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_7705241
_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         'C19 H17 Cl2 Co N5 O2, 2(C2 H6 O S)'
_chemical_formula_sum            'C23 H29 Cl2 Co N5 O4 S2'
_chemical_formula_weight         633.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-23
_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                 95.0990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.84210(10)
_cell_length_b                   13.98040(10)
_cell_length_c                   19.00770(10)
_cell_measurement_reflns_used    14764
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      76.7580
_cell_measurement_theta_min      3.8100
_cell_volume                     5516.56(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_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    -63.00  -5.00   0.50    0.75    --  -18.75 119.00  41.00  116
  2  \w     26.00  94.00   0.50    0.75    --   47.95  77.00 150.00  136
  3  \w     96.00 174.00   0.50    2.50    --  107.11 119.00  41.00  156
  4  \w     91.00 174.00   0.50    2.50    --  107.11  61.00 120.00  166
  5  \w     95.00 174.00   0.50    2.50    --  107.11  45.00-120.00  158
  6  \w     92.00 174.00   0.50    2.50    --  107.11 125.00-150.00  164
  7  \w     85.00 174.00   0.50    2.50    --  107.11  77.00-180.00  178
  8  \w     28.00  93.00   0.50    0.75    --   47.95-119.00 -43.00  130
  9  \w     35.00 113.00   0.50    2.50    --  107.11-119.00 -43.00  156
 10  \w     35.00 102.00   0.50    2.50    --  107.11 -77.00   0.00  134
 11  \w     35.00  68.00   0.50    2.50    --  107.11 -61.00  60.00   66
 12  \w     35.00 109.00   0.50    2.50    --  107.11 -94.00   0.00  148
 13  \w     35.00  68.00   0.50    2.50    --  107.11 -61.00-150.00   66
 14  \w     35.00  68.00   0.50    2.50    --  107.11 -61.00-120.00   66
 15  \w     35.00  68.00   0.50    2.50    --  107.11 -61.00 -60.00   66
 16  \w    -26.00  23.00   0.50    0.75    --   47.95 -19.00 120.00   98
 17  \w    -26.00  23.00   0.50    0.75    --   47.95 -19.00  30.00   98
 18  \w    -26.00  23.00   0.50    0.75    --   47.95 -19.00 -90.00   98
 19  \w    -26.00  23.00   0.50    0.75    --   47.95 -19.00-120.00   98
 20  \w     26.00 120.00   0.50    0.75    --   47.95  77.00-120.00  188
 21  \w     26.00 120.00   0.50    0.75    --   47.95  77.00   0.00  188
 22  \w     35.00  68.00   0.50    2.50    --  107.11 -61.00 150.00   66
 23  \w    -86.00 -26.00   0.50    0.75    --  -18.75 157.00-163.00  120
 24  \w    -90.00   5.00   0.50    0.75    --  -18.75 -77.00 120.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0002586000
_diffrn_orient_matrix_UB_12      0.1092757000
_diffrn_orient_matrix_UB_13      0.0105189000
_diffrn_orient_matrix_UB_21      -0.0737303000
_diffrn_orient_matrix_UB_22      -0.0012546000
_diffrn_orient_matrix_UB_23      0.0020013000
_diffrn_orient_matrix_UB_31      0.0084637000
_diffrn_orient_matrix_UB_32      -0.0142128000
_diffrn_orient_matrix_UB_33      0.0806525000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27154
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.142
_diffrn_reflns_theta_min         3.812
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.409
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            dark
_exptl_crystal_colour_primary    dark
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       needle
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0378P)^2^+7.0215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5254
_reflns_number_total             5678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02482a2.cif
_cod_data_source_block           19MA104_PM313
_cod_depositor_comments
'Adding full bibliography for 7705237--7705245.cif.'
_cod_database_code               7705241
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C19H17Cl2Co1N5O2
_shelx_estimated_absorpt_t_max   0.679
_shelx_estimated_absorpt_t_min   0.284
_diffrn_oxdiff_digest_frames
;
011c851e1d1ec45d472d3f3824a806a905021868970
;
_diffrn_oxdiff_digest_hkl
;
01c447ac8fb2c419465dcc4695b6df0bbd54c4
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C12(H12), C16(H16), C6(H6), C23(H23), C13(H13), C19(H19), C20(H20), C4(H4),
 C22(H22), C15(H15), C5(H5)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              84128
_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 2.151
_oxdiff_exptl_absorpt_empirical_full_min 0.608