A Proton-Switchable Bifunctional Ruthenium Complex That Catalyzes Nitrile Hydroboration.
Geri, Jacob B.; Szymczak, Nathaniel K.; Journal of the American Chemical Society 137 (2015) 12808–12814; doi:10.1021/jacs.5b08406

data_4124546
_publ_section_title
;
 A Proton-Switchable Bifunctional Ruthenium Complex That Catalyzes Nitrile
 Hydroboration.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12808
_journal_page_last               12814
_journal_paper_doi               10.1021/jacs.5b08406
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C54 H41 N5 O2 P2 Ru'
_chemical_formula_sum            'C54 H41 N5 O2 P2 Ru'
_chemical_formula_weight         954.93
_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_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.12 svn.r2899 for OlexSys, GUI svn.r4796)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.748(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8909(2)
_cell_length_b                   20.7560(4)
_cell_length_c                   19.7148(14)
_cell_measurement_temperature    85
_cell_volume                     4309.7(4)
_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      85
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            115261
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         3.147
_exptl_absorpt_coefficient_mu    4.052
_exptl_absorpt_correction_T_max  0.667
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1960.00
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.900
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         7892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7813
_reflns_number_total             7892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08406_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4124543--4124548.cif.'
_cod_database_code               4124546
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Sof(O7A)=Sof(O1A)=Sof(H1A)=1-FVAR(1)
 Sof(O1)=Sof(O7)=Sof(H7)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C23(H23), C29(H29), C31(H31), C5(H5), C11(H11), C2(H2), C19(H19),
 C27(H27), C3(H3), C4(H4), C38(H38), C40(H40), C51(H51), C54(H54), C55(H55),
 C58(H58), C63(H63), C69(H69), C86(H86), C88(H88), C96(H96), C101(H101),
 C103(H103), C106(H106), C115(H115), C120(H120), C121(H121), C126(H126),
 C131(H131), C137(H137), C143(H143), C147(H147), C150(H150), C155(H155),
 C163(H163), C165(H165), C171(H171), C174(H174), C181(H181)
3.b Idealised tetrahedral OH refined as rotating group:
 O7(H7), O1A(H1A)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'