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_7060668
_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         'F6 Sb, C23 H36 N Ni O2 P2'
_chemical_formula_sum            'C23 H36 F6 N Ni O2 P2 Sb'
_chemical_formula_weight         714.93
_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             2021-04-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-29 deposited with the CCDC.	2021-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.032(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6586(3)
_cell_length_b                   26.4721(7)
_cell_length_c                   14.4377(4)
_cell_measurement_reflns_used    9518
_cell_measurement_temperature    120
_cell_measurement_theta_max      60.834
_cell_measurement_theta_min      3.142
_cell_volume                     3164.14(17)
_computing_cell_refinement
;
SAINT (2017) V8.38A; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
'APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_reduction
;
SAINT (2017) 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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57823
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.905
_diffrn_reflns_theta_min         2.905
_diffrn_source                   'Metal Jet'
_diffrn_source_current           2.85
_diffrn_source_power             0.199215
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    8.838
_exptl_absorpt_correction_T_max  0.3747
_exptl_absorpt_correction_T_min  0.1940
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1301 before and 0.0887 after correction.
The Ratio of minimum to maximum transmission is 0.5177.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         7287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0199P)^2^+8.3039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6951
_reflns_number_total             7287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01355f2.cif
_cod_data_source_block           naser54
_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               7060668
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.561
_shelx_estimated_absorpt_t_min   0.304
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.048) H4(0.053) H5(0.052) H7(0.044) H8A(0.071) H8B(0.071)
 H8C(0.071) H9A(0.071) H9B(0.071) H9C(0.071) H10(0.048) H11A(0.078) H11B(0.078)
 H11C(0.078) H12A(0.067) H12B(0.067) H12C(0.067) H13(0.052) H14A(0.084)
 H14B(0.084) H14C(0.084) H15A(0.077) H15B(0.077) H15C(0.077) H16(0.056)
 H17A(0.083) H17B(0.083) H17C(0.083) H18A(0.096) H18B(0.096) H18C(0.096)
 H19(0.042) H20(0.047) H21(0.052) H22(0.048) H23(0.044)
 Fixed X: H3(0.005977) H4(-0.021271) H5(0.090905) H7(0.483095) H8A(0.560621)
 H8B(0.624869) H8C(0.469353) H9A(0.305491) H9B(0.463302) H9C(0.300039)
 H10(0.074562) H11A(-0.090048) H11B(-0.115161) H11C(-0.00524) H12A(0.216203)
 H12B(0.1179) H12C(0.291366) H13(0.520447) H14A(0.569559) H14B(0.733689)
 H14C(0.639864) H15A(0.627306) H15B(0.722102) H15C(0.550325) H16(0.256209)
 H17A(0.031132) H17B(-0.02537) H17C(-0.008772) H18A(0.191837) H18B(0.159987)
 H18C(0.340468) H19(0.596685) H20(0.714132) H21(0.579785) H22(0.324386)
 H23(0.214604)
 Fixed Y: H3(0.524506) H4(0.563323) H5(0.526603) H7(0.365249) H8A(0.428478)
 H8B(0.442308) H8C(0.470379) H9A(0.442373) H9B(0.415145) H9C(0.383665)
 H10(0.359066) H11A(0.370085) H11B(0.314016) H11C(0.323326) H12A(0.274907)
 H12B(0.271947) H12C(0.298578) H13(0.40844) H14A(0.463673) H14B(0.436412)
 H14C(0.417968) H15A(0.327453) H15B(0.347136) H15C(0.320088) H16(0.311273)
 H17A(0.333919) H17B(0.322511) H17C(0.379624) H18A(0.396206) H18B(0.338843)
 H18C(0.358075) H19(0.330738) H20(0.251639) H21(0.180922) H22(0.192011)
 H23(0.27235)
 Fixed Z: H3(0.415788) H4(0.266403) H5(0.15292) H7(0.610974) H8A(0.517231)
 H8B(0.629937) H8C(0.561572) H9A(0.673828) H9B(0.741616) H9C(0.699132)
 H10(0.573821) H11A(0.413682) H11B(0.448132) H11C(0.377874) H12A(0.503322)
 H12B(0.581341) H12C(0.608965) H13(0.129855) H14A(0.262987) H14B(0.261317)
 H14C(0.335656) H15A(0.265382) H15B(0.192429) H15C(0.151085) H16(0.123115)
 H17A(0.173118) H17B(0.059273) H17C(0.097259) H18A(-0.003995) H18B(-0.039435)
 H18C(0.010503) H19(0.475873) H20(0.511286) H21(0.427194) H22(0.314054)
 H23(0.28555)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 110 electrons were 
found in a volume of 408\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[C6H14] (hexanes) per Asymmetric Unit 
which account for 100 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60909
_shelx_fab_checksum              31632
_olex2_submission_special_instructions 'No special instructions were received'