# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

##############################################################################
###      FullProf-generated CIF output file  (version: May 2011)           ###
###      Template of CIF submission form for structure report              ###
##############################################################################
 
# This file has been generated using FullProf.2k taking one example of 
# structure report provided by Acta Cryst. It is given as a 'template' with 
# filled structural items. Many other items are left unfilled and it is the  
# responsibility of the user to properly fill or suppress them. In principle 
# all question marks '?' should be replaced by the appropriate text or 
# numerical value depending on the kind of CIF item. 
# See the document: cif_core.dic (URL: http://www.iucr.org) for details. 
 
# Please notify any error or suggestion to: 
#           Juan Rodriguez-Carvajal (jrc@ill.eu)
# Improvements will be progressively added as needed.
 
#=============================================================================
 data_global
#=============================================================================
 
# PROCESSING SUMMARY (IUCr Office Use Only)
 
_journal_data_validation_number      ?
 
_journal_date_recd_electronic        ?
_journal_date_to_coeditor            ?
_journal_date_from_coeditor          ?
_journal_date_accepted               ?
_journal_date_printers_first         ?
_journal_date_printers_final         ?
_journal_date_proofs_out             ?
_journal_date_proofs_in              ?
_journal_coeditor_name               ?
_journal_coeditor_code               ?
_journal_coeditor_notes
; ?
;
_journal_techeditor_code             ?
_journal_techeditor_notes
; ?
;
_journal_coden_ASTM                  ?
_journal_name_full                   ?
_journal_year                        ?
_journal_volume                      ?
_journal_issue                       ?
_journal_page_first                  ?
_journal_page_last                   ?
_journal_paper_category              ?
_journal_suppl_publ_number           ?
_journal_suppl_publ_pages            ?
 
#=============================================================================
 
# 1. SUBMISSION DETAILS
 
_publ_contact_author_name            Torben R. Jensen
_publ_contact_author_address         University of Aarhus, Langelandsgade 140, DK-8000 Århus C, Denmark.
; ?
;
_publ_contact_author_email           trj@chem.au.dk
_publ_contact_author_fax             ?
_publ_contact_author_phone           +45 8942 3894
 
_publ_contact_letter
; ?
;
 
_publ_requested_journal              Dalton Transactions DOI: 10.1039/c4dt01125b
_publ_requested_coeditor_name        ?
_publ_requested_category             ?   # Acta C: one of CI/CM/CO/FI/FM/FO
 
 
# Definition of non standard CIF items (Reliability indices used in FULLPROF) 
 
loop_ 
_publ_manuscript_incl_extra_item
_publ_manuscript_incl_extra_info
_publ_manuscript_incl_extra_defn
#      Name                               Explanation                 Standard?
#     ------                              -----------                 ---------
 '_pd_proc_ls_prof_cR_factor'    'Prof. R-factor CORRECTED for background'   no
 '_pd_proc_ls_prof_cwR_factor'   'wProf.R-factor CORRECTED for background'   no
 '_pd_proc_ls_prof_cwR_expected' 'wProf.Expected CORRECTED for background'   no
 '_pd_proc_ls_prof_chi2'         'Chi-square for all considered points'      no
 '_pd_proc_ls_prof_echi2'        'Chi-2 for points with Bragg contribution'  no
#=============================================================================
 
# 3. TITLE AND AUTHOR LIST
 
_publ_section_title Novel solvates M(BH4)3S(CH3)2 and properties of halide-free M(BH4)3 (M = Y or Gd)
;
;
_publ_section_title_footnote
;
;
 
# The loop structure below should contain the names and addresses of all 
# authors, in the required order of publication. Repeat as necessary.
 
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
Ley, Morten B.
Center for Materials Crystallography (CMC), Interdisciplinary Nanoscience Center (iNANO), and Department of Chemistry, Aarhus University,
Langelandsgade 140, DK-8000 Aarhus C, Denmark
Paskevicius, Mark
Department of Imaging and Applied Physics, Fuels and Energy Technology Institute, Curtin University, GPO Box U1987, Perth, 6845 WA, Australia
Schouwink, Pascal
Laboratory of Crystallography, Department of Quantum Matter Physics,
University of Geneva, 24, Quai Ernest-Ansermet, CH-1211 Geneva, Switzerland
Richter, Bo
Center for Materials Crystallography (CMC), Interdisciplinary Nanoscience Center (iNANO), and Department of Chemistry, Aarhus University,
Langelandsgade 140, DK-8000 Aarhus C, Denmark
Sheppard, Drew A. 
Department of Imaging and Applied Physics, Fuels and Energy Technology Institute, Curtin University, GPO Box U1987, Perth, 6845 WA, Australia
Buckley, Craig
Department of Imaging and Applied Physics, Fuels and Energy Technology Institute, Curtin University, GPO Box U1987, Perth, 6845 WA, Australia
Jensen, Torben R.
Center for Materials Crystallography (CMC), Interdisciplinary Nanoscience Center (iNANO), and Department of Chemistry, Aarhus University,
Langelandsgade 140, DK-8000 Aarhus C, Denmark
 
#=============================================================================
 
# 4. TEXT
 
_publ_section_synopsis
;  ?
;
_publ_section_abstract
; ?
;          
_publ_section_comment
; ?
;
_publ_section_exptl_prep      # Details of the preparation of the sample(s)
                              # should be given here. 
; ?
;
_publ_section_exptl_refinement
; ?
;
_publ_section_references
; ?
;
_publ_section_figure_captions
; ?
;
_publ_section_acknowledgements
; ?
;
 
#=============================================================================
 
#=============================================================================
# If more than one structure is reported, the remaining sections should be 
# completed per structure. For each data set, replace the '?' in the
# data_? line below by a unique identifier.
 
data_1 Y(BH4)3_DMS                 
 
#=============================================================================
 
# 5. CHEMICAL DATA
 
_chemical_name_systematic
; ?
;
_chemical_name_common             Yttrium borohydride dimethyl sulfide complex
_chemical_formula_moiety          Y(BH4)3S(CH3)2
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_iupac           ?
_chemical_formula_sum             ?
_chemical_formula_weight          ?
_chemical_melting_point           ?
_chemical_compound_source         ?       # for minerals and 
                                          # natural products
 
loop_
    _atom_type_symbol               
    _atom_type_scat_Cromer_Mann_a1 
    _atom_type_scat_Cromer_Mann_b1 
    _atom_type_scat_Cromer_Mann_a2 
    _atom_type_scat_Cromer_Mann_b2 
    _atom_type_scat_Cromer_Mann_a3 
    _atom_type_scat_Cromer_Mann_b3 
    _atom_type_scat_Cromer_Mann_a4 
    _atom_type_scat_Cromer_Mann_b4 
    _atom_type_scat_Cromer_Mann_c 
    _atom_type_scat_dispersion_real 
    _atom_type_scat_dispersion_imag 
    _atom_type_scat_source          
y     17.77600   1.40290  10.29460  12.80060   5.72629   0.12560
       3.26588 104.35400   1.91213  -2.95100   3.54200
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
b      2.05450  23.21850   1.33260   1.02100   1.09790  60.34980
       0.70680   0.14030  -0.19320   0.00000   0.00100
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
h      0.49300  10.51090   0.32291  26.12570   0.14019   3.14236
       0.04081  57.79970   0.00304   0.00000   0.00000
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
s      6.90530   1.46790   5.20340  22.21510   1.43790   0.25360
       1.58630  56.17200   0.86690   0.11000   0.12400
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
c      2.31000  20.84390   1.02000  10.20750   1.58860   0.56870
       0.86500  51.65120   0.21560   0.00200   0.00200
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
 
#=============================================================================
 
# 6. POWDER SPECIMEN AND CRYSTAL DATA
 
_symmetry_cell_setting                Monoclinic
_symmetry_space_group_name_H-M       'P 1 21/c 1'
_symmetry_space_group_name_Hall      '-P 2ybc'
 
loop_
    _symmetry_equiv_pos_as_xyz   #<--must include 'x,y,z'
'x,y,z'
'-x,y+1/2,-z+1/2'
'-x,-y,-z'
'x,-y+1/2,z+1/2'
 
_cell_length_a                       5.52621(8)
_cell_length_b                       22.3255(3)
_cell_length_c                       8.06160(12)
_cell_angle_alpha                    90.00000
_cell_angle_beta                     100.4084(10)
_cell_angle_gamma                    90.00000
_cell_volume                         978.24(3)
_cell_formula_units_Z                ?
_cell_measurement_temperature        ?
_cell_special_details
; ?
;
# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.
 
_pd_spec_size_axial               ?       # perpendicular to 
                                          # equatorial plane
_pd_spec_size_equat               ?       # parallel to 
                                          # scattering vector
                                          # in transmission
_pd_spec_size_thick               ?       # parallel to 
                                          # scattering vector
                                          # in reflection
 
# The next five fields are character fields that describe the specimen.
 
_pd_spec_mounting                         # This field should be
                                          # used to give details of the 
                                          # container.
; ?
;
_pd_spec_mount_mode               ?       # options are 'reflection'
                                          # or 'transmission'
_pd_spec_shape                    ?       # options are 'cylinder' 
                                          # 'flat_sheet' or 'irregular'
_pd_char_particle_morphology      ?
_pd_char_colour                   ?       # use ICDD colour descriptions
 
# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was 
# prepared is in kPa.  The temperature of preparation is in K.        
 
_pd_prep_cool_rate                ?
_pd_prep_pressure                 ?
_pd_prep_temperature              ?
 
# The next four fields are normally only needed for transmission experiments.
 
_exptl_absorpt_coefficient_mu        ?
_exptl_absorpt_correction_type       ?
_exptl_absorpt_process_details       ?
_exptl_absorpt_correction_T_min      ?
_exptl_absorpt_correction_T_max      ?
 
#=============================================================================
 
# 7. EXPERIMENTAL DATA
 
_exptl_special_details
; ?
;
 
# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.
 
_pd_instr_location
; ?
;
_pd_calibration_special_details           # description of the method used
                                          # to calibrate the instrument
; ?
;
 
_diffrn_ambient_temperature          ?
_diffrn_source              ? # Put here: 'rotating-anode X-ray tube' or similar 
_diffrn_radiation_type     'X-ray' 
_diffrn_source_target       ? # Put here the chemical symbol of the anode
 
_diffrn_radiation_monochromator      ?
_diffrn_measurement_device_type      ?
_diffrn_measurement_method           ?
_diffrn_detector_area_resol_mean     ? # Not in version 2.0.1
_diffrn_detector                     ?
_diffrn_detector_type                ? # make or model of detector
_pd_meas_scan_method      ?   # options are 'step', 'cont',
                              # 'tof', 'fixed' or
                              # 'disp' (= dispersive)
_pd_meas_special_details
;  ?
;
 
#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.
 
_pd_meas_number_of_points         4005
_pd_meas_2theta_range_min         1.86063
_pd_meas_2theta_range_max         35.49472
_pd_meas_2theta_range_inc         0.008402
 
#=============================================================================
 
# 8. REFINEMENT DATA
 
_refine_special_details
; ?
;
 
# Use the next field to give any special details about the fitting of the
# powder pattern.
 
_pd_proc_ls_special_details
; ?
;
 
# The next three items are given as text.
 
_pd_proc_ls_profile_function      ?
_pd_proc_ls_background_function   ?
_pd_proc_ls_pref_orient_corr
; ?
;
 
#  The following profile R-factors are NOT CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These are the current CIF standard
 
_pd_proc_ls_prof_R_factor                1.8609
_pd_proc_ls_prof_wR_factor               2.9232
_pd_proc_ls_prof_wR_expected             0.0999
 
#  The following profile R-factors are CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These items are not in the current CIF standard, but are defined above
 
_pd_proc_ls_prof_cR_factor                9.4682
_pd_proc_ls_prof_cwR_factor               9.3150
_pd_proc_ls_prof_cwR_expected             0.3182
 
#  The following items are not in the CIF standard, but are defined above
 
_pd_proc_ls_prof_chi2               856.8841
_pd_proc_ls_prof_echi2             1011.0157
 
#  Items related to LS refinement
 
_refine_ls_R_I_factor                 4.2709
_refine_ls_number_reflns                   427
_refine_ls_number_parameters                56
_refine_ls_number_restraints                 0
 
# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.
 
_pd_proc_2theta_range_min                1.8686
_pd_proc_2theta_range_max               35.5027
_pd_proc_2theta_range_inc              0.008402
_pd_proc_wavelength                    0.822570
 
_pd_block_diffractogram_id        ?  # The id used for the block containing
                                     # the powder pattern profile (section 11)
 
# Give appropriate details in the next two text fields.
 
_pd_proc_info_excluded_regions    ?
_pd_proc_info_data_reduction      ?
 
# The following items are used to identify the programs used.
 
_computing_data_collection           ?
_computing_structure_solution        ?
_computing_structure_refinement      FULLPROF
_computing_molecular_graphics        ?
_computing_publication_material      ?
 
#=============================================================================
 
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
 
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_occupancy
    _atom_site_adp_type              # Not in version 2.0.1
    _atom_site_type_symbol
 Y1  0.6841(3)  0.33623(6)  0.11608(19)  0.0132(6)  1.00000 Uiso Y   
 B1  0.166(2)  0.1643(6)  0.5630(14)  0.031(3)  1.00000 Uiso B   
 H1  0.306(2)  0.1691(6)  0.4761(14)  0.031(3)  1.00000 Uiso H   
 H2  0.226(2)  0.1271(6)  0.6584(14)  0.031(3)  1.00000 Uiso H   
 H3  0.152(2)  0.2084(6)  0.6326(14)  0.031(3)  1.00000 Uiso H   
 H4 -0.022(2)  0.1527(6)  0.4848(14)  0.031(3)  1.00000 Uiso H   
 B2  0.798(3)  0.0794(6)  0.8103(16)  0.031(3)  1.00000 Uiso B   
 H1  0.879(3)  0.0322(6)  0.8243(16)  0.031(3)  1.00000 Uiso H   
 H2  0.954(3)  0.1135(6)  0.8228(16)  0.031(3)  1.00000 Uiso H   
 H3  0.675(3)  0.0841(6)  0.6809(16)  0.031(3)  1.00000 Uiso H   
 H4  0.684(3)  0.0876(6)  0.9130(16)  0.031(3)  1.00000 Uiso H   
 B3  0.325(3)  0.7573(7)  0.1258(20)  0.031(3)  1.00000 Uiso B   
 H1  0.201(3)  0.7712(7)  0.2179(20)  0.031(3)  1.00000 Uiso H   
 H2  0.386(3)  0.7088(7)  0.1513(20)  0.031(3)  1.00000 Uiso H   
 H3  0.219(3)  0.7616(7) -0.0091(20)  0.031(3)  1.00000 Uiso H   
 H4  0.494(3)  0.7877(7)  0.1432(20)  0.031(3)  1.00000 Uiso H   
 S1  0.4945(8)  0.0779(2)  0.3570(5)  0.0427(18)  1.00000 Uiso S   
 C2  0.744(3)  0.0325(6)  0.3027(13)  0.082(4)  1.00000 Uiso C   
 C3  0.378(2)  0.1119(6)  0.1709(16)  0.082(4)  1.00000 Uiso C   
 H4  0.845(3)  0.0099(6)  0.4140(13)  0.082(4)  1.00000 Uiso H   
 H5  0.873(3)  0.0600(6)  0.2473(13)  0.082(4)  1.00000 Uiso H   
 H6  0.663(3) -0.0014(6)  0.2115(13)  0.082(4)  1.00000 Uiso H   
 H7  0.226(2)  0.1413(6)  0.1865(16)  0.082(4)  1.00000 Uiso H   
 H8  0.307(2)  0.0766(6)  0.0809(16)  0.082(4)  1.00000 Uiso H   
 H9  0.515(2)  0.1382(6)  0.1208(16)  0.082(4)  1.00000 Uiso H   
 
# Note: if the displacement parameters were refined anisotropically
# the U matrices should be given as for single-crystal studies.
 
#=============================================================================
 
# 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY 
 
_geom_special_details                ?
 
loop_
    _geom_bond_atom_site_label_1  
    _geom_bond_atom_site_label_2  
    _geom_bond_site_symmetry_1    
    _geom_bond_site_symmetry_2    
    _geom_bond_distance           
    _geom_bond_publ_flag          
    ?   ?   ?   ?   ?   ?
 
loop_
    _geom_contact_atom_site_label_1 
    _geom_contact_atom_site_label_2 
    _geom_contact_distance          
    _geom_contact_site_symmetry_1   
    _geom_contact_site_symmetry_2   
    _geom_contact_publ_flag         
    ?   ?   ?   ?   ?   ?
 
loop_
_geom_angle_atom_site_label_1 
_geom_angle_atom_site_label_2 
_geom_angle_atom_site_label_3 
_geom_angle_site_symmetry_1   
_geom_angle_site_symmetry_2   
_geom_angle_site_symmetry_3   
_geom_angle                   
_geom_angle_publ_flag         
?   ?   ?   ?   ?   ?   ?   ?
 
loop_
_geom_torsion_atom_site_label_1 
_geom_torsion_atom_site_label_2 
_geom_torsion_atom_site_label_3 
_geom_torsion_atom_site_label_4 
_geom_torsion_site_symmetry_1   
_geom_torsion_site_symmetry_2   
_geom_torsion_site_symmetry_3   
_geom_torsion_site_symmetry_4   
_geom_torsion                   
_geom_torsion_publ_flag         
?   ?   ?   ?   ?   ?   ?   ?   ?   ?
 
loop_
_geom_hbond_atom_site_label_D 
_geom_hbond_atom_site_label_H 
_geom_hbond_atom_site_label_A 
_geom_hbond_site_symmetry_D   
_geom_hbond_site_symmetry_H   
_geom_hbond_site_symmetry_A   
_geom_hbond_distance_DH       
_geom_hbond_distance_HA       
_geom_hbond_distance_DA       
_geom_hbond_angle_DHA         
_geom_hbond_publ_flag         
?   ?   ?   ?   ?   ?   ?   ?   ?   ?   ?
 
#=============================================================================
 
#=============================================================================
# Additional structures (last six sections and associated data_? identifiers) 
# may be added at this point.                                                 
#=============================================================================
 
# The following lines are used to test the character set of files sent by     
# network email or other means. They are not part of the CIF data set.        
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789              
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ 
