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_7107448
_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 +,C4 H6 Co Mo12 N2 O40 P 3-,C2 H3 N'
_chemical_formula_sum            'C54 H117 Co Mo12 N6 O40 P'
_chemical_formula_weight         2731.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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            8
_cell_length_a                   17.975(4)
_cell_length_b                   22.382(9)
_cell_length_c                   44.296(16)
_cell_measurement_reflns_used    185
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.50
_cell_volume                     17821(10)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_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      150(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \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  0.0717
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            48140
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.96
_exptl_absorpt_coefficient_mu    1.909
_exptl_absorpt_correction_T_max  0.598
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10792
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.903
_refine_diff_density_min         -1.535
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         7887
_refine_ls_number_restraints     1005
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0409
_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^+186.6674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0870
_reflns_number_gt                6224
_reflns_number_total             7887
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cc17670j.txt
_cod_data_source_block           rje411_salt_of_1
_cod_database_code               7107448
_computing_special_details
;
TITL rje411 in Cmca
CELL 0.71073 17.975 22.382 44.296 90.000 90.000 90.000
ZERR 8.00 0.004 0.009 0.016 0.000 0.000 0.000
LATT 7
SYMM -X, 0.5-Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM X, -Y, -Z
SFAC C H O P MO N Co
UNIT 432 936 320 8 96 48 8

REM blue block
SIZE 0.34 0.30 0.30
TEMP -123
OMIT -3 50
OMIT 4 2 1
OMIT 1 3 36
OMIT 5 25 3

L.S. 8
ACTA
BOND
FMAP 2
PLAN 10

SIMU 0.01 $C $N
DELU 0.01 $C $N

REM EXTI 0.000010
WGHT 0.000000 186.667404
FVAR 0.02151 0.53848
MO1 5 0.598082 0.674713 0.691801 11.00000 0.01841 0.02212 =
0.01765 -0.00478 -0.00229 0.00055
MO2 5 0.500000 0.765379 0.644355 10.50000 0.03328 0.01108 =
0.02237 0.00082 0.00000 0.00000
MO3 5 0.602531 0.698681 0.580679 11.00000 0.02728 0.02427 =
0.02079 0.00135 0.00387 -0.00914
MO4 5 0.604183 0.547369 0.568555 11.00000 0.02674 0.02780 =
0.01783 -0.00537 0.00047 0.00847
MO5 5 0.699729 0.607030 0.627670 11.00000 0.01887 0.05198 =
0.02367 -0.01155 -0.00330 0.01179
MO6 5 0.597534 0.507185 0.679862 11.00000 0.07004 0.02359 =
0.01650 -0.00151 -0.00809 0.02620
MO7 5 0.500000 0.448517 0.620230 10.50000 0.08346 0.01233 =
0.01786 -0.00205 0.00000 0.00000
CO 7 0.500000 0.579889 0.727510 10.50000 0.04306 0.02015 =
0.01481 -0.00006 0.00000 0.00000
P 4 0.500000 0.606946 0.630730 10.50000 0.01762 0.01105 =
0.01218 -0.00008 0.00000 0.00000
O1 3 0.500000 0.499625 0.701761 10.50000 0.07812 0.01892 =
0.01302 0.00429 0.00000 0.00000
O2 3 0.587868 0.588298 0.696810 11.00000 0.03215 0.02442 =
0.01657 -0.00183 -0.00500 0.00864
O3 3 0.500000 0.670274 0.713753 10.50000 0.02615 0.01849 =
0.01446 -0.00119 0.00000 0.00000
O4 3 0.654464 0.474413 0.705302 11.00000 0.09895 0.04767 =
0.02227 0.00035 -0.01143 0.04962
O5 3 0.655374 0.692990 0.720551 11.00000 0.02643 0.04424 =
0.02551 -0.01012 -0.00588 0.00005
O6 3 0.500000 0.840857 0.643875 10.50000 0.08218 0.01941 =
0.02795 -0.00044 0.00000 0.00000
O7 3 0.573183 0.748728 0.676127 11.00000 0.02700 0.02237 =
0.02390 -0.00170 0.00056 -0.00583
O8 3 0.571240 0.444557 0.655108 11.00000 0.09930 0.02232 =
0.02033 0.00012 -0.00598 0.02678
O9 3 0.663945 0.655568 0.660345 11.00000 0.01518 0.03617 =
0.02548 -0.00654 -0.00082 -0.00016
O10 3 0.572837 0.744479 0.613986 11.00000 0.03129 0.01842 =
0.02464 -0.00027 0.00148 -0.00830
O11 3 0.791450 0.603676 0.634374 11.00000 0.02345 0.11661 =
0.03131 -0.02353 -0.00787 0.02426
O12 3 0.637185 0.750052 0.556707 11.00000 0.04942 0.03190 =
0.03300 -0.00130 0.01581 -0.01700
O13 3 0.500000 0.693098 0.568950 10.50000 0.03158 0.02293 =
0.02103 0.00647 0.00000 0.00000
O14 3 0.663584 0.541035 0.652540 11.00000 0.04664 0.04105 =
0.01885 -0.00581 -0.00607 0.02576
O15 3 0.691848 0.672547 0.600782 11.00000 0.02153 0.05078 =
0.02569 -0.00668 0.00385 -0.00927
O16 3 0.500000 0.376384 0.609886 10.50000 0.16373 0.01493 =
0.02340 -0.00240 0.00000 0.00000
O17 3 0.637733 0.507257 0.539442 11.00000 0.04044 0.03729 =
0.02715 -0.00803 0.00115 0.01058
O18 3 0.690544 0.554645 0.593440 11.00000 0.02631 0.05404 =
0.02213 -0.00690 -0.00036 0.01818
O19 3 0.573297 0.482258 0.596788 11.00000 0.05242 0.01896 =
0.02278 -0.00230 -0.00403 0.01280
O20 3 0.500000 0.550467 0.560585 10.50000 0.02863 0.02647 =
0.01967 -0.00315 0.00000 0.00000
O21 3 0.616908 0.625757 0.555335 11.00000 0.02285 0.02981 =
0.02110 -0.00268 0.00314 -0.00027
O24 3 0.500000 0.657739 0.654073 10.50000 0.02002 0.01297 =
0.01273 -0.00093 0.00000 0.00000
O22 3 0.500000 0.545617 0.646099 10.50000 0.03934 0.01530 =
0.01572 -0.00039 0.00000 0.00000
O23 3 0.570255 0.612475 0.611121 11.00000 0.01447 0.01894 =
0.01842 -0.00141 0.00092 0.00229
SAME N5 C51A C52A
SAME N4 C49 C50
N5 6 0.414896 0.572635 0.759502 11.00000 0.06551 0.07849 =
0.02323 0.01605 0.01164 0.04048
PART 5
C51 1 0.352059 0.561826 0.769455 21.00000 0.05707 0.06826 =
0.01603 0.00108 0.00476 0.03004
C52 1 0.278437 0.557638 0.784941 21.00000 0.05797 0.08218 =
0.03009 -0.00322 0.02102 0.01017
AFIX 33
H52A 2 0.249942 0.524363 0.776393 21.00000 -1.50000
H52B 2 0.250905 0.594987 0.782022 21.00000 -1.50000
H52C 2 0.286156 0.550818 0.806569 21.00000 -1.50000
AFIX 0
PART 6
C51A 1 0.371945 0.591654 0.775857 -21.00000 0.05303 0.05589 =
0.01785 -0.00165 0.00182 0.02827
C52A 1 0.304494 0.604430 0.792871 -21.00000 0.04144 0.07318 =
0.03141 -0.00940 0.00670 0.01279
AFIX 33
H52D 2 0.314266 0.636642 0.807323 -21.00000 -1.50000
H52E 2 0.288829 0.568480 0.803784 -21.00000 -1.50000
H52F 2 0.264983 0.616769 0.778960 -21.00000 -1.50000
AFIX 0
SAME N2 > C32
SAME N3 > C48
SAME N1 C5 > C16 C1 > C4
SAME N1 C13 > C16 C9 > C12 C5 > C8 C1 > C4
PART -1
N1 6 0.536238 0.330678 0.736223 10.50000 0.04642 0.02134 =
0.02666 0.00875 -0.00690 0.00075
C1 1 0.590468 0.326508 0.762781 10.50000 0.04914 0.02992 =
0.03188 0.00803 -0.01125 -0.00327
AFIX 23
H1A 2 0.563538 0.310051 0.780415 10.50000 -1.20000
H1B 2 0.630353 0.297880 0.757461 10.50000 -1.20000
AFIX 0
C2 1 0.626390 0.385551 0.772006 10.50000 0.05858 0.04272 =
0.03879 0.00222 -0.01571 -0.00943
AFIX 23
H2A 2 0.588234 0.412539 0.780598 10.50000 -1.20000
H2B 2 0.648281 0.405213 0.754065 10.50000 -1.20000
AFIX 0
C3 1 0.687272 0.373774 0.795525 10.50000 0.05167 0.05225 =
0.04542 0.00389 -0.01297 -0.01130
AFIX 23
H3A 2 0.703903 0.412403 0.804069 10.50000 -1.20000
H3B 2 0.666039 0.349767 0.812202 10.50000 -1.20000
AFIX 0
C4 1 0.753666 0.341371 0.782713 10.50000 0.04407 0.07407 =
0.06493 0.00072 -0.00471 -0.01374
AFIX 33
H4A 2 0.790249 0.334544 0.798751 10.50000 -1.50000
H4B 2 0.776195 0.365592 0.766710 10.50000 -1.50000
H4C 2 0.737718 0.302911 0.774351 10.50000 -1.50000
AFIX 0
C5 1 0.577370 0.347730 0.707681 10.50000 0.04384 0.02332 =
0.02949 0.00811 -0.00713 0.00896
AFIX 23
H5A 2 0.540520 0.352381 0.691237 10.50000 -1.20000
H5B 2 0.601006 0.387172 0.710897 10.50000 -1.20000
AFIX 0
C6 1 0.636563 0.304360 0.697287 10.50000 0.04662 0.03254 =
0.04224 0.00409 -0.00577 0.01359
AFIX 23
H6A 2 0.614342 0.264098 0.695209 10.50000 -1.20000
H6B 2 0.676187 0.302058 0.712767 10.50000 -1.20000
AFIX 0
C7 1 0.670790 0.322838 0.667235 10.50000 0.04305 0.03108 =
0.03160 -0.00079 -0.01005 0.01089
AFIX 23
H7A 2 0.631802 0.323014 0.651449 10.50000 -1.20000
H7B 2 0.690926 0.363868 0.668951 10.50000 -1.20000
AFIX 0
C8 1 0.732390 0.280659 0.658105 10.50000 0.04461 0.04186 =
0.05540 -0.00844 -0.00928 0.01308
AFIX 33
H8A 2 0.753664 0.293692 0.638829 10.50000 -1.50000
H8B 2 0.712260 0.240196 0.655926 10.50000 -1.50000
H8C 2 0.771219 0.280717 0.673636 10.50000 -1.50000
AFIX 0
C9 1 0.476970 0.377451 0.742385 10.50000 0.04931 0.02573 =
0.02699 0.00668 -0.00344 0.00200
AFIX 23
H9A 2 0.443318 0.379121 0.724712 10.50000 -1.20000
H9B 2 0.501674 0.416851 0.744022 10.50000 -1.20000
AFIX 0
C10 1 0.429753 0.368066 0.770564 10.50000 0.05241 0.03200 =
0.02520 0.01046 -0.00016 -0.00062
AFIX 23
H10A 2 0.393969 0.335240 0.766883 10.50000 -1.20000
H10B 2 0.462354 0.356028 0.787520 10.50000 -1.20000
AFIX 0
C11 1 0.387410 0.424073 0.779265 10.50000 0.05253 0.04225 =
0.03258 0.00728 0.00042 0.00370
AFIX 23
H11A 2 0.423295 0.456658 0.783312 10.50000 -1.20000
H11B 2 0.355632 0.436552 0.762135 10.50000 -1.20000
AFIX 0
C12 1 0.339533 0.414836 0.806694 10.50000 0.05066 0.07290 =
0.04736 0.00666 0.01282 0.00957
AFIX 33
H12A 2 0.313830 0.452188 0.811642 10.50000 -1.50000
H12B 2 0.370786 0.402742 0.823761 10.50000 -1.50000
H12C 2 0.302768 0.383555 0.802561 10.50000 -1.50000
AFIX 0
C13 1 0.500199 0.269640 0.733058 10.50000 0.05306 0.02190 =
0.03917 0.00525 -0.00753 -0.00330
AFIX 23
H13A 2 0.540087 0.239177 0.732286 10.50000 -1.20000
H13B 2 0.470374 0.261835 0.751428 10.50000 -1.20000
AFIX 0
C14 1 0.450662 0.261217 0.705896 10.50000 0.05919 0.02945 =
0.04029 0.00645 -0.00970 -0.00886
AFIX 23
H14A 2 0.411223 0.292089 0.706090 10.50000 -1.20000
H14B 2 0.480449 0.266754 0.687306 10.50000 -1.20000
AFIX 0
C15 1 0.415273 0.200529 0.705318 10.50000 0.08140 0.03796 =
0.04513 -0.00312 0.00217 -0.02480
AFIX 23
H15A 2 0.454944 0.169848 0.705511 10.50000 -1.20000
H15B 2 0.385296 0.195357 0.723884 10.50000 -1.20000
AFIX 0
C16 1 0.366803 0.190277 0.678695 10.50000 0.11403 0.06193 =
0.05841 0.00432 -0.01894 -0.03940
AFIX 33
H16A 2 0.345987 0.149851 0.679630 10.50000 -1.50000
H16B 2 0.396156 0.194661 0.660183 10.50000 -1.50000
H16C 2 0.326258 0.219550 0.678692 10.50000 -1.50000
AFIX 0
PART -2
N2 6 0.144658 0.423503 0.583287 10.50000 0.03355 0.02288 =
0.03228 0.00317 0.00092 -0.00669
C17 1 0.124276 0.482603 0.598152 10.50000 0.05476 0.02203 =
0.03805 0.00543 0.00426 -0.00844
AFIX 23
H17A 2 0.170635 0.505313 0.601885 10.50000 -1.20000
H17B 2 0.093849 0.506068 0.583782 10.50000 -1.20000
AFIX 0
C18 1 0.081730 0.477625 0.627814 10.50000 0.05651 0.03386 =
0.03762 -0.00257 0.00498 -0.00455
AFIX 23
H18A 2 0.046757 0.443516 0.626785 10.50000 -1.20000
H18B 2 0.117069 0.470121 0.644532 10.50000 -1.20000
AFIX 0
C19 1 0.038775 0.534822 0.633947 10.50000 0.04670 0.04025 =
0.04407 -0.00876 0.00719 -0.00140
AFIX 23
H19A 2 0.073273 0.569163 0.632387 10.50000 -1.20000
H19B 2 0.000162 0.539707 0.618202 10.50000 -1.20000
AFIX 0
C20 1 0.002114 0.536044 0.664413 10.50000 0.07181 0.05799 =
0.04810 -0.00997 0.01250 -0.00058
AFIX 33
H20A 2 -0.025667 0.573437 0.666733 10.50000 -1.50000
H20B 2 0.040183 0.533361 0.680192 10.50000 -1.50000
H20C 2 -0.032093 0.502131 0.666190 10.50000 -1.50000
AFIX 0
C21 1 0.183985 0.382019 0.605616 10.50000 0.01729 0.01623 =
0.03569 0.00243 -0.00117 -0.01300
AFIX 23
H21A 2 0.148873 0.373093 0.622234 10.50000 -1.20000
H21B 2 0.194504 0.343872 0.595140 10.50000 -1.20000
AFIX 0
C22 1 0.256016 0.404139 0.619501 10.50000 0.03490 0.04123 =
0.03615 0.00255 -0.01337 -0.01364
AFIX 23
H22A 2 0.245133 0.435333 0.634719 10.50000 -1.20000
H22B 2 0.287855 0.421990 0.603651 10.50000 -1.20000
AFIX 0
C23 1 0.296730 0.352177 0.634418 10.50000 0.03694 0.04574 =
0.04255 0.00834 -0.01180 -0.01253
AFIX 23
H23A 2 0.335424 0.368372 0.648056 10.50000 -1.20000
H23B 2 0.260915 0.329444 0.646921 10.50000 -1.20000
AFIX 0
C24 1 0.332655 0.310333 0.612474 10.50000 0.04987 0.07155 =
0.06798 0.00174 -0.00802 0.01222
AFIX 33
H24A 2 0.357690 0.278173 0.623528 10.50000 -1.50000
H24B 2 0.369196 0.332198 0.600328 10.50000 -1.50000
H24C 2 0.294607 0.293224 0.599194 10.50000 -1.50000
AFIX 0
C25 1 0.073404 0.391628 0.572915 10.50000 0.02872 0.02410 =
0.04094 -0.00090 -0.00180 -0.00506
AFIX 23
H25A 2 0.087218 0.350983 0.566110 10.50000 -1.20000
H25B 2 0.040499 0.387023 0.590686 10.50000 -1.20000
AFIX 0
C26 1 0.028947 0.420821 0.548068 10.50000 0.03144 0.02406 =
0.04671 -0.00089 -0.00122 -0.00433
AFIX 23
H26A 2 0.062383 0.431171 0.531096 10.50000 -1.20000
H26B 2 0.006402 0.458238 0.555708 10.50000 -1.20000
AFIX 0
C27 1 -0.032287 0.379084 0.536852 10.50000 0.03139 0.02842 =
0.05255 -0.00523 -0.00805 -0.00122
AFIX 23
H27A 2 -0.058171 0.361869 0.554559 10.50000 -1.20000
H27B 2 -0.069099 0.402912 0.525389 10.50000 -1.20000
AFIX 0
C28 1 -0.005639 0.329001 0.517217 10.50000 0.03225 0.04375 =
0.03932 -0.00233 -0.00774 -0.00056
AFIX 33
H28A 2 -0.048072 0.304291 0.511128 10.50000 -1.50000
H28B 2 0.030048 0.304489 0.528458 10.50000 -1.50000
H28C 2 0.018548 0.345448 0.499215 10.50000 -1.50000
AFIX 0
C29 1 0.193941 0.437794 0.556399 10.50000 0.03557 0.03607 =
0.03328 0.00468 -0.00030 -0.00912
AFIX 23
H29A 2 0.167544 0.466888 0.543413 10.50000 -1.20000
H29B 2 0.239642 0.457514 0.563901 10.50000 -1.20000
AFIX 0
C30 1 0.216325 0.385499 0.537320 10.50000 0.04453 0.04636 =
0.03893 -0.00365 0.00538 -0.01067
AFIX 23
H30A 2 0.175270 0.356015 0.537203 10.50000 -1.20000
H30B 2 0.260254 0.366091 0.546570 10.50000 -1.20000
AFIX 0
C31 1 0.234796 0.402128 0.505158 10.50000 0.05208 0.05978 =
0.03650 -0.00430 0.00790 -0.01903
AFIX 23
H31A 2 0.193483 0.426027 0.496635 10.50000 -1.20000
H31B 2 0.280099 0.427281 0.504992 10.50000 -1.20000
AFIX 0
C32 1 0.247410 0.348362 0.485689 10.50000 0.06904 0.10106 =
0.06160 -0.03475 0.02084 -0.02154
AFIX 33
H32A 2 0.258242 0.361183 0.464997 10.50000 -1.50000
H32B 2 0.202678 0.323330 0.485758 10.50000 -1.50000
H32C 2 0.289563 0.325392 0.493574 10.50000 -1.50000
AFIX 0
PART -3
N3 6 0.677274 0.340712 0.544504 10.50000 0.02762 0.02801 =
0.02642 0.00015 -0.00011 0.00716
C33 1 0.670278 0.276823 0.556529 10.50000 0.03045 0.02822 =
0.02575 0.00246 0.00013 0.00661
AFIX 23
H33A 2 0.652730 0.250825 0.539909 10.50000 -1.20000
H33B 2 0.720359 0.262698 0.562492 10.50000 -1.20000
AFIX 0
C34 1 0.618403 0.269153 0.583140 10.50000 0.03626 0.03797 =
0.03308 0.00676 0.00629 0.00196
AFIX 23
H34A 2 0.641682 0.286836 0.601318 10.50000 -1.20000
H34B 2 0.571601 0.291081 0.579134 10.50000 -1.20000
AFIX 0
C35 1 0.600622 0.204589 0.589235 10.50000 0.04374 0.04316 =
0.03909 0.00864 0.00991 -0.00097
AFIX 23
H35A 2 0.572416 0.188327 0.571886 10.50000 -1.20000
H35B 2 0.647768 0.181930 0.590783 10.50000 -1.20000
AFIX 0
C36 1 0.556186 0.194849 0.617571 10.50000 0.03304 0.05621 =
0.04903 0.01088 0.01433 -0.00012
AFIX 33
H36A 2 0.546644 0.152051 0.620185 10.50000 -1.50000
H36B 2 0.508761 0.216233 0.616036 10.50000 -1.50000
H36C 2 0.584192 0.209914 0.634960 10.50000 -1.50000
AFIX 0
C37 1 0.602076 0.363755 0.534773 10.50000 0.02868 0.03255 =
0.02512 0.00804 0.00128 0.00941
AFIX 23
H37A 2 0.609805 0.402596 0.524550 10.50000 -1.20000
H37B 2 0.572607 0.371726 0.553219 10.50000 -1.20000
AFIX 0
C38 1 0.555366 0.324957 0.514127 10.50000 0.03285 0.06422 =
0.02241 0.00599 -0.00075 0.00473
AFIX 23
H38A 2 0.546173 0.285847 0.523878 10.50000 -1.20000
H38B 2 0.582515 0.317767 0.495023 10.50000 -1.20000
AFIX 0
C39 1 0.481468 0.355456 0.507414 10.50000 0.03924 0.08508 =
0.03909 0.01703 -0.01283 0.00297
AFIX 23
H39A 2 0.491695 0.396153 0.499705 10.50000 -1.20000
H39B 2 0.456024 0.333034 0.491149 10.50000 -1.20000
AFIX 0
C40 1 0.429421 0.360334 0.533958 10.50000 0.03272 0.09657 =
0.07063 -0.01720 -0.00333 0.00487
AFIX 33
H40A 2 0.383901 0.381050 0.527737 10.50000 -1.50000
H40B 2 0.453650 0.382893 0.550171 10.50000 -1.50000
H40C 2 0.416857 0.320233 0.541232 10.50000 -1.50000
AFIX 0
C41 1 0.730713 0.337579 0.517808 10.50000 0.02608 0.02620 =
0.03095 -0.00201 0.00123 0.00508
AFIX 23
H41A 2 0.775859 0.315884 0.524420 10.50000 -1.20000
H41B 2 0.706967 0.313341 0.501788 10.50000 -1.20000
AFIX 0
C42 1 0.754866 0.396044 0.504025 10.50000 0.03039 0.02946 =
0.02662 -0.00208 -0.00016 -0.00356
AFIX 23
H42A 2 0.783422 0.419309 0.519093 10.50000 -1.20000
H42B 2 0.710405 0.419608 0.498348 10.50000 -1.20000
AFIX 0
C43 1 0.802782 0.385668 0.476216 10.50000 0.02476 0.03713 =
0.03062 -0.00085 0.00453 0.00010
AFIX 23
H43A 2 0.843803 0.358240 0.481725 10.50000 -1.20000
H43B 2 0.772167 0.365387 0.460719 10.50000 -1.20000
AFIX 0
C44 1 0.835736 0.440892 0.462508 10.50000 0.03020 0.03726 =
0.04369 0.00387 0.00761 -0.00325
AFIX 33
H44A 2 0.866709 0.429826 0.445180 10.50000 -1.50000
H44B 2 0.866343 0.461467 0.477578 10.50000 -1.50000
H44C 2 0.795698 0.467484 0.455803 10.50000 -1.50000
AFIX 0
C45 1 0.705393 0.382248 0.569056 10.50000 0.02558 0.03623 =
0.03795 -0.01301 0.00474 -0.00218
AFIX 23
H45A 2 0.704123 0.423452 0.560945 10.50000 -1.20000
H45B 2 0.669454 0.380647 0.585972 10.50000 -1.20000
AFIX 0
C46 1 0.782063 0.371788 0.581977 10.50000 0.03535 0.08122 =
0.04323 -0.02308 0.00447 -0.00249
AFIX 23
H46A 2 0.820278 0.375284 0.565980 10.50000 -1.20000
H46B 2 0.785378 0.331422 0.591015 10.50000 -1.20000
AFIX 0
C47 1 0.793704 0.419589 0.606031 10.50000 0.06457 0.11488 =
0.05557 -0.04079 -0.00728 -0.00429
AFIX 23
H47A 2 0.760424 0.453533 0.601239 10.50000 -1.20000
H47B 2 0.777077 0.402903 0.625599 10.50000 -1.20000
AFIX 0
C48 1 0.867973 0.443078 0.610135 10.50000 0.10516 0.13372 =
0.09618 -0.06217 0.03474 -0.05309
AFIX 33
H48A 2 0.867313 0.473784 0.625905 10.50000 -1.50000
H48B 2 0.885394 0.460690 0.591153 10.50000 -1.50000
H48C 2 0.901539 0.410677 0.616127 10.50000 -1.50000
AFIX 0
PART -4
N4 6 0.439695 0.089196 0.548404 10.50000 0.11862 0.06098 =
0.10590 0.02764 0.03399 0.00841
C49 1 0.409856 0.127563 0.561286 10.50000 0.07890 0.05939 =
0.07458 0.03006 0.02136 -0.00212
C50 1 0.373621 0.175595 0.578094 10.50000 0.06226 0.08596 =
0.06592 0.01378 0.00883 0.00859
AFIX 33
H50A 2 0.326948 0.160837 0.586763 10.50000 -1.50000
H50B 2 0.363079 0.209003 0.564448 10.50000 -1.50000
H50C 2 0.406529 0.189165 0.594346 10.50000 -1.50000
PART 0

HKLF 4

REM rje411 in Cmca
REM R1 = 0.0409 for 6224 Fo > 4sig(Fo) and 0.0607 for all 7887 data
REM 794 parameters refined using 1005 restraints

END

;