Metal-Ligand Cooperation Facilitates Bond Activation and Catalytic Hydrogenation with Zinc Pincer Complexes.
Rauch, Michael; Kar, Sayan; Kumar, Amit; Avram, Liat; Shimon, Linda J. W.; Milstein, David; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c05500

data_4135159
_publ_section_title
;
 Metal-Ligand Cooperation Facilitates Bond Activation and Catalytic
 Hydrogenation with Zinc Pincer Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c05500
_journal_year                    2020
_chemical_formula_moiety         'C29 H60 N2 P2 Si2 Zn'
_chemical_formula_sum            'C29 H60 N2 P2 Si2 Zn'
_chemical_formula_weight         620.28
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 92.9540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4697(3)
_cell_length_b                   12.0184(2)
_cell_length_c                   14.2193(2)
_cell_measurement_reflns_used    19262
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.3710
_cell_measurement_theta_min      4.2480
_cell_volume                     3493.49(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov 2016)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29160
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.839
_diffrn_reflns_theta_min         4.267
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.076
_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     343
_refine_ls_number_reflns         7391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0430P)^2^+6.0020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7015
_reflns_number_total             7391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c05500_si_002.cif
_cod_data_source_block           complex4
_cod_original_cell_volume        3493.48(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4135159
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.807
_oxdiff_exptl_absorpt_empirical_full_min 0.699
_oxdiff_exptl_absorpt_empirical_full_max 2.650
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              1372
_shelx_hkl_checksum              36716