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_7061796
_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         'C60 H108 Ag4 Cl2 N8 P4, 2(B F4)'
_chemical_formula_sum            'C60 H108 Ag4 B2 Cl2 F8 N8 P4'
_chemical_formula_weight         1741.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2bv24f
_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
;
2022-08-06 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                77.1240(10)
_cell_angle_beta                 84.4990(10)
_cell_angle_gamma                88.5690(10)
_cell_formula_units_Z            1
_cell_length_a                   12.3096(2)
_cell_length_b                   12.3824(2)
_cell_length_c                   13.0675(2)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.7173
_cell_measurement_theta_min      2.2014
_cell_volume                     1932.74(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 0.996
_diffrn_measured_fraction_theta_max 0.921
_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  0.0207
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34628
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.937
_diffrn_reflns_theta_min         1.662
_diffrn_source                   'fine focus sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6427
_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            colorless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         13342
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.1481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9625
_reflns_number_total             13342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj02651a2.cif
_cod_data_source_block           JCK_NitBu2C_AgBF4_04122022
_cod_depositor_comments
'Adding full bibliography for 7061787--7061798.cif.'
_cod_database_code               7061796
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.680
_exptl_absorpt_special_details   mu*r=0.2000
_olex2_refinement_description
;
1. Restrained distances
 N4-H4
 0.9 with sigma of 0.02
 N2-H2
 0.9 with sigma of 0.02
 P2-H4
 2.1 with sigma of 0.04
 C22-H4
 1.91 with sigma of 0.04
 P1-H2
 2.09 with sigma of 0.04
 C7-H2
 1.91 with sigma of 0.04
 B1-F4 \\sim B1A-F4A
 with sigma of 0.02
 F2-F3 \\sim F2A-F3A
 with sigma of 0.04
 B1-F2 \\sim B1A-F2A
 with sigma of 0.02
 B1-F1 \\sim B1A-F1A
 with sigma of 0.02
 B1-F3 \\sim B1A-F3A
 with sigma of 0.02
 F2-F4 \\sim F2A-F4A
 with sigma of 0.04
 F3-F4 \\sim F3A-F4A
 with sigma of 0.04
 F1-F2 \\sim F1A-F2A
 with sigma of 0.04
 F1-F3 \\sim F1A-F3A
 with sigma of 0.04
 F1-F4 \\sim F1A-F4A
 with sigma of 0.04
2. Rigid body (RIGU) restrains
 B1A, F3A, F4A, F2A, F1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B1, F1, F2, F3, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(B1A)=Sof(F3A)=Sof(F4A)=Sof(F2A)=Sof(F1A)=1-FVAR(1)
 Sof(B1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C21(H21A,H21B), C22(H22A,H22B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3), C4(H4A), C16(H16), C17(H17), C18(H18), C19(H19)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              51220
_olex2_submission_special_instructions 'No special instructions were received'