# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
#=============================================================================

# 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_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        
'Igor Djerdj' # Name of author for correspondence
_publ_contact_author_address     # Address of author for correspondence
; ?
;
_publ_contact_author_email       igor.djerdj@irb.hr
_publ_contact_author_fax         ?
_publ_contact_author_phone       ?

_publ_contact_letter             
; ?
;
_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              
; 'Fox/ObjCryst exported file:vanadium terephthalate'
;
_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
#<--'Last name, first name'
'Igor Djerdj'
; ?
;
; ?
;
'Sreco Skapin' '' ''
'Miran Ceh' '' ''
'Zvonko Jaglicic' '' ''
'Damir Pajic' '' ''
'Bojan Kozlevcar' '' ''
'Bojan Orel' '' ''
'Zorica Crnjak Ore' '' ''

#=============================================================================

# 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_V4O4(OH)2(O2CC6H4CO2)4_DMF
_database_code_depnum_ccdc_archive 'CCDC 818770'
#TrackingRef 'dalton_transaction_publ.cif'

#=============================================================================
# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_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
v 10.29710 6.86570 7.35110 0.43850 2.07030 26.89380 2.05710 102.47800 1.21990
0.26700 0.53000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.00800 0.00600
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900
0.00400 0.00300
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

_chemical_formula_sum            'C35 H25 N O23 V4'
_chemical_formula_weight         1031.33
_cell_length_a                   20.923(4)
_cell_length_b                   5.963(4)
_cell_length_c                   20.425(3)
_cell_angle_alpha                90.000
_cell_angle_beta                 123.701(6)
_cell_angle_gamma                90.000
_cell_volume                     2120.1(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 2/m '
_symmetry_int_tables_number      10
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall  '-P 2y'

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,-z
3 -x,-y,-z
4 x,-y,z
#=============================================================================

# 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      293
_diffrn_source                   Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.70177

_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        2788
_pd_meas_2theta_range_min        1.52940
_pd_meas_2theta_range_max        23.55760
_pd_meas_2theta_range_inc        0.007907

#=============================================================================

# 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        7.5776
_pd_proc_ls_prof_wR_factor       9.7369
_pd_proc_ls_prof_wR_expected     5.5510

# 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       12.2987
_pd_proc_ls_prof_cwR_factor      15.1035
_pd_proc_ls_prof_cwR_expected    8.6322

# The following items are not in the CIF standard, but are defined above

_pd_proc_ls_prof_chi2            3.0812
_pd_proc_ls_prof_echi2           3.0812

# Items related to LS refinement

_refine_ls_R_I_factor            5.5205
_refine_ls_number_reflns         816
_refine_ls_number_parameters     64
_refine_ls_number_restraints     89

# 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        1.5317
_pd_proc_2theta_range_max        23.5599
_pd_proc_2theta_range_inc        0.007907
_pd_proc_wavelength              0.701770

_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_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_attached_hydrogens
_atom_site_calc_flag
_atom_site_thermal_displace_type
_atom_site_u_iso_or_equiv
V1 V 0.5000 1.0000 0.2820(6) 1.000 2 m ? d Uiso 0.09(1)
V2 V 0.5000 0.5000 0.2769(6) 1.000 2 n ? d Uiso 0.09(1)
V3 V 0.0000 0.0000 0.1990(5) 1.000 2 m ? d Uiso 0.09(1)
V4 V 0.0000 0.5000 0.1388(5) 1.000 2 n ? d Uiso 0.09(1)
O1 O 0.452(1) 0.255(1) 0.295(2) 1.000 4 o ? d Uiso 0.06(1)
O2 O 0.367(3) 0.205(4) 0.336(3) 1.000 4 o ? d Uiso 0.06(1)
O3 O 0.147(2) 0.168(4) -0.087(3) 1.000 4 o ? d Uiso 0.06(1)
O4 O 0.072(1) 0.318(1) -0.043(3) 1.000 4 o ? d Uiso 0.06(1)
O5 O 0.5692(3) 0.753(1) 0.299(1) 1.000 4 o ? d Uiso 0.06(1)
O6 O 0.682(2) 0.804(3) 0.294(3) 1.000 4 o ? d Uiso 0.06(1)
O7 O 0.910(3) 0.845(2) 0.700(3) 1.000 4 o ? d Uiso 0.06(1)
O8 O 0.801(4) 0.822(3) 0.696(3) 1.000 4 o ? d Uiso 0.06(1)
O9 O 0.4657(8) 0.244(1) 0.2114(6) 1.000 4 o ? d Uiso 0.06(1)
O10 O -0.004(7) 0.242(5) 0.161(3) 1.000 4 o ? d Uiso 0.06(1)
O11 O -0.0799(8) 0.0000 0.213(1) 1.000 2 m ? d Uiso 0.06(1)
H11 H -0.1017 0.0000 0.2453 1.000 2 m ? d Uiso 0.06
O12 O 0.065(5) 0.5000 0.113(6) 1.000 2 n ? d Uiso 0.06(1)
H12 H 0.1150 0.5000 0.1431 1.000 2 n ? d Uiso 0.06
N1 N 0.2876(3) 0.0000 0.8607(3) 1.000 2 m ? d Uiso 0.05(1)
C1 C 0.3535(3) 0.0000 0.9004(4) 1.000 2 m ? d Uiso 0.03(1)
H1 H 0.4096 0.0000 0.9286 1.000 2 m ? d Uiso 0.03
C2 C 0.233(1) 0.0000 0.872(2) 1.000 2 m ? d Uiso 0.03(1)
H2b H 0.2018 0.1315 0.8482 0.500 4 o ? d Uiso 0.03
H2a H 0.2018 -0.1315 0.8482 0.500 4 o ? d Uiso 0.03
H2c H 0.2542 0.0000 0.9272 1.000 2 m ? d Uiso 0.03
C3 C 0.280(1) 0.0000 0.7836(4) 1.000 2 m ? d Uiso 0.03(1)
H3b H 0.2700 0.1409 0.7556 0.500 4 o ? d Uiso 0.03
H3a H 0.2700 -0.1409 0.7556 0.500 4 o ? d Uiso 0.03
H3c H 0.3342 0.0000 0.8200 1.000 2 m ? d Uiso 0.03
O13 O 0.393(1) 0.0000 0.9944(4) 1.000 2 m ? d Uiso 0.06(1)
C4 C 0.3191 0.2232 0.2007 1.000 4 o ? d Uiso 0.03(1)
C5 C 0.3327 0.2366 0.1444 1.000 4 o ? d Uiso 0.03(1)
H5 H 0.3829 0.2461 0.1576 1.000 4 o ? d Uiso 0.03
C6 C 0.2483 0.2339 0.1831 1.000 4 o ? d Uiso 0.03(1)
H6 H 0.2387 0.2271 0.2225 1.000 4 o ? d Uiso 0.03
C7 C 0.2729 0.2364 0.0676 1.000 4 o ? d Uiso 0.03(1)
H7 H 0.2818 0.2241 0.0279 1.000 4 o ? d Uiso 0.03
C8 C 0.1908 0.2547 0.1079 1.000 4 o ? d Uiso 0.03(1)
H8 H 0.1410 0.2704 0.0954 1.000 4 o ? d Uiso 0.03
C9 C 0.2021 0.2539 0.0501 1.000 4 o ? d Uiso 0.03(1)
C10 C 0.3785 0.2452 0.2776 1.000 4 o ? d Uiso 0.03(1)
C11 C 0.1404 0.2466 -0.0259 1.000 4 o ? d Uiso 0.03(1)
C12 C 0.6970 0.7478 0.4169 1.000 4 o ? d Uiso 0.03(1)
C13 C 0.6653 0.7242 0.4587 1.000 4 o ? d Uiso 0.03(1)
H13 H 0.6122 0.7190 0.4333 1.000 4 o ? d Uiso 0.03
C14 C 0.7725 0.7550 0.4546 1.000 4 o ? d Uiso 0.03(1)
H14 H 0.7948 0.7622 0.4260 1.000 4 o ? d Uiso 0.03
C15 C 0.7116 0.7080 0.5384 1.000 4 o ? d Uiso 0.03(1)
H15 H 0.6910 0.6705 0.5673 1.000 4 o ? d Uiso 0.03
C16 C 0.8173 0.7522 0.5330 1.000 4 o ? d Uiso 0.03(1)
H16 H 0.8704 0.7545 0.5586 1.000 4 o ? d Uiso 0.03
C17 C 0.7864 0.7460 0.5748 1.000 4 o ? d Uiso 0.03(1)
C18 C 0.6506 0.7729 0.3365 1.000 4 o ? d Uiso 0.03(1)
C19 C 0.8316 0.7665 0.6548 1.000 4 o ? d Uiso 0.03(1)
# 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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.92(2) 5_041 ?
V1 O1 1.92(2) 5_011 ?
V1 O5 1.954(8) 9_011 ?
V1 O5 1.954(8) 9_041 ?
V1 O9 1.89(1) 13_011 ?
V1 O9 1.89(1) 13_041 ?

loop_
_geom_bond_atom_site_label_3
_geom_bond_atom_site_label_4
_geom_bond_distance34
_geom_bond_site_symmetry_4
_geom_bond_publ_flag3
V4 O10 1.62(4) 14_041 ?
V4 O10 1.62(4) 14_011 ?
V4 O12 1.70(8) 17_011 ?
V4 O4 2.00(3) 8_031 ?
V4 O4 2.00(3) 8_021 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O1 104.7(3) 5_041 5_011 ?
O1 V1 O5 164.5(3) 5_041 5_041 ?

#=============================================================================