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_7715933
_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         'C26 H16 N2 O'
_chemical_formula_sum            'C26 H16 N2 O'
_chemical_formula_weight         372.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-05
_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                92.468(2)
_cell_angle_beta                 92.260(2)
_cell_angle_gamma                90.330(2)
_cell_formula_units_Z            8
_cell_length_a                   10.4448(3)
_cell_length_b                   16.6554(5)
_cell_length_c                   21.5436(6)
_cell_measurement_reflns_used    20415
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      29.2340
_cell_measurement_theta_min      3.1170
_cell_volume                     3741.28(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    241.00 360.00   1.00   12.50  12.69  12.69  60.00    --   119
  2  \f    240.00 297.00   1.00   12.50  12.69  12.69  40.00    --    57
  3  \f    304.00 356.00   1.00   12.50  12.69  12.69  40.00    --    52
  4  \f    120.00 240.00   1.00   12.50  12.69  12.69  60.00    --   120
  5  \f      0.00 120.00   1.00   12.50  12.69  12.69  60.00    --   120
  6  \f      0.00 120.00   1.00   12.50  12.69  12.69 -20.00    --   120
  7  \f    240.00 283.00   1.00   12.50  12.69  12.69 -20.00    --    43
  8  \f    120.00 240.00   1.00   12.50  12.69  12.69 -20.00    --   120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0383485000
_diffrn_orient_matrix_UB_12      0.0308805000
_diffrn_orient_matrix_UB_13      0.0150494000
_diffrn_orient_matrix_UB_21      0.0120250000
_diffrn_orient_matrix_UB_22      -0.0247942000
_diffrn_orient_matrix_UB_23      0.0255126000
_diffrn_orient_matrix_UB_31      0.0548081000
_diffrn_orient_matrix_UB_32      -0.0157716000
_diffrn_orient_matrix_UB_33      -0.0145029000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21081
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.645
_diffrn_reflns_theta_min         2.135
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.356
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         21081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0719P)^2^+2.0075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15072
_reflns_number_total             21081
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9486\% 
around [1.00 -0.00 -0.00] (reciprocal) or [1.00 0.00 0.02] (direct)
;
_cod_data_source_file            d4dt00749b2.cif
_cod_data_source_block           rodo180531b_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7715932--7715940.cif.'
_cod_database_code               7715933
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C26 H16 N2 O'
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8795(8)
 0.1205(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C66(H66),
 C67(H67), C68(H68), C69(H69), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76),
  C77(H77), C84(H84), C85(H85), C86(H86), C88(H88), C89(H89), C90(H90),
 C92(H92), C93(H93), C94(H94), C95(H95), C97(H97), C98(H98), C100(H100),
 C101(H101), C102(H102), C103(H103), C32(H32), C33(H33), C34(H34), C36(H36),
 C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46),
  C48(H48), C49(H49), C50(H50), C51(H51)
;
_shelx_res_checksum              90728
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.604
_oxdiff_exptl_absorpt_empirical_full_min 0.251
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2