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_7060663
_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         'C29 H35 N3 Ni O2 P, C H2 Cl2, F6 Sb'
_chemical_formula_sum            'C30 H37 Cl2 F6 N3 Ni O2 P Sb'
_chemical_formula_weight         867.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 93.580(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2593(15)
_cell_length_b                   13.5102(12)
_cell_length_c                   29.393(3)
_cell_measurement_reflns_used    5228
_cell_measurement_temperature    130
_cell_measurement_theta_max      54.920
_cell_measurement_theta_min      2.517
_cell_volume                     6840.4(11)
_computing_cell_refinement
;
SAINT (2013) V8.40A; 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) V8.40A; 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      130
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.1164
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_number            13036
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.076
_diffrn_reflns_theta_min         2.516
_diffrn_source                   'Metal Jet'
_diffrn_source_current           2.86
_diffrn_source_power             0.199914
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    8.917
_exptl_absorpt_correction_T_max  0.750824
_exptl_absorpt_correction_T_min  0.378936
_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 201015 reflections, Rint = 0.1164
 (114680 with I > 3sig(I), Rint = 0.0957)
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       plate
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   0.750824
_exptl_transmission_factor_min   0.378936
_refine_diff_density_max         1.115
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         13036
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+41.7206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11380
_reflns_number_total             13036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01355f2.cif
_cod_data_source_block           naser57
_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_original_cell_volume        6840.3(11)
_cod_database_code               7060663
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.175
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.05) H4(0.06) H5(0.053) H7A(0.046) H7B(0.046) H8A(0.043)
 H8B(0.043) H9A(0.051) H9B(0.051) H10A(0.049) H10B(0.049) H11A(0.043)
 H11B(0.043) H12(0.042) H13A(0.063) H13B(0.063) H13C(0.063) H14A(0.064)
 H14B(0.064) H14C(0.064) H15(0.045) H16A(0.067) H16B(0.067) H16C(0.067)
 H17A(0.069) H17B(0.069) H17C(0.069) H18(0.048) H19(0.069) H20(0.077)
 H22(0.084) H23(0.08) H25(0.069) H26(0.07) H27(0.051) H33(0.052) H34(0.054)
 H35(0.057) H37A(0.052) H37B(0.052) H38A(0.047) H38B(0.047) H39A(0.057)
 H39B(0.057) H40A(0.061) H40B(0.061) H41A(0.05) H41B(0.05) H42(0.05)
 H43A(0.072) H43B(0.072) H43C(0.072) H44A(0.08) H44B(0.08) H44C(0.08) H45(0.06)
 H46A(0.084) H46B(0.084) H46C(0.084) H47A(0.129) H47B(0.129) H47C(0.129)
 H48(0.056) H49(0.067) H50(0.069) H52(0.075) H53(0.068) H55(0.059) H56(0.06)
 H57(0.05) H61A(0.093) H61B(0.093) H62A(0.122) H62B(0.122) H62C(0.112)
 H62D(0.112)
 Fixed X: H3(0.436156) H4(0.42306) H5(0.348765) H7A(0.307805) H7B(0.242603)
 H8A(0.127486) H8B(0.172474) H9A(0.118777) H9B(0.049991) H10A(0.115055)
 H10B(0.159239) H11A(0.2358) H11B(0.166098) H12(0.217614) H13A(0.179484)
 H13B(0.164694) H13C(0.23844) H14A(0.327265) H14B(0.250314) H14C(0.318333)
 H15(0.412768) H16A(0.31732) H16B(0.381101) H16C(0.306889) H17A(0.481692)
 H17B(0.492142) H17C(0.433465) H18(0.441985) H19(0.519236) H20(0.48331)
 H22(0.382651) H23(0.274282) H25(0.16055) H26(0.095349) H27(0.149205) H33(-
 0.049944) H34(-0.078172) H35(-0.163485) H37A(-0.277221) H37B(-0.208505) H38A(-
 0.322577) H38B(-0.258212) H39A(-0.350167) H39B(-0.379803) H40A(-0.467042)
 H40B(-0.402423) H41A(-0.344411) H41B(-0.376074) H42(-0.082594) H43A(-0.067444)
 H43B(-0.006145) H43C(-0.019299) H44A(-0.191555) H44B(-0.119689) H44C(-
 0.183575) H45(-0.271598) H46A(-0.258983) H46B(-0.328463) H46C(-0.318132) H47A(-
 0.167498) H47B(-0.23318) H47C(-0.158209) H48(-0.342956) H49(-0.387073) H50(-
 0.321035) H52(-0.205481) H53(-0.098524) H55(-0.00546) H56(0.023052) H57(-
 0.057413) H61A(0.049399) H61B(0.042853) H62A(0.616795) H62B(0.599049)
 H62C(0.615103) H62D(0.676631)
 Fixed Y: H3(0.38757) H4(0.554535) H5(0.662691) H7A(0.661759) H7B(0.673691)
 H8A(0.470738) H8B(0.501422) H9A(0.658609) H9B(0.579247) H10A(0.723346)
 H10B(0.742847) H11A(0.638221) H11B(0.560157) H12(0.180812) H13A(0.312909)
 H13B(0.2101) H13C(0.276388) H14A(0.126075) H14B(0.064404) H14C(0.072139)
 H15(0.161105) H16A(0.216197) H16B(0.130196) H16C(0.118475) H17A(0.312317)
 H17B(0.2385) H17C(0.329988) H18(0.576913) H19(0.630804) H20(0.597926)
 H22(0.519229) H23(0.428954) H25(0.333905) H26(0.28187) H27(0.314994)
 H33(0.69479) H34(0.531554) H35(0.435545) H37A(0.443685) H37B(0.438274)
 H38A(0.557769) H38B(0.474542) H39A(0.375568) H39B(0.400016) H40A(0.539407)
 H40B(0.455341) H41A(0.609682) H41B(0.647753) H42(0.944696) H43A(0.791266)
 H43B(0.877777) H43C(0.792379) H44A(0.996099) H44B(0.991346) H44C(0.905345)
 H45(0.930194) H46A(0.810007) H46B(0.885725) H46C(0.789482) H47A(1.025425)
 H47B(1.024567) H47C(0.955498) H48(0.801042) H49(0.83403) H50(0.773758)
 H52(0.673688) H53(0.580927) H55(0.500024) H56(0.469717) H57(0.532125)
 H61A(0.868019) H61B(0.832286) H62A(0.079713) H62B(0.133484) H62C(0.203862)
 H62D(0.134688)
 Fixed Z: H3(0.512815) H4(0.491753) H5(0.532767) H7A(0.633712) H7B(0.592682)
 H8A(0.620155) H8B(0.576361) H9A(0.576165) H9B(0.576711) H10A(0.689685)
 H10B(0.644145) H11A(0.694169) H11B(0.694676) H12(0.626613) H13A(0.577323)
 H13B(0.551164) H13C(0.540899) H14A(0.561541) H14B(0.569995) H14C(0.609405)
 H15(0.648444) H16A(0.72051) H16B(0.725) H16C(0.68997) H17A(0.663179)
 H17B(0.705701) H17C(0.707232) H18(0.664685) H19(0.727095) H20(0.800232)
 H22(0.851516) H23(0.857192) H25(0.817742) H26(0.750334) H27(0.680596)
 H33(0.509317) H34(0.487607) H35(0.526415) H37A(0.584387) H37B(0.62367)
 H38A(0.695553) H38B(0.689481) H39A(0.647674) H39B(0.697092) H40A(0.588243)
 H40B(0.584234) H41A(0.575666) H41B(0.622556) H42(0.635664) H43A(0.702392)
 H43B(0.695014) H43C(0.657595) H44A(0.671629) H44B(0.7087) H44C(0.706598)
 H45(0.609541) H46A(0.529951) H46B(0.537157) H46C(0.568694) H47A(0.585907)
 H47B(0.544995) H47C(0.542639) H48(0.678379) H49(0.750383) H50(0.815311)
 H52(0.850495) H53(0.840868) H55(0.786032) H56(0.711675) H57(0.651443)
 H61A(0.510243) H61B(0.561844) H62A(0.558341) H62B(0.510057) H62C(0.503547)
 H62D(0.531832)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              43172
_olex2_submission_special_instructions 'No special instructions were received'