Steric influence and controlled dynamic process in a chiral square planar nickel(ii) complex supported by a dipyrromethane-based NNNN tetradentate ligand
Guchhait, Tapas; Giri, Monalisa; Mishra, Soumya; Roy, Satabdi; New Journal of Chemistry 48 (2024) 15240–15247; doi:10.1039/D4NJ03166K

data_7063383
_publ_section_title
;
 Steric influence and controlled dynamic process in a chiral square planar
 nickel(ii) complex supported by a dipyrromethane-based NNNN tetradentate
 ligand
;
_journal_issue                   34
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15240
_journal_page_last               15247
_journal_paper_doi               10.1039/D4NJ03166K
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C25 H32 N6 Ni'
_chemical_formula_sum            'C25 H32 N6 Ni'
_chemical_formula_weight         475.27
_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
_audit_creation_date             2024-07-09
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-09 deposited with the CCDC.	2024-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                108.007(2)
_cell_angle_beta                 93.048(2)
_cell_angle_gamma                114.480(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7367(6)
_cell_length_b                   9.9869(6)
_cell_length_c                   13.6433(10)
_cell_measurement_reflns_used    32856
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      56.578
_cell_measurement_theta_min      4.712
_cell_volume                     1122.80(13)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32856
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.289
_diffrn_reflns_theta_min         2.356
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_T_max  0.7369
_exptl_absorpt_correction_T_min  0.6014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1247 before and 0.1053 after correction.
The Ratio of minimum to maximum transmission is 0.8161.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       'Needle shaped'
_exptl_crystal_F_000             504
_exptl_crystal_recrystallization_method
'Slow evaporation from dichloromethane and hexane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+2.5090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4690
_reflns_number_total             5538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03166k2.cif
_cod_data_source_block           tg2
_cod_depositor_comments
'Adding full bibliography for 7063382--7063383.cif.'
_cod_database_code               7063383
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.916
_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.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C6(H6A,H6B), C14(H14A,H14B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C3(H3), C8(H8), C18(H18), C17(H17), C9(H9)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C25(H25A,H25B,H25C), C21(H21A,H21B,H21C), C5(H5A,H5B,H5C),
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              11702
_olex2_date_sample_completion    2024-04-24
_olex2_date_sample_data_collection 2024-04-24
_olex2_date_sample_submission    2024-04-24
_olex2_submission_original_sample_id 'Ni complex 2'
_olex2_submission_special_instructions 'No special instructions were received'