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_7060667
_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, C22 H32 N2 Ni O2 P'
_chemical_formula_sum            'C22 H32 F6 N2 Ni O2 P Sb'
_chemical_formula_weight         681.92
_chemical_name_systematic        POCN-Ni-py
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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
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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                68.3830(10)
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_cell_angle_gamma                87.0200(10)
_cell_formula_units_Z            4
_cell_length_a                   12.2664(3)
_cell_length_b                   13.2418(3)
_cell_length_c                   17.5270(5)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    120
_cell_measurement_theta_max      60.755
_cell_measurement_theta_min      3.144
_cell_volume                     2638.99(12)
_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)'
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_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'
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_diffrn_measured_fraction_theta_max 0.994
_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  0.0600
_diffrn_reflns_av_unetI/netI     0.0471
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_diffrn_reflns_limit_h_max       15
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_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            92015
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
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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    10.221
_exptl_absorpt_correction_T_max  0.4146
_exptl_absorpt_correction_T_min  0.2141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1395 before and 0.0972 after correction.
The Ratio of minimum to maximum transmission is 0.5164.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       block
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_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         12104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
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_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+1.2403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11575
_reflns_number_total             12104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01355f2.cif
_cod_data_source_block           1b-naser53
_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        2639.00(12)
_cod_database_code               7060667
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_olex2_refinement_description
;
1. Others
 Fixed Uiso: H00C(0.056) H00D(0.056) H00S(0.056) H00V(0.057) H00A(0.054)
 H00B(0.054) H00X(0.058) H00Y(0.062) H00Z(0.056) H010(0.063) H01(0.054)
 H(0.054) H013(0.054) H014(0.06) H01A(0.053) H01B(0.053) H1(0.086) HA(0.086)
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 HK(0.086) H01P(0.061) H01Q(0.061) H01S(0.095) H01T(0.095) H01U(0.095)
 H01V(0.087) H01W(0.077) H01X(0.111) H01Y(0.111) HL(0.111) H01Z(0.091)
 Fixed X: H00C(0.557198) H00D(0.554995) H00S(0.386006) H00V(0.034161)
 H00A(0.591385) H00B(0.57635) H00X(0.257564) H00Y(0.167191) H00Z(0.031403)
 H010(0.36252) H01(0.37069) H(0.382614) H013(0.196683) H014(0.193691)
 H01A(0.391458) H01B(0.420496) H1(-0.068457) HA(-0.124444) HB(-0.09403)
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 HE(0.241131) H01F(0.549804) H01G(0.476464) H6(0.128601) HF(0.032405)
 HG(0.012226) H7(0.55891) HH(0.486672) H8(0.251498) H01L(0.440375)
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 H010(0.106868) H01(0.539866) H(0.56696) H013(0.430412) H014(0.975478)
 H01A(1.033417) H01B(1.058831) H1(0.402591) HA(0.444945) HB(0.321095)
 H018(0.376069) H2(0.434696) HC(0.466534) H3(0.430233) H01C(0.893329)
 H01D(0.923351) H01E(0.686657) H4(0.172565) H5(0.116605) HD(0.025759)
 HE(0.094456) H01F(0.786619) H01G(0.861241) H6(0.158674) HF(0.086672)
 HG(0.211522) H7(0.313109) HH(0.379245) H8(0.199977) H01L(0.918673)
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 Fixed Z: H00C(0.739644) H00D(0.781911) H00S(1.000987) H00V(0.917852)
 H00A(0.266274) H00B(0.309063) H00X(0.078988) H00Y(1.131305) H00Z(0.390916)
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 H018(0.593587) H2(0.945938) HC(0.850407) H3(0.527973) H01C(0.487201)
 H01D(0.391859) H01E(0.524186) H4(0.874072) H5(0.833501) HD(0.909599)
 HE(0.922002) H01F(0.446195) H01G(0.481818) H6(1.018249) HF(1.015794)
 HG(0.9955) H7(0.919551) HH(0.963322) H8(1.209128) H01L(0.034056)
 H01M(0.123016) H01H(0.490936) H01I(0.472245) H01J(0.453864) H01K(0.308576)
 H01N(0.294544) H01O(0.229572) H9(0.60057) H10(0.772926) HI(0.815382)
 H01R(0.332294) H11(0.827024) HJ(0.821668) HK(0.753092) H01P(0.301355)
 H01Q(0.336401) H01S(0.242543) H01T(0.304934) H01U(0.330012) H01V(0.65511)
 H01W(0.579451) H01X(0.307823) H01Y(0.384793) HL(0.396399) H01Z(0.683553)
;
_shelx_res_checksum              21193
_olex2_submission_special_instructions 'No special instructions were received'