Cationic tetra- and pentacoordinate complexes of nickel based on POCN- and POCOP-type pincer ligands: synthesis, characterization, and ligand exchange studies
Rahimi, Naser; Zargarian, Davit; New Journal of Chemistry 45 (2021) 15063–15073; doi:10.1039/D1NJ01355F

data_7060662
_publ_section_title
;
 Cationic tetra- and pentacoordinate complexes of nickel based on POCN-
 and POCOP-type pincer ligands: synthesis, characterization, and ligand
 exchange studies
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15063
_journal_page_last               15073
_journal_paper_doi               10.1039/D1NJ01355F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C44 H62 N4 Ni2 O4 P2, C4 H8 O, 2(F6 Sb)'
_chemical_formula_sum            'C48 H70 F12 N4 Ni2 O5 P2 Sb2'
_chemical_formula_weight         1433.94
_chemical_name_systematic        POCN-Ni-bipy*-Ni-POCN
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-19 deposited with the CCDC.	2021-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.0150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3475(5)
_cell_length_b                   12.6233(4)
_cell_length_c                   24.3404(6)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.94
_cell_measurement_theta_min      2.43
_cell_volume                     5582.3(3)
_computing_cell_refinement
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEX2 CCD'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Quazar MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            52101
_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         70.089
_diffrn_reflns_theta_min         2.432
_diffrn_source                   'Microfocus Source'
_diffrn_source_target            Cu
_diffrn_source_type              'Incoatec I\mS High Brilliance Microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.661
_exptl_absorpt_correction_T_max  0.5220
_exptl_absorpt_correction_T_min  0.3322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1000 before and 0.0548 after correction. The Ratio of minimum to maximum transmission is 0.6364. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       needle
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         10576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+7.2269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9252
_reflns_number_total             10576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01355f2.cif
_cod_data_source_block           1e-naser8
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7060661--7060668.cif.
;
_cod_database_code               7060662
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.760
_shelx_estimated_absorpt_t_min   0.366
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C3(H3), C3A(H3A), C6(H6), C6A(H6A)
1.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C13A(H13C,H13D), C14(H14A,H14B), C14A(H14C,H14D), C15(H15A,
 H15B), C15A(H15C,H15D), C16(H16C,H16D), C16A(H16A,H16B), C17(H17C,H17D),
 C17A(H17A,H17B), C1B(H,HA), C2B(HF,HG), C3B(HB,HC), C4B(HD,HE)
1.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C8A(H8A), C9(H9), C9A(H9A), C10(H10), C10A(H10A), C18(H18),
 C18A(H18A), C19(H19), C19A(H19A), C21(H21), C21A(H21A), C22(H22), C22A(H22A)
1.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC), C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC),
 C4(H4B,H4A,H4C), C4A(H4AA,H4AB,H4AC), C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC)
;
_shelx_res_checksum              97736
_olex2_submission_special_instructions 'No special instructions were received'