P-C reductive elimination in Ru(ii) complexes to convert triarylphosphine ligands into five- or six-membered phosphacycles.
Kuwabara, Takuya; Kato, Takahiro; Takano, Kouichi; Kodama, Shintaro; Manabe, Yuuka; Tsuchida, Noriko; Takano, Keiko; Minami, Yasunori; Hiyama, Tamejiro; Ishii, Youichi; Chemical communications (Cambridge, England) 54 (2018) 5357–5360; doi:10.1039/c8cc02539h

data_7121591
_publ_section_title
;
 P-C reductive elimination in Ru(ii) complexes to convert triarylphosphine
 ligands into five- or six-membered phosphacycles.
;
_journal_issue                   42
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5357
_journal_page_last               5360
_journal_paper_doi               10.1039/c8cc02539h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C70 H52 B F24 P Ru'
_chemical_formula_weight         1491.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-02-28 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;
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_cell_angle_gamma                110.4807(13)
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_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      31.29
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_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
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_computing_molecular_graphics    'Yadokari-XG 2009(Wakita Nemoto et al.)'
_computing_publication_material  'Yadokari-XG 2009(Wakita,Nemoto et al.)'
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_computing_structure_solution    SIR-2014
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_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.963
_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     0.1031
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.963
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_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
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_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            52661
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_min         3.012
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_exptl_crystal_colour            green
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_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.230
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_refine_diff_density_max         1.045
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_refine_ls_extinction_coef       0.00128(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         27980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0760P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18005
_reflns_number_total             27980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02539h2.cif
_cod_data_source_block           aa
_cod_depositor_comments
'Adding full bibliography for 7121586--7121591.cif.'
_cod_original_cell_volume        6340.9(15)
_cod_database_code               7121591
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.930
_exptl_absorpt_special_details   'Jacobson, R. (1998) Private communication'
_shelx_res_checksum              24058