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_7047044
_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(F6 Sb), 2(C56 H83 N6), 2(C H4 O)'
_chemical_formula_sum            'C114 H174 F12 N12 O2 Sb2'
_chemical_formula_weight         2216.14
_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   mixed
_audit_creation_date             2017-09-06
_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                93.48(3)
_cell_angle_beta                 98.319(17)
_cell_angle_gamma                93.55(2)
_cell_formula_units_Z            1
_cell_length_a                   13.287(2)
_cell_length_b                   13.328(2)
_cell_length_c                   17.363(7)
_cell_measurement_reflns_used    57540
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      1.553
_cell_volume                     3029.0(14)
_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 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker-AXS-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  0.0400
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57540
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.553
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.791994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0641 before and 0.0363 after correction.
The Ratio of minimum to maximum transmission is 0.7920.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.037
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         13849
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0280P)^2^+5.0480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9236
_reflns_number_total             13849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02462f2.cif
_cod_data_source_block           nl229120123nico
_cod_depositor_comments
'Adding full bibliography for 7047041--7047045.cif.'
_cod_original_cell_volume        3029.0(15)
_cod_database_code               7047044
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid bond restraints
 F6B, F6A, F5B, F5A, F4B, F4A, F3B, F3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C30, C29, C31, C32, C33, C34, C45, C46, C48, C42, C41, C44, C43, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
F4A \\sim F4B \\sim F5A \\sim F5B \\sim F6A \\sim F6B \\sim F3A \\sim F3B:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
N4 \\sim C30 \\sim C29 \\sim C31 \\sim C33 \\sim C48 \\sim C45 \\sim C46 \\sim
C47 \\sim C41 \\sim C42 \\sim C44 \\sim C43: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Others
 Sof(F5B)=Sof(F6B)=Sof(F4B)=Sof(F3B)=1-FVAR(1)
 Sof(F3A)=Sof(F4A)=Sof(F6A)=Sof(F5A)=FVAR(1)
5.a Free rotating group:
 N4(H4)
5.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C40(H40), C5(H5), C3(H3), C33(H33), C38(H38), C8(H8)
5.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C28(H28A,H28B,
 H28C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C18(H18A,H18B,H18C), C20(H20A,
 H20B,H20C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C44(H44A,H44B,H44C),
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C42(H42A,H42B,H42C), C54(H54A,H54B,
 H54C), C43(H43A,H43B,H43C), C48(H48A,H48B,H48C), C55(H55A,H55B,H55C), C24(H24A,
 H24B,H24C), C47(H47A,H47B,H47C), C23(H23A,H23B,H23C), C56(H56A,H56B,H56C),
 C46(H46A,H46B,H46C), C22(H22A,H22B,H22C), C57(H57A,H57B,H57C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              16467
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'