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_4124547
_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 H43 N5 O2 P2 Ru'
_chemical_formula_sum            'C54 H43 N5 O2 P2 Ru'
_chemical_formula_weight         956.94
_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             2015-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.09 svn.r3130 for OlexSys, GUI svn.r4987)
;
_cell_angle_alpha                90
_cell_angle_beta                 147.951(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7147(14)
_cell_length_b                   20.8591(4)
_cell_length_c                   19.8865(14)
_cell_measurement_temperature    85
_cell_volume                     4339.6(13)
_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  0.0543
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            73206
_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         68.247
_diffrn_reflns_theta_min         3.144
_exptl_absorpt_coefficient_mu    4.025
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968.00
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7948
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0381P)^2^+6.5335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7800
_reflns_number_total             7948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08406_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4124543--4124548.cif.'
_cod_original_cell_volume        4339.6(8)
_cod_database_code               4124547
_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 H(H,H) groups
2. Rigid bond restraints
 C176, C66, C99
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C3, C137, C55
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6, C128
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N8, C141
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O9, C153
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C23(H23), C25(H25), C34(H34), C2(H2), C3(H3), C11(H11),
 C32(H32), C4(H4), C38(H38), C40(H40), C41(H41), C48(H48), C58(H58), C63(H63),
 C66(H66), C71(H71), C74(H74), C75(H75), C81(H81), C86(H86), C90(H90), C91(H91),
  C94(H94), C99(H99), C113(H113), C117(H117), C122(H122), C128(H128),
 C135(H135), C137(H137), C149(H149), C152(H152), C161(H161), C166(H166),
 C171(H171), C176(H176), C177(H177), C187(H187)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'