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_4333324
_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         'C28 H55 N2 P2 Ru 1+; C32 H12 B F24 1-'
_chemical_formula_sum            'C60 H67 B F24 N2 P2 Ru'
_chemical_formula_weight         1445.98
_chemical_name_common
;
[Ru(\h^5^-C~5~Me~5~){P^i^Pr~2~NC~6~H~10~NP^i^Pr~2~-\k^3^-P,P',N}]
[B{C~8~H~3~F~6~}~4~]'
;
_chemical_name_systematic
;
pentahapto-pentamethylcyclopentadienyl-{(R,R)-bis((diisopropylphosphino)amino)
cyclohexane-\k^3^-P,P',N}ruthenium(II) tetrakis{3,5-bis(trifluoromethyl)phenyl}
borate
;
_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                 92.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.259(3)
_cell_length_b                   13.256(3)
_cell_length_c                   17.905(4)
_cell_measurement_reflns_used    7459
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.081
_cell_measurement_theta_min      2.173
_cell_volume                     3143.4(12)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22180
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        -0.0172
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         10971
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.060
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+4.8210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                10829
_reflns_number_total             10971
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700674csup1.cif
_cod_data_source_block           pv0514
_cod_depositor_comments
;
 Replacing the "\K" substring with the "\k" substring in the
 values of the _chemical_name_common and _chemical_name_systematic
 data items.

 Antanas Vaitkus,
 2017-03-29
;
_cod_original_cell_volume        3143.5(11)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4333324