Protonolysis of [((i)PrO)TiMo5O18]3-: access to a family of TiMo5 Lindqvist type polyoxometalates.
Coyle, Laura; Middleton, Paul S.; Murphy, Christopher J.; Clegg, William; Harrington, Ross W.; Errington, R. John; Dalton transactions (Cambridge, England : 2003) 41 (2012) 971–981; doi:10.1039/c1dt11256b

data_7017613
_publ_section_title
;
 Protonolysis of [((i)PrO)TiMo5O18]3-: access to a family of TiMo5
 Lindqvist type polyoxometalates.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              971
_journal_page_last               981
_journal_paper_doi               10.1039/c1dt11256b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         '6 C16 H36 N +,Mo10 O37 Ti2 6-,2 C2 H3 N'
_chemical_formula_sum            'C100 H222 Mo10 N8 O37 Ti2'
_chemical_formula_weight         3184.06
_chemical_name_systematic
;
?
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1864(17)
_cell_length_b                   16.1864(17)
_cell_length_c                   50.752(7)
_cell_measurement_reflns_used    7931
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      2.15
_cell_volume                     13297(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            114405
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.67
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6552
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.892
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_coef       0.000182(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         15970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+26.3651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                14323
_reflns_number_total             15970
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1dt11256b.txt
_cod_data_source_block           rje260_salt_of_7
_cod_database_code               7017613
_computing_special_details
;
TITL rje260 in P4(1)2(1)2
CELL 0.71073 16.1864 16.1864 50.7519 90.000 90.000 90.000
ZERR 4.00 0.0017 0.0017 0.0074 0.000 0.000 0.000
LATT -1
SYMM -X, -Y, 0.5+Z
SYMM 0.5-Y, 0.5+X, 0.25+Z
SYMM 0.5+Y, 0.5-X, 0.75+Z
SYMM 0.5-X, 0.5+Y, 0.25-Z
SYMM 0.5+X, 0.5-Y, 0.75-Z
SYMM Y, X, -Z
SYMM -Y, -X, 0.5-Z
SFAC C H N O TI MO
UNIT 400 888 32 148 8 40

SIZE 0.60 0.48 0.35
TEMP -113

L.S. 8
ACTA 52
BOND $H
FMAP 2
PLAN 10
CONN $TI $MO 6

WGHT 0.032300 26.365095
EXTI 0.000182
FVAR 0.07558
TI1 5 0.490172 0.495603 0.464325 11.00000 0.01464 0.01659 =
0.01224 0.00067 -0.00085 0.00173
MO2 6 0.337771 0.486587 0.424671 11.00000 0.01489 0.02194 =
0.02029 -0.00373 -0.00306 0.00176
MO3 6 0.490257 0.350510 0.421506 11.00000 0.02275 0.01322 =
0.02111 -0.00092 0.00036 0.00306
MO4 6 0.623548 0.504321 0.417960 11.00000 0.01597 0.02200 =
0.01905 0.00228 0.00374 0.00087
MO5 6 0.472195 0.640006 0.421643 11.00000 0.02385 0.01331 =
0.01676 0.00040 -0.00260 0.00261
MO6 6 0.470042 0.494800 0.375597 11.00000 0.03101 0.02404 =
0.01174 -0.00133 -0.00138 0.00487
O1 4 0.497582 0.497582 0.500000 10.50000 0.02948 0.02948 =
0.01486 0.00186 -0.00186 0.00107
O2 4 0.234048 0.470565 0.426517 11.00000 0.01859 0.03331 =
0.03069 -0.00600 -0.00349 0.00056
O3 4 0.501649 0.246394 0.420411 11.00000 0.03643 0.01667 =
0.04100 -0.00169 0.00072 0.00377
O4 4 0.727291 0.518433 0.414492 11.00000 0.02249 0.03508 =
0.03068 0.00581 0.00739 0.00275
O5 4 0.458216 0.743952 0.421594 11.00000 0.03933 0.01914 =
0.02937 0.00111 -0.00768 0.00563
O6 4 0.461952 0.496305 0.342419 11.00000 0.05387 0.04200 =
0.01287 -0.00043 -0.00365 0.00558
O7 4 0.480974 0.495609 0.421486 11.00000 0.01584 0.01549 =
0.01317 0.00022 -0.00270 0.00222
O12 4 0.372268 0.480486 0.459600 11.00000 0.01607 0.02596 =
0.02122 -0.00074 0.00210 0.00040
O13 4 0.505250 0.377643 0.456638 11.00000 0.02262 0.01637 =
0.02077 0.00433 -0.00073 0.00162
O14 4 0.605728 0.510735 0.453948 11.00000 0.01455 0.02524 =
0.01728 0.00178 -0.00249 -0.00007
O15 4 0.473562 0.613594 0.457249 11.00000 0.02054 0.01638 =
0.01827 -0.00237 -0.00042 0.00344
O23 4 0.376945 0.365645 0.422700 11.00000 0.02225 0.01940 =
0.02022 -0.00234 -0.00086 -0.00449
O25 4 0.350276 0.600603 0.423304 11.00000 0.02098 0.02392 =
0.02320 -0.00398 -0.00575 0.00690
O26 4 0.357723 0.480413 0.387001 11.00000 0.02367 0.02791 =
0.02360 -0.00623 -0.00777 0.00140
O34 4 0.610049 0.389855 0.417003 11.00000 0.01914 0.02023 =
0.02887 0.00471 0.00662 0.00817
O36 4 0.487031 0.380849 0.383834 11.00000 0.03010 0.02405 =
0.02318 -0.00682 0.00053 0.00380
O45 4 0.584655 0.625694 0.417509 11.00000 0.02469 0.01883 =
0.02989 0.00185 0.00200 0.00014
O46 4 0.585914 0.510847 0.381667 11.00000 0.03396 0.03482 =
0.01356 -0.00173 0.00317 -0.00259
O56 4 0.456735 0.609675 0.384673 11.00000 0.03231 0.02418 =
0.01565 0.00071 -0.00330 0.00476
N1 3 0.765894 0.795749 0.407621 11.00000 0.02281 0.01721 =
0.01826 0.00086 0.00554 -0.00112
C111 1 0.738930 0.844329 0.383402 11.00000 0.02765 0.02246 =
0.01850 0.00471 0.00578 -0.00170
AFIX 23
H11A 2 0.783582 0.841262 0.370107 11.00000 -1.20000
H11B 2 0.732717 0.903058 0.388476 11.00000 -1.20000
AFIX 0
C112 1 0.658718 0.815878 0.370545 11.00000 0.02835 0.03101 =
0.03014 0.00517 0.00122 -0.00158
AFIX 23
H11C 2 0.663315 0.756908 0.365581 11.00000 -1.20000
H11D 2 0.612584 0.821557 0.383223 11.00000 -1.20000
AFIX 0
C113 1 0.641003 0.867484 0.346128 11.00000 0.02780 0.03155 =
0.02648 0.00358 -0.00087 0.00103
AFIX 23
H11E 2 0.636682 0.926277 0.351325 11.00000 -1.20000
H11F 2 0.688064 0.862297 0.333779 11.00000 -1.20000
AFIX 0
C114 1 0.562324 0.842400 0.331996 11.00000 0.03500 0.06004 =
0.03115 0.00737 -0.00401 -0.00759
AFIX 137
H11G 2 0.565564 0.783918 0.327107 11.00000 -1.50000
H11H 2 0.555681 0.876011 0.316076 11.00000 -1.50000
H11I 2 0.514897 0.851065 0.343676 11.00000 -1.50000
AFIX 0
C121 1 0.697417 0.794879 0.428206 11.00000 0.02330 0.02295 =
0.01972 0.00465 0.00567 0.00374
AFIX 23
H12A 2 0.646697 0.772261 0.420033 11.00000 -1.20000
H12B 2 0.713692 0.757079 0.442636 11.00000 -1.20000
AFIX 0
C122 1 0.677619 0.878432 0.439884 11.00000 0.03707 0.03063 =
0.03196 0.00421 0.01445 0.00334
AFIX 23
H12C 2 0.668334 0.918668 0.425494 11.00000 -1.20000
H12D 2 0.725216 0.897852 0.450453 11.00000 -1.20000
AFIX 0
C123 1 0.601606 0.874578 0.457177 11.00000 0.03556 0.04653 =
0.03360 0.00176 0.01445 0.00474
AFIX 23
H12E 2 0.553047 0.860789 0.446163 11.00000 -1.20000
H12F 2 0.608623 0.829901 0.470310 11.00000 -1.20000
AFIX 0
C124 1 0.585581 0.954877 0.471377 11.00000 0.06946 0.06207 =
0.06158 -0.01233 0.03326 0.01576
AFIX 137
H12G 2 0.635318 0.971430 0.481039 11.00000 -1.50000
H12H 2 0.539751 0.947594 0.483779 11.00000 -1.50000
H12I 2 0.571264 0.997768 0.458536 11.00000 -1.50000
AFIX 0
C131 1 0.842989 0.838554 0.418170 11.00000 0.02628 0.02555 =
0.01504 -0.00104 0.00270 -0.00174
AFIX 23
H13A 2 0.885465 0.838658 0.404135 11.00000 -1.20000
H13B 2 0.829040 0.896838 0.422067 11.00000 -1.20000
AFIX 0
C132 1 0.880109 0.800207 0.442707 11.00000 0.02667 0.03757 =
0.02686 0.00510 0.00102 -0.00028
AFIX 23
H13C 2 0.835604 0.787420 0.455451 11.00000 -1.20000
H13D 2 0.908023 0.747815 0.438011 11.00000 -1.20000
AFIX 0
C133 1 0.941426 0.858105 0.455232 11.00000 0.04065 0.06024 =
0.04259 0.00504 -0.01274 -0.00799
AFIX 23
H13E 2 0.913049 0.909899 0.460305 11.00000 -1.20000
H13F 2 0.984927 0.872133 0.442270 11.00000 -1.20000
AFIX 0
C134 1 0.981299 0.819581 0.479602 11.00000 0.05188 0.08842 =
0.03195 0.00586 -0.01732 -0.00578
AFIX 137
H13G 2 0.938137 0.802864 0.492050 11.00000 -1.50000
H13H 2 1.017741 0.860116 0.488008 11.00000 -1.50000
H13I 2 1.013590 0.771056 0.474378 11.00000 -1.50000
AFIX 0
C141 1 0.783352 0.706152 0.400962 11.00000 0.02647 0.01704 =
0.02702 0.00300 0.00402 -0.00064
AFIX 23
H14A 2 0.731196 0.680239 0.395002 11.00000 -1.20000
H14B 2 0.800723 0.677508 0.417282 11.00000 -1.20000
AFIX 0
C142 1 0.848807 0.691503 0.380002 11.00000 0.02777 0.02332 =
0.02582 0.00035 0.00307 0.00222
AFIX 23
H14C 2 0.901567 0.717182 0.385506 11.00000 -1.20000
H14D 2 0.831349 0.717203 0.363200 11.00000 -1.20000
AFIX 0
C143 1 0.860971 0.598594 0.376099 11.00000 0.03843 0.02360 =
0.03629 0.00307 0.01347 0.00069
AFIX 23
H14E 2 0.876027 0.573507 0.393229 11.00000 -1.20000
H14F 2 0.807850 0.573989 0.370451 11.00000 -1.20000
AFIX 0
C144 1 0.926418 0.576764 0.356126 11.00000 0.04469 0.02873 =
0.03675 -0.00348 0.01156 0.00325
AFIX 137
H14G 2 0.913326 0.603139 0.339253 11.00000 -1.50000
H14H 2 0.928142 0.516684 0.353803 11.00000 -1.50000
H14I 2 0.980313 0.596286 0.362342 11.00000 -1.50000
AFIX 0
N2 3 0.218175 0.188296 0.406618 11.00000 0.03461 0.02634 =
0.02226 -0.00503 -0.01047 0.00038
C211 1 0.249740 0.142249 0.382511 11.00000 0.03727 0.02488 =
0.02537 -0.00394 -0.00997 -0.00097
AFIX 23
H21A 2 0.209708 0.150061 0.367975 11.00000 -1.20000
H21B 2 0.251397 0.082504 0.386652 11.00000 -1.20000
AFIX 0
C212 1 0.334795 0.168548 0.372875 11.00000 0.03621 0.04310 =
0.04056 0.00089 -0.00498 -0.01035
AFIX 23
H21C 2 0.336345 0.229445 0.371129 11.00000 -1.20000
H21D 2 0.376835 0.152269 0.386058 11.00000 -1.20000
AFIX 0
C213 1 0.355586 0.129959 0.346849 11.00000 0.04622 0.03419 =
0.04004 0.00516 0.00248 -0.00770
AFIX 23
H21E 2 0.314507 0.147895 0.333577 11.00000 -1.20000
H21F 2 0.351714 0.069133 0.348479 11.00000 -1.20000
AFIX 0
C214 1 0.440909 0.152610 0.337357 11.00000 0.04896 0.07627 =
0.04267 0.00461 0.00300 -0.01113
AFIX 137
H21G 2 0.448552 0.212514 0.338737 11.00000 -1.50000
H21H 2 0.447328 0.135566 0.318941 11.00000 -1.50000
H21I 2 0.482299 0.124470 0.348222 11.00000 -1.50000
AFIX 0
C221 1 0.280650 0.180298 0.428861 11.00000 0.03932 0.03332 =
0.02790 -0.00595 -0.01591 -0.00020
AFIX 23
H22A 2 0.334628 0.201257 0.422579 11.00000 -1.20000
H22B 2 0.262798 0.216000 0.443641 11.00000 -1.20000
AFIX 0
C222 1 0.292447 0.093229 0.439153 11.00000 0.03918 0.03331 =
0.03835 -0.00339 -0.01216 -0.00092
AFIX 23
H22C 2 0.239559 0.073404 0.446637 11.00000 -1.20000
H22D 2 0.307051 0.056541 0.424257 11.00000 -1.20000
AFIX 0
C223 1 0.358448 0.087056 0.459872 11.00000 0.05789 0.04864 =
0.04267 -0.00559 -0.02406 0.00438
AFIX 23
H22E 2 0.347301 0.127815 0.473975 11.00000 -1.20000
H22F 2 0.412710 0.100461 0.451951 11.00000 -1.20000
AFIX 0
C224 1 0.361593 0.000414 0.471768 11.00000 0.07440 0.06378 =
0.03770 -0.00427 -0.02159 0.01804
AFIX 137
H22G 2 0.306024 -0.016049 0.477353 11.00000 -1.50000
H22H 2 0.398673 0.000380 0.487033 11.00000 -1.50000
H22I 2 0.382101 -0.038669 0.458550 11.00000 -1.50000
AFIX 0
C231 1 0.135821 0.149586 0.414201 11.00000 0.03404 0.03398 =
0.03101 -0.00156 -0.00854 -0.00019
AFIX 23
H23A 2 0.143727 0.089483 0.416790 11.00000 -1.20000
H23B 2 0.096283 0.157151 0.399515 11.00000 -1.20000
AFIX 0
C232 1 0.098649 0.186691 0.439369 11.00000 0.04489 0.05014 =
0.04731 -0.00691 -0.00097 0.00988
AFIX 23
H23C 2 0.142551 0.191047 0.452879 11.00000 -1.20000
H23D 2 0.078887 0.243276 0.435483 11.00000 -1.20000
AFIX 0
C233 1 0.029246 0.137887 0.450300 11.00000 0.07478 0.07977 =
0.05862 -0.02495 0.00870 -0.01675
AFIX 23
H23E 2 0.047668 0.080005 0.452579 11.00000 -1.20000
H23F 2 -0.016555 0.137848 0.437372 11.00000 -1.20000
AFIX 0
C234 1 -0.002915 0.168940 0.476129 11.00000 0.06830 0.15546 =
0.08225 -0.05307 0.03009 -0.04779
AFIX 137
H23G 2 0.041826 0.169015 0.489138 11.00000 -1.50000
H23H 2 -0.047611 0.132861 0.482232 11.00000 -1.50000
H23I 2 -0.024008 0.225268 0.473921 11.00000 -1.50000
AFIX 0
C241 1 0.208032 0.280151 0.400723 11.00000 0.03841 0.02436 =
0.02881 0.00001 -0.01196 -0.00020
AFIX 23
H24A 2 0.186930 0.307741 0.416778 11.00000 -1.20000
H24B 2 0.263222 0.303618 0.396893 11.00000 -1.20000
AFIX 0
C242 1 0.151151 0.300927 0.378087 11.00000 0.03193 0.02442 =
0.02869 -0.00260 -0.00754 0.00104
AFIX 23
H24C 2 0.094702 0.280713 0.381938 11.00000 -1.20000
H24D 2 0.170807 0.273519 0.361814 11.00000 -1.20000
AFIX 0
C243 1 0.149643 0.394261 0.374113 11.00000 0.03684 0.02634 =
0.03556 -0.00381 -0.00679 -0.00532
AFIX 23
H24E 2 0.206636 0.414036 0.370898 11.00000 -1.20000
H24F 2 0.129310 0.420959 0.390421 11.00000 -1.20000
AFIX 0
C244 1 0.094670 0.420144 0.351032 11.00000 0.04255 0.02832 =
0.03838 0.00524 -0.00301 0.00068
AFIX 137
H24G 2 0.116283 0.396316 0.334674 11.00000 -1.50000
H24H 2 0.094223 0.480525 0.349624 11.00000 -1.50000
H24I 2 0.038282 0.400173 0.354011 11.00000 -1.50000
AFIX 0
N3 3 0.299759 0.710338 0.499828 11.00000 0.02623 0.03229 =
0.01997 0.00080 0.00297 0.01224
C311 1 0.303353 0.752323 0.472707 11.00000 0.02998 0.03808 =
0.01971 -0.00288 0.00438 0.00918
AFIX 23
H31A 2 0.348509 0.793558 0.473080 11.00000 -1.20000
H31B 2 0.318566 0.709935 0.459509 11.00000 -1.20000
AFIX 0
C312 1 0.224848 0.795756 0.463103 11.00000 0.03531 0.03964 =
0.02161 0.00461 0.00304 0.00534
AFIX 23
H31C 2 0.211520 0.842590 0.474907 11.00000 -1.20000
H31D 2 0.177835 0.756642 0.463378 11.00000 -1.20000
AFIX 0
C313 1 0.238803 0.827505 0.434880 11.00000 0.04246 0.04636 =
0.01828 0.00001 0.00097 0.00086
AFIX 23
H31E 2 0.291162 0.859051 0.434226 11.00000 -1.20000
H31F 2 0.244087 0.779800 0.422790 11.00000 -1.20000
AFIX 0
C314 1 0.168578 0.882355 0.425621 11.00000 0.06325 0.04584 =
0.04573 0.00948 -0.00620 0.00223
AFIX 137
H31G 2 0.116913 0.850790 0.425681 11.00000 -1.50000
H31H 2 0.180100 0.901871 0.407715 11.00000 -1.50000
H31I 2 0.163354 0.929839 0.437485 11.00000 -1.50000
AFIX 0
C321 1 0.387963 0.714910 0.510903 11.00000 0.02450 0.02808 =
0.03548 -0.00634 -0.00267 0.01059
AFIX 23
H32A 2 0.392909 0.674236 0.525385 11.00000 -1.20000
H32B 2 0.426892 0.698018 0.496855 11.00000 -1.20000
AFIX 0
C322 1 0.414867 0.799389 0.521325 11.00000 0.03794 0.02979 =
0.03326 -0.00365 -0.00054 0.00887
AFIX 23
H32C 2 0.396551 0.843229 0.509041 11.00000 -1.20000
H32D 2 0.388938 0.809701 0.538683 11.00000 -1.20000
AFIX 0
C323 1 0.508202 0.801634 0.524021 11.00000 0.04200 0.02543 =
0.03577 0.00805 0.00380 -0.00302
AFIX 23
H32E 2 0.533371 0.801820 0.506243 11.00000 -1.20000
H32F 2 0.526928 0.751065 0.533226 11.00000 -1.20000
AFIX 0
C324 1 0.538118 0.877215 0.539209 11.00000 0.05290 0.03841 =
0.05021 0.00610 -0.00569 -0.00680
AFIX 137
H32G 2 0.513189 0.927095 0.531687 11.00000 -1.50000
H32H 2 0.598416 0.880988 0.537951 11.00000 -1.50000
H32I 2 0.521973 0.872135 0.557748 11.00000 -1.50000
AFIX 0
C331 1 0.238890 0.754386 0.517618 11.00000 0.03150 0.03238 =
0.01792 0.00120 0.00042 0.01234
AFIX 23
H33A 2 0.183887 0.753285 0.509094 11.00000 -1.20000
H33B 2 0.255857 0.812961 0.519112 11.00000 -1.20000
AFIX 0
C332 1 0.230547 0.718862 0.545238 11.00000 0.03619 0.03947 =
0.02123 0.00438 0.00217 0.00758
AFIX 23
H33C 2 0.285962 0.710492 0.553050 11.00000 -1.20000
H33D 2 0.202205 0.664714 0.544488 11.00000 -1.20000
AFIX 0
C333 1 0.180364 0.779339 0.562281 11.00000 0.03457 0.04441 =
0.01774 -0.00358 0.00036 0.00402
AFIX 23
H33E 2 0.182048 0.760330 0.580813 11.00000 -1.20000
H33F 2 0.206953 0.834372 0.561547 11.00000 -1.20000
AFIX 0
C334 1 0.090111 0.788033 0.553812 11.00000 0.03215 0.05391 =
0.05171 -0.00956 0.00511 0.00468
AFIX 137
H33G 2 0.087703 0.808674 0.535675 11.00000 -1.50000
H33H 2 0.061904 0.826958 0.565552 11.00000 -1.50000
H33I 2 0.062888 0.734040 0.554782 11.00000 -1.50000
AFIX 0
C341 1 0.279951 0.619305 0.497580 11.00000 0.02472 0.02821 =
0.03126 -0.00132 0.00091 0.01011
AFIX 23
H34A 2 0.281509 0.595008 0.515474 11.00000 -1.20000
H34B 2 0.324212 0.592592 0.487156 11.00000 -1.20000
AFIX 0
C342 1 0.197558 0.597596 0.485130 11.00000 0.03121 0.03915 =
0.02538 0.00067 0.00180 0.01240
AFIX 23
H34C 2 0.197888 0.613015 0.466254 11.00000 -1.20000
H34D 2 0.152648 0.628567 0.493950 11.00000 -1.20000
AFIX 0
C343 1 0.182794 0.505160 0.487957 11.00000 0.02954 0.04523 =
0.03681 0.00313 0.00604 -0.00225
AFIX 23
H34E 2 0.230715 0.475138 0.480524 11.00000 -1.20000
H34F 2 0.179267 0.491291 0.506922 11.00000 -1.20000
AFIX 0
C344 1 0.104704 0.475566 0.474318 11.00000 0.03132 0.05886 =
0.05474 0.00076 0.01050 -0.00561
AFIX 137
H34G 2 0.057074 0.506085 0.481201 11.00000 -1.50000
H34H 2 0.097170 0.416403 0.477642 11.00000 -1.50000
H34I 2 0.109474 0.485114 0.455311 11.00000 -1.50000
AFIX 0
N4 3 0.754714 0.754714 0.500000 10.50000 0.06393 0.06393 =
0.03482 -0.00118 0.00118 -0.03611
C41 1 0.705693 0.705693 0.500000 10.50000 0.04029 0.04029 =
0.02499 -0.00292 0.00292 -0.00707
C42 1 0.640774 0.640774 0.500000 10.50000 0.03992 0.03992 =
0.06527 -0.01180 0.01180 -0.01185
N5 3 0.222800 0.222800 0.500000 10.50000 0.10682 0.10682 =
0.04650 -0.01559 0.01559 -0.06222
C51 1 0.271867 0.271867 0.500000 10.50000 0.04783 0.04783 =
0.03428 -0.00147 0.00147 -0.01104
C52 1 0.334930 0.334930 0.500000 10.50000 0.04019 0.04019 =
0.11791 0.02673 -0.02673 -0.01704
HKLF 4

REM rje260 in P4(1)2(1)2
REM R1 = 0.0400 for 14323 Fo > 4sig(Fo) and 0.0484 for all 15970 data
REM 724 parameters refined using 0 restraints

END

WGHT 0.0308 27.8009
REM Highest difference peak 0.892, deepest hole -1.333, 1-sigma level 0.117
Q1 1 0.5288 0.5141 0.3842 11.00000 0.05 0.89
Q2 1 0.5379 0.4986 0.3873 11.00000 0.05 0.87
Q3 1 0.6611 0.5167 0.4324 11.00000 0.05 0.84
Q4 1 0.5741 0.5149 0.4188 11.00000 0.05 0.76
Q5 1 0.4560 0.4399 0.3774 11.00000 0.05 0.73
Q6 1 0.2810 0.4975 0.4233 11.00000 0.05 0.73
Q7 1 0.3650 0.4877 0.4092 11.00000 0.05 0.72
Q8 1 0.5936 0.4522 0.4208 11.00000 0.05 0.72
Q9 1 0.4199 0.6455 0.4225 11.00000 0.05 0.72
Q10 1 0.4997 0.3947 0.4328 11.00000 0.05 0.70
;