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_7244345
_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 H38 Cl F6 N Ni O2 P4'
_chemical_formula_weight         908.76
_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-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                 91.166(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4860(7)
_cell_length_b                   13.2706(9)
_cell_length_c                   29.888(2)
_cell_measurement_reflns_used    81157
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.199
_cell_measurement_theta_min      2.350
_cell_volume                     4158.2(5)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0845
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            81157
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.199
_diffrn_reflns_theta_min         2.350
_diffrn_source                   'Fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6969
_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            red
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       needle
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.042
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6969
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         9234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+4.5194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5465
_reflns_number_total             9234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra08961g2.cif
_cod_data_source_block           LNiClCNXylyl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7244345
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              55299