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_7061794
_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 Co N2 P'
_chemical_formula_sum            'C14 H25 Cl2 Co N2 P'
_chemical_formula_weight         382.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2bs74j
_audit_creation_date             2022-08-06
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5503(2)
_cell_length_b                   11.6343(2)
_cell_length_c                   14.8131(3)
_cell_measurement_reflns_used    9247
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.3283
_cell_measurement_theta_min      2.2259
_cell_volume                     1818.24(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.969
_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  0.0179
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32966
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.806
_diffrn_reflns_theta_min         2.226
_diffrn_source                   'fine focus sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    1.318
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4864
_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            blue
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.930
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 2401 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         6389
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0420P)^2^+0.1061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                5802
_reflns_number_total             6389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj02651a2.cif
_cod_data_source_block           JCK_tBu1C1H_CoCl2_02082020
_cod_depositor_comments
'Adding full bibliography for 7061787--7061798.cif.'
_cod_database_code               7061794
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details   mu*r=0.2000
_olex2_refinement_description
;
1. Restrained distances
 N2-H2N
 0.9 with sigma of 0.02
 P1-H2N
 2.12 with sigma of 0.04
 C6-H2N
 1.94 with sigma of 0.04
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              68123
_olex2_submission_special_instructions 'No special instructions were received'