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_1550561
_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         'C45 H72 Lu N6 Ni P3'
_chemical_formula_sum            'C45 H72 Lu N6 Ni P3'
_chemical_formula_weight         1023.67
_chemical_name_common            16087_Complex-2
_chemical_name_systematic        NiLu(iPr2PCH2NAr)3tacn
_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                78.2730(10)
_cell_angle_beta                 79.6030(10)
_cell_angle_gamma                78.3390(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7814(2)
_cell_length_b                   10.8562(2)
_cell_length_c                   20.1873(4)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.53
_cell_measurement_theta_min      4.22
_cell_volume                     2241.69(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ShelXle Rev. 712 (Huebschle, 2011)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker PHOTON-II CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33217
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.588
_diffrn_reflns_theta_min         4.222
_diffrn_source                   'I\uS Microfocus Tube'
_exptl_absorpt_coefficient_mu    5.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             1056
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran/hexanes'
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.7538
_exptl_transmission_factor_min   0.6117
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         9120
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0265P)^2^+1.5513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8162
_reflns_number_total             9120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04712j3.cif
_cod_data_source_block           16087_Complex-4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1550561
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.125
_shelx_estimated_absorpt_t_max   0.588
_shelx_res_checksum              51574