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_7717174
_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            'C62 H86 Al N6'
_chemical_formula_weight         942.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0207(7)
_cell_length_b                   20.0834(8)
_cell_length_c                   15.5972(7)
_cell_measurement_reflns_used    10447
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0380
_cell_measurement_theta_min      2.5900
_cell_volume                     5331.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.43.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.43.93a (Rigaku OD, 2020)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1010
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64257
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.028
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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            black
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         8351
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0709P)^2^+1.1939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5637
_reflns_number_total             8351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02597k2.cif
_cod_data_source_block           albiancynchncy
_cod_depositor_comments
'Adding full bibliography for 7717170--7717178.cif.'
_cod_database_code               7717174
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.982
_oxdiff_exptl_absorpt_empirical_full_min 0.780
_oxdiff_exptl_absorpt_empirical_full_max 1.641
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              5015
_shelx_hkl_checksum              99086