High-spin, tetrahedral cobalt(ii) and nickel(ii) complexes supported by monoprotic aminophosphine ligands, and attempted extension to copper(ii) complexes: synthesis, characterization, and unexpected reactivity
Kelly, Jordan C.; Bloomfield, Aaron J.; New Journal of Chemistry 46 (2022) 18647–18651; doi:10.1039/D2NJ02651A

data_7061789
_publ_section_title
;
 High-spin, tetrahedral cobalt(ii) and nickel(ii) complexes supported by
 monoprotic aminophosphine ligands, and attempted extension to copper(ii)
 complexes: synthesis, characterization, and unexpected reactivity
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18647
_journal_page_last               18651
_journal_paper_doi               10.1039/D2NJ02651A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C14 H25 Cl2 N2 Ni P'
_chemical_formula_sum            'C14 H25 Cl2 N2 Ni P'
_chemical_formula_weight         381.94
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2bs6x8
_audit_creation_date             2022-08-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-08 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.837(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.3712(10)
_cell_length_b                   12.0474(9)
_cell_length_c                   23.5918(18)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5295
_cell_measurement_theta_min      2.3110
_cell_volume                     3673.6(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker Instrument Service V2017.5.0.0'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            49071
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         1.600
_diffrn_source                   'fine focus sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    1.427
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6951
_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            purple
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         8444
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0437P)^2^+0.8654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6409
_reflns_number_total             8444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj02651a2.cif
_cod_data_source_block           JCK_NiCl2tBu1C1H_03252022
_cod_depositor_comments
'Adding full bibliography for 7061787--7061798.cif.'
_cod_database_code               7061789
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.723
_exptl_absorpt_special_details   mu*r=0.2000
_olex2_refinement_description
;
1. Restrained distances
 N2B-H2BN
 0.9 with sigma of 0.02
 N2A-H2AN
 0.9 with sigma of 0.02
 P1B-H2BN
 2.13 with sigma of 0.04
 C6B-H2BN
 1.94 with sigma of 0.04
 P1A-H2AN
 2.12 with sigma of 0.04
 C6A-H2AN
 1.92 with sigma of 0.04
2.a Secondary CH2 refined with riding coordinates:
 C6A(H6AA,H6AB), C6B(H6BA,H6BB)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1B(H1B), C2A(H2A), C2B(H2B), C3A(H3A), C3B(H3B), C4A(H4A), C4B(H4B)
2.c Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C8B(H8BA,H8BB,H8BC), C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,
 H9BC), C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C12A(H12A,H12B,H12C),
 C12B(H12D,H12E,H12F), C13A(H13A,H13B,H13C), C13B(H13D,H13E,H13F), C14A(H14A,
 H14B,H14C), C14B(H14D,H14E,H14F)
;
_shelx_res_checksum              29101
_olex2_submission_special_instructions 'No special instructions were received'