PNP-Ligated Heterometallic Rare-Earth/Ruthenium Hydride Complexes Bearing Phosphinophenyl and Phosphinomethyl Bridging Ligands
O, Wylie W. N.; Kang, Xiaohui; Luo, Yi; Hou, Zhaomin; Organometallics 33 (2014) 1030–1043; doi:10.1021/om401216v

data_4086349
_publ_section_title
;
 PNP-Ligated Heterometallic Rare-Earth/Ruthenium Hydride Complexes Bearing
 Phosphinophenyl and Phosphinomethyl Bridging Ligands
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1030
_journal_page_last               1043
_journal_paper_doi               10.1021/om401216v
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C59 H80 N2 P3 Ru Y'
_chemical_formula_weight         1100.14
_chemical_name_common            PNP(iPr)Y(tBuCN)(H)2Ru(C5Me5)PPh2(C6H4)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.276(5)
_cell_angle_beta                 79.828(6)
_cell_angle_gamma                85.762(6)
_cell_formula_units_Z            2
_cell_length_a                   13.366(2)
_cell_length_b                   13.892(2)
_cell_length_c                   15.558(2)
_cell_measurement_reflns_used    65058
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      25.64
_cell_measurement_theta_min      1.45
_cell_volume                     2831.7(7)
_computing_cell_refinement       'APEX2 (Bruker, 2013); SAINT (Bruker, 2012)'
_computing_data_collection       'GIS (Bruker)'
_computing_data_reduction
'SAINT (Bruker, 2012); XPREP (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker D8 QUEST diffractometer with a CMOS area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'doubly curved silicon crystal'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            65058
_diffrn_reflns_theta_full        25.64
_diffrn_reflns_theta_max         25.64
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  0.9203
_exptl_absorpt_correction_T_min  0.6028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2012) SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         10687
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+1.6866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                9179
_reflns_number_total             10687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401216v_si_002.cif
_cod_data_source_block           4a-Y
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4093 2015-10-18 17:28:56Z antanas 
;
_cod_database_code               4086349