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_7705238
_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, 2(F6 P)'
_chemical_formula_sum            'C38 H34 Co F12 N10 O4 P2'
_chemical_formula_weight         1043.62
_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             2019-02-07
_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                 93.1440(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.94056(17)
_cell_length_b                   21.9377(4)
_cell_length_c                   16.2425(2)
_cell_measurement_reflns_used    28565
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      27.5570
_cell_measurement_theta_min      1.9290
_cell_volume                     4248.29(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.37a (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 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.944
_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   25.00    --   27.42  57.00 -30.00  113
  2  \w    -10.00 103.00   1.00   25.00    --   27.42  57.00-180.00  113
  3  \w     35.00 122.00   1.00   25.00    --   27.42 178.00 -30.00   87
  4  \w    -54.00  83.00   1.00   25.00    --   27.42 -38.00  90.00  137
  5  \w    -20.00  32.00   1.00   25.00    --  -23.50 -99.00-150.00   52
  6  \w     35.00 122.00   1.00   25.00    --   27.42 178.00-180.00   87
  7  \w    -10.00 103.00   1.00   25.00    --   27.42  57.00-120.00  113
  8  \w    -20.00  82.00   1.00   25.00    --   27.42 -99.00 -60.00  102
  9  \w    -49.00  65.00   1.00   25.00    --   27.42 -57.00 -30.00  114
 10  \w    -10.00 103.00   1.00   25.00    --   27.42  57.00  90.00  113
 11  \w    -16.00 104.00   1.00   25.00    --   27.42  77.00  30.00  120
;
_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      -0.0222114000
_diffrn_orient_matrix_UB_12      0.0077816000
_diffrn_orient_matrix_UB_13      0.0382125000
_diffrn_orient_matrix_UB_21      -0.0342123000
_diffrn_orient_matrix_UB_22      -0.0265042000
_diffrn_orient_matrix_UB_23      -0.0021626000
_diffrn_orient_matrix_UB_31      0.0432937000
_diffrn_orient_matrix_UB_32      -0.0168014000
_diffrn_orient_matrix_UB_33      0.0211814000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73492
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.194
_diffrn_reflns_theta_min         1.561
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  0.89258
_exptl_absorpt_correction_T_min  0.89258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.348
_exptl_crystal_size_min          0.163
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         9855
_refine_ls_number_restraints     618
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0549P)^2^+6.7788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8281
_reflns_number_total             9855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02482a2.cif
_cod_data_source_block           19ma017_pm293
_cod_depositor_comments
'Adding full bibliography for 7705237--7705245.cif.'
_cod_original_cell_volume        4248.28(12)
_cod_database_code               7705238
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.773
_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. Uiso/Uaniso restraints and constraints
F3A \\sim P1 \\sim F2 \\sim F2A \\sim F6A \\sim F3 \\sim F5A \\sim F5 \\sim F6
\\sim F1A \\sim F1 \\sim F4 \\sim F4A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
F9 \\sim P2 \\sim F10 \\sim F12 \\sim F8 \\sim F11 \\sim F7 \\sim F9A \\sim P2A
\\sim F12A \\sim F10A \\sim F8A \\sim F11A \\sim F7A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 F6, P1, F4, F1A, F3A, F5A, F2, F3, F6A, F2A, F5, F1, F4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F10, P2, F9, F8, F7, F11, F12, F11A, F8A, P2A, F12A, F10A, F7A, F9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F8A)=Sof(P2A)=Sof(F10A)=Sof(F12A)=Sof(F11A)=Sof(F7A)=Sof(F9A)=1-FVAR(1)
 Sof(P2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F4A)=Sof(F3A)=Sof(F5A)=Sof(F6A)=Sof(F1A)=Sof(F2A)=1-FVAR(2)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F1)=Sof(F2)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C28(H28),
  C29(H29), C30(H30), C34(H34), C35(H35), C36(H36), C37(H37)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C19(H19A,H19B,H19C), C25(H25A,H25B,H25C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              11802
_olex2_submission_special_instructions 'No special instructions were received'