# 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_Nb7Fe3B8
_database_code_depnum_ccdc_archive 'CCDC 1470521'
_audit_update_record             
;
2016-03-28 deposited with the CCDC.
2016-05-16 downloaded from the CCDC.
;

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

_audit_creation_date             ?
_audit_creation_method           'WinCSD program'

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

_chemical_formula_sum            'B8 Fe3 Nb7'
_chemical_formula_weight         904.39
_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
Nb Nb 7.00 -2.044 .625 International_Tables_Vol_IV_Table_2.3.1
Fe Fe 3.00 .348 .850 International_Tables_Vol_IV_Table_2.3.1
B B 8.00 .002 .001 International_Tables_Vol_IV_Table_2.3.1

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

loop_
_symmetry_equiv_pos_as_xyz
' x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
' y, -x+y, z'
' x-y, x, z'
'-y, -x, z'
'-x+y, y, z'
' x, x-y, z'
' y, x, z'
' x-y, -y, z'
'-x, -x+y, z'
'-x, -y, -z'
' y, -x+y, -z'
' x-y, x, -z'
' x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
' y, x, -z'
' x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z'
'-x+y, y, -z'
' x, x-y, -z'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 6/m m m'

_cell_length_a                   8.3346(2)
_cell_length_b                   8.3346(2)
_cell_length_c                   3.2941(1)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     198.17(2)
_cell_formula_units_Z            1


#------------------ 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  0.767
_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    7.5776
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             405
_exptl_absorpt_coefficient_mu    14.953

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

_cell_measurement_temperature    295.0
_cell_measurement_reflns_used    4160
_cell_measurement_theta_min      4.8
_cell_measurement_theta_max      65.9

_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       
;
R-axis RAPID
;
_diffrn_measurement_device_details 
;
Crystal Goniometer
;
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measurement_method       'profile data from φ-scans'
_diffrn_reflns_theta_full        65.9
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measured_fraction_theta_full 1.0

_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_measurement_details      
;
scan:
	Number of images: 75
	           Slice: 80.0000 - 192.5000
	     Image width: 1.5000
	        Exp time: 1200.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 48.0000
	             Phi: 240.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 75
	           Slice: 80.0000 - 192.5000
	     Image width: 1.5000
	        Exp time: 1200.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 48.0000
	             Phi: 60.0000
	             XTD: 127.4000
	          2theta: 0.0000

;
_diffrn_orient_matrix_UB_11      -0.0381
_diffrn_orient_matrix_UB_12      -0.1164
_diffrn_orient_matrix_UB_13      -0.0642
_diffrn_orient_matrix_UB_21      0.0213
_diffrn_orient_matrix_UB_22      -0.0141
_diffrn_orient_matrix_UB_23      -0.1359
_diffrn_orient_matrix_UB_31      0.2727
_diffrn_orient_matrix_UB_32      -0.1198
_diffrn_orient_matrix_UB_33      0.0552
_diffrn_orient_matrix_type       d*Trek

_diffrn_radiation_wavelength     0.710730
_diffrn_radiation_type           MoK\a

_diffrn_reflns_number            5932
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_sigmaI/netI    0.023

_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         ?
_diffrn_reflns_theta_max         65.9

_reflns_number_total             719
_reflns_number_gt                614
_reflns_threshold_expression     I>2σ(I)

#------------------ 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 :
#L. Akselrud, Yu. Grin.
#WinCSD: software package for crystallographic calculations (Version 4).
#J. Appl. Crystallogr., 2014, 47.

#------------------ 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     4.9923Log(Fₒ)⁴
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     Sheldrick
_refine_ls_extinction_coef       0.063(4)
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         719
_refine_ls_number_parameters     17
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          ?
_refine_ls_R_factor_gt           0.047
_refine_ls_wR_factor_all         ?
_refine_ls_wR_factor_ref         0.053
_refine_ls_goodness_of_fit_ref   1.01
_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_occupancy
Nb1 Nb 0 0 0 Bani 0.30(2) 1.0
Nb2 Nb 0.21202(3) 0.42404(6) 0 Bani 0.313(8) 1.0
Fe1 Fe 0.5 0 0.5 Bani 0.41(2) 1.0
B1 B 0.33333 0.66666 0.5 Bani 0.50(1) 1.0
B2 B 0.2186(8) 0 0.5 Bani 0.51(9) 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
Nb1 0.26(1) 0.26(1) 0.29(3) 0.129(7) 0 0
Nb2 0.24(1) 0.29(1) 0.32(1) 0.143(6) 0 0
Fe1 0.27(2) 0.35(2) 0.50(3) 0.17(1) 0 0
B1 0.4(1) 0.4(1) 0.4(2) 0.20(6) 0 0
B2 0.5(1) 0.6(1) 0.4(1) 0.29(7) 0 0


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
Nb1 B2 2.456(3) . yes
Nb1 Nb2 3.0607(4) . yes
Nb1 Nb1 3.2941(1) 1_556 yes
Nb2 B2 2.396(2) 2_555 yes
Nb2 B1 2.4041(3) . yes
Nb2 Fe1 2.7120(2) 2_555 yes
Nb2 Nb2 3.0333(6) 2_665 yes
Nb2 Nb2 3.0607(4) 5_555 yes
Nb2 Nb2 3.2941(1) 1_554 yes
Fe1 B2 2.345(3) . yes
Fe1 B1 2.4060(1) 1_545 yes
Fe1 Fe1 3.2941(1) 1_556 yes
B2 B2 1.822(5) 5_555 yes

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
B1 Nb1 B1 180.0
####################################################################### 
# 
# 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_Ta7Fe3B8
_database_code_depnum_ccdc_archive 'CCDC 1470522'
_audit_update_record             
;
2016-03-28 deposited with the CCDC.
2016-05-16 downloaded from the CCDC.
;

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

_audit_creation_date             ?
_audit_creation_method           'WinCSD program'

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

_chemical_formula_sum            'B8 Fe3 Ta7'
_chemical_formula_weight         1520.67
_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
Ta Ta 7.00 -.626 6.553 International_Tables_Vol_IV_Table_2.3.1
Fe Fe 3.00 .348 .850 International_Tables_Vol_IV_Table_2.3.1
B B 8.00 .002 .001 International_Tables_Vol_IV_Table_2.3.1

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

loop_
_symmetry_equiv_pos_as_xyz
' x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
' y, -x+y, z'
' x-y, x, z'
'-y, -x, z'
'-x+y, y, z'
' x, x-y, z'
' y, x, z'
' x-y, -y, z'
'-x, -x+y, z'
'-x, -y, -z'
' y, -x+y, -z'
' x-y, x, -z'
' x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
' y, x, -z'
' x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z'
'-x+y, y, -z'
' x, x-y, -z'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 6/m m m'

_cell_length_a                   8.2788(3)
_cell_length_b                   8.2788(3)
_cell_length_c                   3.2934(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     195.48(3)
_cell_formula_units_Z            1


#------------------ 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  0.5708
_exptl_absorpt_correction_T_max  1.0000
_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    12.916
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             629
_exptl_absorpt_coefficient_mu    102.784

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

_cell_measurement_temperature    295.0
_cell_measurement_reflns_used    1697
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      33.20

_diffrn_ambient_temperature      295.0
_diffrn_source_power             1.7
_diffrn_source_voltage           50.0
_diffrn_source_current           34.0
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details 
;
AFC7: Eulerian 3 circle
;
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measurement_method       'profile data from φ-scans'
_diffrn_reflns_theta_full        33.2
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measured_fraction_theta_full 1.0

_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_measurement_details      
;
scan:
	Number of images: 600
	           Slice: 0.0000 - 360.0000
	     Image width: 0.6000
	        Exp time: 46.0000
	   Rotation axis: Phi
	           Omega: -20.0000
	             Chi: -30.0000
	             Phi: 0.0000
	             XTD: 48.2900
	          2theta: -28.0000

;
_diffrn_orient_matrix_UB_11      0.0101
_diffrn_orient_matrix_UB_12      0.0117
_diffrn_orient_matrix_UB_13      -0.1387
_diffrn_orient_matrix_UB_21      -0.0367
_diffrn_orient_matrix_UB_22      0.1191
_diffrn_orient_matrix_UB_23      -0.0628
_diffrn_orient_matrix_UB_31      0.2838
_diffrn_orient_matrix_UB_32      0.1030
_diffrn_orient_matrix_UB_33      0.0293
_diffrn_orient_matrix_type       d*Trek

_diffrn_radiation_wavelength     0.710730
_diffrn_radiation_type           MoK\a

_diffrn_reflns_number            1774
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_sigmaI/netI    0.016

_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       2
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         33.2

_reflns_number_total             179
_reflns_number_gt                174
_reflns_threshold_expression     I>2σ(I)

#------------------ 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 :
#L. Akselrud, Yu. Grin.
#WinCSD: software package for crystallographic calculations (Version 4).
#J. Appl. Crystallogr., 2014, 47.

#------------------ 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     5.2059Log(Fₒ)⁴
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     Sheldrick
_refine_ls_extinction_coef       0.026(1)
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         179
_refine_ls_number_parameters     14
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          ?
_refine_ls_R_factor_gt           0.017
_refine_ls_wR_factor_all         ?
_refine_ls_wR_factor_ref         0.017
_refine_ls_goodness_of_fit_ref   1.04
_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_occupancy
Ta1 Ta 0 0 0 Bani 0.20(2) 1.0
Ta2 Ta 0.21233(3) 0.42466(6) 0 Bani 0.27(2) 1.0
Fe1 Fe 0.5 0 0.5 Bani 0.34(5) 1.0
B1 B 0.33333 0.66666 0.5 Biso 0.3(1) 1.0
B2 B 0.221(1) 0 0.5 Biso 0.4(1) 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
Ta1 0.07(2) 0.07(2) 0.41(4) 0.03(1) 0 0
Ta2 0.12(2) 0.17(2) 0.44(2) 0.087(9) 0 0
Fe1 0.14(5) 0.24(7) 0.58(7) 0.12(3) 0 0


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
Ta1 B2 2.462(3) . yes
Ta1 Ta2 3.0447(7) . yes
Ta1 Ta1 3.2934(3) 1_556 yes
Ta2 B2 2.383(6) 2_555 yes
Ta2 B1 2.3921(3) . yes
Ta2 Fe1 2.6995(3) 2_555 yes
Ta2 Ta2 3.0053(6) 2_665 yes
Ta2 Ta2 3.0447(7) 5_555 yes
Ta2 Ta2 3.2934(3) 1_554 yes
Fe1 B2 2.310(4) . yes
Fe1 B1 2.3899(1) 1_545 yes
Fe1 Fe1 3.2934(3) 1_556 yes
B2 B2 1.830(6) 5_555 yes


loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
B1 Ta1 B1 180.0
