Structural snapshots of the rearrangement of the bis(di-tert-butyl-aminophenyl)amine pincer ligand in the presence of transition metal ions.
Leconte, N.; Baptiste, B.; Philouze, C.; Thomas, F.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11303–11307; doi:10.1039/c8dt02462f

data_7047043
_publ_section_title
;
 Structural snapshots of the rearrangement of the
 bis(di-tert-butyl-aminophenyl)amine pincer ligand in the presence of
 transition metal ions.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11303
_journal_page_last               11307
_journal_paper_doi               10.1039/c8dt02462f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C56 H86 Co N6'
_chemical_formula_sum            'C56 H86 Co N6'
_chemical_formula_weight         902.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-09-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2017-10-09 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.90(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.417(6)
_cell_length_b                   9.7021(19)
_cell_length_c                   19.879(4)
_cell_measurement_reflns_used    24321
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.219
_cell_volume                     5460.7(19)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            KappaCCD
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker kappaCCD'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24321
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.219
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.783687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0706 before and 0.0370 after correction.
The Ratio of minimum to maximum transmission is 0.7837.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_description       block
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4735
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0365P)^2^+12.1065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3750
_reflns_number_total             4735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02462f2.cif
_cod_data_source_block           nanny_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7047041--7047045.cif.'
_cod_original_cell_volume        5460.8(19)
_cod_database_code               7047043
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H3BA,H3BB} of N3B, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H3AA,H3AB} of N3A
2. Rigid bond restraints
 C21, C23A, C22A, C24A, C24B, C23B, C22B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C21 \\sim C23A \\sim C22A \\sim C24A \\sim C24B \\sim C23B \\sim C22B: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(H12)=Sof(N3B)=Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(H8)=Sof(N3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C14A)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(2)
 Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23B)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(3)
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(3)
5.a Free rotating group:
 N3A(H3AA,H3AB), N3B(H3BA,H3BB)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C10(H10), C12(H12), C8(H8), C3(H3), C5(H5)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C16A(H16A,H16B,H16C),
 C23A(H23A,H23B,H23C), C22A(H22A,H22B,H22C), C24A(H24A,H24B,H24C), C14A(H14A,
 H14B,H14C), C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C16B(H16D,H16E,H16F),
 C14B(H14D,H14E,H14F), C24B(H24D,H24E,H24F), C23B(H23D,H23E,H23F), C22B(H22D,
 H22E,H22F)
;
_shelx_res_checksum              41268
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'