Rational selection of co-catalysts for the deaminative hydrogenation of amides.
Artús Suàrez, Lluís; Jayarathne, Upul; Balcells, David; Bernskoetter, Wesley H.; Hazari, Nilay; Jaraiz, Martín; Nova, Ainara; Chemical science 11 (2020) 2225–2230; doi:10.1039/c9sc03812d

data_1557075
_publ_section_title
;
 Rational selection of co-catalysts for the deaminative hydrogenation of
 amides.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              2225
_journal_page_last               2230
_journal_paper_doi               10.1039/c9sc03812d
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C36 H36 N2 O2 P2 Ru, 3(C4 H8 O), C7 H7 N O'
_chemical_formula_sum            'C55 H67 N3 O6 P2 Ru'
_chemical_formula_weight         1029.12
_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
_audit_creation_date             2018-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-25 deposited with the CCDC.	2020-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.113(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5623(6)
_cell_length_b                   13.9340(4)
_cell_length_c                   20.8795(7)
_cell_measurement_reflns_used    9014
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.63
_cell_measurement_theta_min      3.15
_cell_volume                     5106.0(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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            249738
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.747
_diffrn_reflns_theta_min         1.488
_diffrn_source                   'Sealed Source Mo with TRIUMPH optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         3.209
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         18813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0535P)^2^+15.2897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14781
_reflns_number_total             18813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03812d2.cif
_cod_data_source_block           s1_a
_cod_depositor_comments
;Adding full bibliography for 1557075.cif.

 Adding full bibliography for 1557075.cif.
;
_cod_database_code               1557075
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.877
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All Ru(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C13(H13A,H13B), C16(H16A,H16B), C14(H14A,H14B), C3S(H3SA,
 H3SB), C4S(H4SA,H4SB), C10S(H10A,H10B), C1S(H1SA,H1SB), C2S(H2SA,H2SB),
 C8S(H8SA,H8SB), C12S(H12A,H12B), C9S(H9SA,H9SB), C11S(H11A,H11B), C7S(H7SA,
 H7SB), C5S(H5SA,H5SB), C6S(H6SA,H6SB)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C28(H28), C18(H18), C30(H30), C27(H27), C26(H26), C12(H12),
 C35(H35), C9(H9), C19(H19), C34(H34), C33(H33), C25(H25), C21(H21), C20(H20),
 C6(H6), C8(H8), C31(H31), C11(H11), C24(H24), C2(H2), C10(H10), C4(H4), C5(H5),
  C32(H32), C40(H40), C43(H43), C38(H38), C41(H41), C3(H3), C42(H42), C39(H39)
;
_shelx_res_checksum              22857
_olex2_submission_special_instructions 'No special instructions were received'