Four- and five-coordinate nickel(ii) complexes bearing new diphosphine–phosphonite and triphosphine–phosphite ligands: catalysts for N-alkylation of amines
Panigrahi, Dipankar; Mondal, Munmun; Gupta, Rohit; Mani, Ganesan; RSC Advances 12 (2022) 4510–4520; doi:10.1039/D1RA08961G

data_7244344
_publ_section_title
;
 Four- and five-coordinate nickel(ii) complexes bearing new
 diphosphine--phosphonite and triphosphine--phosphite ligands: catalysts
 for N-alkylation of amines
;
_journal_issue                   8
_journal_name_full               'RSC Advances'
_journal_page_first              4510
_journal_page_last               4520
_journal_paper_doi               10.1039/D1RA08961G
_journal_volume                  12
_journal_year                    2022
_chemical_formula_sum            'C41 H45 Cl2 F12 N2 Ni O2 P5'
_chemical_formula_weight         1110.25
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-09 deposited with the CCDC.	2021-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.369(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6099(10)
_cell_length_b                   22.192(2)
_cell_length_c                   20.122(2)
_cell_measurement_reflns_used    59211
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.413
_cell_measurement_theta_min      1.835
_cell_volume                     4736.5(8)
_computing_molecular_graphics    ORTEP
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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  0.0649
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59211
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_min         1.835
_diffrn_source                   'Fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6138
_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            orange-red
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       prism
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.043
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6138
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0482P)^2^+2.7604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7886
_reflns_number_total             9639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra08961g2.cif
_cod_data_source_block           LNiCNPr2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7244344
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.937
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              77567