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_4124548
_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
'C48 H50 B2 N5 O6 P Ru, 0.9(C7 H14), C3.15 H6.30'
_chemical_formula_sum            'C57.45 H68.9 B2 N5 O6 P Ru'
_chemical_formula_weight         1079.14
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.389(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.5276(2)
_cell_length_b                   15.2452(2)
_cell_length_c                   31.182(2)
_cell_measurement_reflns_used    57657
_cell_measurement_temperature    85
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      2.90
_cell_volume                     5406.5(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_detector_area_resol_mean 29.257
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Saturn70 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            83666
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.060
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2262.4
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.186
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         9792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+11.8367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9372
_reflns_number_total             9792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08406_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4124543--4124548.cif.'
_cod_original_formula_sum        'C57.45 H68.90 B2 N5 O6 P Ru'
_cod_database_code               4124548
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H10O,H10P,H} of C106, {H1AD,H1AE,H1B} of C1, All C(H,H)
  groups
 At 1.5 times of:
  {H24A,H24B,H24C} of C24, {H33A,H33B,H33C} of C33, {H6AA,H6AB,H6AC} of C6AA,
  {H10A,H10B,H10C} of C10, {H1AA,H1AB,H1AC} of C1AA, {H46A,H46B,H46C} of C46,
  {H61A,H61B,H61C} of C61, {H78A,H78B,H78C} of C78, {H10D,H10E,H10F} of C100,
  {H4A,H4B,H4C} of C4
2. Others
 Fixed Sof: C101(0.9) H101(0.9) C100(0.9) H10D(0.9) H10E(0.9) H10F(0.9)
 C1(0.9) H1AD(0.45) H1AE(0.45) H1B(0.45) C4(0.45) H4A(0.45) H4B(0.45) H4C(0.45)
 C102(0.9) H10G(0.9) H10H(0.9) C103(0.9) H10I(0.9) H10J(0.9) C104(0.9)
 H10K(0.9) H10L(0.9) C105(0.9) H10M(0.9) H10N(0.9) C2(0.9) H2A(0.9) H2B(0.9)
 C3(0.9) H3A(0.9) H3B(0.9) C106(0.9) H10O(0.9) H10P(0.9)
3.a Ternary CH refined with riding coordinates:
 C101(H101), C1(H1B)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1AD,H1AE), C102(H10G,H10H), C103(H10I,H10J), C104(H10K,H10L), C105(H10M,
 H10N), C2(H2A,H2B), C3(H3A,H3B), C106(H10O,H10P)
3.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C3AA(H3AA), C4AA(H4AA), C17(H17), C20(H20), C28(H28), C30(H30),
 C34(H34), C36(H36), C43(H43), C45(H45), C52(H52), C53(H53), C64(H64), C67(H67),
  C69(H69), C74(H74), C94(H94), C95(H95), C107(H107), C109(H109), C118(H118),
 C119(H119), C132(H132), C136(H136)
3.d Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC), C6AA(H6AA,H6AB,H6AC), C10(H10A,H10B,H10C), C24(H24A,
 H24B,H24C), C33(H33A,H33B,H33C), C46(H46A,H46B,H46C), C61(H61A,H61B,H61C),
 C78(H78A,H78B,H78C), C100(H10D,H10E,H10F), C4(H4A,H4B,H4C)
;
_olex2_submission_original_sample_id RuBPin
_olex2_submission_special_instructions 'No special instructions were received'