Dipyrromethane-Diphosphine: The effect of meso substituents on the formation of nickel complexes and on their performance in the transfer hydrogenation of ketones
Mani, Ganesan; Gupta, Rohit; Kumar, Ashok; Dalton Transactions  (2023) –; doi:10.1039/D3DT03163B

data_7714490
_publ_section_title
;
 Dipyrromethane-Diphosphine: The effect of meso substituents on the
 formation of nickel complexes and on their performance in the transfer
 hydrogenation of ketones
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03163B
_journal_year                    2023
_chemical_formula_sum            'C47 H40 Cl2 N2 Ni P2'
_chemical_formula_weight         824.36
_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   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-09-26 deposited with the CCDC.	2023-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.2620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4431(7)
_cell_length_b                   15.2942(6)
_cell_length_c                   17.7753(7)
_cell_measurement_reflns_used    83247
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.087
_cell_measurement_theta_min      1.904
_cell_volume                     4068.9(3)
_computing_molecular_graphics    ortep
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-D8 Venture APEX3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            83247
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.087
_diffrn_reflns_theta_min         1.904
_diffrn_source                   'Fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       prism
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.076
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6896
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         8944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0365P)^2^+1.8519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6557
_reflns_number_total             8944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03163b2.cif
_cod_data_source_block           L1NiCl2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7714490
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              43664