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_7705245
_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 Co N10 O4, 3(F6 P), 2(H2 O)'
_chemical_formula_sum            'C38 H38 Co F18 N10 O6 P3'
_chemical_formula_weight         1224.62
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-07-13 deposited with the CCDC.	2020-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3165(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.05781(13)
_cell_length_b                   14.7905(2)
_cell_length_c                   24.4665(3)
_cell_measurement_reflns_used    13124
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.4710
_cell_measurement_theta_min      1.6780
_cell_volume                     4662.92(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 0.984
_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  58.00   1.00   32.50    --  -23.50  70.00  97.00  121
  2  \w     35.00 122.00   1.00   32.50    --   27.42 178.00-150.00   87
  3  \w    -10.00 103.00   1.00   32.50    --   27.42  57.00 -60.00  113
  4  \w    -49.00  65.00   1.00   32.50    --   27.42 -57.00   0.00  114
  5  \w     35.00 122.00   1.00   32.50    --   27.42 178.00 -90.00   87
  6  \w    -44.00  25.00   1.00   32.50    --   27.42 -70.00 -33.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0241485000
_diffrn_orient_matrix_UB_12      -0.0323790000
_diffrn_orient_matrix_UB_13      0.0151070000
_diffrn_orient_matrix_UB_21      0.0490119000
_diffrn_orient_matrix_UB_22      -0.0199381000
_diffrn_orient_matrix_UB_23      0.0095950000
_diffrn_orient_matrix_UB_31      0.0067004000
_diffrn_orient_matrix_UB_32      0.0292183000
_diffrn_orient_matrix_UB_33      0.0232977000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39769
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.049
_diffrn_reflns_theta_min         1.580
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       needle
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         10068
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0813P)^2^+5.2501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7551
_reflns_number_total             10068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02482a2.cif
_cod_data_source_block           17MA133_PM107-H2O
_cod_depositor_comments
'Adding full bibliography for 7705237--7705245.cif.'
_cod_original_cell_volume        4662.91(10)
_cod_database_code               7705245
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C38H34Co1F12N10O4P2
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.840
_reflns_odcompleteness_completeness 99.97
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H2WA-O43
 1.97 with sigma of 0.02
 H2WB-O35_$1
 2.11 with sigma of 0.02
 H2WA-H2WB
 1.44 with sigma of 0.02
3.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C14(H14), C30(H30), C7(H7), C13(H13), C37(H37), C4(H4), C38(H38),
 C01F(H01F), C28(H28), C01I(H01I), C29(H29), C3(H3), C01P(H01P), C5(H5),
 C25(H25), C01U(H01U), C21(H21), C12(H12), C39(H39), C23(H23), C24(H24)
3.c Idealised Me refined as rotating group:
 C019(H01A,H01B,H01C), C0AA(H0AA,H0AB,H0AC), C26(H26A,H26B,H26C), C1(H1A,H1B,
 H1C)
;
_olex2_date_sample_data_collection 2017-09-12
_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 1.624
_oxdiff_exptl_absorpt_empirical_full_min 0.661