A strained intramolecular P/Al-FLP and its reactivity toward allene
Federmann, Patrick; Bosse, Tamino; Wolff, Siad; Cula, Beatrice; Herwig, Christian; Limberg, Christian; Chemical Communications  (2022) –; doi:10.1039/D2CC05640B

data_7130960
_publ_section_title
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 A strained intramolecular P/Al-FLP and its reactivity toward allene
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC05640B
_journal_year                    2022
_chemical_formula_sum            'C25 H16 Al Cl2 O2 P'
_chemical_formula_weight         477.23
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-06-17 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                88.302(7)
_cell_angle_beta                 86.483(8)
_cell_angle_gamma                87.468(8)
_cell_formula_units_Z            4
_cell_length_a                   12.083(3)
_cell_length_b                   13.097(3)
_cell_length_c                   13.743(3)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.25
_cell_volume                     2167.8(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10812
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.425
_diffrn_reflns_theta_min         2.123
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.745687
_exptl_absorpt_correction_T_min  0.674425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       fragment
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         10812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0485P)^2^+1.5665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8696
_reflns_number_total             10812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05640b2.cif
_cod_data_source_block           mo_b22_pf309wh_0m_5
_cod_depositor_comments
;

2025-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C100 H64 Al4 Cl8 O8 P4'
_cod_original_formula_weight         1908.91
_cod_original_formula_units_Z            1
_cod_original_cell_volume        2167.9(8)
_cod_database_code               7130960
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.835
_shelx_estimated_absorpt_t_max   0.914
_shelx_res_checksum              96545
_shelx_hkl_checksum              56312