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_7715937
_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         'C54 H32 Cu2 F6 N4 O8 S2, 2(C H2 Cl2)'
_chemical_formula_sum            'C56 H36 Cl4 Cu2 F6 N4 O8 S2'
_chemical_formula_weight         1339.89
_chemical_properties_physical    Air-sensitive,Moisture-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   mixed
_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                 96.3972(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9485(3)
_cell_length_b                   17.6987(3)
_cell_length_c                   17.5363(3)
_cell_measurement_reflns_used    21079
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.3520
_cell_measurement_theta_min      2.5620
_cell_volume                     5227.55(16)
_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(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.861
_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     16.00 114.00   1.00   17.50  12.17  12.17 -20.00    --    98
  2  \f    261.00 345.00   1.00   17.50  12.17  12.17  20.00    --    84
  3  \f      0.00  53.00   1.00   17.50  40.00  12.17   0.00    --    53
  4  \f    120.00 240.00   1.00   17.50  40.00  12.17   0.00    --   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      0.0367564000
_diffrn_orient_matrix_UB_12      0.0192662000
_diffrn_orient_matrix_UB_13      0.0073770000
_diffrn_orient_matrix_UB_21      0.0006481000
_diffrn_orient_matrix_UB_22      -0.0079857000
_diffrn_orient_matrix_UB_23      0.0397068000
_diffrn_orient_matrix_UB_31      0.0205386000
_diffrn_orient_matrix_UB_32      -0.0342201000
_diffrn_orient_matrix_UB_33      -0.0051060000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49209
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.841
_diffrn_reflns_theta_min         2.337
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.483
_exptl_crystal_size_mid          0.307
_exptl_crystal_size_min          0.186
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         12941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0298P)^2^+4.7100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10816
_reflns_number_total             12941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00749b2.cif
_cod_data_source_block           rodo180531a
_cod_depositor_comments
'Adding full bibliography for 7715932--7715940.cif.'
_cod_original_cell_volume        5227.53(16)
_cod_database_code               7715937
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N Cu O S F'
_chemical_oxdiff_usercomment     'orange block'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C56(H56A,H56B)
2.b 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), C22(H22), C23(H23), C24(H24), C25(H25), C32(H32), C33(H33),
  C34(H34), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42),
 C43(H43), C48(H48), C49(H49), C50(H50), C51(H51)
;
_shelx_res_checksum              21789
_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 1.314
_oxdiff_exptl_absorpt_empirical_full_min 0.713