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_7133679
_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 H47 N7 Ni O, 3(C H2 Cl2)'
_chemical_formula_sum            'C44 H53 Cl6 N7 Ni O'
_chemical_formula_weight         967.34
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-06-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-27 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.462(2)
_cell_angle_beta                 93.570(2)
_cell_angle_gamma                100.750(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6855(4)
_cell_length_b                   13.1657(4)
_cell_length_c                   13.8011(5)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      66.683
_cell_measurement_theta_min      3.209
_cell_volume                     2259.67(13)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1057
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            58726
_diffrn_reflns_theta_full        66.98
_diffrn_reflns_theta_max         66.98
_diffrn_reflns_theta_min         3.21
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.222
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1136 before and 0.0943 after correction. The Ratio of minimum to maximum transmission is 0.8434. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         8018
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+6.3293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.2090
_reflns_number_gt                6040
_reflns_number_total             8018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4cc03186e2.cif
_cod_data_source_block           2_data
_cod_depositor_comments
'Adding full bibliography for 7133679--7133683.cif.'
_cod_database_code               7133679
_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, All O(H,H) groups
2. Restrained distances
 Cl5-C44 \\sim Cl5A-C44A
 with sigma of 0.02
 Cl6-C44 \\sim Cl6A-C44A
 with sigma of 0.02
 Cl5-Cl6 \\sim Cl5A-Cl6A
 with sigma of 0.04
3. Others
 Sof(Cl5A)=Sof(Cl6A)=Sof(C44A)=Sof(H44C)=Sof(H44D)=1-FVAR(1)
 Sof(Cl5)=Sof(Cl6)=Sof(C44)=Sof(H44A)=Sof(H44B)=FVAR(1)
4.a Rotating group:
 O1(H1A,H1B)
4.b Ternary CH refined with riding coordinates:
 C25(H25), C36(H36)
4.c Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C43(H43A,H43B), C42(H42A,H42B), C44(H44A,H44B), C44A(H44C,H44D)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C21(H21), C22(H22), C24(H24), C32(H32), C33(H33), C35(H35)
4.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C19(H19A,H19B,H19C)
;
_olex2_submission_special_instructions 'No special instructions were received'