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_7047042
_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         '2(C28 H40 N2)'
_chemical_formula_sum            'C56 H80 N4'
_chemical_formula_weight         809.24
_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   geom
_audit_creation_date             2018-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2018-05-04 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.15(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.936(5)
_cell_length_b                   18.585(4)
_cell_length_c                   12.560(3)
_cell_measurement_reflns_used    20881
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.430
_cell_volume                     5175(2)
_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  'olex2.refine (Bourhis et al., 2013)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            KappaCCD
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '4 circles diffractometer'
_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  0.0455
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20881
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.430
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.696984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0504 before and 0.0339 after correction.
The Ratio of minimum to maximum transmission is 0.6970.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4540
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0544P)^2^+4.7800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1468
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2691
_reflns_number_total             4540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02462f2.cif
_cod_data_source_block           nanny
_cod_depositor_comments
'Adding full bibliography for 7047041--7047045.cif.'
_cod_database_code               7047042
_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. Restrained distances
 C23A-C21
 1.53 with sigma of 0.02
 C21-C23B
 1.53 with sigma of 0.02
 C21-C22A
 1.53 with sigma of 0.02
 C21-C22B
 1.53 with sigma of 0.02
 C21-C24A
 1.53 with sigma of 0.02
 C21-C24B
 1.53 with sigma of 0.02
3. Rigid bond restraints
 C24B, C24A, C22B, C22A, C23B, C23A, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C23A \\sim C23B \\sim C24B \\sim C21 \\sim C24A \\sim C22B \\sim C22A: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C24A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C23A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C22B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23B)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 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(1)
6.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C5(H5), C10(H10)
6.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C14(H14A,H14B,
 H14C), C19(H19A,H19B,H19C), C28(H28A,H28B,H28C), C15(H15A,H15B,H15C), C16(H16A,
 H16B,H16C), C18(H18A,H18B,H18C), C23A(H23A,H23B,H23C), C22A(H22A,H22B,H22C),
 C24A(H24A,H24B,H24C), C22B(H22D,H22E,H22F), C23B(H23D,H23E,H23F), C24B(H24D,
 H24E,H24F)
;
_shelx_res_checksum              53680
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'