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_1574959
_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         'C50 H87 Al Cl Cu N5 P Si, 2(C6 H6)'
_chemical_formula_sum            'C62 H99 Al Cl Cu N5 P Si'
_chemical_formula_weight         1099.49
_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   geom
_atom_sites_solution_primary     'Intrinsic Phasing'
_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
_cell_angle_beta                 109.228(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8337(12)
_cell_length_b                   10.5705(5)
_cell_length_c                   25.3214(12)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.4751
_cell_measurement_theta_min      2.169
_cell_measurement_wavelength     0.71073
_cell_volume                     6276.2(5)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'APEX 5'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      193(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.391
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;<Phi   scan: start= 224.5; len= 214.5; end= 439.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   2.349 deg omega= 268.623 deg chi=  24.000 deg] 
measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Phi   scan: start= 156.0; len= 184.0; end= 340.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   2.349 deg omega=   2.755 deg chi= -44.500 deg] 
measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   3.8; len= 105.5; end= 109.3 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   2.349 deg phi= 144.000 deg chi= -44.500 deg] 
measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start= 324.6; len=  45.5; end= 370.1 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   1.175 deg phi= 360.000 deg chi=  68.500 deg] 
measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   3.8; len= 105.5; end= 109.3 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   2.349 deg phi=  72.000 deg chi= -44.500 deg] 
measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   0.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
;
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_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  0.1221
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            167766
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.316
_diffrn_reflns_theta_min         2.169
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_target            Mo
_diffrn_source_type              'INCOATEC I\mS 3.0'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6811
_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    1.164
_exptl_crystal_description       needle
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         15556
_refine_ls_number_restraints     1218
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0606
_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^)+(0.0692P)^2^+8.0650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10892
_reflns_number_total             15556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03846d2.cif
_cod_data_source_block           11
_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_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1574959
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.9134
_shelx_estimated_absorpt_t_min   0.867
_shelx_estimated_absorpt_t_max   0.981
_bruker_diffrn_measurement_temperature_device 'Oxford Cryostream 700'
_diffrn_measurement_bruker_total_exposure_time 6730.0
_diffrn_reflns_bruker_av_norm_i  214.764
_diffrn_reflns_bruker_number_gt  78456
_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              84693