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_4084822
_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 H44 B Cl N2 O P2 Ru, 2(C4 H8 O)'
_chemical_formula_sum            'C33 H60 B Cl N2 O3 P2 Ru'
_chemical_formula_weight         742.10
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
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_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'
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_cell_angle_alpha                90
_cell_angle_beta                 115.1418(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   15.856(2)
_cell_length_c                   17.075(3)
_cell_measurement_reflns_used    7099
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      31.3686
_cell_measurement_theta_min      2.6355
_cell_volume                     3631.5(9)
_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      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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
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_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.467
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_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       Block
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_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.140
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_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 2487 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.041(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     2
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_refine_ls_R_factor_all          0.0329
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.757
_reflns_Friedel_fraction_full    0.805
_reflns_Friedel_fraction_max     0.755
_reflns_number_gt                6663
_reflns_number_total             7288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500585j_si_002.cif
_cod_data_source_block           2
_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        3631.6(9)
_cod_database_code               4084822
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.917
_shelxl_version_number           2014-1
_shelx_res_checksum              91937
_shelx_hkl_checksum              81763