Synthesis and Characterization of Primary Aluminum Parent Amides and Phosphides
Melton, Christopher E.; Dube, Jonathan W.; Ragogna, Paul J.; Fettinger, James C.; Power, Philip P.; Organometallics 33 (2014) 329–; doi:10.1021/om4010675

data_4082536
_publ_section_title
;
 Synthesis and Characterization of Primary Aluminum Parent Amides and
 Phosphides
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              329
_journal_paper_doi               10.1021/om4010675
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C72 H75 Al3 P5'
_chemical_formula_sum            'C72 H75 Al3 P5'
_chemical_formula_weight         1176.1
_chemical_name_systematic
;
 ?
;
_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-2012
_cell_angle_alpha                90
_cell_angle_beta                 93.253(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.728(5)
_cell_length_b                   21.383(7)
_cell_length_c                   26.915(8)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.47
_cell_volume                     7888(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      150(2)
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            100254
_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         25.728
_diffrn_reflns_theta_min         1.790
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.990
_exptl_crystal_description       block
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.208
_platon_squeeze_details
;
;
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         15003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1242P)^2^+0.4160P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9628
_reflns_number_total             15003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4010675_si_002.cif
_cod_data_source_block           4
_cod_original_cell_volume        7888(4)
_cod_database_code               4082536
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.947
_shelxl_version_number           2012-9
_shelx_res_checksum              7881