Ambidentate bonding and electrochemical implications of pincer-type pyridylidene amide ligands in complexes of nickel, cobalt and zinc.
Melle, Philipp; Ségaud, Nathalie; Albrecht, Martin; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12662–12673; doi:10.1039/d0dt02482a

data_7705243
_publ_section_title
;
 Ambidentate bonding and electrochemical implications of pincer-type
 pyridylidene amide ligands in complexes of nickel, cobalt and zinc.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12662
_journal_page_last               12673
_journal_paper_doi               10.1039/d0dt02482a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C38 H34 N10 Ni O4, 2(F6 P)'
_chemical_formula_sum            'C38 H34 F12 N10 Ni O4 P2'
_chemical_formula_weight         1043.40
_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             2019-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-13 deposited with the CCDC.	2020-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.2670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9760(2)
_cell_length_b                   21.8343(3)
_cell_length_c                   16.1933(2)
_cell_measurement_reflns_used    6188
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      24.6440
_cell_measurement_theta_min      1.8580
_cell_volume                     4231.03(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -16.00 112.00   1.00   50.00    --   27.42  77.00 150.00  128
  2  \w     35.00 122.00   1.00   50.00    --   27.42 178.00 120.00   87
  3  \w    -49.00  65.00   1.00   50.00    --   27.42 -57.00 120.00  114
  4  \w    -10.00 103.00   1.00   50.00    --   27.42  57.00 -90.00  113
  5  \w    -47.00  -6.00   1.00   50.00    --   27.42 132.00-149.82   41
  6  \w    -10.00  79.00   1.00   50.00    --   27.42  57.00  60.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0405869000
_diffrn_orient_matrix_UB_12      0.0014329000
_diffrn_orient_matrix_UB_13      -0.0306647000
_diffrn_orient_matrix_UB_21      0.0113804000
_diffrn_orient_matrix_UB_22      -0.0316294000
_diffrn_orient_matrix_UB_23      0.0056551000
_diffrn_orient_matrix_UB_31      -0.0416823000
_diffrn_orient_matrix_UB_32      -0.0072517000
_diffrn_orient_matrix_UB_33      -0.0308118000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36391
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.151
_diffrn_reflns_theta_min         1.566
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       needle
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         9541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0651
_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^)+(0.0544P)^2^+5.7171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6036
_reflns_number_total             9541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02482a2.cif
_cod_data_source_block           19MA33_PM295
_cod_depositor_comments
'Adding full bibliography for 7705237--7705245.cif.'
_cod_database_code               7705243
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C38H34F12N10Ni1O4P2
_chemical_oxdiff_usercomment     PM295
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C42(H42), C40(H40), C20(H20), C15(H15), C41(H41), C14(H14), C31(H31),
 C13(H13), C47(H47), C5(H5), C50(H50), C21(H21), C23(H23), C4(H4), C22(H22),
 C2(H2), C48(H48), C30(H30), C3(H3), C49(H49), C28(H28), C29(H29)
2.b Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C26(H26A,H26B,H26C), C33(H33A,H33B,H33C), C25(H25A,H25B,
 H25C)
;
_shelx_res_checksum              82863
_olex2_date_sample_data_collection 2019-02-25
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.226
_oxdiff_exptl_absorpt_empirical_full_min 0.855