Aluminacyclopropene-phosphine complex: a carbene-exchange reagent.
Xu, Huihui; León Baeza, José Miguel; Baceiredo, Antoine; Rojas Guerrero, René Segundo; Saffon-Merceron, Nathalie; Branchadell, Vicenç; Kato, Tsuyoshi; Chemical science 16 (2025) 14225–14230; doi:10.1039/d5sc03846d

data_1574962
_publ_section_title
;
 Aluminacyclopropene-phosphine complex: a carbene-exchange reagent.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              14225
_journal_page_last               14230
_journal_paper_doi               10.1039/d5sc03846d
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C58 H93 Al N5 P Si, C4 H8 O'
_chemical_formula_sum            'C62 H101 Al N5 O P Si'
_chemical_formula_weight         1018.51
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method
;FinalCif 2024.9-0 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-04-04 deposited with the CCDC.	2025-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.561(2)
_cell_angle_beta                 92.765(2)
_cell_angle_gamma                98.516(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0584(9)
_cell_length_b                   13.9968(9)
_cell_length_c                   18.0629(13)
_cell_measurement_reflns_used    9442
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.142
_cell_measurement_theta_min      2.3985
_cell_measurement_wavelength     0.71073
_cell_volume                     3011.1(4)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'APEX 2'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_computing_molecular_graphics    'Bruker SHELXTL, XP (G. Sheldrick)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      193(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;<Phi   scan: start=   0.1; len= 359.8; end= 359.9 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  10.236 deg omega= 285.627 deg chi=  23.000 deg] 
measure for 20.0 seconds; frame angle 0.70 degrees, wavelength=0.71073>
<Phi   scan: start=   0.1; len= 359.8; end= 359.9 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  10.236 deg omega=  14.885 deg chi= -57.063 deg] 
measure for 20.0 seconds; frame angle 0.70 degrees, wavelength=0.71073>
<Phi   scan: start=   0.1; len= 359.8; end= 359.9 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  10.236 deg omega=   7.187 deg chi= -23.000 deg] 
measure for 20.0 seconds; frame angle 0.70 degrees, wavelength=0.71073>
<Omega scan: start=  15.9; len= 114.1; end= 130.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  10.236 deg phi= 240.000 deg chi= -54.740 deg] 
measure for 20.0 seconds; frame angle 0.70 degrees, wavelength=0.71073>
<Omega scan: start= 308.6; len=  75.6; end= 384.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  10.236 deg phi=  60.000 deg chi=  64.875 deg] 
measure for 20.0 seconds; frame angle 0.70 degrees, wavelength=0.71073>
<Omega scan: start=  15.9; len= 114.1; end= 130.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  10.236 deg phi= 180.000 deg chi= -54.740 deg] 
measure for 20.0 seconds; frame angle 0.70 degrees, wavelength=0.71073>
<Omega scan: start=  15.9; len= 114.1; end= 130.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  10.236 deg phi=  60.001 deg chi= -54.740 deg] 
measure for 20.0 seconds; frame angle 0.70 degrees, wavelength=0.71073>
<Omega scan: start= 308.6; len=  75.6; end= 384.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  10.236 deg phi= 180.000 deg chi=  64.875 deg] 
measure for 20.0 seconds; frame angle 0.70 degrees, wavelength=0.71073>
;
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker QUAZAR'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            91728
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.443
_diffrn_reflns_theta_min         2.001
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.6
_diffrn_source_target            Mo
_diffrn_source_type              'INCOATEC I\mS'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         12350
_refine_ls_number_restraints     464
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0661
_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^)+(0.1005P)^2^+1.2333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.2024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7515
_reflns_number_total             12350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03846d2.cif
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1574958--1574964.cif.
;
_cod_database_code               1574962
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.9261
_shelx_estimated_absorpt_t_min   0.985
_shelx_estimated_absorpt_t_max   0.990
_bruker_diffrn_measurement_temperature_device 'Oxford Cryostream 700'
_diffrn_measurement_bruker_total_exposure_time 44941.028514
_diffrn_reflns_bruker_av_norm_i  120.725
_diffrn_reflns_bruker_number_gt  37422
_computing_bruker_data_scaling
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_geom_details
; All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_shelx_res_checksum              51434