Phosphine-Pyridonate Ligands Containing Octahedral Ruthenium Complexes : Access to Esters and Formic Acid
Sahoo, Apurba Ranjan; Jiang, Fan; Bruneau, Christian; Gangavaram, Sharma; Surisetti, Suresh; Roisnel, Thierry; Dorcet, Vincent; Achard, Mathieu; Catal. Sci. Technol.  (2017) –; doi:10.1039/C7CY00932A

data_1546515
_publ_section_title
;
 Phosphine-Pyridonate Ligands Containing Octahedral Ruthenium Complexes :
 Access to Esters and Formic Acid
;
_journal_name_full               'Catal. Sci. Technol.'
_journal_paper_doi               10.1039/C7CY00932A
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38 H35 N3 O3 P2 Ru, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C38.5 H36 Cl N3 O3 P2 Ru'
_chemical_formula_weight         787.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2016-03-16 deposited with the CCDC.
2017-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.190(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1179(19)
_cell_length_b                   16.1688(19)
_cell_length_c                   15.2936(18)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.65
_cell_measurement_wavelength     0.71073
_cell_volume                     3807.6(8)
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2014)'
_computing_publication_material  'CRYSCALc (T. Roisnel, local program, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            72636
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.685
_diffrn_reflns_theta_min         2.519
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.301
_refine_diff_density_min         -3.850
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details
;
Flack x determined using 6769 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.049(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         72636
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0732
_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^)+(0.1180P)^2^+13.2728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2105
_reflns_number_gt                63493
_reflns_number_total             72636
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cy00932a2.cif
_cod_data_source_block           MAARS772
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group_crystal_system' value 'Monoclinic' changed to
'monoclinic' according to
/home/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 4973 2017-02-22 13:04:09Z antanas 

2019-01-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C38 H35 N3 O3 P2 Ru), C H2 Cl2'
_cod_original_formula_sum        'C77 H72 Cl2 N6 O6 P4 Ru2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1574.32
_cod_database_code               1546515
_shelx_res_checksum              34088