Ruthenium Hydrides Containing the Superhindered Polydentate Polyphosphine Ligand P(CH2CH2P(t)Bu2)3.
Gilbert-Wilson, Ryan; Field, Leslie D.; Bhadbhade, Mohan; Inorganic chemistry  (2014) 141112150820006–; doi:10.1021/ic501895s

data_4341650
_publ_section_title
;
 Ruthenium Hydrides Containing the Superhindered Polydentate Polyphosphine
 Ligand P(CH2CH2P(t)Bu2)3.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141112150820006
_journal_paper_doi               10.1021/ic501895s
_journal_year                    2014
_chemical_formula_sum            'C30 H67 Cl N2 P4 Ru'
_chemical_formula_weight         716.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 92.0640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4338(4)
_cell_length_b                   20.2875(7)
_cell_length_c                   21.5007(8)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.774
_cell_measurement_theta_min      2.564
_cell_volume                     3676.4(3)
_computing_cell_refinement       '<i>APEX2</i>  '
_computing_data_collection       '<i>APEX2</i> (Bruker, 2007)'
_computing_data_reduction        '<i>APEX2</i>  '
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Area Detector'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31508
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.220
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            'Orange red'
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.109
_refine_diff_density_max         1.482
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         8012
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+7.7073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6638
_reflns_number_total             8012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501895s_si_002.cif
_cod_data_source_block           RuHClN2
_cod_database_code               4341650
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.928
_shelxl_version_number           2014/6