3-Methylindole-Based Tripodal Tetraphosphine Ruthenium Complexes in N2 Coordination and Reduction and Formic Acid Dehydrogenation
Van de Watering, F.F.; Heijtbrink, N.; Van der Vlugt, J.I.; Dzik, W.I.; De Bruin, B.; Reek, J.N.H.; Inorganics 5 (2017) 73–; doi:10.3390/inorganics5040073

data_1556550
_publ_section_title
;
 3-Methylindole-Based Tripodal Tetraphosphine Ruthenium Complexes in N2
 Coordination and Reduction and Formic Acid Dehydrogenation
;
_journal_name_full               Inorganics
_journal_page_first              73
_journal_paper_doi               10.3390/inorganics5040073
_journal_volume                  5
_journal_year                    2017
_chemical_formula_sum            'C65 H55 Cl6 N3 P4 Ru'
_chemical_formula_weight         1315.77
_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'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 91.012(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1879(9)
_cell_length_b                   18.1604(8)
_cell_length_c                   19.7879(9)
_cell_measurement_reflns_used    133
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.3389
_cell_measurement_theta_min      4.6154
_cell_volume                     6894.2(5)
_computing_structure_refinement  'SHELXL-2016/3 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Quest ECO Photon 50'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56511
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.030
_diffrn_reflns_theta_max         25.030
_diffrn_reflns_theta_min         2.468
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.483
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.253
_refine_diff_density_max         3.100
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         12141
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1435
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10290
_reflns_number_total             12141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ff400_0m_a_sq.cif
_cod_data_source_block           ff400_0m_a_sq
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1556550
_shelx_res_checksum              64651
_shelx_hkl_checksum              63372
_shelx_fab_checksum              90187