hydroboration of carbon dioxide.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11842
_journal_page_last               11845
_journal_paper_doi               10.1039/c6cc06278d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C31 H30 Cl3 F6 N6 O P Ru'
_chemical_formula_sum            'C31 H30 Cl3 F6 N6 O P Ru'
_chemical_formula_weight         855.00
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1lnp0y
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-01 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                77.336(14)
_cell_angle_beta                 74.113(10)
_cell_angle_gamma                79.124(10)
_cell_formula_units_Z            2
_cell_length_a                   10.630(4)
_cell_length_b                   12.402(5)
_cell_length_c                   14.118(5)
_cell_measurement_reflns_used    4040
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.232
_cell_measurement_theta_min      2.209
_cell_volume                     1730.1(11)
_computing_cell_refinement
'SHELXTL, Acta Cryst., Sect. A 2008, 64, 112-122.'
_computing_data_collection       'APEX3 v2016.5.0'
_computing_data_reduction        'Saint, APEX v2014.11.0.'
_computing_molecular_graphics    Ortep3
_computing_publication_material  'APEX3 v2016.5.0'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT, Acta Cryst., Sect. A 2015, A71, 3-8.'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker AXS D8 Venture '
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42950
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.232
_diffrn_reflns_theta_min         2.209
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       rod
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.092
_platon_squeeze_details
; 
In the last stage of the refinement some residuals electronic density peaks 
were located in the solvent region, near to the dichloromethane molecule. 
SQUEEZE details:  Solvent accessible volume = 37.9 \%A^3^, (2.2 %) 
for a total volume of: 1730.1(11) \%A^3^, 
electrons found in the Solvent accessible volume. = 3.1.  
These peaks were first attributed to an ether molecule: C~2~H~5~-O-C~2~H~5~, 
in statistic occupancy with CH~2~Cl~2~ molecule.  
However owing to the low intensity of the electronic peaks 
it was not possible to stabilize a chemically correct model, 
even using strong restraints on interatomic lengths and angles.  
No disorder could be resolved.   
Since the solvent region could not be modelled satisfactorily, 
we resorted to the program SQUEEZE  
integrated in the Crystallographic tools:  Platon .  
Then the model was refined using the squeezed data.
;
_refine_diff_density_max         1.228
_refine_diff_density_min         -1.320
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0017(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         8519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+4.3410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7146
_reflns_number_total             8519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06278d2.cif
_cod_data_source_block           g672
_cod_original_cell_volume        1730.0(11)
_cod_database_code               7125036
_shelx_estimated_absorpt_t_min   0.783
_shelx_estimated_absorpt_t_max   0.930
_shelx_res_checksum              93687