Ruthenium-catalyzed Hydrogenation of CO2 as a Route to Methyl Esters for use as Biofuels or fine Chemicals
Wang, Zheng; Zhao, Ziwei; Li, Yong; Zhong, Yanxia; Zhang, Qiuyue; Liu, Qingbin; Solan, Gregory; Ma, Yanping; Sun, Wen Hua; Chemical Science  (2020) –; doi:10.1039/D0SC02942D

data_1558257
_publ_section_title
;
 Ruthenium-catalyzed Hydrogenation of CO2 as a Route to Methyl Esters for
 use as Biofuels or fine Chemicals
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02942D
_journal_year                    2020
_chemical_formula_moiety         'C51 H53 Cl2 P3 Ru'
_chemical_formula_sum            'C51 H53 Cl2 P3 Ru'
_chemical_formula_weight         930.81
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-10-29 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.826(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4966(4)
_cell_length_b                   21.3798(7)
_cell_length_c                   17.4791(6)
_cell_measurement_reflns_used    10584
_cell_measurement_temperature    173
_cell_measurement_theta_max      31.1200
_cell_measurement_theta_min      1.8870
_cell_volume                     4601.5(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_unetI/netI     0.1437
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36309
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.469
_diffrn_reflns_theta_min         1.518
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39110
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.114
_refine_diff_density_max         2.930
_refine_diff_density_min         -1.805
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         13650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1426
_refine_ls_R_factor_gt           0.0771
_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^)+(0.0878P)^2^+6.0654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.2175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7921
_reflns_number_total             13650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02942d2.cif
_cod_data_source_block           Ru2
_cod_database_code               1558257
_shelx_shelxl_version_number     2017/1
_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:
 C01A(H01A)
2.b Secondary CH2 refined with riding coordinates:
 C00B(H00B,H00C), C00C(H00D,H00E), C00E(H00G,H00H)
2.c Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00D(H00F), C00H(H00I), C00J(H00J), C00K(H00K), C00L(H00L),
 C00M(H00M), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00U(H00U),
 C00V(H00V), C00W(H00W), C00X(H00X), C00Z(H00Z), C010(H010), C011(H011),
 C012(H012), C013(H013), C014(H014), C015(H015), C016(H016), C018(H018),
 C01B(H01B), C01C(H01C), C01E(H01E), C01G(H01H), C01H(H01I), C01J(H01M),
 C01K(H01N), C01L(H01O), C01M(H01P), C01N(H01Q)
2.d Idealised Me refined as rotating group:
 C00T(H00N,H00S,H00T), C00Y(H00Y,H,HA), C01F(H01D,H01F,H01G), C01I(H01J,H01K,
 H01L)
;
_shelx_res_checksum              3996
_shelx_fab_checksum              29207
_olex2_submission_special_instructions 'No special instructions were received'