Ruthenium molecular complexes immobilized on graphene as active catalysts for the synthesis of carboxylic acids from alcohol dehydrogenation
Ventura-Espinosa, David; Vicent, Cristian; Baya, Miguel; Mata, Jose A.; Catal. Sci. Technol. 6 (2016) 8024–; doi:10.1039/C6CY01455K

data_1544219
_publ_section_title
;
 Ruthenium molecular complexes immobilized on graphene as active catalysts
 for the synthesis of carboxylic acids from alcohol dehydrogenation
;
_journal_issue                   22
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              8024
_journal_paper_doi               10.1039/C6CY01455K
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C21 H21 Cl2 F5 N2 Ru, C H Cl3'
_chemical_formula_sum            'C22 H22 Cl5 F5 N2 Ru'
_chemical_formula_weight         687.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-23
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4963)
;
_audit_update_record
;
2016-07-01 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.922(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9690(4)
_cell_length_b                   10.6225(4)
_cell_length_c                   15.6395(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2651.45(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.899
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29917
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.46
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.146
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.561
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0500P)^2^+6.3950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                5534
_reflns_number_total             6622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cy01455k3.cif
_cod_data_source_block           str1733
_cod_depositor_comments
'Adding full bibliography for 1544219--1544220.cif.'
_cod_original_cell_volume        2651.44(15)
_cod_database_code               1544219
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl33(0.5) Cl34(0.5) Cl32(0.5) H2AA(0.5) H2AB(0.5) Cl(0.5) Cl1(0.5)
 Cl2(0.5)
3.a Ternary CH refined with riding coordinates:
 C2AA(H2AA), C2AA(H2AB), C29(H29)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C8(H8), C28(H28), C27(H27), C7(H7), C24(H24)
3.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'