Phosphaaluminirenes: Synthons for Main Group Heterocycles.
Liu, Liu Leo; Zhou, Jiliang; Cao, Levy L.; Stephan, Douglas W.; Journal of the American Chemical Society 141 (2019) 16971–16982; doi:10.1021/jacs.9b09330

data_4127968
_publ_section_title
;
 Phosphaaluminirenes: Synthons for Main Group Heterocycles.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16971
_journal_page_last               16982
_journal_paper_doi               10.1021/jacs.9b09330
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C40 H56 Al N2 P'
_chemical_formula_sum            'C40 H56 Al N2 P'
_chemical_formula_weight         622.81
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.081(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8796(8)
_cell_length_b                   19.0921(13)
_cell_length_c                   17.8224(13)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.089
_cell_measurement_theta_min      2.486
_cell_volume                     3633.0(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            65213
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.763
_diffrn_reflns_theta_min         1.579
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1488 before and 0.0787 after correction.
The Ratio of minimum to maximum transmission is 0.9199.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+1.5464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4919
_reflns_number_total             6938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09330_si_002.cif
_cod_data_source_block           3
_cod_database_code               4127968
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C26(H26), C35(H35), C6(H6), C4(H4), C24(H24), C8(H8), C38(H38)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C11(H11A,H11B), C10(H10A,H10B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,
 H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C31(H31), C33(H33), C21(H21), C19(H19), C32(H32), C20(H20)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C), C23(H23A,H23B,H23C), C37(H37A,H37B,H37C), C25(H25A,H25B,H25C), C36(H36A,
 H36B,H36C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              64471
_shelx_hkl_checksum              90549
_olex2_submission_special_instructions 'No special instructions were received'