The Partial Dehydrogenation of Aluminium Dihydrides
Hooper, Thomas; Lau, Samantha; Chen, Wenyi; Brown, Ryan; Garçon, Martí; Luong, Karen; Barrow, Nathan; Tatton, Andrew; Sackman, George A.; Richardson, Christopher; White, Andrew J. P.; Cooper, Richard Ian; Edwards, Alison; Casely, Ian; Crimmin, Mark Richard; Chemical Science  (2019) –; doi:10.1039/C9SC02750E

data_1552214
_publ_section_title
;
 The Partial Dehydrogenation of Aluminium Dihydrides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02750E
_journal_year                    2019
_chemical_formula_moiety         'C78 H118 Al2 N4 P2 Pd2 , 2(C6 H6)'
_chemical_formula_sum            'C90 H130 Al2 N4 P2 Pd2'
_chemical_formula_weight         1596.67
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-04-05 deposited with the CCDC.    2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                114.468(5)
_cell_angle_beta                 101.107(3)
_cell_angle_gamma                101.892(3)
_cell_formula_units_Z            1
_cell_length_a                   12.5660(4)
_cell_length_b                   13.8938(6)
_cell_length_c                   14.1192(7)
_cell_measurement_reflns_used    6478
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.3770
_cell_measurement_theta_min      2.8030
_cell_volume                     2085.85(19)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.789
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0114
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.789
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11999
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.343
_diffrn_reflns_theta_min         2.472
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       blocks
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.712
_exptl_crystal_size_mid          0.475
_exptl_crystal_size_min          0.409
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         8225
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+1.0591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7510
_reflns_number_total             8225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02750e3.cif
_cod_data_source_block           7
_cod_original_cell_volume        2085.84(17)
_cod_database_code               1552214
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              52887