Bimetallic nickel-lutetium complexes: Tuning the properties and catalytic hydrogenation activity of the Ni site by varying the Lu coordination environment
Lu, Connie; Ramirez, Bianca L.; Sharma, Prachi; Eisenhart, Reed; Gagliardi, Laura; Chemical Science  (2019) –; doi:10.1039/C8SC04712J

data_1550560
_publ_section_title
;
 Bimetallic nickel-lutetium complexes: Tuning the properties and catalytic
 hydrogenation activity of the Ni site by varying the Lu coordination
 environment
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04712J
_journal_year                    2019
_chemical_formula_moiety         'C43 H75 Lu N3 Ni O P3'
_chemical_formula_sum            'C43 H71 Lu N3 Ni O P3'
_chemical_formula_weight         972.61
_chemical_name_common            16244_Complex-3-THF
_chemical_name_systematic        NiLu(iPr2PCH2NPh)3(C4H8O)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-09-27 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                76.8410(10)
_cell_angle_beta                 81.2330(10)
_cell_angle_gamma                68.2440(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4262(10)
_cell_length_b                   12.1111(11)
_cell_length_c                   17.7291(16)
_cell_measurement_reflns_used    6372
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      2.21
_cell_volume                     2212.5(3)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX3, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'Shelxle-(Rev. 712) (Huebschle, C. B., 2011)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Photon-II CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25794
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.250
_diffrn_reflns_theta_min         1.183
_diffrn_source                   micro
_exptl_absorpt_coefficient_mu    2.787
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangualar block'
_exptl_crystal_F_000             1004
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran/hexanes'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         9816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0236P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8608
_reflns_number_total             9816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04712j3.cif
_cod_data_source_block           16244_Complex-3-THF
_cod_database_code               1550560
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              10338