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_4127975
_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_sum            'C56.5 H72 Al N4 P'
_chemical_formula_weight         865.13
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.962(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.6729(16)
_cell_length_b                   11.0531(5)
_cell_length_c                   33.7785(16)
_cell_measurement_reflns_used    7667
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.37
_cell_volume                     10026.6(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep 3'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1185
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            85088
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.711
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         0.758
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       block
_exptl_crystal_F_000             3736
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         17055
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.0756
_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^)+(0.0549P)^2^+12.1415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10009
_reflns_number_total             17055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09330_si_002.cif
_cod_data_source_block           10
_cod_original_formula_sum        'C56.50 H72 Al N4 P'
_cod_database_code               4127975
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              98159
_shelx_hkl_checksum              89517