# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AlPd15B7
_database_code_depnum_ccdc_archive 'CCDC 1440657'
_audit_update_record             
;
2015-12-04 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

_audit_creation_date             ?
_audit_creation_method           'WinCSD program'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_sum            'Al B7 Pd15'
_chemical_formula_weight         1698.65
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Al Al 16.00 .065 .052 International_Tables_Vol_IV_Table_2.3.1
Pd Pd 240.00 -.977 1.012 International_Tables_Vol_IV_Table_2.3.1
B B 112.00 .002 .001 International_Tables_Vol_IV_Table_2.3.1

#------------------ UNIT CELL INFORMATION -----------------------------------#

loop_
_symmetry_equiv_pos_as_xyz
' x, y, z'
' z, x, y'
' y, z, x'
' 1/2+x, y, 1/2-z'
' 1/2+z, x, 1/2-y'
' 1/2+y, z, 1/2-x'
' 1/2-x, 1/2+y, z'
' 1/2-z, 1/2+x, y'
' 1/2-y, 1/2+z, x'
'-x, 1/2+y, 1/2-z'
'-z, 1/2+x, 1/2-y'
'-y, 1/2+z, 1/2-x'
' 1/4+y, 1/4+x, 1/4+z'
' 1/4+x, 1/4+z, 1/4+y'
' 1/4+z, 1/4+y, 1/4+x'
' 1/4+y, 3/4+x, 3/4-z'
' 1/4+x, 3/4+z, 3/4-y'
' 1/4+z, 3/4+y, 3/4-x'
' 3/4+y, 3/4-x, 1/4+z'
' 3/4+x, 3/4-z, 1/4+y'
' 3/4+z, 3/4-y, 1/4+x'
' 3/4+y, 1/4-x, 3/4-z'
' 3/4+x, 1/4-z, 3/4-y'
' 3/4+z, 1/4-y, 3/4-x'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
' 1/2-x, -y, 1/2+z'
' 1/2-z, -x, 1/2+y'
' 1/2-y, -z, 1/2+x'
' 1/2+x, 1/2-y, -z'
' 1/2+z, 1/2-x, -y'
' 1/2+y, 1/2-z, -x'
' x, 1/2-y, 1/2+z'
' z, 1/2-x, 1/2+y'
' y, 1/2-z, 1/2+x'
' 3/4-y, 3/4-x, 3/4-z'
' 3/4-x, 3/4-z, 3/4-y'
' 3/4-z, 3/4-y, 3/4-x'
' 3/4-y, 1/4-x, 1/4+z'
' 3/4-x, 1/4-z, 1/4+y'
' 3/4-z, 1/4-y, 1/4+x'
' 1/4-y, 1/4+x, 3/4-z'
' 1/4-x, 1/4+z, 3/4-y'
' 1/4-z, 1/4+y, 3/4-x'
' 1/4-y, 3/4+x, 1/4+z'
' 1/4-x, 3/4+z, 1/4+y'
' 1/4-z, 3/4+y, 1/4+x'
' 1/2+x, 1/2+y, 1/2+z'
' 1/2+z, 1/2+x, 1/2+y'
' 1/2+y, 1/2+z, 1/2+x'
' x, 1/2+y, -z'
' z, 1/2+x, -y'
' y, 1/2+z, -x'
'-x, y, 1/2+z'
'-z, x, 1/2+y'
'-y, z, 1/2+x'
' 1/2-x, y, -z'
' 1/2-z, x, -y'
' 1/2-y, z, -x'
' 3/4+y, 3/4+x, 3/4+z'
' 3/4+x, 3/4+z, 3/4+y'
' 3/4+z, 3/4+y, 3/4+x'
' 3/4+y, 1/4+x, 1/4-z'
' 3/4+x, 1/4+z, 1/4-y'
' 3/4+z, 1/4+y, 1/4-x'
' 1/4+y, 1/4-x, 3/4+z'
' 1/4+x, 1/4-z, 3/4+y'
' 1/4+z, 1/4-y, 3/4+x'
' 1/4+y, 3/4-x, 1/4-z'
' 1/4+x, 3/4-z, 1/4-y'
' 1/4+z, 3/4-y, 1/4-x'
' 1/2-x, 1/2-y, 1/2-z'
' 1/2-z, 1/2-x, 1/2-y'
' 1/2-y, 1/2-z, 1/2-x'
'-x, 1/2-y, z'
'-z, 1/2-x, y'
'-y, 1/2-z, x'
' x, -y, 1/2-z'
' z, -x, 1/2-y'
' y, -z, 1/2-x'
' 1/2+x, -y, z'
' 1/2+z, -x, y'
' 1/2+y, -z, x'
' 1/4-y, 1/4-x, 1/4-z'
' 1/4-x, 1/4-z, 1/4-y'
' 1/4-z, 1/4-y, 1/4-x'
' 1/4-y, 3/4-x, 3/4+z'
' 1/4-x, 3/4-z, 3/4+y'
' 1/4-z, 3/4-y, 3/4+x'
' 3/4-y, 3/4+x, 1/4-z'
' 3/4-x, 3/4+z, 1/4-y'
' 3/4-z, 3/4+y, 1/4-x'
' 3/4-y, 1/4+x, 3/4+z'
' 3/4-x, 1/4+z, 3/4+y'
' 3/4-z, 1/4+y, 3/4+x'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I a -3 d'

_cell_length_a                   16.4466(3)
_cell_length_b                   16.4466(3)
_cell_length_c                   16.4466(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4448.7(3)
_cell_formula_units_Z            16


#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_description       Block
_exptl_crystal_colour            Grey
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_chemical_formula_analytical     ?
_exptl_crystal_size_rad          ?
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'Blessing, R. H. (1995) Acta Cryst. A51, 33-38'
_exptl_absorpt_correction_type   Multi-scan
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    10.14
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             11808
_exptl_absorpt_coefficient_mu    23.07

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_cell_measurement_temperature    295.0
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.8
_cell_measurement_theta_max      33.4

_diffrn_ambient_temperature      295.0
_diffrn_source_power             1.8
_diffrn_source_voltage           50.0
_diffrn_source_current           36.0
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
AFC7: Eulerian 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from φ-scans'
_diffrn_reflns_theta_full        33.7
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993

_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_measurement_details      
;
scan:
	Number of images: 600
	           Slice: -90.0000 - 270.0000
	     Image width: 0.6000
	        Exp time: 50.0000
	   Rotation axis: Phi
	           Omega: -30.0000
	             Chi: -40.0000
	             Phi: 0.0000
	             XTD: 48.9400
	          2theta: -28.0000

;
_diffrn_orient_matrix_UB_11      0.004964
_diffrn_orient_matrix_UB_12      0.030599
_diffrn_orient_matrix_UB_13      -0.052284
_diffrn_orient_matrix_UB_21      0.031017
_diffrn_orient_matrix_UB_22      -0.046346
_diffrn_orient_matrix_UB_23      -0.024179
_diffrn_orient_matrix_UB_31      -0.052037
_diffrn_orient_matrix_UB_32      -0.024706
_diffrn_orient_matrix_UB_33      -0.019399
_diffrn_orient_matrix_type       d*Trek

_diffrn_radiation_wavelength     0.710730
_diffrn_radiation_type           MoK\a

_diffrn_reflns_number            18108
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.053

_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.8
_diffrn_reflns_theta_max         33.7

_reflns_number_total             730
_reflns_number_gt                718
_reflns_threshold_expression     'Fₒ > 4σ(Fₒ)'

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       ?
_computing_cell_refinement       WinCSD
_computing_data_reduction        WinCSD
_computing_structure_solution    WinCSD
_computing_structure_refinement  WinCSD
_computing_molecular_graphics    ?
_computing_publication_material  'WinCSD (Akselrud et al, 1993)'

#### PLEASE do not forget the following reference :
#Akselrud, L.G., Zavalii, P.Y., Grin, Yu.N.,
#Pecharsky, V.K., Baumgartner, B., Wolfel, E.
#(1993) Materials Science Forum, v.133-136, 335-340

#------------------ REFINEMENT INFORMATION ----------------------------------#

_refine_special_details          
; ?
;

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle

_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     0.0468Log(Fₒ)⁴
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     Sheldrick
_refine_ls_extinction_coef       0.00026(2)
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         730
_refine_ls_number_parameters     32
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          ?
_refine_ls_R_factor_gt           0.058
_refine_ls_wR_factor_all         ?
_refine_ls_wR_factor_ref         0.064
_refine_ls_goodness_of_fit_ref   1.02
_refine_diff_density_max         ?
_refine_diff_density_min         ?

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_B_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
Al Al 0 0 0 Bani 1.08(8) 16 1.0
Pd1 Pd 0.125 0.24484(6) 0.00516(6) Bani 1.23(2) 48 1.0
Pd2 Pd 0.00090(6) 0.14693(6) 0.07718(6) Bani 0.99(2) 96 1.0
Pd3 Pd 0.10758(6) 0.24514(6) 0.33770(6) Bani 1.13(2) 96 1.0
B1 B 0.125 0.125 0.125 Biso 1.4(5) 16 1.0
B2 B 0.263(2) 0 0.25 Biso 1.5(3) 48 1.0
B3 B 0.125 0.619(1) 0.631(1) Biso 1.4(3) 48 1.0


loop_
_atom_site_aniso_label
_atom_site_aniso_B_11
_atom_site_aniso_B_22
_atom_site_aniso_B_33
_atom_site_aniso_B_12
_atom_site_aniso_B_13
_atom_site_aniso_B_23
Al 1.1(1) 1.1(1) 1.1(1) -0.06(15) -0.06(15) -0.06(15)
Pd1 1.09(5) 1.31(4) 1.31(4) -0.11(3) -0.11(3) 0.12(4)
Pd2 0.93(4) 1.09(4) 0.96(4) 0.01(2) -0.02(2) 0
Pd3 1.26(4) 1.08(4) 1.06(4) -0.09(3) -0.02(3) -0.14(3)

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al Pd2 2.729(1) . yes
Al Pd3 2.752(1) 61_444 yes
Pd1 B2 2.079(3) 2_555 yes
Pd1 Pd3 2.774(2) 34_554 yes
Pd1 Pd2 2.782(1) 3_555 yes
Pd1 B1 2.787(1) . yes
Pd1 B3 2.844(11) 5_455 yes
Pd1 Pd2 2.857(1) . yes
Pd1 Pd2 2.976(1) 68_554 yes
Pd1 Pd3 3.012(1) 3_555 yes
Pd1 B3 3.159(15) 47_544 yes
Pd1 Pd3 3.214(1) 60_555 yes
Pd2 B3 2.145(14) 9_545 yes
Pd2 B1 2.217(1) . yes
Pd2 B2 2.254(15) 66_455 yes
Pd2 Pd3 2.713(1) 85_555 yes
Pd2 Pd2 2.850(1) 85_555 yes
Pd2 Pd2 2.885(1) 64_455 yes
Pd2 Pd3 2.885(1) 62_444 yes
Pd2 Pd2 2.942(1) 2_555 yes
Pd2 Pd3 2.955(1) 87_555 yes
Pd2 Pd2 3.391(1) 76_555 yes
Pd3 B3 2.152(15) 52_546 yes
Pd3 B2 2.154(13) 3_555 yes
Pd3 B3 2.281(6) 32_456 yes
Pd3 Pd3 2.789(1) 22_455 yes
Pd3 Pd3 2.921(1) 74_555 yes
Pd3 B2 3.03(2) 24_455 yes
Pd3 Pd3 3.542(1) 76_555 yes
Pd3 Pd3 3.706(1) 47_545 yes
_chemical_name_systematic        AlPd15B7
_exptl_crystal_preparation       Superconductor
