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_1550559
_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 P3, 0.5(C6 H14)'
_chemical_formula_sum            'C48 H79 Lu N6 P3'
_chemical_formula_weight         1008.05
_chemical_name_common            16056_Complex-2
_chemical_name_systematic        Lu(iPr2PCH2NAr)3tacn
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   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                90
_cell_angle_beta                 112.211(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5369(5)
_cell_length_b                   38.7027(14)
_cell_length_c                   11.8500(4)
_cell_measurement_reflns_used    2918
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.58
_cell_measurement_theta_min      4.57
_cell_volume                     4898.5(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      123(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0721
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43324
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.647
_diffrn_reflns_theta_min         4.139
_diffrn_source                   micro
_exptl_absorpt_coefficient_mu    5.066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/hexanes'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7538
_exptl_transmission_factor_min   0.6086
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         9881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0239P)^2^+3.1422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7815
_reflns_number_total             9883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04712j3.cif
_cod_data_source_block           16056_Complex-2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_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               1550559
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              10848