Homogeneous polymetallic ruthenium(ii)^zinc(ii) complexes: robust catalysts for the efficient hydrogenation of levulinic acid to γ-valerolactone
Amenuvor, Gershon; Darkwa, James; Makhubela, Banothile C. E.; Catalysis Science & Technology 8 (2018) 2370–; doi:10.1039/C8CY00265G

data_1554191
_publ_section_title
;
 Homogeneous polymetallic ruthenium(ii)^zinc(ii) complexes: robust
 catalysts for the efficient hydrogenation of levulinic acid to
 \g-valerolactone
;
_journal_issue                   9
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              2370
_journal_paper_doi               10.1039/C8CY00265G
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C25 H29 Cl2 O2 P Ru'
_chemical_formula_sum            'C25 H29 Cl2 O2 P Ru'
_chemical_formula_weight         564.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-10-20 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.74
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.595(2)
_cell_length_b                   12.873(3)
_cell_length_c                   18.387(4)
_cell_measurement_reflns_used    2244
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.93
_cell_measurement_theta_min      2.56
_cell_volume                     2401.5(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.781
_diffrn_measured_fraction_theta_max 0.811
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_av_unetI/netI     0.2111
_diffrn_reflns_Laue_measured_fraction_full 0.781
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16618
_diffrn_reflns_point_group_measured_fraction_full 0.781
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.666
_diffrn_reflns_theta_min         1.960
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6614
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1358 before and 0.0797 after correction.
The Ratio of minimum to maximum transmission is 0.8870.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_refine_diff_density_max         0.672
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.577
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         5026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.577
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2700
_reflns_number_total             5026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cy00265g2.cif
_cod_data_source_block           15lm_darkwa_ga058
_cod_original_cell_volume        2401.4(9)
_cod_database_code               1554191
_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.a Ternary CH refined with riding coordinates:
 C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              35862
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'