Coordinatively Unsaturated Semisandwich Complexes of Ruthenium with Phosphinoamine Ligands and Related Species: A Complex Containing (R,R)-1,2-Bis((diisopropylphosphino)amino)cyclohexane in a New Coordination Form κ3P,P‘,N-η2-P,N
Palacios, M. Dolores; Puerta, M. Carmen; Valerga, Pedro; Lledós, Agustí; Veilly, Edouard; Inorganic Chemistry 46 (2007) 6958–6967; doi:10.1021/ic700674c

data_4333325
_publ_section_title
;
 Coordinatively Unsaturated Semisandwich Complexes of Ruthenium with
 Phosphinoamine Ligands and Related Species:&#x00A0; A Complex Containing
 (R,R)-1,2-Bis((diisopropylphosphino)amino)cyclohexane in a New
 Coordination Form \k3P,P&#x2018;,N-\h2-P,N
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6958
_journal_page_last               6967
_journal_paper_doi               10.1021/ic700674c
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C23 H45 N4 P2 Ru 1+; C32 H12 B F24 1-'
_chemical_formula_sum            'C55 H57 B F24 N4 P2 Ru'
_chemical_formula_weight         1403.87
_chemical_name_common
;
[Ru(\h^5^C~5~H~5~)(N~2~){(\K^2^-P,P')-^i^Pr~2~PNH(C~6~H~10~)NHP^i^Pr~2~}]
[B{(C~6~H~3~(CF~3~)~2~}~4~]
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.51(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.079(3)
_cell_length_b                   17.540(4)
_cell_length_c                   26.037(5)
_cell_measurement_reflns_used    9599
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.012
_cell_measurement_theta_min      2.437
_cell_volume                     5962(2)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3 vers. 1.08 (Faruggia, 2005)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.831
_diffrn_measured_fraction_theta_max 0.831
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '1700 omega scan frames, 0.3 deg, 10 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42054
_diffrn_reflns_theta_full        26.69
_diffrn_reflns_theta_max         26.69
_diffrn_reflns_theta_min         0.78
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0110
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.588
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(2)
_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     1559
_refine_ls_number_reflns         19589
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+24.7082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1382
_reflns_number_gt                19132
_reflns_number_total             19589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700674csup1.cif
_cod_data_source_block           pv0505
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4333325