Ruthenium Complexes Stabilized by Bidentate Enamido-Phosphine Ligands: Aspects of Cooperative H2 Activation.
Wambach, Truman C.; Fryzuk, Michael D.; Inorganic chemistry 54 (2015) 5888–5896; doi:10.1021/acs.inorgchem.5b00672

data_4343262
_publ_section_title
;
 Ruthenium Complexes Stabilized by Bidentate Enamido-Phosphine Ligands:
 Aspects of Cooperative H2 Activation.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5888
_journal_page_last               5896
_journal_paper_doi               10.1021/acs.inorgchem.5b00672
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C33 H59 N O P2 Ru'
_chemical_formula_sum            'C33 H59 N O P2 Ru'
_chemical_formula_weight         648.82
_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     direct
_audit_creation_date             2015-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 101.445(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   12.507(5)
_cell_length_b                   16.903(5)
_cell_length_c                   16.260(5)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.638
_cell_measurement_theta_min      2.586
_cell_volume                     3369(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX DUO'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37019
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.639
_diffrn_reflns_theta_min         1.661
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1075 before and 0.0373 after correction. The Ratio of minimum to maximum transmission is 0.9236. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_recrystallization_method
'Crystalized from a concentrated, cold pentane solution at -32 C'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         9463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+1.5813P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8114
_reflns_number_total             9463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00672_si_002.cif
_cod_data_source_block           mo_mf934_0mco
_cod_depositor_comments
'Adding full bibliography for 4343262--4343264.cif.'
_cod_database_code               4343262
_shelxl_version_number           2012-9
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C7(H7), C31(H31), C22(H22), C25(H25), C19(H19), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C27(H27A,H27B,H27C), C30(H30A,H30B,
 H30C), C021(H02A,H02B,H02C), C6(H6A,H6B,H6C), C29(H29A,H29B,H29C), C24(H24A,
 H24B,H24C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C21(H21A,H21B,H21C),
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'