Rational addition of capping groups to the phosphomolybdate Keggin anion [PMo<sub>12</sub>O<sub>40</sub>]<sup>3-</sup> by mild, non-aqueous reductive aggregation
Ridla Bakri; Andrew Booth; Gavin Harle; Paul S. Middleton; Corinne Wills; William Clegg; Ross W. Harrington; R. John Errington; Chem. Commun. 48 (2012) 2779–; doi:10.1039/c2cc17670j

data_7107449
_publ_section_title
;
 Rational addition of capping groups to the phosphomolybdate Keggin anion
 [PMo<sub>12</sub>O<sub>40</sub>]<sup>3-</sup> by mild, non-aqueous
 reductive aggregation
;
_journal_name_full               'Chem. Commun.'
_journal_page_first              2779
_journal_paper_doi               10.1039/c2cc17670j
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         '3 C16 H36 N +,Mo12 V2 P O42 3-,C2 H3 N'
_chemical_formula_sum            'C50 H111 Mo12 N4 O42 P V2'
_chemical_formula_weight         2724.56
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 95.462(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.8622(17)
_cell_length_b                   14.4740(17)
_cell_length_c                   49.226(4)
_cell_measurement_reflns_used    979
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.23
_cell_volume                     16925(3)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6393
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_sigmaI/netI    0.1252
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            37547
_diffrn_reflns_theta_full        25.27
_diffrn_reflns_theta_max         25.27
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.420
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             10720
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1010
_refine_ls_number_reflns         20469
_refine_ls_number_restraints     980
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0429P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1485
_reflns_number_gt                11207
_reflns_number_total             20469
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cc17670j.txt
_cod_data_source_block           rje422_salt_of_2
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7107449
_computing_special_details
;
TITL PM166 (RJE422) in I2/a
CELL 0.6393 23.8622 14.4740 49.226 90.000 95.462 90.000
ZERR 8.00 0.0017 0.0017 0.004 0.000 0.007 0.000
LATT 2
SYMM 0.5-X, Y, -Z
SFAC C H N O P V MO
DISP P 0.08539 0.07631 274.94
DISP V 0.27018 0.43544 1568.86
DISP Mo -2.88896 0.56746 2044.55
UNIT 400 888 32 336 8 16 96
TEMP -153
SIZE 0.02 0.03 0.10
OMIT 16 1 13
OMIT -16 10 26

SIMU $N $C
DELU $N $C

L.S. 20
CONN $MO 6
CONN $V 5
ACTA
BOND
FMAP 2
PLAN 10

REM EXTI 0.000052
WGHT 0.042900
FVAR 0.01628 0.49751
MO1 7 0.691872 0.076687 0.442009 11.00000 0.02922 0.03260 =
0.02400 -0.00080 -0.00157 0.00257
MO2 7 0.740146 -0.073302 0.388993 11.00000 0.02551 0.02782 =
0.03220 0.00268 0.00208 0.00341
MO3 7 0.773698 0.117762 0.354195 11.00000 0.02347 0.03053 =
0.02920 0.00044 0.00296 -0.00120
MO4 7 0.681322 -0.056054 0.322929 11.00000 0.02624 0.03024 =
0.02914 -0.00520 0.00247 -0.00061
MO5 7 0.569945 0.132266 0.302585 11.00000 0.02541 0.03400 =
0.02525 0.00285 -0.00053 -0.00075
MO6 7 0.535240 -0.072780 0.341040 11.00000 0.02570 0.03266 =
0.02752 -0.00046 0.00004 -0.00390
MO7 7 0.488529 0.066679 0.389623 11.00000 0.02331 0.04329 =
0.02999 0.00108 0.00357 0.00221
MO8 7 0.660959 0.304000 0.336242 11.00000 0.03256 0.02729 =
0.03032 0.00304 -0.00033 0.00044
MO9 7 0.588957 0.252134 0.423159 11.00000 0.03372 0.03557 =
0.02905 -0.00556 0.00363 0.00695
MO10 7 0.593917 -0.106606 0.406342 11.00000 0.02609 0.03144 =
0.02836 0.00397 0.00280 -0.00100
MO11 7 0.724864 0.268317 0.406898 11.00000 0.03120 0.02808 =
0.02846 -0.00344 -0.00096 0.00013
MO12 7 0.526017 0.272117 0.351830 11.00000 0.03133 0.03649 =
0.03430 0.00354 0.00133 0.01013
V1 6 0.563729 0.055006 0.443877 11.00000 0.03434 0.04970 =
0.03009 0.00056 0.00691 0.00309
V2 6 0.698092 0.142337 0.300630 11.00000 0.03216 0.04186 =
0.02899 0.00206 0.00431 -0.00323
P1 5 0.631585 0.098640 0.372261 11.00000 0.02597 0.02684 =
0.02593 0.00040 0.00185 0.00084
O1 4 0.423571 0.071488 0.399724 11.00000 0.03557 0.05480 =
0.04813 -0.00072 0.00747 0.00157
O2 4 0.536974 0.036737 0.472044 11.00000 0.04018 0.05704 =
0.03878 -0.00106 0.00921 -0.00189
O3 4 0.724991 0.161599 0.272745 11.00000 0.04982 0.05289 =
0.02458 0.01001 0.00634 -0.00114
O4 4 0.692944 -0.121481 0.296087 11.00000 0.04232 0.04414 =
0.03823 -0.00976 0.00612 0.00261
O5 4 0.534938 0.031621 0.317963 11.00000 0.02778 0.04179 =
0.03432 0.00278 0.00337 -0.00327
O6 4 0.782658 -0.157164 0.401396 11.00000 0.03975 0.02851 =
0.04739 0.00999 0.00561 0.00770
O7 4 0.474686 0.350097 0.348894 11.00000 0.03841 0.05262 =
0.05179 0.00469 -0.00071 0.02008
O8 4 0.771006 0.351115 0.416589 11.00000 0.04185 0.03543 =
0.05009 -0.00363 -0.00208 -0.00087
O9 4 0.555805 0.316544 0.444945 11.00000 0.04568 0.05667 =
0.04538 -0.00811 0.00924 0.00936
O10 4 0.526781 -0.029120 0.415389 11.00000 0.02961 0.04597 =
0.02909 0.00076 0.00785 -0.00049
O11 4 0.544801 0.128815 0.269668 11.00000 0.04283 0.04919 =
0.03531 0.00136 -0.00169 -0.00445
O12 4 0.656783 0.311503 0.423569 11.00000 0.04622 0.03565 =
0.03781 -0.00286 0.00509 0.00715
O13 4 0.589712 0.345896 0.339987 11.00000 0.03886 0.03330 =
0.04544 0.00436 -0.00244 0.01025
O14 4 0.649439 0.149192 0.399006 11.00000 0.03039 0.03015 =
0.03386 -0.00187 0.00185 0.00464
O15 4 0.491456 0.166782 0.366483 11.00000 0.02998 0.04722 =
0.04021 0.00278 -0.00069 0.00217
O16 4 0.555632 -0.147500 0.374591 11.00000 0.03034 0.03709 =
0.03801 0.00620 0.00406 0.00126
O17 4 0.560825 0.290286 0.389226 11.00000 0.03949 0.04111 =
0.03708 0.00183 0.00022 0.00616
O18 4 0.682905 0.047283 0.363080 11.00000 0.03260 0.03090 =
0.02526 0.00024 0.00455 0.00404
O19 4 0.723404 0.211350 0.332924 11.00000 0.03267 0.03743 =
0.03081 0.00197 0.00199 -0.00006
O20 4 0.498737 -0.148854 0.321174 11.00000 0.03484 0.04313 =
0.04158 -0.00145 -0.00135 -0.00849
O21 4 0.584614 0.029419 0.376385 11.00000 0.03017 0.03037 =
0.02898 -0.00163 -0.00026 0.00081
O22 4 0.522677 0.219362 0.316429 11.00000 0.02991 0.04715 =
0.03693 0.00319 0.00113 0.00495
O23 4 0.687391 0.315239 0.371972 11.00000 0.03403 0.03259 =
0.03625 0.00581 -0.00297 0.00084
O24 4 0.716987 0.046871 0.473381 11.00000 0.05171 0.05362 =
0.03179 0.00491 -0.00505 -0.00512
O25 4 0.688817 0.395665 0.321195 11.00000 0.05968 0.03148 =
0.03606 0.00943 -0.00364 -0.00641
O26 4 0.723174 -0.115638 0.350778 11.00000 0.03621 0.03291 =
0.03389 -0.00187 0.00130 -0.00193
O27 4 0.664978 -0.120653 0.395563 11.00000 0.03309 0.03397 =
0.04188 -0.00290 0.00459 -0.00298
O28 4 0.532532 0.146096 0.418329 11.00000 0.03332 0.05004 =
0.03501 0.00518 0.00328 0.00258
O29 4 0.733557 0.184020 0.436727 11.00000 0.03000 0.03740 =
0.03472 -0.00352 -0.00254 0.00048
O30 4 0.790741 0.010549 0.374279 11.00000 0.02574 0.03295 =
0.03350 -0.00266 0.00223 0.00229
O31 4 0.836364 0.146648 0.344447 11.00000 0.02842 0.04125 =
0.03752 -0.00275 0.00487 -0.00383
O32 4 0.612824 -0.094476 0.332104 11.00000 0.03329 0.02557 =
0.04215 0.00165 0.00436 -0.00092
O33 4 0.632841 0.226584 0.302901 11.00000 0.03124 0.03800 =
0.03363 -0.00057 -0.00037 -0.00174
O34 4 0.627906 -0.014371 0.434091 11.00000 0.03473 0.04277 =
0.03673 -0.00340 0.00774 -0.00046
O35 4 0.622773 0.152338 0.449287 11.00000 0.03994 0.03787 =
0.03054 -0.00130 0.00533 0.00414
O36 4 0.732392 0.004290 0.419313 11.00000 0.02501 0.04356 =
0.03626 0.00581 0.00143 -0.00066
O37 4 0.587150 -0.197324 0.427273 11.00000 0.04124 0.04376 =
0.03514 0.01322 0.00354 -0.00537
O38 4 0.479230 -0.021028 0.361538 11.00000 0.02642 0.04174 =
0.03751 0.00482 -0.00123 0.00064
O39 4 0.766203 0.191198 0.384767 11.00000 0.02971 0.03602 =
0.03652 -0.00007 0.00302 -0.00028
O40 4 0.608977 0.167902 0.350399 11.00000 0.03298 0.03510 =
0.02690 0.00354 -0.00069 0.00154
O41 4 0.741310 0.042536 0.321379 11.00000 0.03423 0.03294 =
0.02788 -0.00091 0.00292 -0.00414
O42 4 0.639336 0.050918 0.303018 11.00000 0.03430 0.04239 =
0.02755 0.00106 0.00260 -0.00474
SAME N2 > C32
SAME N3 > C48
SAME N2 > C31 C32A
SAME N1 C5 > C16 C1 > C4
SAME N1 C13 > C16 C9 > C12 C5 > C8 C1 > C4
N1 3 0.323189 1.097915 0.110580 11.00000 0.05418 0.03855 =
0.11469 0.00367 0.01420 -0.00866
C1 1 0.350296 1.156705 0.133533 11.00000 0.05605 0.03771 =
0.10146 0.02267 -0.00338 -0.00581
AFIX 23
H1A 2 0.320524 1.194034 0.140968 11.00000 -1.20000
H1B 2 0.376595 1.200191 0.125805 11.00000 -1.20000
AFIX 0
C2 1 0.382245 1.105372 0.156967 11.00000 0.05690 0.05259 =
0.11715 0.02706 0.00029 0.00608
AFIX 23
H2A 2 0.355474 1.067982 0.166536 11.00000 -1.20000
H2B 2 0.409502 1.062639 0.149646 11.00000 -1.20000
AFIX 0
C3 1 0.413003 1.169789 0.176816 11.00000 0.05810 0.07001 =
0.14675 0.04032 -0.03711 -0.02585
AFIX 23
H3A 2 0.432820 1.216015 0.166404 11.00000 -1.20000
H3B 2 0.384922 1.203435 0.186610 11.00000 -1.20000
AFIX 0
C4 1 0.454848 1.126899 0.197486 11.00000 0.05881 0.10590 =
0.13126 0.06003 -0.01177 -0.01956
AFIX 33
H4A 2 0.469926 1.174195 0.210429 11.00000 -1.50000
H4B 2 0.485642 1.099946 0.188290 11.00000 -1.50000
H4C 2 0.436470 1.078373 0.207320 11.00000 -1.50000
AFIX 0
C5 1 0.366968 1.034128 0.099334 11.00000 0.09719 0.04052 =
0.20362 -0.00982 0.03751 0.01394
AFIX 23
H5A 2 0.385284 0.996625 0.114489 11.00000 -1.20000
H5B 2 0.347455 0.991238 0.085913 11.00000 -1.20000
AFIX 0
C6 1 0.411375 1.085559 0.085911 11.00000 0.10969 0.11742 =
0.21640 -0.01119 0.07829 0.00164
AFIX 23
H6A 2 0.424962 1.135843 0.098491 11.00000 -1.20000
H6B 2 0.392471 1.115455 0.069419 11.00000 -1.20000
AFIX 0
C7 1 0.462402 1.037210 0.077356 11.00000 0.08798 0.07252 =
0.30911 -0.00906 0.02959 0.01885
AFIX 23
H7A 2 0.450561 0.987433 0.064255 11.00000 -1.20000
H7B 2 0.485717 1.081632 0.068073 11.00000 -1.20000
AFIX 0
C8 1 0.494814 0.998848 0.100298 11.00000 0.14043 0.10165 =
0.29793 -0.05147 -0.03199 -0.00946
AFIX 33
H8A 2 0.534181 0.993550 0.096365 11.00000 -1.50000
H8B 2 0.480203 0.937469 0.104197 11.00000 -1.50000
H8C 2 0.492431 1.039045 0.116166 11.00000 -1.50000
AFIX 0
C9 1 0.297179 1.163860 0.089015 11.00000 0.06298 0.04194 =
0.07414 -0.01427 0.01915 0.00068
AFIX 23
H9A 2 0.268289 1.200922 0.097240 11.00000 -1.20000
H9B 2 0.326872 1.207072 0.084242 11.00000 -1.20000
AFIX 0
C10 1 0.270129 1.121724 0.062838 11.00000 0.06565 0.06368 =
0.11227 -0.03768 0.00541 -0.00794
AFIX 23
H10A 2 0.241816 1.075350 0.067177 11.00000 -1.20000
H10B 2 0.299170 1.089837 0.053215 11.00000 -1.20000
AFIX 0
C11 1 0.241829 1.195922 0.044371 11.00000 0.06489 0.09355 =
0.06997 -0.03745 -0.00193 -0.02254
AFIX 23
H11A 2 0.223378 1.165842 0.027804 11.00000 -1.20000
H11B 2 0.212004 1.225633 0.053996 11.00000 -1.20000
AFIX 0
C12 1 0.280403 1.268897 0.035855 11.00000 0.11665 0.16896 =
0.05076 0.00129 -0.01513 -0.07426
AFIX 33
H12A 2 0.261248 1.304958 0.020883 11.00000 -1.50000
H12B 2 0.314160 1.240068 0.029723 11.00000 -1.50000
H12C 2 0.291218 1.309748 0.051348 11.00000 -1.50000
AFIX 0
C13 1 0.279473 1.034718 0.121442 11.00000 0.06830 0.05742 =
0.10319 0.00179 0.00225 -0.02092
AFIX 23
H13A 2 0.262761 0.996453 0.106081 11.00000 -1.20000
H13B 2 0.299317 0.992272 0.134888 11.00000 -1.20000
AFIX 0
C14 1 0.232146 1.079362 0.134707 11.00000 0.05543 0.08462 =
0.07444 0.01876 -0.00887 -0.01138
AFIX 23
H14A 2 0.212681 1.125191 0.122205 11.00000 -1.20000
H14B 2 0.246943 1.111510 0.151643 11.00000 -1.20000
AFIX 0
C15 1 0.191226 1.002794 0.141287 11.00000 0.05374 0.08487 =
0.09763 0.02233 -0.00172 -0.00080
AFIX 23
H15A 2 0.178889 0.968573 0.124354 11.00000 -1.20000
H15B 2 0.210983 0.958764 0.154280 11.00000 -1.20000
AFIX 0
C16 1 0.141905 1.039152 0.153053 11.00000 0.06966 0.08259 =
0.13182 0.01076 0.02177 0.00676
AFIX 33
H16A 2 0.121878 0.988435 0.161105 11.00000 -1.50000
H16B 2 0.116854 1.068979 0.138733 11.00000 -1.50000
H16C 2 0.153844 1.084470 0.167227 11.00000 -1.50000
AFIX 0
N2 3 0.616400 0.432077 0.236875 11.00000 0.03419 0.04640 =
0.03754 0.00134 0.00331 0.00950
PART 0
C17 1 0.626010 0.469814 0.208890 11.00000 0.03571 0.05760 =
0.04738 0.00313 0.00679 0.00626
AFIX 23
H17A 2 0.664329 0.451657 0.204823 11.00000 -1.20000
H17B 2 0.599042 0.439171 0.195239 11.00000 -1.20000
AFIX 0
C18 1 0.620292 0.572959 0.204909 11.00000 0.04482 0.04867 =
0.05690 0.00592 -0.00857 0.01154
AFIX 23
H18A 2 0.581312 0.591873 0.207551 11.00000 -1.20000
H18B 2 0.646024 0.604983 0.218810 11.00000 -1.20000
AFIX 0
C19 1 0.633832 0.601626 0.176945 11.00000 0.06509 0.06972 =
0.05259 0.01923 -0.02423 -0.02722
AFIX 23
H19A 2 0.669448 0.571063 0.173265 11.00000 -1.20000
H19B 2 0.603913 0.577198 0.163546 11.00000 -1.20000
AFIX 0
C20 1 0.639666 0.700492 0.171751 11.00000 0.04379 0.06521 =
0.09584 0.02682 -0.00749 -0.01080
AFIX 33
H20A 2 0.647734 0.709925 0.152797 11.00000 -1.50000
H20B 2 0.670605 0.725614 0.184082 11.00000 -1.50000
H20C 2 0.604568 0.732182 0.174892 11.00000 -1.50000
AFIX 0
C21 1 0.553950 0.436635 0.240872 11.00000 0.03839 0.05489 =
0.05106 0.00532 0.00758 0.01527
AFIX 23
H21A 2 0.542977 0.502573 0.241098 11.00000 -1.20000
H21B 2 0.532880 0.408208 0.224693 11.00000 -1.20000
AFIX 0
C22 1 0.534673 0.391811 0.265769 11.00000 0.05072 0.06187 =
0.05529 0.00286 0.01568 0.01159
AFIX 23
H22A 2 0.556132 0.418117 0.282168 11.00000 -1.20000
H22B 2 0.543099 0.324890 0.265287 11.00000 -1.20000
AFIX 0
C23 1 0.472224 0.404707 0.268145 11.00000 0.04642 0.08137 =
0.07361 0.01439 0.02308 0.01437
AFIX 23
H23A 2 0.464235 0.388949 0.286963 11.00000 -1.20000
H23B 2 0.462607 0.470649 0.265057 11.00000 -1.20000
AFIX 0
C24 1 0.436014 0.348589 0.248947 11.00000 0.07716 0.19183 =
0.11700 0.00866 -0.03138 -0.02242
AFIX 33
H24A 2 0.397410 0.349650 0.254181 11.00000 -1.50000
H24B 2 0.449853 0.284811 0.249320 11.00000 -1.50000
H24C 2 0.436545 0.373747 0.230490 11.00000 -1.50000
AFIX 0
C25 1 0.635852 0.330481 0.238078 11.00000 0.03735 0.05752 =
0.04968 -0.00130 0.00527 0.01029
AFIX 23
H25A 2 0.675670 0.328227 0.234013 11.00000 -1.20000
H25B 2 0.634376 0.307799 0.256970 11.00000 -1.20000
AFIX 0
C26 1 0.602243 0.265028 0.218880 11.00000 0.04877 0.05235 =
0.04740 0.00542 0.00592 -0.00712
AFIX 23
H26A 2 0.599605 0.291039 0.200202 11.00000 -1.20000
H26B 2 0.563555 0.260134 0.224435 11.00000 -1.20000
AFIX 0
C27 1 0.627987 0.168425 0.218446 11.00000 0.03893 0.05448 =
0.04435 0.00457 0.00223 -0.00401
AFIX 23
H27A 2 0.637271 0.147204 0.237461 11.00000 -1.20000
H27B 2 0.599712 0.125334 0.209540 11.00000 -1.20000
AFIX 0
C28 1 0.679776 0.164675 0.203811 11.00000 0.05930 0.04513 =
0.05127 -0.00050 0.01088 -0.00091
AFIX 33
H28A 2 0.689730 0.100063 0.200758 11.00000 -1.50000
H28B 2 0.710789 0.195162 0.214835 11.00000 -1.50000
H28C 2 0.672882 0.196332 0.186212 11.00000 -1.50000
AFIX 0
C29 1 0.649364 0.486650 0.259178 11.00000 0.05735 0.05275 =
0.03682 0.00172 -0.00386 -0.00479
AFIX 23
H29A 2 0.631983 0.548605 0.259882 11.00000 -1.20000
H29B 2 0.644818 0.455854 0.276791 11.00000 -1.20000
AFIX 0
C30 1 0.710713 0.499412 0.257043 11.00000 0.05461 0.06081 =
0.05677 0.00436 -0.00252 0.00080
AFIX 23
H30A 2 0.716603 0.521236 0.238468 11.00000 -1.20000
H30B 2 0.730186 0.439335 0.259975 11.00000 -1.20000
AFIX 0
C31 1 0.736242 0.569621 0.278163 11.00000 0.06701 0.06368 =
0.05416 0.00398 -0.01249 -0.01793
PART 1
AFIX 23
H31A 2 0.711817 0.624997 0.277698 21.00000 -1.20000
H31B 2 0.736921 0.542105 0.296604 21.00000 -1.20000
AFIX 23
PART 2
H31C 2 0.721575 0.556669 0.295922 -21.00000 -1.20000
H31D 2 0.777564 0.560850 0.280543 -21.00000 -1.20000
AFIX 0
PART 1
C32 1 0.793330 0.597907 0.273416 21.00000 0.07818 0.05544 =
0.05437 -0.00077 0.01161 -0.01116
AFIX 33
H32A 2 0.810060 0.632892 0.289199 21.00000 -1.50000
H32B 2 0.791964 0.636801 0.257070 21.00000 -1.50000
H32C 2 0.816223 0.542985 0.270797 21.00000 -1.50000
AFIX 0
PART 2
C32A 1 0.724298 0.665355 0.270869 -21.00000 0.07542 0.05768 =
0.14756 -0.00882 -0.01271 0.02053
AFIX 33
H32D 2 0.749451 0.705895 0.282371 -21.00000 -1.50000
H32E 2 0.685105 0.679593 0.273657 -21.00000 -1.50000
H32F 2 0.730281 0.675155 0.251659 -21.00000 -1.50000
AFIX 0
N3 3 0.582872 0.297535 0.040321 11.00000 0.03727 0.04647 =
0.03790 0.00212 0.01070 0.01035
C33 1 0.576814 0.401852 0.041378 11.00000 0.04691 0.04800 =
0.04720 -0.00267 0.00164 0.01291
AFIX 23
H33A 2 0.564372 0.424436 0.022795 11.00000 -1.20000
H33B 2 0.546837 0.417064 0.053231 11.00000 -1.20000
AFIX 0
C34 1 0.629363 0.452878 0.051710 11.00000 0.06211 0.04503 =
0.11038 -0.02678 0.00495 0.00562
AFIX 23
H34A 2 0.662306 0.423932 0.044323 11.00000 -1.20000
H34B 2 0.634752 0.448716 0.071863 11.00000 -1.20000
AFIX 0
C35 1 0.625513 0.554195 0.043140 11.00000 0.06120 0.05161 =
0.09825 -0.00986 0.01665 0.00158
AFIX 23
H35A 2 0.586137 0.575256 0.043576 11.00000 -1.20000
H35B 2 0.649329 0.591404 0.056596 11.00000 -1.20000
AFIX 0
C36 1 0.642912 0.571474 0.016218 11.00000 0.08422 0.13213 =
0.10212 0.01054 0.02957 0.02653
AFIX 33
H36A 2 0.610614 0.593393 0.004149 11.00000 -1.50000
H36B 2 0.657326 0.514195 0.008863 11.00000 -1.50000
H36C 2 0.672574 0.618531 0.017417 11.00000 -1.50000
AFIX 0
C37 1 0.622671 0.271164 0.019314 11.00000 0.04637 0.05066 =
0.04805 0.00369 0.01603 0.00876
AFIX 23
H37A 2 0.661143 0.290739 0.026256 11.00000 -1.20000
H37B 2 0.611939 0.306693 0.002432 11.00000 -1.20000
AFIX 0
C38 1 0.624581 0.168928 0.011844 11.00000 0.04548 0.05890 =
0.04823 -0.01381 0.00814 0.00535
AFIX 23
H38A 2 0.627725 0.131097 0.028675 11.00000 -1.20000
H38B 2 0.589329 0.151492 0.000793 11.00000 -1.20000
AFIX 0
C39 1 0.674269 0.150144 -0.004145 11.00000 0.04949 0.07124 =
0.05382 -0.00870 0.01291 0.01546
AFIX 23
H39A 2 0.672989 0.193971 -0.019632 11.00000 -1.20000
H39B 2 0.709246 0.162664 0.007767 11.00000 -1.20000
AFIX 0
C40 1 0.677146 0.054918 -0.014975 11.00000 0.08064 0.09409 =
0.08376 -0.04903 0.00937 0.02052
AFIX 33
H40A 2 0.710752 0.048564 -0.024820 11.00000 -1.50000
H40B 2 0.643491 0.042452 -0.027444 11.00000 -1.50000
H40C 2 0.679097 0.010757 0.000177 11.00000 -1.50000
AFIX 0
C41 1 0.524676 0.254993 0.033155 11.00000 0.03983 0.05978 =
0.04954 0.00536 0.00691 -0.00113
AFIX 23
H41A 2 0.528280 0.187083 0.034976 11.00000 -1.20000
H41B 2 0.499753 0.276074 0.046885 11.00000 -1.20000
AFIX 0
C42 1 0.495894 0.275887 0.005215 11.00000 0.04827 0.07009 =
0.04333 -0.00164 0.00413 0.00702
AFIX 23
H42A 2 0.522420 0.264450 -0.008704 11.00000 -1.20000
H42B 2 0.485058 0.341914 0.004240 11.00000 -1.20000
AFIX 0
C43 1 0.443692 0.216351 -0.000973 11.00000 0.05085 0.09932 =
0.06138 0.00960 -0.00929 -0.00095
AFIX 23
H43A 2 0.419769 0.221891 0.014311 11.00000 -1.20000
H43B 2 0.421881 0.240399 -0.017590 11.00000 -1.20000
AFIX 0
C44 1 0.456287 0.116804 -0.005176 11.00000 0.10210 0.09092 =
0.08574 -0.00990 0.00706 -0.03454
AFIX 33
H44A 2 0.420945 0.082464 -0.008691 11.00000 -1.50000
H44B 2 0.477693 0.092192 0.011215 11.00000 -1.50000
H44C 2 0.478505 0.110295 -0.020816 11.00000 -1.50000
AFIX 0
C45 1 0.607196 0.258763 0.067607 11.00000 0.05328 0.06644 =
0.03643 0.00181 0.00300 0.01582
AFIX 23
H45A 2 0.644652 0.287221 0.072121 11.00000 -1.20000
H45B 2 0.613296 0.191709 0.065226 11.00000 -1.20000
AFIX 0
C46 1 0.573453 0.271364 0.092167 11.00000 0.06776 0.05548 =
0.03851 -0.00224 0.00703 0.01494
AFIX 23
H46A 2 0.576928 0.335960 0.098724 11.00000 -1.20000
H46B 2 0.533165 0.258656 0.086764 11.00000 -1.20000
AFIX 0
C47 1 0.595170 0.206028 0.114833 11.00000 0.05677 0.05697 =
0.03726 -0.00207 0.00149 -0.00438
AFIX 23
H47A 2 0.592629 0.141817 0.107896 11.00000 -1.20000
H47B 2 0.635348 0.219713 0.120206 11.00000 -1.20000
AFIX 0
C48 1 0.563265 0.213316 0.139308 11.00000 0.06385 0.06651 =
0.04509 0.01202 0.01484 0.00648
AFIX 33
H48A 2 0.577517 0.167452 0.152896 11.00000 -1.50000
H48B 2 0.523234 0.201887 0.134013 11.00000 -1.50000
H48C 2 0.568046 0.275407 0.147126 11.00000 -1.50000
AFIX 0
N4 3 0.630022 0.947091 0.068131 11.00000 0.11796 0.14425 =
0.14629 0.01807 0.01256 -0.04633
C49 1 0.611938 0.877703 0.075107 11.00000 0.08302 0.12165 =
0.09757 0.00802 0.02128 -0.01596
C50 1 0.590718 0.788642 0.085098 11.00000 0.09271 0.11850 =
0.10415 -0.00512 0.00430 -0.02707
AFIX 33
H50A 2 0.562990 0.800799 0.098120 11.00000 -1.50000
H50B 2 0.622184 0.753224 0.094121 11.00000 -1.50000
H50C 2 0.572982 0.753157 0.069643 11.00000 -1.50000

HKLF 4

REM PM166 (RJE422) in I2/a
REM R1 = 0.0588 for 11207 Fo > 4sig(Fo) and 0.1175 for all 20469 data
REM 1010 parameters refined using 980 restraints

END

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