Dibenzoazepine hydrazine is a building block for <i>N</i>-alkene hybrid ligands: exploratory syntheses of complexes of Cu, Fe, and Li.
Grasruck, Alexander; Schall, Kristina; Heinemann, Frank W.; Langer, Jens; Herrera, Alberto; Frieß, Sybille; Schmid, Günter; Dorta, Romano; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8642–8656; doi:10.1039/d4dt00749b

data_7715939
_publ_section_title
;
 Dibenzoazepine hydrazine is a building block for <i>N</i>-alkene hybrid
 ligands: exploratory syntheses of complexes of Cu, Fe, and Li.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8642
_journal_page_last               8656
_journal_paper_doi               10.1039/d4dt00749b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C29 H39 Li N2 O3'
_chemical_formula_sum            'C29 H39 Li N2 O3'
_chemical_formula_weight         470.56
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2023-10-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-07 deposited with the CCDC.	2024-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.616(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8126(17)
_cell_length_b                   16.863(3)
_cell_length_c                   17.707(4)
_cell_measurement_reflns_used    9219
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      2.31
_cell_volume                     2626.1(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_collection       'Bruker APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2016)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa ImuS Duo Photon II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS high brilliance micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            84572
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.090
_diffrn_reflns_theta_min         2.305
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1133 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.9044.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuan, n-hexane'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5790
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+2.4510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4596
_reflns_number_total             5790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00749b2.cif
_cod_data_source_block           rd1905
_cod_depositor_comments
'Adding full bibliography for 7715932--7715940.cif.'
_cod_original_cell_volume        2626.2(9)
_cod_database_code               7715939
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.986
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H18A,H18B} of C18, {H19A,H19B} of C19, {H21A,H21B} of C21,
   {H20A,H20B} of C20, {H29C,H29D} of C29A, {H28C,H28D} of C28A, {H27C,H27D} of
  C27A, {H26C,H26D} of C26A, {H27A,H27B} of C27, {H29A,H29B} of C29, {H28A,
  H28B} of C28, {H26A,H26B} of C26, {H22A,H22B} of C22, {H24A,H24B} of C24,
  {H25A,H25B} of C25, {H23A,H23B} of C23
 At 1.5 times of:
  All C(H,H,H) groups, {H16A,H16B} of C16
2. Uiso/Uaniso restraints and constraints
O3 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim O3A \\sim C26A \\sim C27A
\\sim C28A \\sim C29A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
3. Others
 Sof(O3A)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27C)=Sof(H27D)=
 Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=1-FVAR(1)
 Sof(O3)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C26A(H26C,H26D), C27A(H27C,
 H27D), C28A(H28C,H28D), C29A(H29C,H29D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13)
4.c X=CH2 refined with riding coordinates:
 C16(H16A,H16B)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              3274
_olex2_submission_special_instructions 'No special instructions were received'