Vanadium fluoroarsenates-folding sheets into highly corrugated layers and crystalline arrays of large inorganic tubes
Eleni Kotsapa; Mark T. Weller; Chem.Commun. 47 (2011) 6132–6134; doi:10.1039/c1cc11513h

data_7106415
_publ_section_title
;
 Vanadium fluoroarsenates-folding sheets into highly corrugated layers and
 crystalline arrays of large inorganic tubes
;
_journal_issue                   21
_journal_name_full               Chem.Commun.
_journal_page_first              6132
_journal_page_last               6134
_journal_paper_doi               10.1039/c1cc11513h
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C6 H21 As2 F3 N3 O13 V3'
_chemical_formula_weight         702.92
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.5917(14)
_cell_angle_beta                 79.8934(13)
_cell_angle_gamma                72.0654(14)
_cell_formula_units_Z            2
_cell_length_a                   8.5594(2)
_cell_length_b                   10.8001(2)
_cell_length_c                   12.0616(2)
_cell_measurement_reflns_used    13957
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     964.51(4)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics
;
Images generated using CrystalMaker: a crystal and molecular
structures program for Mac and Windows. CrystalMaker Software Ltd,
Oxford, England (www.crystalmaker.com)
;
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15708
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.926
_exptl_absorpt_correction_T_max  0.6386
_exptl_absorpt_correction_T_min  0.6386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.8059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                3000
_reflns_number_total             3397
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1cc11513h.txt
_cod_data_source_block           2009ek00166trip-1
_cod_original_cell_volume
'964.51(3) TITL 2009ek00166triP-1 in P-1 CELL 0.71073 8.5594 10.8001 12.0616 65.5917 79.8934 72.0654 ZERR 2.00 0.0002 0.0002 0.0002 0.0014 0.0013 0.0014 LATT 1 SFAC C H As F N O V UNIT 12 42 4 6 6 26 6 MERG 2 SHEL 7 0.84 FMAP 2 PLAN 25 SIZE 0.10 0.10 0.10 ACTA BOND L.S. 4 TEMP -153.00 WGHT 0.000000 3.805900 FVAR 0.45369 AS1 3 0.492495 0.232100 0.054344 11.00000 0.00949 0.00648 = 0.00725 -0.00296 -0.00050 -0.00286 AS2 3 0.520004 0.769617 0.351882 11.00000 0.01074 0.00784 = 0.00774 -0.00245 -0.00056 -0.00315 V1 7 0.629467 0.439732 0.117801 11.00000 0.00863 0.00692 = 0.00835 -0.00284 -0.00164 -0.00261 V2 7 0.640036 0.432506 0.407631 11.00000 0.00817 0.00727 = 0.00662 -0.00260 -0.00036 -0.00175 V3 7 0.660303 0.024330 -0.093141 11.00000 0.00817 0.00734 = 0.00864 -0.00353 -0.00051 -0.00247 F1 4 0.383405 0.546620 0.434574 11.00000 0.00807 0.00946 = 0.00899 -0.00329 -0.00178 -0.00169 F2 4 0.381203 0.550510 0.054152 11.00000 0.01069 0.00755 = 0.00946 -0.00367 0.00081 -0.00322 F3 4 0.606988 -0.098809 0.070784 11.00000 0.00963 0.01063 = 0.01001 -0.00383 -0.00075 -0.00214 O1 6 0.649410 0.176096 -0.034090 11.00000 0.01022 0.00998 = 0.01162 -0.00717 0.00186 -0.00321 O2 6 0.832035 0.353689 0.403378 11.00000 0.01126 0.01136 = 0.01407 -0.00542 -0.00001 -0.00019 O3 6 0.855857 -0.036503 -0.102136 11.00000 0.01139 0.01334 = 0.01122 -0.00449 0.00015 -0.00282 O4 6 0.663456 0.631287 0.334266 11.00000 0.01124 0.00818 = 0.01056 -0.00326 0.00295 -0.00450 O5 6 0.566074 0.452329 0.257450 11.00000 0.01400 0.00810 = 0.00546 -0.00240 -0.00133 -0.00417 O6 6 0.621953 0.896141 0.319055 11.00000 0.01696 0.00828 = 0.01682 -0.00345 -0.00037 -0.00453 AFIX 3 H901 2 0.572153 0.960741 0.283155 11.00000 -1.50000 AFIX 0 O7 6 0.409023 0.098689 0.150078 11.00000 0.01110 0.00705 = 0.01126 -0.00438 0.00246 -0.00589 O8 6 0.553760 0.271908 0.159174 11.00000 0.01403 0.00985 = 0.00572 -0.00300 -0.00164 -0.00629 O9 6 0.342690 0.367507 -0.028381 11.00000 0.01032 0.00765 = 0.01125 -0.00210 -0.00309 -0.00354 O10 6 0.550372 0.263718 0.501193 11.00000 0.01536 0.00825 = 0.00517 -0.00164 -0.00027 -0.00457 O11 6 0.821638 0.363756 0.131502 11.00000 0.01098 0.00970 = 0.01264 -0.00388 -0.00120 -0.00332 O12 6 0.361015 0.833940 0.264019 11.00000 0.00829 0.01169 = 0.00988 -0.00211 -0.00318 -0.00212 N1 5 0.199130 0.620999 0.246405 11.00000 0.01209 0.01632 = 0.00701 -0.00510 0.00071 -0.00581 AFIX 3 H1A 2 0.266230 0.589099 0.309705 11.00000 -1.20000 H1B 2 0.259730 0.652399 0.174305 11.00000 -1.20000 AFIX 0 N2 5 -0.106669 0.682760 0.144800 11.00000 0.01020 0.03012 = 0.01211 -0.00660 -0.00057 -0.00505 AFIX 3 H2A 2 -0.179069 0.658160 0.211100 11.00000 -1.20000 H2B 2 -0.163269 0.716860 0.075500 11.00000 -1.20000 AFIX 0 C1 1 0.057967 0.738099 0.255446 11.00000 0.01444 0.01776 = 0.01928 -0.00986 0.00188 -0.00595 AFIX 23 H1C 2 0.098298 0.813183 0.258542 11.00000 -1.20000 H1D 2 -0.010582 0.703397 0.330962 11.00000 -1.20000 AFIX 0 C2 1 -0.042321 0.795753 0.146300 11.00000 0.01396 0.01844 = 0.01855 -0.00240 -0.00011 -0.00805 AFIX 23 H2C 2 -0.135121 0.876192 0.149659 11.00000 -1.20000 H2D 2 0.026597 0.829901 0.070867 11.00000 -1.20000 AFIX 0 C3 1 0.027519 0.555369 0.147850 11.00000 0.01477 0.03047 = 0.02441 -0.02085 0.00278 -0.00932 AFIX 23 H3C 2 0.094196 0.577684 0.069721 11.00000 -1.20000 H3D 2 -0.021155 0.479416 0.156737 11.00000 -1.20000 AFIX 0 C4 1 0.137197 0.504231 0.251314 11.00000 0.01814 0.01634 = 0.02092 -0.00492 -0.00065 -0.00605 AFIX 23 H4A 2 0.074878 0.468702 0.330010 11.00000 -1.20000 H4B 2 0.231215 0.425652 0.245713 11.00000 -1.20000 AFIX 0 N3 5 0.172408 -0.002554 0.471489 11.00000 0.02293 0.02050 = 0.03242 -0.01434 0.00602 -0.00582 AFIX 3 H3A 2 0.253108 0.044746 0.447589 11.00000 -1.20000 H3B 2 0.221808 -0.095154 0.482489 11.00000 -1.20000 AFIX 0 C5 1 0.052370 0.060908 0.373750 11.00000 0.02398 0.02274 = 0.02117 -0.01261 0.00341 -0.00167 AFIX 23 H5A 2 0.109228 0.047671 0.298989 11.00000 -1.20000 H5B 2 0.010385 0.163431 0.354317 11.00000 -1.20000 AFIX 0 C6 1 0.089933 0.004800 0.587891 11.00000 0.02807 0.03123 = 0.02647 -0.01659 -0.00153 -0.00911 AFIX 23 H6A 2 0.049697 0.104628 0.578828 11.00000 -1.20000 H6B 2 0.170411 -0.044554 0.652208 11.00000 -1.20000 AFIX 0 OW1 6 0.376360 0.169174 0.386009 11.00000 0.02836 0.02845 = 0.01241 -0.01028 0.00068 -0.01368 AFIX 3 H902 2 0.420960 0.188974 0.323009 11.00000 -1.50000 H903 2 0.417960 0.188974 0.430009 11.00000 -1.50000 HKLF 4 REM 2009ek00166triP-1 in P-1 REM R1 = 0.0291 for 3000 Fo > 4sig(Fo) and 0.0371 for all 3397 data REM 271 parameters refined using 0 restraints END WGHT 0.0000 3.7670 REM Highest difference peak 0.562, deepest hole -0.493, 1-sigma level 0.114 Q1 1 0.0737 0.1072 0.4414 11.00000 0.05 0.56 Q2 1 0.6476 0.2049 0.5199 11.00000 0.05 0.49 Q3 1 0.6168 0.6935 0.3260 11.00000 0.05 0.46 Q4 1 0.4293 0.8065 0.3034 11.00000 0.05 0.45 Q5 1 0.5246 0.3608 0.4625 11.00000 0.05 0.44 Q6 1 0.7239 0.3554 0.1136 11.00000 0.05 0.42 Q7 1 0.1045 0.2471 0.2682 11.00000 0.05 0.41 Q8 1 0.5221 0.9969 0.2180 11.00000 0.05 0.41 Q9 1 0.1290 0.6804 0.2597 11.00000 0.05 0.40 Q10 1 0.6490 0.4752 0.2413 11.00000 0.05 0.40 Q11 1 0.7888 -0.1447 -0.0750 11.00000 0.05 0.40 Q12 1 0.5646 0.4477 0.2058 11.00000 0.05 0.40 Q13 1 0.5428 0.2629 0.1054 11.00000 0.05 0.39 Q14 1 0.6841 0.7083 0.2449 11.00000 0.05 0.39 Q15 1 0.4064 -0.0932 0.4251 11.00000 0.05 0.39 Q16 1 0.3977 0.0811 0.1955 11.00000 0.05 0.39 Q17 1 0.5296 0.2503 0.4539 11.00000 0.05 0.39 Q18 1 0.7444 0.6228 0.3335 11.00000 0.05 0.37 Q19 1 0.1737 -0.1250 0.7825 11.00000 0.05 0.37 Q20 1 0.4170 0.0205 0.4264 11.00000 0.05 0.37 Q21 1 0.1263 -0.0558 0.7634 11.00000 0.05 0.37 Q22 1 0.2748 0.3325 0.4355 11.00000 0.05 0.37 Q23 1 0.4994 0.3407 0.1553 11.00000 0.05 0.37 Q24 1 0.2572 0.3618 -0.0209 11.00000 0.05 0.37 Q25 1 0.9107 0.0019 -0.1020 11.00000 0.05 0.36'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7106415