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_7060665
_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         'C30 H39 N2 Ni O2 P2, F6 Sb'
_chemical_formula_sum            'C30 H39 F6 N2 Ni O2 P2 Sb'
_chemical_formula_weight         816.03
_chemical_name_systematic        POCOP-Ni-phen
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             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                104.063(2)
_cell_angle_beta                 100.134(2)
_cell_angle_gamma                90.206(2)
_cell_formula_units_Z            4
_cell_length_a                   12.6698(6)
_cell_length_b                   13.6736(6)
_cell_length_c                   20.1046(9)
_cell_measurement_reflns_used    5436
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.975
_cell_measurement_theta_min      2.304
_cell_volume                     3321.9(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 0.977
_diffrn_measured_fraction_theta_max 0.969
_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  0.077
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22257
_diffrn_reflns_point_group_measured_fraction_full 0.858
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.325
_diffrn_reflns_theta_min         2.304
_diffrn_source                   'Microfocus Source'
_diffrn_source_target            Cu
_diffrn_source_type              'Incoatec I\mS High Brilliance Microsource'
_exptl_absorpt_coefficient_mu    8.632
_exptl_absorpt_correction_T_max  0.190058
_exptl_absorpt_correction_T_min  0.071111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 266080 reflections, Rint = 0.0862
 (227847 with I > 3sig(I), Rint = 0.0852)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   0.753572
_exptl_transmission_factor_min   0.581089
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.0024(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1618
_refine_ls_number_reflns         22257
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0745P)^2^+0.5845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_full    0.738
_reflns_Friedel_fraction_max     0.731
_reflns_number_gt                22086
_reflns_number_total             22257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01355f2.cif
_cod_data_source_block           2d-naser6
_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               7060665
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.510
_shelx_estimated_absorpt_t_min   0.253
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.58965
 0.41035
2.a Ternary CH refined with riding coordinates:
 C3A(H3A), C6A(H6A), C15A(H15A), C18A(H18A), C3B(H3B), C6B(H6B), C15B(H15B),
 C18B(H18B), C3C(H3C), C6C(H6C), C15C(H15C), C18C(H18C), C3D(H3D), C6D(H6D),
 C15D(H15D), C18D(H18D)
2.b Aromatic/amide H refined with riding coordinates:
 C8A(H8A), C9A(H9A), C10A(H10A), C19A(H19A), C20A(H20A), C21A(H21A),
 C23A(H23A), C24A(H24A), C26A(H26A), C27A(H27A), C28A(H28A), C8B(H8B), C9B(H9B),
  C10B(H10B), C19B(H19B), C20B(H20B), C21B(H21B), C23B(H23B), C24B(H24B),
 C26B(H26B), C27B(H27B), C28B(H28B), C8C(H8C), C9C(H9C), C10C(H10C), C19C(H19C),
  C20C(H20C), C21C(H21C), C23C(H23C), C24C(H24C), C26C(H26C), C27C(H27C),
 C28C(H28C), C8D(H8D), C9D(H9D), C10D(H10D), C19D(H19D), C20D(H20D), C21D(H21D),
  C23D(H23D), C24D(H24D), C26D(H26D), C27D(H27D), C28D(H28D)
2.c Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,
 H5AC), C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C), C16A(H16A,H16B,H16C),
 C17A(H17A,H17B,H17C), C1B(H1BA,H1BB,H1BC), C2B(H2BA,H2BB,H2BC), C4B(H4BA,H4BB,
 H4BC), C5B(H5BA,H5BB,H5BC), C13B(H13D,H13E,H13F), C14B(H14D,H14E,H14F),
 C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F), C1C(H1CA,H1CB,H1CC), C2C(H2CA,H2CB,
 H2CC), C4C(H4CA,H4CB,H4CC), C5C(H5CA,H5CB,H5CC), C13C(H13G,H13H,H13I),
 C14C(H14G,H14H,H14I), C16C(H16G,H16H,H16I), C17C(H17G,H17H,H17I), C1D(H1DA,
 H1DB,H1DC), C2D(H2DA,H2DB,H2DC), C4D(H4DA,H4DB,H4DC), C5D(H5DA,H5DB,H5DC),
 C13D(H13J,H13K,H13L), C14D(H14J,H14K,H14L), C16D(H16J,H16K,H16L), C17D(H17J,
 H17K,H17L)
;
_shelx_res_checksum              17605
_olex2_submission_special_instructions 'No special instructions were received'