##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
# Software is freely available for graphical display of the structure(s) #
# in this CIF. For information consult the CIF software page #
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# #
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data_global
_audit_creation_method SHELXL-97
_journal_date_recd_electronic 2013-09-10
_journal_date_accepted 2013-09-26
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2013
_journal_volume 69
_journal_issue 11
_journal_page_first o1602
_journal_page_last o1602
_journal_paper_category QO
_journal_paper_doi 10.1107/S1600536813026561
_journal_coeditor_code HB7138
_publ_contact_author_name 'Devadasan Velmurugan'
_publ_contact_author_address
; CAS in Crystallography and Biophysics
University of madras
Maraimalai campus(guindy campus)
Chennai - 600 025
India.
;
_publ_contact_author_email 'shirai2011@gmail.com'
_publ_contact_author_fax '044 091 2499 3057'
_publ_contact_author_phone '044 091 24484170'
_publ_section_title
;
N-(4-Fluorophenyl)-2,6-dimethyl-1,3-dioxan-4-amine
;
loop_
_publ_author_name
_publ_author_address
' Gottimukkala Rambabu'
;
Chemistry Department
GEBH
Sree Vidyanikethan Engineering College
A. Rangampet
Tirupati 517 102
India
;
'Zeenat Fatima'
;
Centre of Advanced Study in Crystallography and Biophysics
University of Madras
Guindy Campus
Chennai 600 025
India
;
' Bandapalli Palakshi Reddy'
;
Chemistry Department
GEBH
Sree Vidyanikethan Engineering College
A. Rangampet
Tirupati 517 102
India
;
' Vijayaparthasarathi Vijayakumar'
;
Centre for Organic and Medicinal Chemistry
VIT University
Vellore 632 014
India
;
'Devadasan Velmurugan'
;
Centre of Advanced Study in Crystallography and Biophysics
University of Madras
Guindy Campus
Chennai 600 025
India
;
data_I
_database_code_depnum_ccdc_archive 'CCDC 963313'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
N-(4-Fluorophenyl)-2,6-dimethyl-1,3-dioxan-4-amine
;
_chemical_name_common ?
_chemical_formula_moiety 'C12 H16 F N O2'
_chemical_formula_sum 'C12 H16 F N O2'
_chemical_formula_iupac 'C12 H16 F N O2'
_chemical_formula_weight 225.26
_chemical_melting_point ?
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_space_group_name_Hall '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 10.4924(10)
_cell_length_b 10.0614(10)
_cell_length_c 11.0379(11)
_cell_angle_alpha 90.00
_cell_angle_beta 90.136(2)
_cell_angle_gamma 90.00
_cell_volume 1165.2(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2910
_cell_measurement_theta_min 2.68
_cell_measurement_theta_max 28.35
_cell_measurement_temperature 293(2)
_exptl_crystal_description Block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.15
_exptl_crystal_density_diffrn 1.284
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 480
_exptl_absorpt_coefficient_mu 0.098
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Bruker, 2008)'
_exptl_absorpt_correction_T_min 0.6485
_exptl_absorpt_correction_T_max 0.7457
_exptl_special_details
;
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART APEXII area-detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 10977
_diffrn_reflns_av_R_equivalents 0.0204
_diffrn_reflns_av_sigmaI/netI 0.0184
_diffrn_reflns_theta_min 2.68
_diffrn_reflns_theta_max 28.35
_diffrn_reflns_theta_full 28.35
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F^2^, conventional
R-factors R are based on F, with F set to zero for
negative F^2^. The threshold expression of F^2^ >
\s(F^2^) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F^2^ are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total 2910
_reflns_number_gt 2179
_reflns_threshold_expression I>2sigma(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0558
_refine_ls_R_factor_gt 0.0407
_refine_ls_wR_factor_gt 0.1141
_refine_ls_wR_factor_ref 0.1293
_refine_ls_goodness_of_fit_ref 1.014
_refine_ls_restrained_S_all 1.014
_refine_ls_number_reflns 2910
_refine_ls_number_parameters 147
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+0.1851P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.150
_refine_diff_density_min -0.183
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection 'APEX2 (Bruker, 2008)'
_computing_cell_refinement 'SAINT (Bruker, 2008)'
_computing_data_reduction 'SAINT (Bruker, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.85420(8) 0.16432(8) 0.95248(8) 0.0469(2) Uani d . 1 1 . .
O O2 0.91002(9) 0.28191(9) 0.77911(8) 0.0509(2) Uani d . 1 1 . .
C C3 0.91619(12) 0.04131(13) 0.77606(11) 0.0491(3) Uani d . 1 1 . .
H H3A 0.8970 -0.0356 0.7263 0.059 Uiso calc R 1 1 . .
H H3B 1.0045 0.0351 0.8018 0.059 Uiso calc R 1 1 . .
C C5 0.82700(12) 0.27629(12) 0.87937(12) 0.0482(3) Uani d . 1 1 . .
H H5 0.7386 0.2718 0.8509 0.058 Uiso calc R 1 1 . .
N N1 0.84979(10) -0.06797(11) 0.96310(10) 0.0525(3) Uani d . 1 1 . .
H H1 0.9177 -0.1148 0.9546 0.063 Uiso calc R 1 1 . .
C C4 0.83024(11) 0.04228(11) 0.88605(11) 0.0453(3) Uani d . 1 1 . .
H H4 0.7413 0.0421 0.8587 0.054 Uiso calc R 1 1 . .
C C2 0.89697(13) 0.16759(13) 0.70224(12) 0.0514(3) Uani d . 1 1 . .
H H2 0.8111 0.1669 0.6672 0.062 Uiso calc R 1 1 . .
F F1 0.49573(9) -0.21970(11) 1.30521(8) 0.0788(3) Uani d . 1 1 . .
C C7 0.76261(11) -0.10329(11) 1.05237(11) 0.0442(3) Uani d . 1 1 . .
C C8 0.77421(13) -0.22492(13) 1.11186(14) 0.0556(3) Uani d . 1 1 . .
H H8 0.8424 -0.2806 1.0939 0.067 Uiso calc R 1 1 . .
C C9 0.68551(15) -0.26374(15) 1.19728(14) 0.0622(4) Uani d . 1 1 . .
H H9 0.6935 -0.3450 1.2367 0.075 Uiso calc R 1 1 . .
C C12 0.66199(11) -0.02028(12) 1.08440(12) 0.0497(3) Uani d . 1 1 . .
H H12 0.6546 0.0628 1.0481 0.060 Uiso calc R 1 1 . .
C C11 0.57272(13) -0.05951(14) 1.16951(12) 0.0539(3) Uani d . 1 1 . .
H H11 0.5051 -0.0041 1.1898 0.065 Uiso calc R 1 1 . .
C C6 0.84563(15) 0.39947(14) 0.95358(14) 0.0630(4) Uani d . 1 1 . .
H H6A 0.9318 0.4026 0.9830 0.095 Uiso calc R 1 1 . .
H H6B 0.7879 0.3985 1.0209 0.095 Uiso calc R 1 1 . .
H H6C 0.8292 0.4763 0.9044 0.095 Uiso calc R 1 1 . .
C C10 0.58580(13) -0.18076(15) 1.22298(12) 0.0553(3) Uani d . 1 1 . .
C C1 0.99285(17) 0.18267(17) 0.60184(14) 0.0693(4) Uani d . 1 1 . .
H H1A 0.9765 0.2637 0.5585 0.104 Uiso calc R 1 1 . .
H H1B 0.9860 0.1086 0.5474 0.104 Uiso calc R 1 1 . .
H H1C 1.0772 0.1854 0.6357 0.104 Uiso calc R 1 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0494(5) 0.0386(4) 0.0529(5) -0.0015(3) -0.0005(4) 0.0021(3)
O2 0.0567(5) 0.0407(5) 0.0551(5) -0.0081(4) -0.0008(4) 0.0033(4)
C3 0.0510(7) 0.0415(6) 0.0550(7) -0.0041(5) 0.0010(5) -0.0027(5)
C5 0.0448(6) 0.0382(6) 0.0615(7) 0.0007(5) -0.0030(5) 0.0043(5)
N1 0.0438(5) 0.0426(5) 0.0712(7) 0.0076(4) 0.0087(5) 0.0123(5)
C4 0.0402(6) 0.0372(6) 0.0584(7) -0.0023(4) -0.0015(5) 0.0035(5)
C2 0.0558(7) 0.0469(7) 0.0514(7) -0.0082(5) -0.0057(6) 0.0004(5)
F1 0.0799(6) 0.0875(7) 0.0691(6) -0.0231(5) 0.0156(5) 0.0142(5)
C7 0.0412(6) 0.0360(6) 0.0555(7) -0.0029(4) -0.0031(5) 0.0024(5)
C8 0.0480(7) 0.0442(7) 0.0747(9) 0.0025(5) -0.0051(6) 0.0114(6)
C9 0.0643(8) 0.0516(7) 0.0705(9) -0.0076(6) -0.0097(7) 0.0214(7)
C12 0.0499(6) 0.0372(6) 0.0621(7) 0.0001(5) 0.0030(5) 0.0039(5)
C11 0.0503(7) 0.0510(7) 0.0603(8) -0.0029(5) 0.0048(6) -0.0042(6)
C6 0.0729(9) 0.0416(7) 0.0746(9) -0.0004(6) 0.0029(7) -0.0027(6)
C10 0.0554(7) 0.0602(8) 0.0502(7) -0.0158(6) 0.0003(6) 0.0050(6)
C1 0.0872(11) 0.0654(9) 0.0554(8) -0.0120(8) 0.0075(8) 0.0026(7)
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C5 . 1.4145(14) ?
O1 C4 . 1.4517(14) ?
O2 C5 . 1.4111(16) ?
O2 C2 . 1.4357(15) ?
C3 C4 . 1.5141(17) ?
C3 C2 . 1.5226(18) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C5 C6 . 1.4981(19) ?
C5 H5 . 0.9800 ?
N1 C7 . 1.3922(15) ?
N1 C4 . 1.4125(15) ?
N1 H1 . 0.8600 ?
C4 H4 . 0.9800 ?
C2 C1 . 1.5061(19) ?
C2 H2 . 0.9800 ?
F1 C10 . 1.3691(15) ?
C7 C8 . 1.3940(17) ?
C7 C12 . 1.3924(17) ?
C8 C9 . 1.383(2) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.369(2) ?
C9 H9 . 0.9300 ?
C12 C11 . 1.3856(17) ?
C12 H12 . 0.9300 ?
C11 C10 . 1.362(2) ?
C11 H11 . 0.9300 ?
C6 H6A . 0.9600 ?
C6 H6B . 0.9600 ?
C6 H6C . 0.9600 ?
C1 H1A . 0.9600 ?
C1 H1B . 0.9600 ?
C1 H1C . 0.9600 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C5 O1 C4 . . 110.55(9) ?
C5 O2 C2 . . 111.92(9) ?
C4 C3 C2 . . 110.20(10) ?
C4 C3 H3A . . 109.6 ?
C2 C3 H3A . . 109.6 ?
C4 C3 H3B . . 109.6 ?
C2 C3 H3B . . 109.6 ?
H3A C3 H3B . . 108.1 ?
O2 C5 O1 . . 110.80(9) ?
O2 C5 C6 . . 108.40(10) ?
O1 C5 C6 . . 108.73(11) ?
O2 C5 H5 . . 109.6 ?
O1 C5 H5 . . 109.6 ?
C6 C5 H5 . . 109.6 ?
C7 N1 C4 . . 122.13(10) ?
C7 N1 H1 . . 118.9 ?
C4 N1 H1 . . 118.9 ?
N1 C4 O1 . . 109.60(10) ?
N1 C4 C3 . . 113.06(10) ?
O1 C4 C3 . . 107.92(9) ?
N1 C4 H4 . . 108.7 ?
O1 C4 H4 . . 108.7 ?
C3 C4 H4 . . 108.7 ?
O2 C2 C1 . . 106.93(10) ?
O2 C2 C3 . . 109.87(10) ?
C1 C2 C3 . . 112.96(12) ?
O2 C2 H2 . . 109.0 ?
C1 C2 H2 . . 109.0 ?
C3 C2 H2 . . 109.0 ?
C8 C7 N1 . . 120.04(11) ?
C8 C7 C12 . . 118.19(12) ?
N1 C7 C12 . . 121.77(11) ?
C9 C8 C7 . . 120.73(13) ?
C9 C8 H8 . . 119.6 ?
C7 C8 H8 . . 119.6 ?
C10 C9 C8 . . 119.02(13) ?
C10 C9 H9 . . 120.5 ?
C8 C9 H9 . . 120.5 ?
C11 C12 C7 . . 121.03(12) ?
C11 C12 H12 . . 119.5 ?
C7 C12 H12 . . 119.5 ?
C10 C11 C12 . . 118.78(13) ?
C10 C11 H11 . . 120.6 ?
C12 C11 H11 . . 120.6 ?
C5 C6 H6A . . 109.5 ?
C5 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
C5 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
C11 C10 C9 . . 122.19(12) ?
C11 C10 F1 . . 118.33(13) ?
C9 C10 F1 . . 119.47(13) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 O2 C5 O1 . . . . 61.43(13) ?
C2 O2 C5 C6 . . . . -179.33(10) ?
C4 O1 C5 O2 . . . . -64.23(12) ?
C4 O1 C5 C6 . . . . 176.73(10) ?
C7 N1 C4 O1 . . . . 74.98(14) ?
C7 N1 C4 C3 . . . . -164.58(11) ?
C5 O1 C4 N1 . . . . -176.11(9) ?
C5 O1 C4 C3 . . . . 60.37(12) ?
C2 C3 C4 N1 . . . . -175.84(10) ?
C2 C3 C4 O1 . . . . -54.45(12) ?
C5 O2 C2 C1 . . . . -178.06(10) ?
C5 O2 C2 C3 . . . . -55.13(13) ?
C4 C3 C2 O2 . . . . 52.25(14) ?
C4 C3 C2 C1 . . . . 171.55(11) ?
C4 N1 C7 C8 . . . . 168.84(12) ?
C4 N1 C7 C12 . . . . -10.76(19) ?
N1 C7 C8 C9 . . . . -177.40(13) ?
C12 C7 C8 C9 . . . . 2.2(2) ?
C7 C8 C9 C10 . . . . -0.1(2) ?
C8 C7 C12 C11 . . . . -2.58(19) ?
N1 C7 C12 C11 . . . . 177.03(12) ?
C7 C12 C11 C10 . . . . 0.8(2) ?
C12 C11 C10 C9 . . . . 1.4(2) ?
C12 C11 C10 F1 . . . . -178.74(12) ?
C8 C9 C10 C11 . . . . -1.7(2) ?
C8 C9 C10 F1 . . . . 178.39(12) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1 F1 4_655 0.86 2.48 3.1556(14) 136
_iucr_refine_instructions_details
;
TITL PF in P2(1)/n
CELL 0.71073 10.4924 10.0614 11.0379 90.000 90.136 90.000
ZERR 4.00 0.0010 0.0010 0.0011 0.000 0.002 0.000
LATT 1
SYMM 1/2 - X, 1/2 + Y, 1/2 - Z
SFAC C H N O F
UNIT 48 64 4 8 4
MERG 2
FMAP 2
PLAN 20
BOND $H
ACTA
CONF
SIZE 0.20 0.25 0.30
EQIV $1 1/2+x,-1/2-y,-1/2+z
HTAB N1, F1_$1
L.S. 10
WGHT 0.064400 0.185100
FVAR 0.19287
MOLE 1
O1 4 0.854196 0.164315 0.952476 11.00000 0.04935 0.03857 =
0.05287 0.00212 -0.00051 -0.00155
O2 4 0.910015 0.281910 0.779114 11.00000 0.05675 0.04074 =
0.05511 0.00326 -0.00081 -0.00811
C3 1 0.916193 0.041306 0.776062 11.00000 0.05095 0.04152 =
0.05498 -0.00267 0.00100 -0.00414
AFIX 23
H3A 2 0.896968 -0.035622 0.726302 11.00000 -1.20000
H3B 2 1.004453 0.035079 0.801789 11.00000 -1.20000
AFIX 0
C5 1 0.826997 0.276294 0.879374 11.00000 0.04482 0.03816 =
0.06153 0.00430 -0.00300 0.00075
AFIX 13
H5 2 0.738570 0.271797 0.850882 11.00000 -1.20000
AFIX 0
N1 3 0.849790 -0.067974 0.963096 11.00000 0.04382 0.04259 =
0.07119 0.01228 0.00867 0.00759
AFIX 43
H1 2 0.917747 -0.114808 0.954585 11.00000 -1.20000
AFIX 0
C4 1 0.830243 0.042283 0.886046 11.00000 0.04022 0.03721 =
0.05836 0.00347 -0.00154 -0.00232
AFIX 13
H4 2 0.741330 0.042095 0.858655 11.00000 -1.20000
AFIX 0
C2 1 0.896971 0.167587 0.702239 11.00000 0.05575 0.04692 =
0.05139 0.00039 -0.00566 -0.00820
AFIX 13
H2 2 0.811071 0.166861 0.667192 11.00000 -1.20000
AFIX 0
F1 5 0.495727 -0.219703 1.305210 11.00000 0.07992 0.08751 =
0.06912 0.01424 0.01564 -0.02309
C7 1 0.762609 -0.103286 1.052372 11.00000 0.04117 0.03601 =
0.05549 0.00240 -0.00305 -0.00293
C8 1 0.774214 -0.224916 1.111859 11.00000 0.04795 0.04419 =
0.07475 0.01141 -0.00514 0.00246
AFIX 43
H8 2 0.842372 -0.280563 1.093895 11.00000 -1.20000
AFIX 0
C9 1 0.685514 -0.263744 1.197277 11.00000 0.06434 0.05162 =
0.07049 0.02144 -0.00974 -0.00759
AFIX 43
H9 2 0.693485 -0.345032 1.236678 11.00000 -1.20000
AFIX 0
C12 1 0.661990 -0.020276 1.084401 11.00000 0.04988 0.03721 =
0.06208 0.00388 0.00298 0.00014
AFIX 43
H12 2 0.654590 0.062789 1.048103 11.00000 -1.20000
AFIX 0
C11 1 0.572722 -0.059507 1.169511 11.00000 0.05033 0.05104 =
0.06031 -0.00422 0.00476 -0.00292
AFIX 43
H11 2 0.505122 -0.004067 1.189754 11.00000 -1.20000
AFIX 0
C6 1 0.845632 0.399469 0.953576 11.00000 0.07291 0.04163 =
0.07461 -0.00271 0.00293 -0.00044
AFIX 137
H6A 2 0.931755 0.402568 0.982996 11.00000 -1.50000
H6B 2 0.787919 0.398511 1.020929 11.00000 -1.50000
H6C 2 0.829162 0.476263 0.904354 11.00000 -1.50000
AFIX 0
C10 1 0.585797 -0.180761 1.222983 11.00000 0.05538 0.06024 =
0.05016 0.00498 0.00028 -0.01584
C1 1 0.992846 0.182674 0.601842 11.00000 0.08718 0.06544 =
0.05538 0.00256 0.00750 -0.01199
AFIX 137
H1A 2 0.976506 0.263651 0.558508 11.00000 -1.50000
H1B 2 0.985960 0.108637 0.547356 11.00000 -1.50000
H1C 2 1.077183 0.185350 0.635666 11.00000 -1.50000
HKLF 4
REM PF in P2(1)/n
REM R1 = 0.0407 for 2179 Fo > 4sig(Fo) and 0.0558 for all 2910 data
REM 147 parameters refined using 0 restraints
END
WGHT 0.0530 0.1890
REM Highest difference peak 0.150, deepest hole -0.183, 1-sigma level 0.035
Q1 1 0.8628 0.0400 0.8219 11.00000 0.05 0.15
Q2 1 0.7256 -0.0565 1.0810 11.00000 0.05 0.15
Q3 1 1.0637 0.1464 0.6280 11.00000 0.05 0.14
Q4 1 0.9352 -0.0819 0.9876 11.00000 0.05 0.14
Q5 1 0.7826 -0.1502 1.1076 11.00000 0.05 0.14
Q6 1 0.8178 -0.0670 1.0268 11.00000 0.05 0.14
Q7 1 0.5706 -0.2513 1.3203 11.00000 0.05 0.14
Q8 1 0.9323 0.1697 0.6414 11.00000 0.05 0.13
Q9 1 0.6410 -0.0323 1.1522 11.00000 0.05 0.12
Q10 1 0.6607 -0.2007 1.2392 11.00000 0.05 0.12
Q11 1 0.7460 -0.2208 1.1756 11.00000 0.05 0.12
Q12 1 0.9116 0.1070 0.7381 11.00000 0.05 0.11
Q13 1 0.7428 0.2484 0.8067 11.00000 0.05 0.11
Q14 1 0.5588 -0.1395 1.1689 11.00000 0.05 0.10
Q15 1 0.6075 -0.1051 1.2292 11.00000 0.05 0.10
Q16 1 0.7115 -0.2515 1.1236 11.00000 0.05 0.10
Q17 1 0.6896 -0.0784 1.0438 11.00000 0.05 0.09
Q18 1 0.6183 0.0463 1.0050 11.00000 0.05 0.09
Q19 1 0.8427 0.3976 1.0606 11.00000 0.05 0.09
Q20 1 0.9192 0.3792 1.0247 11.00000 0.05 0.09
;