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_7705240
_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'
_chemical_formula_sum            'C19 H17 Cl2 Co N5 O2'
_chemical_formula_weight         477.20
_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             2019-03-03
_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                102.016(2)
_cell_angle_beta                 99.280(2)
_cell_angle_gamma                104.188(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9978(2)
_cell_length_b                   9.2730(2)
_cell_length_c                   14.4181(4)
_cell_measurement_reflns_used    5682
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.0170
_cell_measurement_theta_min      2.3290
_cell_volume                     988.23(5)
_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 0.929
_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    -10.00 103.00   1.00   27.50    --   27.42  57.00   0.00  113
  2  \w    -16.00 112.00   1.00   27.50    --   27.42  77.00 -90.00  128
  3  \w    -16.00 112.00   1.00   27.50    --   27.42  77.00  30.00  128
  4  \w    -10.00 103.00   1.00   27.50    --   27.42  57.00-180.00  113
  5  \w     35.00 122.00   1.00   27.50    --   27.42 178.00 -90.00   87
  6  \w     35.00 122.00   1.00   27.50    --   27.42 178.00-180.00   87
  7  \w   -108.00 -55.00   1.00   27.50    --  -23.50-153.00-144.00   53
  8  \w    -54.00  83.00   1.00   27.50    --   27.42 -38.00  30.00  137
  9  \w     35.00 122.00   1.00   27.50    --   27.42 178.00 -30.00   87
 10  \w    -16.00  63.00   1.00   27.50    --   27.42  77.00 120.00   79
 11  \w    -49.00  65.00   1.00   27.50    --   27.42 -57.00 -90.00  114
;
_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      0.0587525000
_diffrn_orient_matrix_UB_12      0.0269970000
_diffrn_orient_matrix_UB_13      -0.0287144000
_diffrn_orient_matrix_UB_21      -0.0685854000
_diffrn_orient_matrix_UB_22      -0.0347918000
_diffrn_orient_matrix_UB_23      -0.0425092000
_diffrn_orient_matrix_UB_31      -0.0255688000
_diffrn_orient_matrix_UB_32      0.0687950000
_diffrn_orient_matrix_UB_33      0.0056342000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16903
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.103
_diffrn_reflns_theta_min         2.345
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78321
_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 blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       prism
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0303P)^2^+0.3672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3596
_reflns_number_total             4480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02482a2.cif
_cod_data_source_block           19ma035_PM305
_cod_depositor_comments
'Adding full bibliography for 7705237--7705245.cif.'
_cod_original_cell_volume        988.23(4)
_cod_database_code               7705240
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C19H17Cl2Co1N5O2
_chemical_oxdiff_usercomment     PM305
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.845
_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, {H22A,H22B,H22C} of C22
 At 1.5 times of:
  {H29A,H29B,H29C} of C29
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C17(H17), C24(H24), C7(H7), C27(H27), C18(H18), C25(H25),
 C20(H20), C19(H19), C26(H26)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              74595
_olex2_date_sample_data_collection 2019-03-01
_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 1.647
_oxdiff_exptl_absorpt_empirical_full_min 0.750