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_7060661
_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, C28 H39 N2 Ni O2 P2, C4 H8 O'
_chemical_formula_sum            'C32 H47 F6 N2 Ni O3 P2 Sb'
_chemical_formula_weight         864.11
_chemical_name_systematic        POCOP-Ni-bipy
_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
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;
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                 91.766(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9127(6)
_cell_length_b                   9.2788(3)
_cell_length_c                   23.5436(8)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    130
_cell_measurement_theta_max      60.529
_cell_measurement_theta_min      2.275
_cell_volume                     3692.9(2)
_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)'
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_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0844
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
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_diffrn_reflns_limit_l_min       -28
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_max         54.987
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_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    7.662
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.4805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1655 before and 0.0867 after correction.
The Ratio of minimum to maximum transmission is 0.6390.
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    1.554
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.741
_refine_diff_density_min         -1.800
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         7057
_refine_ls_number_restraints     254
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0323P)^2^+6.5544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5792
_reflns_number_total             7057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01355f2.cif
_cod_data_source_block           2c-naser56
_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               7060661
_shelx_shelxl_version_number     2017/1
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;
1. Others
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 H51D(0.121) H52C(0.122) H52D(0.122) H53C(0.109) H53D(0.109) H50C(0.133)
 H50D(0.133)
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 H50C(0.567231) H50D(0.594721)
 Fixed Y: H00J(0.837834) H00L(1.059928) H00M(0.815676) H00N(1.112147)
 H00P(1.002625) H00Q(1.138502) H00R(0.636357) H00S(0.591666) H00T(0.552146)
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 H5C(0.920698) H6A(0.721662) H6B(0.856058) H6C(0.74108) H51C(1.003035)
 H51D(1.056197) H52C(0.837105) H52D(0.770802) H53C(0.692227) H53D(0.807235)
 H50C(1.028106) H50D(0.87047)
 Fixed Z: H00J(0.665797) H00L(0.544749) H00M(0.674975) H00N(0.537564)
 H00P(0.599553) H00Q(0.749869) H00R(0.612253) H00S(0.695846) H00T(0.545059)
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 H00X(0.471411) H00D(0.702462) H00E(0.764314) H00F(0.712628) H00Z(0.462022)
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 H01I(0.581423) H53A(0.800166) H53B(0.765689) H01J(0.513895) H01K(0.470908)
 H01L(0.452157) H01M(0.460559) H01N(0.4993) H01O(0.432996) H50A(0.786322)
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 H51D(0.867714) H52C(0.896807) H52D(0.887002) H53C(0.806265) H53D(0.807254)
 H50C(0.81171) H50D(0.827275)
;
_shelx_res_checksum              48719
_olex2_submission_special_instructions 'No special instructions were received'