Synthesis and characterization of tetrapodal nickel complexes with adaptable ligand binding geometries.
Cho, Hsien-Liang; Gullett, Kelly L.; Fout, Alison R.; Chemical communications (Cambridge, England) 60 (2024) 10564–10567; doi:10.1039/d4cc03186e

data_7133682
_publ_section_title
;
 Synthesis and characterization of tetrapodal nickel complexes with
 adaptable ligand binding geometries.
;
_journal_issue                   76
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10564
_journal_page_last               10567
_journal_paper_doi               10.1039/d4cc03186e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C41 H45 Ag N7 Ni, 1(C F3 O3 S)'
_chemical_formula_sum            'C42 H45 Ag F3 N7 Ni O3 S'
_chemical_formula_weight         951.49
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-28 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.067(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8971(10)
_cell_length_b                   15.1770(14)
_cell_length_c                   24.243(2)
_cell_measurement_reflns_used    9753
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      70.284
_cell_measurement_theta_min      3.458
_cell_volume                     3920.8(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Venture (Photon 3)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0211
_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       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            54684
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.374
_diffrn_reflns_theta_min         3.458
_diffrn_source                   'Bruker Venture Cu-IuS'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.647
_exptl_absorpt_correction_T_max  0.3841
_exptl_absorpt_correction_T_min  0.2705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0810 before and 0.0579 after correction. 
The Ratio of minimum to maximum transmission is 0.7042. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.679
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         7470
_refine_ls_number_restraints     1025
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0756P)^2^+11.6885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7261
_reflns_number_total             7470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03186e2.cif
_cod_data_source_block           af_hlc_pi2ni_agotf
_cod_depositor_comments
'Adding full bibliography for 7133679--7133683.cif.'
_cod_original_cell_volume        3920.9(6)
_cod_database_code               7133682
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.793
_shelx_estimated_absorpt_t_min   0.597
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5C-F8C \\sim C5C-F7C \\sim C5C-F6C
 with sigma of 0.02
 F8C-F7C \\sim F7C-F6C \\sim F6C-F8C
 with sigma of 0.04
 S1C-F8C \\sim S1C-F7C \\sim S1C-F6C
 with sigma of 0.04
 S1C-O3C \\sim S1C-O2C \\sim S1C-O4C
 with sigma of 0.02
 O3C-O2C \\sim O2C-O4C \\sim O3C-O4C
 with sigma of 0.04
 C5C-O3C \\sim C5C-O2C \\sim C5C-O4C
 with sigma of 0.04
 C14C-F16C \\sim C14C-F15C \\sim C14C-F17C
 with sigma of 0.02
 F16C-F15C \\sim F15C-F17C \\sim F17C-F16C
 with sigma of 0.04
 S10C-F16C \\sim S10C-F15C \\sim S10C-F17C
 with sigma of 0.04
 S10C-O11C \\sim S10C-O13C \\sim S10C-O12C
 with sigma of 0.02
 O11C-O13C \\sim O13C-O12C \\sim O11C-O12C
 with sigma of 0.04
 C14C-O11C \\sim C14C-O13C \\sim C14C-O12C
 with sigma of 0.04
 C25C-F28C \\sim C25C-F26C \\sim C25C-F27C
 with sigma of 0.02
 F28C-F26C \\sim F26C-F27C \\sim F27C-F28C
 with sigma of 0.04
 S21C-F28C \\sim S21C-F26C \\sim S21C-F27C
 with sigma of 0.04
 S21C-O22C \\sim S21C-O23C \\sim S21C-O24C
 with sigma of 0.02
 O22C-O23C \\sim O23C-O24C \\sim O22C-O24C
 with sigma of 0.04
 C25C-O22C \\sim C25C-O23C \\sim C25C-O24C
 with sigma of 0.04
 C4-C5 \\sim C5-C6 \\sim C6-C1 \\sim C1-C2 \\sim C2-C3 \\sim C3-C4
 with sigma of 0.02
 C4-C2 \\sim C6-C2 \\sim C5-C3 \\sim C5-C1 \\sim C1-C3 \\sim C4-C6
 with sigma of 0.04
 C1A-C2A \\sim C2A-C3A \\sim C3A-C4A \\sim C4A-C5A \\sim C5A-C6A \\sim C6A-C1A
 with sigma of 0.02
 C1A-C5A \\sim C3A-C5A \\sim C2A-C6A \\sim C2A-C4A \\sim C4A-C6A \\sim C1A-C3A
 with sigma of 0.04
 N7-C1 \\sim N7-C1A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
S1C \\sim F6C \\sim F7C \\sim F8C \\sim O2C \\sim O3C \\sim O4C \\sim C5C \\sim
S21C \\sim F26C \\sim F27C \\sim F28C \\sim O22C \\sim O23C \\sim O24C \\sim
C25C \\sim S10C \\sim F15C \\sim F16C \\sim F17C \\sim O11C \\sim O12C \\sim
O13C \\sim C14C: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C1A \\sim C2A \\sim C3A
\\sim C4A \\sim C5A \\sim C6A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(S10C) = Uanis(O13C)
4. Rigid body (RIGU) restrains
 S1C, F6C, F7C, F8C, O2C, O3C, O4C, C5C, S21C, F26C, F27C, F28C, O22C, O23C,
 O24C, C25C, S10C, F15C, F16C, F17C, O11C, O12C, O13C, C14C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2, C3, C4, C5, C6, C1A, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 1*[Sof(C5C)+Sof(S1C)+Sof(F6C)+Sof(F7C)+Sof(F8C)+Sof(O2C)+Sof(O3C)+Sof(O4C)]+1*
 [Sof(C25C)+Sof(S21C)+Sof(F26C)+Sof(F27C)+Sof(F28C)+Sof(O22C)+Sof(O23C)+
 Sof(O24C)]+1*[Sof(C14C)+Sof(S10C)+Sof(F15C)+Sof(F16C)+Sof(F17C)+Sof(O11C)+
 Sof(O12C)+Sof(O13C)]=1 with esd of 0.0001
 Sof(C5C)=Sof(S1C)=Sof(F6C)=Sof(F7C)=Sof(F8C)=Sof(O2C)=Sof(O3C)=Sof(O4C)=FVAR(1)
 Sof(C14C)=Sof(S10C)=Sof(F15C)=Sof(F16C)=Sof(F17C)=Sof(O11C)=Sof(O12C)=
 Sof(O13C)=FVAR(2)
 Sof(C25C)=Sof(S21C)=Sof(F26C)=Sof(F27C)=Sof(F28C)=Sof(O22C)=Sof(O23C)=
 Sof(O24C)=FVAR(3)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=1-FVAR(4)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(4)
6.a Free rotating group:
 C4(C1,C2,C3,C5,C6), C1A(C2A,C3A,C4A,C5A,C6A), C5C(S1C,F6C,F7C,F8C,O2C,O3C,
 O4C), C25C(S21C,F26C,F27C,F28C,O22C,O23C,O24C), C14C(S10C,F15C,F16C,F17C,O11C,
 O12C,O13C)
6.b Ternary CH refined with riding coordinates:
 C7(H7), C1(H1), C1A(H1A)
6.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C4(H4A,H4B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C2A(H2AA,
 H2AB), C3A(H3AA,H3AB), C4A(H4AA,H4AB), C5A(H5AA,H5AB), C6A(H6AA,H6AB)
6.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C16(H16), C21(H21), C22(H22), C24(H24), C26(H26),
 C27(H27), C28(H28), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41)
6.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              72210
_shelx_hkl_checksum              46354
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder'
_olex2_submission_original_sample_id AFB_HC_240625_dV_HLC_pi2Ni_AgOTf_20230712
_olex2_submission_special_instructions 'No special instructions were received'