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_1554189
_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         'C29 H29 Cl2 O2 P Ru, H2 O'
_chemical_formula_sum            'C29 H31 Cl2 O3 P Ru'
_chemical_formula_weight         630.51
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2016-06-12
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.11.03 svn.r3071 for OlexSys, GUI svn.r4932)
;
_audit_update_record
;
2017-10-20 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.550(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0354(5)
_cell_length_b                   12.4751(12)
_cell_length_c                   22.0590(13)
_cell_volume                     2756.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9954
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39789
_diffrn_reflns_theta_full        67.0000
_diffrn_reflns_theta_max         72.41
_diffrn_reflns_theta_min         4.02
_exptl_absorpt_coefficient_mu    7.169
_exptl_crystal_density_diffrn    1.5193
_exptl_crystal_F_000             1295.3795
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.5822
_refine_diff_density_min         -0.2508
_refine_diff_density_rms         0.0787
_refine_ls_d_res_high            0.8087
_refine_ls_d_res_low             11.0083
_refine_ls_goodness_of_fit_ref   1.0449
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5435
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0446
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+1.0373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0641
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -10
_reflns_number_gt                5007
_reflns_number_total             5435
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8cy00265g2.cif
_cod_data_source_block           darkwa164
_cod_original_cell_volume        2756.3(4)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1554189
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-H2 = O3-H3b = O3-H3a
 0.79698 with sigma of 0.005
3.a Ternary CH refined with riding coordinates:
 C2(H2a), C7(H7)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29)
3.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c)
;
_olex2_submission_special_instructions 'No special instructions were received'