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_7047041
_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         'F6 Sb, C56 H82 Co N6, 2.03(C7 H8)'
_chemical_formula_sum            'C70.23 H98.26 Co F6 N6 Sb'
_chemical_formula_weight         1321.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-09-12
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.171(4)
_cell_length_b                   18.080(4)
_cell_length_c                   40.633(8)
_cell_measurement_reflns_used    92780
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.00
_cell_volume                     14084(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0675
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            92780
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.002
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.742878
_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 0.0341 after correction. The Ratio of minimum to maximum transmission is 0.7429. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       needle
_exptl_crystal_F_000             5549
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.646
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         12411
_refine_ls_number_restraints     325
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+20.2449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7689
_reflns_number_total             12411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02462f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7047041--7047045.cif.'
_cod_database_code               7047041
_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
2. Restrained distances
 C57-C58
 1.45 with sigma of 0.02
 C58-C59
 1.45 with sigma of 0.02
 C59-C60
 1.45 with sigma of 0.02
 C57-C59
 2.45 with sigma of 0.02
 C58-C60
 2.45 with sigma of 0.02
 C58-C58_$1
 2.45 with sigma of 0.02
 C59-C59_$1
 2.45 with sigma of 0.02
 C61-C59
 1.5 with sigma of 0.02
 C61-C58
 2.5 with sigma of 0.02
 C61-C60
 2.5 with sigma of 0.02
 C69-C70
 1.5 with sigma of 0.02
 C69-C71
 2.5 with sigma of 0.02
 C69-C75
 2.5 with sigma of 0.02
 C70-C71
 1.45 with sigma of 0.02
 C71-C72
 1.45 with sigma of 0.02
 C72-C73
 1.45 with sigma of 0.02
 C74-C75
 1.45 with sigma of 0.02
 C70-C75
 1.45 with sigma of 0.02
 C70-C72
 2.45 with sigma of 0.02
 C71-C73
 2.45 with sigma of 0.02
 C72-C74
 2.45 with sigma of 0.02
 C73-C75
 2.45 with sigma of 0.02
 C74-C70
 2.45 with sigma of 0.02
 C75-C71
 2.45 with sigma of 0.02
 C21-C23B
 1.5 with sigma of 0.02
 C21-C22B
 1.5 with sigma of 0.02
 C21-C24B
 1.5 with sigma of 0.02
 C23B-C24B
 2.5 with sigma of 0.02
 C23B-C22B
 2.5 with sigma of 0.02
 C22B-C24B
 2.5 with sigma of 0.02
 C52B-C51B
 2.5 with sigma of 0.02
 C51B-C50B
 2.5 with sigma of 0.02
 C50B-C52B
 2.5 with sigma of 0.02
 C52B-C49
 1.5 with sigma of 0.02
 C49-C50B
 1.5 with sigma of 0.02
 C51B-C49
 1.5 with sigma of 0.02
 C50A-C49
 1.5 with sigma of 0.02
 C49-C51A
 1.5 with sigma of 0.02
 C49-C52A
 1.5 with sigma of 0.02
 C51A-C50A
 2.5 with sigma of 0.02
 C50A-C52A
 2.5 with sigma of 0.02
 C51A-C52A
 2.5 with sigma of 0.02
 C62-C68
 2.5 with sigma of 0.02
 C62-C64
 2.5 with sigma of 0.02
 C62-C63
 1.5 with sigma of 0.02
 C63-C68
 1.45 with sigma of 0.02
 C68-C67
 1.45 with sigma of 0.02
 C67-C66
 1.45 with sigma of 0.02
 C66-C65
 1.45 with sigma of 0.02
 C65-C64
 1.45 with sigma of 0.02
 C64-C63
 1.45 with sigma of 0.02
 C63-C67
 2.45 with sigma of 0.02
 C68-C66
 2.45 with sigma of 0.02
 C67-C65
 2.45 with sigma of 0.02
 C66-C64
 2.45 with sigma of 0.02
 C65-C63
 2.45 with sigma of 0.02
 C64-C68
 2.45 with sigma of 0.02
3. Restrained planarity
 C65, C63, C64, C62, C68, C66, C67
 with sigma of 0.1
 C69, C70, C75, C71, C74, C72, C73
 with sigma of 0.1
4. Rigid bond restraints
 C65, C63, C64, C62, C68, C66, C67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C59, C57, C58, C60, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C67, C68, C63, C66, C64, C62, C65
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C70, C69, C75, C71, C74, C72, C73
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C23B, C23A, C24B, C24A, C22B, C22A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C52B, C51A, C51B, C50A, C50B, C52A, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C59 \\sim C57 \\sim C58 \\sim C60 \\sim C61: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C63 \\sim C68 \\sim C67 \\sim C66 \\sim C64 \\sim C62 \\sim C65: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C70 \\sim C69 \\sim C75 \\sim C71 \\sim C74 \\sim C72 \\sim C73: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C23A \\sim C24B \\sim C24A \\sim C22B \\sim C22A \\sim C23B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C52A \\sim C52B \\sim C51A \\sim C49 \\sim C51B \\sim C50A \\sim C50B: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C50B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C57) = Uanis(C60)
Uanis(C24A) = Uanis(C24B)
Uanis(C24B) = Uanis(C24A)
Uanis(C23A) = Uanis(C22B)
Uanis(C51A) = Uanis(C51B)
Uanis(C50A) = Uanis(C50B)
Uanis(C52B) = Uanis(C52A)
6. Others
 Sof(C68)=Sof(H68)=Sof(C66)=Sof(H66)=Sof(C67)=Sof(H67)=Sof(C65)=Sof(H65)=
 Sof(C63)=Sof(C64)=Sof(H64)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=FVAR(1)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C75)=Sof(H75)=Sof(C70)=Sof(C71)=
 Sof(H71)=Sof(C72)=Sof(H72)=Sof(C74)=Sof(H74)=Sof(C73)=Sof(H73)=FVAR(2)
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=1-FVAR(3)
 Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=FVAR(3)
 Sof(C51B)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52B)=Sof(H52A)=Sof(H52B)=
 Sof(H52C)=Sof(C50B)=Sof(H50A)=Sof(H50B)=Sof(H50C)=1-FVAR(4)
 Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C50A)=Sof(H50D)=Sof(H50E)=
 Sof(H50F)=Sof(C52A)=Sof(H52D)=Sof(H52E)=Sof(H52F)=FVAR(4)
 Fixed Sof: H59(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5)
7.a Free rotating group:
 N1(H1), N4(H4)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C31(H31), C10(H10), C8(H8), C33(H33), C5(H5), C38(H38), C36(H36),
 C68(H68), C66(H66), C67(H67), C65(H65), C64(H64), C57(H57), C58(H58), C59(H59),
  C60(H60), C75(H75), C71(H71), C72(H72), C74(H74), C73(H73)
7.c Idealised Me refined with riding coordinates:
 C50B(H50A,H50B,H50C), C69(H69A,H69B,H69C), C24B(H24D,H24E,H24F), C22B(H22D,
 H22E,H22F)
7.d Idealised Me refined as rotating group:
 C51B(H51A,H51B,H51C), C23A(H23A,H23B,H23C), C55(H55A,H55B,H55C), C48(H48A,
 H48B,H48C), C26(H26A,H26B,H26C), C43(H43A,H43B,H43C), C18(H18A,H18B,H18C),
 C46(H46A,H46B,H46C), C56(H56A,H56B,H56C), C20(H20A,H20B,H20C), C42(H42A,H42B,
 H42C), C52B(H52A,H52B,H52C), C47(H47A,H47B,H47C), C44(H44A,H44B,H44C),
 C27(H27A,H27B,H27C), C15(H15A,H15B,H15C), C28(H28A,H28B,H28C), C14(H14A,H14B,
 H14C), C54(H54A,H54B,H54C), C22A(H22A,H22B,H22C), C19(H19A,H19B,H19C),
 C16(H16A,H16B,H16C), C24A(H24A,H24B,H24C), C62(H62A,H62B,H62C), C61(H61A,H61B,
 H61C), C23B(H23D,H23E,H23F), C51A(H51D,H51E,H51F), C50A(H50D,H50E,H50F),
 C52A(H52D,H52E,H52F)
;
_shelx_res_checksum              35561
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'