Reaction of an N/Al FLP-based aluminum hydride toward alkynes: deprotonated alumination versus hydroalumination with regioselective cis-addition character.
Chen, Yilin; Jiang, Wenjun; Li, Bin; Fu, Gang; Chen, Shimin; Zhu, Hongping; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9152–9160; doi:10.1039/c9dt00903e

data_7700016
_publ_section_title
;
 Reaction of an N/Al FLP-based aluminum hydride toward alkynes:
 deprotonated alumination versus hydroalumination with regioselective
 cis-addition character.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9152
_journal_page_last               9160
_journal_paper_doi               10.1039/c9dt00903e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C41 H45 Al N P'
_chemical_formula_weight         609.73
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-02-28 deposited with the CCDC.    2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.469(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9919(3)
_cell_length_b                   14.7539(4)
_cell_length_c                   18.7760(4)
_cell_measurement_reflns_used    4281
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.1280
_cell_measurement_theta_min      3.8120
_cell_volume                     3872.43(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12606
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        62.117
_diffrn_reflns_theta_max         62.117
_diffrn_reflns_theta_min         3.812
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  0.8202
_exptl_absorpt_correction_T_min  0.7472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr.
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         6022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0696
_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^)+(0.1482P)^2^+1.4850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5170
_reflns_number_total             6022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00903e2.cif
_cod_data_source_block           cyl-170712
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7700016--7700019.cif.
;
_cod_database_code               7700016
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.747
_shelx_estimated_absorpt_t_max   0.820
_shelx_res_checksum              42688