Synthesis, Structure, and Bonding Properties of Ruthenium Complexes Possessing a Boron-Based PBP Pincer Ligand and Their Application for Catalytic Hydrogenation
Miyada, Takuma; Huang Kwan, Enrique; Yamashita, Makoto; Organometallics 33 (2014) 6760–; doi:10.1021/om500585j

data_4084823
_publ_section_title
;
 Synthesis, Structure, and Bonding Properties of Ruthenium Complexes
 Possessing a Boron-Based PBP Pincer Ligand and Their Application for
 Catalytic Hydrogenation
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6760
_journal_paper_doi               10.1021/om500585j
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C25 H48 B2 N2 O P2 Ru, C4 H8 O'
_chemical_formula_sum            'C29 H56 B2 N2 O2 P2 Ru'
_chemical_formula_weight         649.38
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_alpha                90
_cell_angle_beta                 109.855(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.318(4)
_cell_length_b                   16.123(3)
_cell_length_c                   11.440(3)
_cell_measurement_reflns_used    4900
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4971
_cell_measurement_theta_min      1.6886
_cell_volume                     3351.3(13)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    'Yadokari-XG 2009(Wakita Nemoto et al.)'
_computing_publication_material  'Yadokari-XG 2009(Wakita,Nemoto et al.)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 99.2000
_diffrn_measured_fraction_theta_max 27.4971
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10436
_diffrn_reflns_point_group_measured_fraction_full 0.755
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_theta_full        27.4971
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.689
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       Block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 1486 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4588
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+7.9106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.565
_reflns_Friedel_fraction_full    0.547
_reflns_Friedel_fraction_max     0.563
_reflns_number_gt                4391
_reflns_number_total             4588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500585j_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4084822--4084825.cif.
;
_cod_original_cell_volume        3351.4(12)
_cod_database_code               4084823
_shelx_estimated_absorpt_t_min   0.737
_shelx_estimated_absorpt_t_max   0.891
_shelxl_version_number           2014-1
_shelx_res_checksum              85050
_shelx_hkl_checksum              59647