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_1552212
_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 H116 D2 Al2 N4 P2 Pd2'
_chemical_formula_sum            'C78 H116 Al2 D2 N4 P2 Pd2'
_chemical_formula_weight         1442.54
_chemical_melting_point          ?
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2019-06-05 deposited with the CCDC.    2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                95.322(3)
_cell_angle_beta                 95.111(3)
_cell_angle_gamma                112.036(4)
_cell_formula_units_Z            2
_cell_length_a                   12.6182(5)
_cell_length_b                   13.8635(5)
_cell_length_c                   22.8654(10)
_cell_measurement_radiation      X-ray
_cell_measurement_reflns_used    7553
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      28.2660
_cell_measurement_theta_min      2.6320
_cell_measurement_wavelength     0.71073
_cell_volume                     3658.3(3)
_computing_cell_refinement       'CrysAlisPro (Agilent, 2011)'
_computing_data_collection       'MAATEL/ANSTO control program'
_computing_data_reduction
'argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Refinement of X-ray structure'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.819
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measurement_details
;
'35 images, exposure time 5000 seconds, 12 images, exposure time 8000 seconds'
;
_diffrn_measurement_device       'Laue image-plate diffractometer'
_diffrn_measurement_device_type  KOALA
_diffrn_measurement_method       Laue
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_reflns_av_R_equivalents  0.3319
_diffrn_reflns_av_unetI/netI     0.4093
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60469
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_theta_full        56.34
_diffrn_reflns_theta_max         56.45
_diffrn_reflns_theta_min         2.101
_diffrn_source                   'nuclear reactor'
_diffrn_source_details           'thermal neutrons, supermirror guides'
_diffrn_source_type
'OPAL reactor, ANSTO, Lucas Heights, Australia'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shard'
_exptl_crystal_F_000             328.79
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.74
_refine_diff_density_min         -1.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2306
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1275
_refine_ls_number_reflns         2736
_refine_ls_number_restraints     1146
_refine_ls_R_factor_all          0.2298
_refine_ls_R_factor_gt           0.1143
_refine_ls_shift/su_max          0.0008277
_refine_ls_shift/su_mean         0.0000424
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method = Chebychev polynomial, (Carruthers & Watkin, 1979) 
 W = 1.0/[A[0]*T[0]'(X)+A[1]*T[1]'(X) ... +A[NP-1]*T[NP-1]'(X)] 
 3.23 2.87 0.591 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4986
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1218
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3280
_reflns_number_total             6009
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.57
_oxford_diffrn_Wilson_scale      152.77
_oxford_refine_ls_r_factor_ref   0.0903
_oxford_refine_ls_scale          0.1124(7)
_oxford_reflns_number_all        6009
_oxford_structure_analysis_title mrc1961
_cod_data_source_file            c9sc02750e3.cif
_cod_data_source_block           7c-d2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C78 H116 D2 Al2 N4 P2 Pd2'
_cod_database_code               1552212
_oxford_refine_reflns_threshold_expression_ref I>3.0\s(I)