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_7060664
_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
'C27 H35 N3 Ni O2 P, C0.69 H1.38 Cl1.38, F6 Sb'
_chemical_formula_sum            'C27.69 H36.38 Cl1.38 F6 N3 Ni O2 P Sb'
_chemical_formula_weight         817.61
_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
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;
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
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5548(7)
_cell_length_b                   15.2342(7)
_cell_length_c                   14.8051(8)
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.512
_cell_measurement_theta_min      4.173
_cell_volume                     3269.9(3)
_computing_cell_refinement
;
SAINT (2020) V8.40B; 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 (2020) V8.40B; 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 2018/2 (Sheldrick, 2018)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.972
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.990
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_diffrn_reflns_limit_h_max       17
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_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
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_diffrn_reflns_number            40637
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.618
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_diffrn_source                   'Microfocus Source'
_diffrn_source_current           0.65
_diffrn_source_power             0.0291265
_diffrn_source_target            Cu
_diffrn_source_type              'Incoatec I\mS High Brilliance Microsource'
_diffrn_source_voltage           44.81
_exptl_absorpt_coefficient_mu    9.343
_exptl_absorpt_correction_T_max  0.2260
_exptl_absorpt_correction_T_min  0.0798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1463 before and 0.0755 after correction.
The Ratio of minimum to maximum transmission is 0.3531.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.098
_refine_diff_density_max         2.047
_refine_diff_density_min         -1.791
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6314
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0856
_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^)+47.6774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1873
_refine_ls_wR_factor_ref         0.1882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6061
_reflns_number_total             6314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01355f2.cif
_cod_data_source_block           naser79
_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               7060664
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_shelx_estimated_absorpt_t_max   0.461
_shelx_estimated_absorpt_t_min   0.327
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.064) H4(0.067) H5(0.058) H7A(0.052) H7B(0.052) H8A(0.052)
 H8B(0.052) H9A(0.055) H9B(0.055) H10A(0.059) H10B(0.059) H11A(0.052)
 H11B(0.052) H12(0.059) H13A(0.082) H13B(0.082) H13C(0.082) H14A(0.087)
 H14B(0.087) H14C(0.087) H15(0.06) H16A(0.097) H16B(0.097) H16C(0.097)
 H17A(0.097) H17B(0.097) H17C(0.097) H18(0.06) H19(0.062) H20(0.059) H21(0.052)
 H24(0.058) H25(0.063) H26(0.056) H27(0.057) H30C(0.082) H30D(0.082)
 H30A(0.082) H30B(0.082)
 Fixed X: H3(0.33751) H4(0.289346) H5(0.283456) H7A(0.244371) H7B(0.32921)
 H8A(0.374945) H8B(0.274448) H9A(0.323046) H9B(0.338558) H10A(0.552114)
 H10B(0.451868) H11A(0.486015) H11B(0.508863) H12(0.552559) H13A(0.56476)
 H13B(0.647753) H13C(0.562608) H14A(0.524917) H14B(0.620875) H14C(0.530082)
 H15(0.367028) H16A(0.454339) H16B(0.353775) H16C(0.383257) H17A(0.229944)
 H17B(0.218678) H17C(0.226264) H18(0.141282) H19(0.000541) H20(-0.001996)
 H21(0.136343) H24(0.267587) H25(0.416549) H26(0.544226) H27(0.520866)
 H30C(0.42572) H30D(0.455198) H30A(0.500622) H30B(0.410564)
 Fixed Y: H3(-0.08898) H4(-0.129192) H5(-0.023902) H7A(0.17588) H7B(0.135714)
 H8A(0.3636) H8B(0.324451) H9A(0.274594) H9B(0.378483) H10A(0.21741)
 H10B(0.178005) H11A(0.153184) H11B(0.254784) H12(0.235656) H13A(0.072023)
 H13B(0.139936) H13C(0.165312) H14A(0.15351) H14B(0.121623) H14C(0.063188)
 H15(0.168475) H16A(0.296923) H16B(0.323161) H16C(0.345031) H17A(0.26304)
 H17B(0.222523) H17C(0.158867) H18(0.17243) H19(0.238414) H20(0.382787)
 H21(0.464948) H24(0.53006) H25(0.591094) H26(0.498574) H27(0.347726)
 H30C(0.435432) H30D(0.406795) H30A(0.430689) H30B(0.409843)
 Fixed Z: H3(0.665891) H4(0.514151) H5(0.39931) H7A(0.40518) H7B(0.356362)
 H8A(0.442972) H8B(0.415119) H9A(0.275376) H9B(0.284955) H10A(0.326773)
 H10B(0.297472) H11A(0.453172) H11B(0.470396) H12(0.766829) H13A(0.675069)
 H13B(0.696274) H13C(0.625234) H14A(0.898013) H14B(0.864186) H14C(0.843501)
 H15(0.875123) H16A(0.882448) H16B(0.909172) H16C(0.810027) H17A(0.764923)
 H17B(0.863062) H17C(0.778056) H18(0.554624) H19(0.57659) H20(0.619805)
 H21(0.638215) H24(0.633348) H25(0.637677) H26(0.637482) H27(0.624926)
 H30C(0.066196) H30D(0.169056) H30A(0.173904) H30B(0.107149)
;
_shelx_res_checksum              31082
_olex2_submission_special_instructions 'No special instructions were received'