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_7017609
_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         '3 C16 H36 N +,C H3 Mo5 O19 Ti 3-'
_chemical_formula_sum            'C49 H111 Mo5 N3 O19 Ti'
_chemical_formula_weight         1574.01
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 113.343(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.4619(7)
_cell_length_b                   18.6123(7)
_cell_length_c                   27.2737(9)
_cell_measurement_reflns_used    42495
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.69
_cell_measurement_theta_min      2.30
_cell_volume                     13731.5(8)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            48667
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6480
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.42
_refine_diff_density_max         2.417
_refine_diff_density_min         -2.481
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         12093
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.266
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+192.2561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1389
_reflns_number_gt                11036
_reflns_number_total             12093
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1dt11256b.txt
_cod_data_source_block           rje253_salt_of_3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7017609
_computing_special_details
;
TITL rje253 in C2/c
CELL 0.71073 29.4619 18.6123 27.2737 90.000 113.343 90.000
ZERR 8.00 0.0007 0.0007 0.0009 0.000 0.002 0.000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC C H N O TI MO
UNIT 392 888 24 152 8 40
TEMP -113
SIZE 0.42 0.44 0.62

OMIT -3 50
L.S. 8
ACTA
BOND $H
FMAP 2
PLAN 10

EXYZ TI1 MO1
EADP TI1 MO1
EXYZ TI2 MO4
EADP TI2 MO4
CONN $TI $MO 6
SIMU C3 > C14X C23 > C26X C35 > C42X
DELU C3 > C14X C23 > C26X C35 > C42X

REM EXTI 0.000016 INSIGNIFICANT
WGHT 0.024000 192.256104
FVAR 0.03070 0.65994 0.68155 0.55355 0.56910 0.59109 0.67588
PART 1
TI1 5 0.237798 0.363468 0.521531 10.50000 0.02260 0.02549 =
0.02214 -0.00714 0.00909 0.00034
PART 2
MO1 6 0.237798 0.363468 0.521531 10.50000 0.02260 0.02549 =
0.02214 -0.00714 0.00909 0.00034
PART 0
MO2 6 0.335276 0.267821 0.538190 11.00000 0.01737 0.03347 =
0.02582 -0.00689 0.00841 -0.00100
MO3 6 0.252335 0.209578 0.582194 11.00000 0.02629 0.03321 =
0.02080 -0.00009 0.01154 0.00201
PART 1
TI2 5 0.082155 0.250354 0.777240 10.50000 0.02443 0.05571 =
0.03912 0.00091 0.01340 0.00787
PART 2
MO4 6 0.082155 0.250354 0.777240 10.50000 0.02443 0.05571 =
0.03912 0.00091 0.01340 0.00787
PART 0
MO5 6 -0.005077 0.340407 0.687669 11.00000 0.04916 0.03121 =
0.04057 0.01224 0.02690 0.00633
MO6 6 -0.005598 0.163604 0.687259 11.00000 0.09406 0.03302 =
0.06285 -0.02043 0.05965 -0.02172
O1 4 0.257874 0.179546 0.642911 11.00000 0.04066 0.03689 =
0.02398 -0.00111 0.01647 0.00055
O2 4 0.184694 0.202553 0.538865 11.00000 0.02502 0.03477 =
0.02124 -0.00798 0.01076 -0.00208
O3 4 0.323996 0.232430 0.596859 11.00000 0.02137 0.03060 =
0.01831 -0.00467 0.00585 0.00209
O4 4 0.397190 0.281738 0.562163 11.00000 0.02332 0.04514 =
0.03146 -0.00887 0.01156 -0.00307
O5 4 0.309653 0.358177 0.545780 11.00000 0.02397 0.02828 =
0.02720 -0.00629 0.00918 -0.00323
O6 4 0.235638 0.375577 0.450390 11.00000 0.02842 0.02675 =
0.02414 -0.00268 0.00980 0.00290
O7 4 0.228417 0.449485 0.541132 11.00000 0.03558 0.02617 =
0.04353 -0.01103 0.01182 0.00221
O8 4 0.171448 0.327598 0.489988 11.00000 0.02045 0.03151 =
0.02863 -0.00368 0.00839 0.00190
O9 4 0.245558 0.310700 0.586601 11.00000 0.03177 0.02950 =
0.02947 -0.00895 0.01710 0.00353
O10 4 0.250000 0.250000 0.500000 10.50000 0.02093 0.02877 =
0.02301 -0.00219 0.01125 0.00046
O12 4 0.063470 0.324023 0.722204 11.00000 0.04354 0.03330 =
0.06483 -0.00217 0.03634 -0.00378
O15 4 0.000000 0.396884 0.750000 10.50000 0.06238 0.02092 =
0.09395 0.00000 0.05495 0.00000
O16 4 -0.008706 0.251121 0.648871 11.00000 0.05838 0.06422 =
0.03487 -0.00487 0.02605 -0.01201
O17 4 -0.071755 0.179287 0.677842 11.00000 0.07015 0.08948 =
0.06440 -0.04718 0.04013 -0.04156
O19 4 0.000000 0.107778 0.750000 10.50000 0.11432 0.02324 =
0.11324 0.00000 0.09253 0.00000
O20 4 0.062894 0.180134 0.720969 11.00000 0.06880 0.03379 =
0.07239 -0.00048 0.04891 0.00873
O21 4 0.000000 0.252006 0.750000 10.50000 0.04351 0.02157 =
0.03263 0.00000 0.02202 0.00000
PART 1
C1 1 0.205978 0.475203 0.578212 10.50000 0.04445 0.06407 =
0.07356 -0.02685 0.01914 0.00419
AFIX 33
H1A 2 0.207255 0.527798 0.579880 10.50000 -1.50000
H1B 2 0.224433 0.455412 0.613926 10.50000 -1.50000
H1C 2 0.171484 0.459319 0.565225 10.50000 -1.50000
AFIX 0
C2 1 0.197543 0.244616 0.839767 10.50000 0.04197 0.06859 =
0.11309 -0.02518 0.01153 0.00335
AFIX 33
H2A 2 0.220314 0.252532 0.822093 10.50000 -1.50000
H2B 2 0.202626 0.196294 0.855293 10.50000 -1.50000
H2C 2 0.203837 0.280351 0.868102 10.50000 -1.50000
AFIX 0
PART 0
SAME N1 C3 C4 C5 C6
SAME N1 C3 C4 C5 C6X
SAME N1 C7 C8 C9 C10
SAME N1 C7 C8 C9 C10X
SAME N1 C11 C12 C13 C14
SAME N1 C11 C12 C13 C14X
N1 3 -0.066121 0.728209 0.438964 11.00000 0.04911 0.06334 =
0.04923 -0.00006 0.03773 0.00537
C3 1 -0.079241 0.803732 0.449814 11.00000 0.04493 0.06055 =
0.05452 -0.00720 0.03348 0.00108
AFIX 23
H3A 2 -0.115198 0.805805 0.441041 11.00000 -1.20000
H3B 2 -0.061871 0.813869 0.488441 11.00000 -1.20000
AFIX 0
C4 1 -0.066343 0.861660 0.418951 11.00000 0.05995 0.06485 =
0.09334 0.00239 0.04471 -0.00933
AFIX 23
H4A 2 -0.029953 0.866177 0.432198 11.00000 -1.20000
H4B 2 -0.079094 0.848236 0.380725 11.00000 -1.20000
AFIX 0
C5 1 -0.088033 0.932152 0.424763 11.00000 0.08716 0.06236 =
0.14895 0.00014 0.06009 -0.00981
PART 1
AFIX 23
H5A 2 -0.080830 0.967151 0.401463 21.00000 -1.20000
H5B 2 -0.124383 0.926191 0.410336 21.00000 -1.20000
AFIX 23
PART 2
H5C 2 -0.123529 0.931854 0.400729 -21.00000 -1.20000
H5D 2 -0.086025 0.935530 0.461793 -21.00000 -1.20000
AFIX 0
PART 1
C6 1 -0.073706 0.962746 0.474414 21.00000 0.20496 0.06743 =
0.14126 -0.00455 0.05030 0.03796
AFIX 33
H6A 2 -0.092163 1.007407 0.471717 21.00000 -1.50000
H6B 2 -0.038229 0.973297 0.488503 21.00000 -1.50000
H6C 2 -0.080493 0.929381 0.498478 21.00000 -1.50000
AFIX 0
PART 2
C6X 1 -0.066945 0.993935 0.414155 -21.00000 0.09896
AFIX 33
H6X1 2 -0.084445 1.036276 0.419113 -21.00000 -1.50000
H6X2 2 -0.069466 0.992530 0.377244 -21.00000 -1.50000
H6X3 2 -0.032064 0.996533 0.438634 -21.00000 -1.50000
AFIX 0
PART 0
C7 1 -0.011151 0.722122 0.451641 11.00000 0.05008 0.09214 =
0.05439 0.00357 0.03900 0.00914
AFIX 23
H7A 2 -0.004490 0.673082 0.442085 11.00000 -1.20000
H7B 2 -0.002998 0.756188 0.428452 11.00000 -1.20000
AFIX 0
C8 1 0.023142 0.736432 0.508654 11.00000 0.06133 0.11908 =
0.05540 -0.00243 0.03464 0.01411
AFIX 23
H8A 2 0.016388 0.784862 0.519196 11.00000 -1.20000
H8B 2 0.016856 0.700893 0.532241 11.00000 -1.20000
AFIX 0
C9 1 0.076120 0.731986 0.515894 11.00000 0.05854 0.12547 =
0.09832 -0.00646 0.02863 0.00879
PART 1
AFIX 23
H9A 2 0.082405 0.682773 0.506302 31.00000 -1.20000
H9B 2 0.081077 0.765344 0.490173 31.00000 -1.20000
AFIX 23
PART 2
H9C 2 0.096808 0.726982 0.554496 -31.00000 -1.20000
H9D 2 0.080578 0.687881 0.497999 -31.00000 -1.20000
AFIX 0
PART 1
C10 1 0.111774 0.747733 0.567077 31.00000 0.07248 0.21530 =
0.08807 -0.01936 0.01630 0.00766
AFIX 33
H10A 2 0.144908 0.741943 0.567276 31.00000 -1.50000
H10B 2 0.107776 0.714875 0.593162 31.00000 -1.50000
H10C 2 0.107494 0.797359 0.576477 31.00000 -1.50000
AFIX 0
PART 2
C10X 1 0.093490 0.790280 0.496309 -31.00000 0.07097 0.16119 =
0.10787 0.00101 0.02816 -0.02176
AFIX 33
H10D 2 0.128318 0.782559 0.502840 -31.00000 -1.50000
H10E 2 0.090315 0.834244 0.514470 -31.00000 -1.50000
H10F 2 0.074056 0.795040 0.457840 -31.00000 -1.50000
AFIX 0
PART 0
C11 1 -0.093513 0.707798 0.380635 11.00000 0.05330 0.06893 =
0.05209 -0.00368 0.03606 -0.00096
AFIX 23
H11A 2 -0.080593 0.737338 0.358834 11.00000 -1.20000
H11B 2 -0.086213 0.656904 0.376083 11.00000 -1.20000
AFIX 0
C12 1 -0.148957 0.717270 0.359360 11.00000 0.05246 0.09638 =
0.06199 -0.01789 0.03501 -0.01744
AFIX 23
H12A 2 -0.161247 0.698777 0.385876 11.00000 -1.20000
H12B 2 -0.157077 0.769063 0.354027 11.00000 -1.20000
AFIX 0
C13 1 -0.174246 0.678392 0.307616 11.00000 0.08156 0.14972 =
0.07015 -0.03294 0.01916 -0.01786
PART 1
AFIX 23
H13A 2 -0.161752 0.698144 0.281621 41.00000 -1.20000
H13B 2 -0.164122 0.627321 0.313384 41.00000 -1.20000
AFIX 23
PART 2
H13C 2 -0.200137 0.709479 0.282108 -41.00000 -1.20000
H13D 2 -0.149995 0.666729 0.292002 -41.00000 -1.20000
AFIX 0
PART 1
C14 1 -0.224659 0.680774 0.284850 41.00000 0.07192 0.10284 =
0.06553 -0.03386 0.02438 -0.00007
AFIX 33
H14A 2 -0.236653 0.654183 0.251075 41.00000 -1.50000
H14B 2 -0.235573 0.730883 0.278035 41.00000 -1.50000
H14C 2 -0.237950 0.658966 0.309091 41.00000 -1.50000
AFIX 0
PART 2
C14X 1 -0.196164 0.613503 0.316453 -41.00000 0.07959 0.15371 =
0.10174 -0.07941 0.05335 -0.04592
AFIX 33
H14D 2 -0.212269 0.587864 0.282545 -41.00000 -1.50000
H14E 2 -0.220757 0.625349 0.331043 -41.00000 -1.50000
H14F 2 -0.170444 0.582959 0.341810 -41.00000 -1.50000
AFIX 0
PART 0
C15 1 -0.080761 0.678376 0.474661 11.00000 0.07275 0.05722 =
0.05071 -0.00561 0.04847 0.00705
AFIX 23
H15A 2 -0.063747 0.694638 0.512104 11.00000 -1.20000
H15B 2 -0.116763 0.683191 0.464886 11.00000 -1.20000
AFIX 0
C16 1 -0.069059 0.600242 0.471770 11.00000 0.09900 0.06623 =
0.08459 0.01436 0.06931 0.01581
AFIX 23
H16A 2 -0.091226 0.580760 0.436641 11.00000 -1.20000
H16B 2 -0.034627 0.595682 0.474605 11.00000 -1.20000
AFIX 0
C17 1 -0.074970 0.556747 0.515197 11.00000 0.15824 0.06307 =
0.13300 0.02892 0.11506 0.03440
AFIX 23
H17A 2 -0.053271 0.577675 0.549989 11.00000 -1.20000
H17B 2 -0.109494 0.562027 0.511914 11.00000 -1.20000
AFIX 0
C18 1 -0.063976 0.480378 0.516228 11.00000 0.12819 0.12036 =
0.10610 0.04703 0.07479 0.04652
AFIX 33
H18A 2 -0.069299 0.457487 0.545875 11.00000 -1.50000
H18B 2 -0.029454 0.473932 0.521033 11.00000 -1.50000
H18C 2 -0.085774 0.458300 0.482470 11.00000 -1.50000
AFIX 0
O13 4 -0.011259 0.401844 0.639818 11.00000 0.09056 0.06732 =
0.08423 0.04400 0.05543 0.02410
O11 4 0.147116 0.251516 0.801094 11.00000 0.03499 0.15232 =
0.07419 0.00528 0.02311 0.01970
SAME N2 C23 C24 C25 C26X
SAME N2 C23 C24 C25 C26
N2 3 -0.127627 -0.026751 0.671206 11.00000 0.05112 0.03182 =
0.02669 -0.00747 0.01087 -0.00963
C19 1 -0.130473 0.026338 0.712346 11.00000 0.06353 0.04228 =
0.03532 -0.01352 0.02182 -0.01435
AFIX 23
H19A 2 -0.111075 0.006946 0.748440 11.00000 -1.20000
H19B 2 -0.114666 0.071858 0.708777 11.00000 -1.20000
AFIX 0
C20 1 -0.182178 0.042810 0.708068 11.00000 0.07468 0.06375 =
0.05838 -0.02278 0.03462 -0.01119
AFIX 23
H20A 2 -0.199713 -0.002713 0.707637 11.00000 -1.20000
H20B 2 -0.200625 0.068348 0.674112 11.00000 -1.20000
AFIX 0
C21 1 -0.180975 0.089141 0.754824 11.00000 0.08887 0.06832 =
0.07576 -0.02720 0.05809 -0.02478
AFIX 23
H21A 2 -0.164996 0.061968 0.788544 11.00000 -1.20000
H21B 2 -0.161037 0.132790 0.757091 11.00000 -1.20000
AFIX 0
C22 1 -0.232083 0.110589 0.748284 11.00000 0.12643 0.11243 =
0.11045 -0.03417 0.08501 -0.00514
AFIX 33
H22A 2 -0.230234 0.140371 0.778651 11.00000 -1.50000
H22B 2 -0.251645 0.067436 0.746799 11.00000 -1.50000
H22C 2 -0.247793 0.137987 0.715126 11.00000 -1.50000
AFIX 0
C23 1 -0.157558 -0.001471 0.614606 11.00000 0.04630 0.03980 =
0.02960 -0.00917 0.01122 -0.00577
AFIX 23
H23A 2 -0.155017 -0.038293 0.589621 11.00000 -1.20000
H23B 2 -0.192713 0.001292 0.609475 11.00000 -1.20000
AFIX 0
C24 1 -0.142821 0.070254 0.599357 11.00000 0.06010 0.04658 =
0.04420 0.00313 0.00926 -0.01485
AFIX 23
H24A 2 -0.107774 0.068743 0.603955 11.00000 -1.20000
H24B 2 -0.146456 0.108403 0.622838 11.00000 -1.20000
AFIX 0
C25 1 -0.175480 0.086795 0.541692 11.00000 0.09776 0.09106 =
0.06287 0.02988 -0.00656 -0.02756
PART 1
AFIX 23
H25A 2 -0.210381 0.082165 0.537214 51.00000 -1.20000
H25B 2 -0.170097 0.137575 0.534603 51.00000 -1.20000
AFIX 23
PART 2
H25C 2 -0.180730 0.041826 0.520772 -51.00000 -1.20000
H25D 2 -0.208122 0.102840 0.539950 -51.00000 -1.20000
AFIX 0
PART 1
C26 1 -0.168450 0.043272 0.502163 51.00000 0.20891 0.10298 =
0.04016 0.01811 0.02639 -0.06077
AFIX 33
H26A 2 -0.191604 0.058298 0.466589 51.00000 -1.50000
H26B 2 -0.174451 -0.007198 0.507928 51.00000 -1.50000
H26C 2 -0.134471 0.048841 0.504838 51.00000 -1.50000
AFIX 0
PART 2
C26X 1 -0.156301 0.141619 0.516216 -51.00000 0.15765 0.08859 =
0.07657 0.03079 0.03343 -0.02494
AFIX 33
H26D 2 -0.179828 0.148782 0.479262 -51.00000 -1.50000
H26E 2 -0.124487 0.125746 0.516485 -51.00000 -1.50000
H26F 2 -0.151782 0.186934 0.535892 -51.00000 -1.50000
AFIX 0
PART 0
C27 1 -0.073329 -0.033501 0.681191 11.00000 0.03832 0.04338 =
0.02998 -0.00556 0.00504 -0.00601
AFIX 23
H27A 2 -0.059900 0.015456 0.682040 11.00000 -1.20000
H27B 2 -0.055780 -0.054773 0.717055 11.00000 -1.20000
AFIX 0
C28 1 -0.061178 -0.077549 0.641586 11.00000 0.04438 0.05279 =
0.04012 -0.01434 0.00530 -0.00315
AFIX 23
H28A 2 -0.073276 -0.052425 0.606749 11.00000 -1.20000
H28B 2 -0.078188 -0.124549 0.636356 11.00000 -1.20000
AFIX 0
C29 1 -0.005789 -0.089501 0.661074 11.00000 0.04419 0.05560 =
0.05648 -0.01382 0.00834 -0.00222
AFIX 23
H29A 2 0.011203 -0.042436 0.669762 11.00000 -1.20000
H29B 2 0.005537 -0.118326 0.694285 11.00000 -1.20000
AFIX 0
C30 1 0.008888 -0.127670 0.620335 11.00000 0.04808 0.12864 =
0.08318 -0.02944 0.01629 0.01310
AFIX 33
H30A 2 0.044791 -0.134679 0.635190 11.00000 -1.50000
H30B 2 -0.001011 -0.098494 0.587843 11.00000 -1.50000
H30C 2 -0.007645 -0.174464 0.611685 11.00000 -1.50000
AFIX 0
C31 1 -0.148713 -0.099473 0.676608 11.00000 0.05918 0.02933 =
0.03802 -0.01328 0.01522 -0.01930
AFIX 23
H31A 2 -0.184447 -0.093078 0.667829 11.00000 -1.20000
H31B 2 -0.145718 -0.131789 0.649212 11.00000 -1.20000
AFIX 0
C32 1 -0.126371 -0.137399 0.729783 11.00000 0.07068 0.03910 =
0.02848 -0.00495 0.01625 -0.01459
AFIX 23
H32A 2 -0.090860 -0.146509 0.738782 11.00000 -1.20000
H32B 2 -0.129094 -0.106328 0.757956 11.00000 -1.20000
AFIX 0
C33 1 -0.152333 -0.207454 0.728082 11.00000 0.09825 0.04606 =
0.06205 -0.00205 0.03092 -0.02447
AFIX 23
H33A 2 -0.188014 -0.197774 0.717464 11.00000 -1.20000
H33B 2 -0.148845 -0.238256 0.700185 11.00000 -1.20000
AFIX 0
C34 1 -0.133577 -0.248059 0.779825 11.00000 0.11410 0.04423 =
0.06499 0.00649 0.03372 -0.01093
AFIX 33
H34A 2 -0.152835 -0.292255 0.775661 11.00000 -1.50000
H34B 2 -0.136959 -0.218208 0.807786 11.00000 -1.50000
H34C 2 -0.098684 -0.260241 0.789832 11.00000 -1.50000
AFIX 0
O14 4 -0.071690 0.322710 0.677295 11.00000 0.03540 0.10571 =
0.05647 0.04184 0.02015 0.01853
O18 4 -0.010696 0.099489 0.641452 11.00000 0.12932 0.07560 =
0.10921 -0.05697 0.09609 -0.05007
SAME N3 C39 C40 C41 C42X
SAME N3 C39 C40 C41 C42
SAME N3 C35 C36 C37 C38
SAME N3 C35 C36 C37 C38X
N3 3 0.147753 0.496402 0.336725 11.00000 0.04453 0.03838 =
0.05379 0.01457 0.02211 0.01670
C35 1 0.127664 0.426121 0.348766 11.00000 0.04836 0.05055 =
0.05975 0.02339 0.02180 0.01464
AFIX 23
H35A 2 0.135547 0.387026 0.328803 11.00000 -1.20000
H35B 2 0.145161 0.415519 0.387305 11.00000 -1.20000
AFIX 0
C36 1 0.072659 0.425094 0.335038 11.00000 0.04786 0.07617 =
0.07331 0.03177 0.02702 0.01575
AFIX 23
H36A 2 0.054525 0.437306 0.296868 11.00000 -1.20000
H36B 2 0.064393 0.461497 0.356664 11.00000 -1.20000
AFIX 0
C37 1 0.056987 0.351149 0.346058 11.00000 0.04763 0.09608 =
0.11168 0.03843 0.02319 0.00283
PART 1
AFIX 23
H37A 2 0.067305 0.315578 0.325503 61.00000 -1.20000
H37B 2 0.075615 0.340343 0.384394 61.00000 -1.20000
AFIX 23
PART 2
H37C 2 0.079090 0.337004 0.382792 -61.00000 -1.20000
H37D 2 0.023129 0.354983 0.345098 -61.00000 -1.20000
AFIX 0
PART 1
C38 1 0.006194 0.340329 0.334077 61.00000 0.05043 0.15848 =
0.21817 0.10237 0.03004 -0.00134
AFIX 33
H38A 2 0.000964 0.290957 0.343197 61.00000 -1.50000
H38B 2 -0.012919 0.348497 0.295884 61.00000 -1.50000
H38C 2 -0.004668 0.374033 0.354844 61.00000 -1.50000
AFIX 0
PART 2
C38X 1 0.057294 0.295415 0.310999 -61.00000 0.07132
AFIX 33
H38D 2 0.047322 0.250246 0.322324 -61.00000 -1.50000
H38E 2 0.090660 0.290269 0.311727 -61.00000 -1.50000
H38F 2 0.034115 0.307083 0.274636 -61.00000 -1.50000
AFIX 0
PART 0
C39 1 0.141653 0.556036 0.371505 11.00000 0.06558 0.05011 =
0.07531 0.00206 0.03857 0.02114
AFIX 23
H39A 2 0.151272 0.601827 0.359808 11.00000 -1.20000
H39B 2 0.106105 0.559640 0.364561 11.00000 -1.20000
AFIX 0
C40 1 0.170280 0.549349 0.431111 11.00000 0.09361 0.08023 =
0.07197 0.00122 0.04385 0.02239
AFIX 23
H40A 2 0.205696 0.541309 0.438945 11.00000 -1.20000
H40B 2 0.157970 0.507548 0.444678 11.00000 -1.20000
AFIX 0
C41 1 0.164392 0.618168 0.459386 11.00000 0.13876 0.13638 =
0.08825 -0.03325 0.05862 0.03841
PART 1
AFIX 23
H41A 2 0.128671 0.628626 0.447484 71.00000 -1.20000
H41B 2 0.177537 0.608751 0.498274 71.00000 -1.20000
AFIX 23
PART 2
H41C 2 0.172733 0.659441 0.441606 -71.00000 -1.20000
H41D 2 0.128972 0.622775 0.452805 -71.00000 -1.20000
AFIX 0
PART 1
C42 1 0.187814 0.679440 0.450709 71.00000 0.19368 0.07923 =
0.08376 -0.01461 0.01544 0.04446
AFIX 33
H42A 2 0.181162 0.720476 0.469387 71.00000 -1.50000
H42B 2 0.175126 0.689661 0.412352 71.00000 -1.50000
H42C 2 0.223539 0.671049 0.464316 71.00000 -1.50000
AFIX 0
PART 2
C42X 1 0.192024 0.625640 0.515220 -71.00000 0.13304 0.17004 =
0.10397 -0.05482 0.03985 0.06131
AFIX 33
H42D 2 0.183986 0.671682 0.527281 -71.00000 -1.50000
H42E 2 0.227425 0.624094 0.522807 -71.00000 -1.50000
H42F 2 0.183722 0.586300 0.534083 -71.00000 -1.50000
AFIX 0
PART 0
C43 1 0.201668 0.483405 0.348214 11.00000 0.04632 0.04115 =
0.04730 0.01048 0.02227 0.01690
AFIX 23
H43A 2 0.218236 0.466088 0.385438 11.00000 -1.20000
H43B 2 0.203800 0.444512 0.324455 11.00000 -1.20000
AFIX 0
C44 1 0.229846 0.547648 0.341195 11.00000 0.05565 0.05288 =
0.06606 0.01607 0.02246 0.00584
AFIX 23
H44A 2 0.226924 0.587792 0.363581 11.00000 -1.20000
H44B 2 0.215270 0.563421 0.303449 11.00000 -1.20000
AFIX 0
C45 1 0.283875 0.529601 0.356804 11.00000 0.06475 0.07291 =
0.12325 -0.00506 0.05327 -0.00657
AFIX 23
H45A 2 0.298476 0.516049 0.395027 11.00000 -1.20000
H45B 2 0.286316 0.487381 0.335902 11.00000 -1.20000
AFIX 0
C46 1 0.313467 0.589908 0.347973 11.00000 0.07342 0.12233 =
0.13641 0.02650 0.03768 -0.02290
AFIX 33
H46A 2 0.347861 0.574516 0.358552 11.00000 -1.50000
H46B 2 0.312249 0.631462 0.369486 11.00000 -1.50000
H46C 2 0.299650 0.603197 0.310105 11.00000 -1.50000
AFIX 0
C47 1 0.119410 0.519170 0.279004 11.00000 0.05505 0.03737 =
0.06052 0.02121 0.01880 0.01411
AFIX 23
H47A 2 0.084606 0.528229 0.273479 11.00000 -1.20000
H47B 2 0.133376 0.565158 0.273115 11.00000 -1.20000
AFIX 0
C48 1 0.119944 0.466375 0.237690 11.00000 0.06662 0.05441 =
0.05252 0.01560 0.01507 0.01630
AFIX 23
H48A 2 0.109991 0.418305 0.245430 11.00000 -1.20000
H48B 2 0.153732 0.462705 0.238428 11.00000 -1.20000
AFIX 0
C49 1 0.084437 0.491391 0.183211 11.00000 0.12492 0.05713 =
0.05998 0.01289 0.00926 -0.00496
AFIX 23
H49A 2 0.092202 0.541620 0.177408 11.00000 -1.20000
H49B 2 0.050242 0.490110 0.181480 11.00000 -1.20000
AFIX 0
C50 1 0.088100 0.443328 0.139310 11.00000 0.18862 0.09134 =
0.05275 0.00517 0.02175 -0.00804
AFIX 33
H50A 2 0.064747 0.460181 0.104368 11.00000 -1.50000
H50B 2 0.080103 0.393695 0.144887 11.00000 -1.50000
H50C 2 0.121793 0.445366 0.140599 11.00000 -1.50000

HKLF 4

REM rje253 in C2/c
REM R1 = 0.0682 for 11036 Fo > 4sig(Fo) and 0.0747 for all 12093 data
REM 756 parameters refined using 261 restraints

END

WGHT 0.0239 192.2869
REM Highest difference peak 2.417, deepest hole -2.481, 1-sigma level 0.128
Q1 1 0.0253 0.1640 0.7112 11.00000 0.05 2.42
Q2 1 -0.0170 0.1987 0.6706 11.00000 0.05 1.36
Q3 1 0.0910 0.2867 0.7997 11.00000 0.05 1.03
Q4 1 0.2558 0.2206 0.8980 11.00000 0.05 0.93
Q5 1 0.3704 0.2617 0.5485 11.00000 0.05 0.79
Q6 1 0.2873 0.2187 0.5902 11.00000 0.05 0.76
Q7 1 -0.0391 0.3442 0.6808 11.00000 0.05 0.74
Q8 1 0.1819 0.6421 0.6105 11.00000 0.05 0.65
Q9 1 0.2402 0.2522 0.8569 11.00000 0.05 0.63
Q10 1 0.0155 0.4323 0.6671 11.00000 0.05 0.63
;