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_7715936
_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_absolute_configuration ad
_chemical_formula_moiety         'C38 H34 Cu N4 O2'
_chemical_formula_sum            'C38 H34 Cu N4 O2'
_chemical_formula_weight         642.23
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.66630(10)
_cell_length_b                   39.1923(5)
_cell_length_c                   15.0354(2)
_cell_measurement_reflns_used    19990
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.5380
_cell_measurement_theta_min      4.4810
_cell_volume                     6285.35(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -114.00 -16.00   1.00    1.60    --  -40.61 -38.00 120.00   98
  2  \w   -104.00 -17.00   1.00    1.60    --  -40.61 -38.00-150.00   87
  3  \w   -110.00 -68.00   1.00    1.60    --  -40.61-147.00 -72.00   42
  4  \w      1.00  60.00   1.00    1.60    --   40.61 -99.00   0.00   59
  5  \w     41.00  95.00   1.00    1.60    --   40.61-125.00-180.00   54
  6  \w     56.00 178.00   1.00    6.00    --  107.07  15.00-180.00  122
  7  \w     97.00 178.00   1.00    6.00    --  107.07  30.00  60.00   81
  8  \w     53.00 123.00   1.00    6.00    --  107.07 -45.00-120.00   70
  9  \w     37.00 110.00   1.00    6.00    --  107.07 -94.00  30.00   73
 10  \w     68.00 109.00   1.00    6.00    --  107.07-125.00 -90.00   41
 11  \w     25.00 105.00   1.00    6.00    --  107.07 -94.00 -60.00   80
 12  \w     46.00 109.00   1.00    6.00    --  107.07-125.00-180.00   63
 13  \w     36.00 129.00   1.00    6.00    --  107.07 -45.00 120.00   93
 14  \w     46.00 106.00   1.00    6.00    --  107.07 -45.00   0.00   60
 15  \w    -43.00 -13.00   1.00    1.60    --  -40.86 -57.00  30.00   30
 16  \w   -114.00 -89.00   1.00    1.60    --  -40.86-147.00 -72.00   25
 17  \w    -61.00  10.00   1.00    1.60    --  -40.86  57.00 -60.00   71
 18  \w    -74.00  24.00   1.00    1.60    --  -40.86  19.00-120.00   98
 19  \w      7.00  32.00   1.00    1.60    --   42.00  86.00  55.24   25
 20  \w      6.00  31.00   1.00    1.60    --   42.00  88.00 173.80   25
 21  \w     11.00  37.00   1.00    1.60    --   46.00  84.00 -53.03   26
 22  \w     17.00  44.00   1.00    1.60    --   50.00  79.00-111.08   27
 23  \w     17.00  42.00   1.00    1.60    --   50.00  80.00 131.13   25
 24  \w     25.00  50.00   1.00    1.60    --   58.00  77.00  -3.98   25
 25  \w     27.00  61.00   1.00    1.60    --   58.00  77.00 -62.64   34
 26  \w     30.00  63.00   1.00    1.60    --   62.00  74.00 121.22   33
 27  \w     35.00  61.00   1.00    1.60    --   62.00  75.00  76.61   26
 28  \w     33.00  60.00   1.00    1.60    --   66.00  77.00 169.04   27
 29  \w     76.00 102.00   1.00    1.60    --   66.00  77.00 169.04   26
 30  \w     34.00  96.00   1.00    1.60    --   66.00  75.00  46.31   62
 31  \w     40.00  66.00   1.00    1.60    --   70.00  76.00-166.72   26
 32  \w     39.00  73.00   1.00    1.60    --   70.00  77.00  12.58   34
 33  \w    105.00 145.00   1.00    6.00    --   74.00  77.00-133.08   40
 34  \w     41.00  72.00   1.00    6.00    --   74.00  77.00-133.08   31
 35  \w     45.00  81.00   1.00    6.00    --   78.00  77.00 -40.14   36
 36  \w    133.00 175.00   1.00    6.00    --  107.07  77.00   0.00   42
 37  \w     74.00 146.00   1.00    6.00    --  107.07  77.00 -30.00   72
 38  \w     76.00 116.00   1.00    6.00    --  107.07  77.00   0.00   40
 39  \w     74.00 101.00   1.00    6.00    --  107.07  77.00  90.00   27
 40  \w    145.00 171.00   1.00    6.00    --  107.07  61.00  90.00   26
 41  \w    135.00 160.00   1.00    6.00    --  107.07  77.00 120.00   25
 42  \w     80.00 107.00   1.00    6.00    --  107.07  61.00  90.00   27
 43  \w     74.00 100.00   1.00    6.00    --  107.07  77.00  30.00   26
 44  \w    153.00 178.00   1.00    6.00    --  107.07  77.00  30.00   25
 45  \w     75.00 101.00   1.00    6.00    --  107.07  77.00 120.00   26
 46  \w     79.00 104.00   1.00    6.00    --  107.07  61.00-120.00   25
 47  \w    113.00 162.00   1.00    6.00    --  107.07  77.00-150.00   49
 48  \w     82.00 108.00   1.00    6.00    --  107.07  61.00-180.00   26
 49  \w     74.00  99.00   1.00    6.00    --  107.07  77.00-150.00   25
 50  \w     78.00 106.00   1.00    6.00    --  107.07  77.00-180.00   28
 51  \w     74.00  99.00   1.00    6.00    --  107.07  77.00  60.00   25
 52  \w     74.00 152.00   1.00    6.00    --  107.07  77.00 -90.00   78
 53  \w    107.00 146.00   1.00    6.00    --  107.07  77.00 -60.00   39
 54  \w     74.00 103.00   1.00    6.00    --  107.07  77.00 -60.00   29
 55  \w    147.00 176.00   1.00    6.00    --  107.07  77.00 150.00   29
 56  \w    135.00 161.00   1.00    6.00    --  107.07  61.00-180.00   26
 57  \w    153.00 178.00   1.00    6.00    --  107.07  77.00-120.00   25
 58  \w     76.00 141.00   1.00    6.00    --  107.07  77.00-120.00   65
 59  \w     74.00  99.00   1.00    6.00    --  107.07  77.00 150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0901786000
_diffrn_orient_matrix_UB_12      0.0261609000
_diffrn_orient_matrix_UB_13      0.0419023000
_diffrn_orient_matrix_UB_21      0.0882053000
_diffrn_orient_matrix_UB_22      -0.0291914000
_diffrn_orient_matrix_UB_23      0.0282451000
_diffrn_orient_matrix_UB_31      0.0703215000
_diffrn_orient_matrix_UB_32      0.0030898000
_diffrn_orient_matrix_UB_33      -0.0891064000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23807
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.634
_diffrn_reflns_theta_min         4.513
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       plate
_exptl_crystal_F_000             2680
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, n-hexane'
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 1491 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3152
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0281P)^2^+10.4509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                3151
_reflns_number_total             3152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00749b2.cif
_cod_data_source_block           rodo180915a
_cod_depositor_comments
'Adding full bibliography for 7715932--7715940.cif.'
_cod_database_code               7715936
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N P Cu O '
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.714
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              12954
_olex2_date_sample_data_collection 2021-07-01
_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 1.572
_oxdiff_exptl_absorpt_empirical_full_min 0.751