A Highly Reactive Ruthenium Phosphido Complex Exhibiting Ru−P π-Bonding
Derrah, Eric J.; Pantazis, Dimitrios A.; McDonald, Robert; Rosenberg, Lisa; Organometallics 26 (2007) 1473–; doi:10.1021/om0700056

data_4073000
_publ_section_title
;
 A Highly Reactive Ruthenium Phosphido Complex Exhibiting Ru&#x2212;P
 \p-Bonding
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1473
_journal_paper_doi               10.1021/om0700056
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C39 H43 P2 Ru, 0.25(C5 H12)'
_chemical_formula_sum            'C40.25 H47 P2 Ru'
_chemical_formula_weight         693.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.432(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3907(13)
_cell_length_b                   13.5621(16)
_cell_length_c                   25.866(3)
_cell_measurement_reflns_used    5560
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.20
_cell_volume                     3584.8(7)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_sigmaI/netI    0.0899
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26806
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.9316
_exptl_absorpt_correction_T_min  0.7851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1450
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;

 Attempts to refine peaks of residual electron density as solvent n-pentane

 carbon atoms were unsuccessful.  The data were corrected for disordered

 electron density through use of the SQUEEZE procedure (Sluis, P. van der;

 Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON

 (Spek, A.L. Acta Crystallogr. 1990, A46, C34.  PLATON - a multipurpose

 crystallographic tool.  Utrecht University, Utrecht, The Netherlands).

 A total solvent-accessible void volume of 521.7 A^3^ with a total electron

 count of 91 (consistent with one molecule of solvent n-pentane) was found

 in the unit cell.

;
_refine_diff_density_max         1.929
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                4859
_reflns_number_total             7309
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om0700056si20070102_062649.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3584.8(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4073000