Phosphine-free pincer-ruthenium catalyzed biofuel production: high rates, yields and turnovers of solventless alcohol alkylation
Das, Kanu; Yasmin, Eileen; Das, Babulal; Srivastava, Hemant Kumar; Kumar, Akshai; Catalysis Science & Technology 10 (2020) 8347–8358; doi:10.1039/D0CY01679A

data_1559301
_publ_section_title
;
 Phosphine-free pincer-ruthenium catalyzed biofuel production: high rates,
 yields and turnovers of solventless alcohol alkylation
;
_journal_issue                   24
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              8347
_journal_page_last               8358
_journal_paper_doi               10.1039/D0CY01679A
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C20 H27 Cl2 N3 O Ru, H2 O, 0.5(C3 H6 O)'
_chemical_formula_sum            'C21.5 H32 Cl2 N3 O2.5 Ru'
_chemical_formula_weight         544.47
_chemical_name_systematic        (Cy2NNN)RuCl2(CO)
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2020-02-27 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.020(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.5519(9)
_cell_length_b                   23.6646(18)
_cell_length_c                   16.9746(12)
_cell_measurement_reflns_used    8853
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.48
_cell_volume                     5029.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1575
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            166251
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2178
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0329P)^2^+58.4231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                6633
_reflns_number_total             8853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0cy01679a2.cif
_cod_data_source_block           kd-481_0ma_a
_cod_depositor_comments
;
Adding full bibliography for 1559301--1559302.cif.

2022-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C43 H64 Cl4 N6 O5 Ru2'
_cod_original_formula_weight         1088.94
_cod_original_formula_moiety         'C43 H64 Cl4 N6 O5 Ru2'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1559301