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_4086342
_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            'C54 H71 N P3 Ru Y'
_chemical_formula_weight         1017.01
_chemical_name_common            PNP(iPr)Y(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                84.350(2)
_cell_angle_beta                 75.826(2)
_cell_angle_gamma                89.237(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3723(14)
_cell_length_b                   14.7572(19)
_cell_length_c                   18.146(2)
_cell_measurement_reflns_used    15271
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      1.82
_cell_volume                     2938.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15271
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  0.8230
_exptl_absorpt_correction_T_min  0.7034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;

Electron density peaks were located during structural refinement. These were believed to be a disordered hexane molecule per unit of the title complex. Several attempts were made to model the solvent molecule but were not successful. 
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a solvent cavity of volume 523.0A^3^ containing approximately 102 electrons. This contribution to the electron density was removed from the observed data uisng the SQUEEZE option in PLATON (Spek, 2003). 

Similar treatments of disordered solvent molecules were carried out by St\"ahler et al. (2001),  Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:

Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13

Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005). Acta Cryst. E61, m2014-m2017.

Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M. (2003). Acta Cryst. E59, o975-o977.

Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M. (2003). Acta Cryst. C59, m84-m86.

St\"ahler, R., N\"ather, C. & Bensch, W. (2001). Acta Cryst. C57, 26-27.
;
_refine_diff_density_max         1.514
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         10228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0641P)^2^+0.8855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                8364
_reflns_number_total             10228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401216v_si_002.cif
_cod_data_source_block           2a-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_original_sg_symbol_H-M      P-1
_cod_database_code               4086342