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_7047045
_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 H80 N6 O, C2 H4 O2'
_chemical_formula_sum            'C58 H84 N6 O3'
_chemical_formula_weight         913.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-09-11
_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                101.99(3)
_cell_angle_beta                 95.68(3)
_cell_angle_gamma                107.23(3)
_cell_formula_units_Z            4
_cell_length_a                   15.004(3)
_cell_length_b                   15.758(3)
_cell_length_c                   25.923(5)
_cell_measurement_reflns_used    81884
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.397
_cell_volume                     5641(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  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            KappaCCD
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Enraf Nonius 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  0.0283
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            81884
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.397
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.809312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1144 before and 0.0274 after correction.
The Ratio of minimum to maximum transmission is 0.8093.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       plate
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.63
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1358
_refine_ls_number_reflns         19429
_refine_ls_number_restraints     590
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0524P)^2^+2.9515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13891
_reflns_number_total             19429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02462f2.cif
_cod_data_source_block           sadnico
_cod_depositor_comments
'Adding full bibliography for 7047041--7047045.cif.'
_cod_database_code               7047045
_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
2. Restrained distances
 C25-C27B
 1.5 with sigma of 0.02
 C28B-C25
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C51B, C51A, C52B, C52A, C50B, C50A, C79A, C77, C80A, C78A, C105, C107, C117,
 C106, C116, C108, C118, C109, C112, C111, C110, C99, C97, C100, C98, C81, C83,
 C84, C82, C17, C19, C20, C18, C71, C70, C69, C72, C101, C102, C103, C104, C73,
 C75, C74, C76, C41, C42, C44, C43, C49, C55, C53, C54, C56, C22, C21, C24, C23,
  C13, C15, C16, C1A, C48, C45, C47, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C80B, C78A, C78B, C79A, C79B, C80A, C77
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C78B, C78A, C80B, C80A, C79B, C79A, C77
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25, C27A, C28A, C26A, C26B, C28B, C27B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C52B \\sim C51A \\sim C51B \\sim C50A \\sim C50B \\sim C52A \\sim C82 \\sim C83
\\sim C84 \\sim C81 \\sim C80A \\sim C77 \\sim C79A \\sim C78A \\sim C46 \\sim
C48 \\sim C47 \\sim C45 \\sim C1A \\sim C15 \\sim C16 \\sim C13 \\sim C17 \\sim
C18 \\sim C20 \\sim C19 \\sim C24 \\sim C21 \\sim C23 \\sim C22 \\sim C56 \\sim
C53 \\sim C55 \\sim C54 \\sim C42 \\sim C43 \\sim C44 \\sim C98 \\sim C97 \\sim
C41 \\sim C49 \\sim C99 \\sim C100 \\sim C74 \\sim C76 \\sim C73 \\sim C75
\\sim C109 \\sim C111 \\sim C112 \\sim C110 \\sim C105 \\sim C107 \\sim C117
\\sim C106 \\sim C116 \\sim C108 \\sim C118 \\sim C102 \\sim C101 \\sim C104
\\sim C103 \\sim C71 \\sim C72 \\sim C69 \\sim C70: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C80B \\sim C78A \\sim C78B \\sim C79A \\sim C79B \\sim C80A \\sim C77: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C78B \\sim C78A \\sim C80B \\sim C80A \\sim C79B \\sim C79A \\sim C77: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C25 \\sim C27A \\sim C28A \\sim C26A \\sim C26B \\sim C28B \\sim C27B: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C78A) = Uanis(C79B)
Uanis(C80B) = Uanis(C79A)
Uanis(C78B) = Uanis(C80A)
Uanis(C27B) = Uanis(C27A)
5. Others
 Sof(C79B)=Sof(H79D)=Sof(H79E)=Sof(H79F)=Sof(C78B)=Sof(H78D)=Sof(H78E)=
 Sof(H78F)=Sof(C80B)=Sof(H80D)=Sof(H80E)=Sof(H80F)=1-FVAR(1)
 Sof(C78A)=Sof(H78A)=Sof(H78B)=Sof(H78C)=Sof(C79A)=Sof(H79A)=Sof(H79B)=
 Sof(H79C)=Sof(C80A)=Sof(H80A)=Sof(H80B)=Sof(H80C)=FVAR(1)
 Sof(C52B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(C51B)=Sof(H51D)=Sof(H51E)=
 Sof(H51F)=Sof(C50B)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(2)
 Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C50A)=Sof(H50A)=Sof(H50B)=
 Sof(H50C)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(2)
 Sof(C118)=Sof(H11J)=Sof(H11K)=Sof(H11L)=Sof(C117)=Sof(H11M)=Sof(H11N)=
 Sof(H11O)=Sof(C116)=Sof(H11P)=Sof(H11Q)=Sof(H11R)=1-FVAR(3)
 Sof(C108)=Sof(H10M)=Sof(H10N)=Sof(H10O)=Sof(C106)=Sof(H10P)=Sof(H10Q)=
 Sof(H10R)=Sof(C107)=Sof(H10S)=Sof(H10T)=Sof(H10U)=FVAR(3)
 Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C28B)=Sof(H28D)=Sof(H28E)=
 Sof(H28F)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(4)
 Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28A)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(4)
6.a Aromatic/amide H refined with riding coordinates:
 C92(H92), C66(H66), C64(H64), C36(H36), C8(H8), C10(H10), C59(H59), C3(H3),
 C94(H94), C31(H31), C87(H87), C61(H61), C89(H89), C38(H38), C33(H33), C5(H5)
6.b Idealised Me refined with riding coordinates:
 C79B(H79D,H79E,H79F)
6.c Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C47(H47A,H47B,H47C), C18(H18A,H18B,H18C), C84(H84A,H84B,
 H84C), C82(H82A,H82B,H82C), C48(H48A,H48B,H48C), C110(H11A,H11B,H11C),
 C16(H16A,H16B,H16C), C112(H11D,H11E,H11F), C103(H10A,H10B,H10C), C20(H20A,H20B,
 H20C), C24(H24A,H24B,H24C), C111(H11G,H11H,H11I), C75(H75A,H75B,H75C),
 C76(H76A,H76B,H76C), C46(H46A,H46B,H46C), C15(H15A,H15B,H15C), C27A(H27A,H27B,
 H27C), C99(H99A,H99B,H99C), C104(H10D,H10E,H10F), C19(H19A,H19B,H19C),
 C42(H42A,H42B,H42C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C22(H22A,H22B,
 H22C), C102(H10G,H10H,H10I), C14(H14A,H14B,H14C), C1A(H1AA,H1AB,H1AC),
 C54(H54A,H54B,H54C), C114(H11S,H11T,H11U), C28A(H28A,H28B,H28C), C55(H55A,H55B,
 H55C), C23(H23A,H23B,H23C), C44(H44A,H44B,H44C), C78A(H78A,H78B,H78C),
 C79A(H79A,H79B,H79C), C80A(H80A,H80B,H80C), C26A(H26A,H26B,H26C), C70(H70A,
 H70B,H70C), C100(H10J,H10K,H10L), C43(H43A,H43B,H43C), C56(H56A,H56B,H56C),
 C71(H71A,H71B,H71C), C51A(H51A,H51B,H51C), C98(H98A,H98B,H98C), C50A(H50A,H50B,
 H50C), C52A(H52A,H52B,H52C), C108(H10M,H10N,H10O), C106(H10P,H10Q,H10R),
 C107(H10S,H10T,H10U), C118(H11J,H11K,H11L), C117(H11M,H11N,H11O), C116(H11P,
 H11Q,H11R), C52B(H52D,H52E,H52F), C51B(H51D,H51E,H51F), C50B(H50D,H50E,H50F),
 C78B(H78D,H78E,H78F), C80B(H80D,H80E,H80F), C26B(H26D,H26E,H26F), C28B(H28D,
 H28E,H28F), C27B(H27D,H27E,H27F)
6.d Idealised tetrahedral OH refined as rotating group:
 O5(H5A), O3(H3A)
;
_shelx_res_checksum              27370
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'