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_4337911
_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         'C57 H53 N P4 Ru, 0.5(C6 H14 O3)'
_chemical_formula_sum            'C60 H60 N O1.5 P4 Ru'
_chemical_formula_weight         1044.04
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 102.4134(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2200(2)
_cell_length_b                   20.1647(3)
_cell_length_c                   22.2859(3)
_cell_measurement_reflns_used    14110
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.9000
_cell_measurement_theta_min      2.6820
_cell_volume                     5363.15(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.872
_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  0.0275
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39598
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.164
_diffrn_reflns_theta_min         2.226
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.917
_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    1.293
_exptl_crystal_description       tablets
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
SQUEEZE suggested 161 e/cell = 40.3 e/asu
The solvents used were ether (C4H10O, 42e), diglyme (C6H14O3, 74e) and
methanol (CH4O, 18e).
Before the use of SQUEEZE the solvent most resembled diglyme, though
translationally disordered ether would look very similar.
1/2diglyme = 37e, so this was used as the solvent present.
 
So, the atom list is low by 1/2(C6 H14 O3) = C3 H7 O1.5, and the UNIT
is low by C12 H28 O6, i.e. C228 H212 N4 O0 P16 Ru4
;
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         12637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+0.2997P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10085
_reflns_number_total             12637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500030k_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4337910--4337915.cif.'
_cod_original_formula_sum        'C60 H60 N O1.50 P4 Ru'
_cod_database_code               4337911
_shelxl_version_number           2013-2