Attempted Reduction of a Carbazolyl-Diiodoalane
Hinz, Alexander; Müller, Maximilian P.; Chemical Communications  (2021) –; doi:10.1039/D1CC05557G

data_7129158
_publ_section_title
;
 Attempted Reduction of a Carbazolyl-Diiodoalane
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05557G
_journal_year                    2021
_chemical_formula_sum            'C48 H64 Al N'
_chemical_formula_weight         681.98
_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
;
2021-09-07 deposited with the CCDC.	2021-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                94.863(9)
_cell_angle_beta                 95.352(7)
_cell_angle_gamma                94.833(8)
_cell_formula_units_Z            2
_cell_length_a                   12.0243(9)
_cell_length_b                   12.3868(15)
_cell_length_c                   14.3602(13)
_cell_measurement_reflns_used    13711
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      63.85
_cell_measurement_theta_min      2.70
_cell_volume                     2112.7(4)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.161.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.0.0 (STOE, 2020)
X-Area LANA 1.78.0.0 (STOE, 2020)
;
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.89, Darmstadt 2020
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 EIGER4M
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      ' 1465 frames, detector distance = 80 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24511
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         57.486
_diffrn_reflns_theta_min         2.701
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.1498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.000
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.030
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1405
_refine_ls_number_reflns         8607
_refine_ls_number_restraints     2067
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5486
_reflns_number_total             8607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05557g2.cif
_cod_data_source_block           RAl
_cod_database_code               7129158
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              38849
_shelx_hkl_checksum              87078