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_4124544
_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 H42 N5 O2 P2 Ru, C2 F3 O2'
_chemical_formula_sum            'C56 H42 F3 N5 O4 P2 Ru'
_chemical_formula_weight         1068.96
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   35.8458(7)
_cell_length_b                   35.8458(7)
_cell_length_c                   23.3820(16)
_cell_measurement_temperature    85
_cell_volume                     26018.9(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_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  0.0699
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            258927
_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         68.230
_diffrn_reflns_theta_min         2.366
_exptl_absorpt_coefficient_mu    3.175
_exptl_absorpt_correction_T_max  0.9246
_exptl_absorpt_correction_T_min  0.8699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       plate
_exptl_crystal_F_000             9828.00
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.504
_refine_diff_density_min         -2.182
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         10594
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10022
_reflns_number_total             10594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08406_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4124543--4124548.cif.'
_cod_original_cell_volume        26019(2)
_cod_database_code               4124544
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 P21, C681
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 P21, C681
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 N54(H54), C23(H23), C21(H21), C45(H45), C49(H49), C105(H105), C123(H123),
 C138(H138), C142(H142), C145(H145), C211(H211), C284(H284), C334(H334),
 C351(H351), C385(H385), C407(H407), C436(H436), C443(H443), C488(H488),
 C537(H537), C562(H562), C576(H576), C633(H633), C640(H640), C701(H701),
 C731(H731), C741(H741), C753(H753), C764(H764), C783(H783), C819(H819),
 C853(H853), C870(H870), C906(H906), C907(H907), C933(H933), C937(H937),
 C966(H966), C983(H983), C101(H101), C1(H1)
3.b Idealised tetrahedral OH refined as rotating group:
 O34(H34)
;
_shelx_fab_checksum              38618
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'