Hydro-coupling of isocyanates promoted by 1,2-bis(arylimino)acenaphthene aluminum hydrides.
Koptseva, Tatyana S.; Skatova, Alexandra A.; Moskalev, Mikhail V.; Rumyantcev, Roman V.; Fedushkin, Igor L.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17308–17312; doi:10.1039/d4dt02597k

data_7717171
_publ_section_title
;
 Hydro-coupling of isocyanates promoted by 1,2-bis(arylimino)acenaphthene
 aluminum hydrides.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17308
_journal_page_last               17312
_journal_paper_doi               10.1039/d4dt02597k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C116 H102 Al N6 O6.5'
_chemical_formula_weight         1711.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-06-20 deposited with the CCDC.	2024-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.597(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9292(10)
_cell_length_b                   35.073(3)
_cell_length_c                   18.3381(13)
_cell_measurement_reflns_used    4712
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.0480
_cell_measurement_theta_min      1.9690
_cell_volume                     8941.2(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_molecular_graphics
'Diamond. Ver. 3.2k. (Putz & Brandernburg, 2014)'
_computing_publication_material
'Diamond. Ver. 3.2k. (Putz & Brandernburg, 2014)'
_computing_structure_refinement  SHELXL-2019/3
_computing_structure_solution    SHELXT-2014/5
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0704
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1383
_diffrn_reflns_av_unetI/netI     0.2090
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48777
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.875
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
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            brown
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       stick
_exptl_crystal_F_000             3620
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1215
_refine_ls_number_reflns         15800
_refine_ls_number_restraints     321
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1988
_refine_ls_R_factor_gt           0.0812
_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^)+(0.0396P)^2^+6.6562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7481
_reflns_number_total             15800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02597k2.cif
_cod_data_source_block           alarbianocnphocnph
_cod_depositor_comments
'Adding full bibliography for 7717170--7717178.cif.'
_cod_original_cell_volume        8941.1(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C116 H102 Al N6 O6.50'
_cod_database_code               7717171
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.951
_shelx_estimated_absorpt_t_max   0.994
_oxdiff_exptl_absorpt_empirical_full_min 0.917
_oxdiff_exptl_absorpt_empirical_full_max 1.135
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              2689
_shelx_hkl_checksum              19628