Synthesis, Characterization, and Reactivity of Ruthenium Hydride Complexes of N-Centered Triphosphine Ligands.
Phanopoulos, Andreas; Brown, Neil J.; White, Andrew J. P.; Long, Nicholas J.; Miller, Philip W.; Inorganic chemistry 53 (2014) 3742–; doi:10.1021/ic500030k

data_4337913
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of Ruthenium Hydride
 Complexes of N-Centered Triphosphine Ligands.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3742
_journal_paper_doi               10.1021/ic500030k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C36 H60 N O3 P3 Ru'
_chemical_formula_sum            'C36 H60 N O3 P3 Ru'
_chemical_formula_weight         748.83
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.438(2)
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   56.2065(11)
_cell_length_b                   28.0254(4)
_cell_length_c                   19.0501(4)
_cell_measurement_reflns_used    29686
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.8790
_cell_measurement_theta_min      2.2470
_cell_volume                     30007.0(10)
_computing_cell_refinement       CrysAlisPro,
_computing_data_collection       CrysAlisPro,
_computing_data_reduction        CrysAlisPro,
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            71424
_diffrn_reflns_point_group_measured_fraction_full 0.754
_diffrn_reflns_point_group_measured_fraction_max 0.655
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.209
_diffrn_reflns_theta_min         2.232
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       blocks
_exptl_crystal_F_000             12672
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
; 
 Flack x determined using 12216 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 

 Results of chirality/polarity tests
  _refine_ls_R_factor_obs+         0.0340
  _refine_ls_wR_factor_obs+        0.0762
  _refine_ls_abs_structure_Flack+  0.437(9)
  _refine_ls_R_factor_obs-         0.0344
  _refine_ls_wR_factor_obs-        0.0772
  _refine_ls_abs_structure_Flack-  0.562(9)
;
_refine_ls_abs_structure_Flack   0.437(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3316
_refine_ls_number_reflns         43859
_refine_ls_number_restraints     1125
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+38.7753P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.474
_reflns_Friedel_fraction_full    0.510
_reflns_Friedel_fraction_max     0.421
_reflns_number_gt                40026
_reflns_number_total             43859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500030k_si_002.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 4337910--4337915.cif.'
_cod_database_code               4337913
_shelxl_version_number           2013-2