# Ms. No.:
#
# Title: Exceptional Steric Congestion in an in,in-Bis(hydrosilane)
#
# Authors: Jie Zong, Joel T. Mague, and Robert A. Pascal, Jr.
#
# Contents: This file (rap059_0m_a.cif) contains CIF data for compound 2
#
#=======================================================================
data_global
#=======================================================================
_audit_creation_date 'July 12, 2013'
_audit_creation_method
;
APEX2 v2013.4-1 and manual editing
;
_audit_update_record
;
June 13, 2013 Initial CIF created by JTM.
July 12, 2013 Sent to CheckCIF See rp059_0m_a_checkcif.pdf for alerts
that were generated. Comments on these
alerts are given below.
------------------------------------------------------------------------
ALERT level A = In general: serious problem
ALERT level B = Potentially serious problem
ALERT level C = Check and explain
ALERT level G = General alerts; check
------------------------------------------------------------------------
PLAT410_ALERT_2_B Short Intra H...H Contact H1A .. H2A .. 1.88 Ang.
Comment/Explanation:
The extraordinarily close H...H contact is the point of the paper!!
------------------------------------------------------------------------
PLAT420_ALERT_2_C D-H Without Acceptor Si1 - H1A ... ? Check
PLAT420_ALERT_2_C D-H Without Acceptor Si2 - H2A ... ? Check
Comment/Explanation:
Hydrosilanes are not hydrogen bond donors!!
------------------------------------------------------------------------
DIFMN02_ALERT_2_B The minimum difference density is < -0.1*ZMAX*1.00
_refine_diff_density_min given = -1.835
Test value = -1.700
DIFMX01_ALERT_2_C The maximum difference density is > 0.1*ZMAX*0.75
_refine_diff_density_max given = 1.382
Test value = 1.275
PLAT098_ALERT_2_B Large Reported Min. (Negative) Resid. Dens. -1.84 eA-3
PLAT097_ALERT_2_C Large Reported Max. (Positive) Resid. Dens. 1.38 eA-3
DIFMN03_ALERT_1_C The minimum difference density is < -0.1*ZMAX*0.75
The relevant atom site should be identified.
DIFMX02_ALERT_1_C The maximum difference density is > 0.1*ZMAX*0.75
The relevant atom site should be identified.
Comment/Explanation:
The large difference density peaks are located on the C3 axis in
the region of the included solvent molecules. Large difference
density peaks on special positions in trigonal and hexagonal
space groups seem to be common artifacts of refinement.
------------------------------------------------------------------------
PLAT340_ALERT_3_C Low Bond Precision on C-C Bonds .......... 0.0095 Ang.
Comment/Explanation:
The low precision bond is for the benzene included solvent only.
------------------------------------------------------------------------
RFACR01_ALERT_3_C The value of the weighted R factor is > 0.25
Weighted R factor given 0.254
Comment/Explanation:
The difference is not significant.
------------------------------------------------------------------------
;
_publ_section_references
;
Brandenburg, K. & Putz, H. (2012). DIAMOND, Crystal Impact GbR,
Bonn, Germany.
Bruker AXS (2008). SHELXTL, Madison, WI.
Bruker AXS (2013). APEX2, Madison, WI.
Bruker AXS (2013a). SAINT, Madison, WI.
Bruker AXS (2013b). SADABS, Madison, WI.
Bruker AXS (2013c). SHELXT, Madison, WI.
Sheldrick, G, M. (2008). CELL_NOW, University
of G\"ottingen, Germany.
Sheldrick, G, M. (2009). TWINABS, University
of G\"ottingen, Germany.
Sheldrick, G, M. (2013). SHELXL--2013, University
of G\"ottingen, Germany.
;
_publ_section_comment
;
;
#=======================================================================
data_rap059_0m_a
#=======================================================================
_audit_creation_method SHELXL-2013
_chemical_name_systematic
;
?
;
_chemical_name_common 'in,in-bis(hydrosilane)'
_chemical_melting_point ?
_chemical_formula_moiety
'C39 H32 S3 Si2, 0.5(C6 H6), C H Cl3'
_chemical_formula_sum
'C43 H36 Cl3 S3 Si2'
_chemical_formula_weight 811.43
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091
'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'
'Si' 'Si' 0.2541 0.3302
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'S' 'S' 0.3331 0.5567
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.3639 0.7018
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system trigonal
_space_group_IT_number 147
_space_group_name_H-M_alt 'P -3'
_space_group_name_Hall '-P 3'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
_cell_length_a 14.0183(5)
_cell_length_b 14.0183(5)
_cell_length_c 11.3948(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 1939.22(16)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9982
_cell_measurement_theta_min 3.8793
_cell_measurement_theta_max 66.7086
_exptl_crystal_description plate
_exptl_crystal_colour colourless
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_density_diffrn 1.390
_exptl_crystal_F_000 842
_exptl_transmission_factor_min 0.639
_exptl_transmission_factor_max 0.979
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.02
_exptl_absorpt_coefficient_mu 4.482
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.64
_exptl_absorpt_correction_T_max 0.98
_exptl_absorpt_process_details 'TWINABS (Sheldrick, 2009)'
_exptl_special_details
;
Analysis of 769 reflections having I/\s(I) > 13 and chosen from
the full data set with CELL_NOW (Sheldrick, 2008) showed the
crystal to belong to the trigonal system and to be twinned by a
180 \% rotation about a*. The raw data were processed using
the multi-component version of SAINT under control of the
two-component orientation file generated by CELL_NOW.
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_radiation_monochromator mirror
_diffrn_source 'INCOATEC I\mS micro--focus source'
_diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number 4981
_diffrn_reflns_av_unetI/netI 0.0353
_diffrn_reflns_av_R_equivalents ?
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 3.641
_diffrn_reflns_theta_max 66.703
_diffrn_reflns_theta_full 66.700
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total 4981
_reflns_number_gt 4366
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'APEX2 (Bruker AXS, 2013)'
_computing_cell_refinement 'SAINT (Bruker AXS, 2013a)'
_computing_data_reduction 'SAINT (Bruker AXS, 2013a)'
_computing_structure_solution 'SHELXT (Bruker AXS 2013c)'
_computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics
'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material 'SHELXTL (Bruker AXS, 2008)'
_refine_special_details
;
Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.1414P)^2^+4.7553P]
where P=(Fo^2^+2Fc^2^)/3
;
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 4981
_refine_ls_number_parameters 157
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0905
_refine_ls_R_factor_gt 0.0822
_refine_ls_wR_factor_ref 0.2544
_refine_ls_wR_factor_gt 0.2456
_refine_ls_goodness_of_fit_ref 1.094
_refine_ls_restrained_S_all 1.109
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.80616(10) 0.23620(10) 0.52699(11) 0.0234(4) Uani 1 1 d . . . . .
Si1 Si 0.6667 0.3333 0.3847(2) 0.0194(6) Uani 1 3 d S T P . .
H1A H 0.6667 0.3333 0.496(9) 0.023 Uiso 1 3 d S U P . .
Si2 Si 0.6667 0.3333 0.7738(2) 0.0211(6) Uani 1 3 d S T P . .
H2A H 0.6667 0.3333 0.661(9) 0.025 Uiso 1 3 d S U P . .
C1 C 0.8027(4) 0.3541(4) 0.3308(4) 0.0214(10) Uani 1 1 d . . . . .
C2 C 0.8511(4) 0.4129(4) 0.2282(5) 0.0262(11) Uani 1 1 d . . . . .
H2 H 0.8161 0.4459 0.1869 0.031 Uiso 1 1 calc R U . . .
C3 C 0.9490(4) 0.4247(4) 0.1845(5) 0.0284(12) Uani 1 1 d . . . . .
H3 H 0.9801 0.4647 0.1142 0.034 Uiso 1 1 calc R U . . .
C4 C 1.0003(4) 0.3773(4) 0.2448(5) 0.0293(12) Uani 1 1 d . . . . .
H4 H 1.0666 0.3839 0.2149 0.035 Uiso 1 1 calc R U . . .
C5 C 0.9564(4) 0.3209(4) 0.3475(5) 0.0262(11) Uani 1 1 d . . . . .
H5 H 0.9931 0.2897 0.3889 0.031 Uiso 1 1 calc R U . . .
C6 C 0.8578(4) 0.3093(4) 0.3917(4) 0.0214(10) Uani 1 1 d . . . . .
C7 C 0.8775(4) 0.3503(4) 0.6316(4) 0.0237(11) Uani 1 1 d . . . . .
H7A H 0.9576 0.3902 0.6152 0.028 Uiso 1 1 calc R U . . .
H7B H 0.8501 0.4028 0.6232 0.028 Uiso 1 1 calc R U . . .
C8 C 0.8564(4) 0.3042(4) 0.7561(5) 0.0239(11) Uani 1 1 d . . . . .
C9 C 0.9274(4) 0.2697(4) 0.8009(5) 0.0300(12) Uani 1 1 d . . . . .
H9 H 0.9854 0.2752 0.7530 0.036 Uiso 1 1 calc R U . . .
C10 C 0.9146(5) 0.2281(5) 0.9132(5) 0.0323(13) Uani 1 1 d . . . . .
H10 H 0.9648 0.2071 0.9426 0.039 Uiso 1 1 calc R U . . .
C11 C 0.8287(5) 0.2169(4) 0.9831(5) 0.0297(12) Uani 1 1 d . . . . .
H11 H 0.8190 0.1875 1.0601 0.036 Uiso 1 1 calc R U . . .
C12 C 0.7570(4) 0.2492(4) 0.9387(5) 0.0257(11) Uani 1 1 d . . . . .
H12 H 0.6979 0.2413 0.9865 0.031 Uiso 1 1 calc R U . . .
C13 C 0.7691(4) 0.2935(4) 0.8253(4) 0.0223(11) Uani 1 1 d . . . . .
C14 C 0.9494(8) 0.8858(7) 0.5025(12) 0.087(3) Uani 1 1 d . U . . .
H14 H 0.9150 0.8079 0.5094 0.105 Uiso 1 1 calc R U . . .
C15 C 1.0000 1.0000 0.772(2) 0.094(7) Uani 1 3 d S T P . .
H15 H 1.0000 1.0000 0.6846 0.112 Uiso 1 3 calc R U P . .
Cl1 Cl 0.86847(19) 0.97121(18) 0.8153(3) 0.0895(10) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0246(7) 0.0203(6) 0.0258(7) 0.0022(5) 0.0010(5) 0.0117(5)
Si1 0.0195(7) 0.0195(7) 0.0193(11) 0.000 0.000 0.0097(4)
Si2 0.0228(8) 0.0228(8) 0.0177(11) 0.000 0.000 0.0114(4)
C1 0.020(2) 0.020(2) 0.022(2) -0.0029(19) -0.0016(19) 0.009(2)
C2 0.027(3) 0.025(3) 0.024(3) -0.003(2) -0.002(2) 0.011(2)
C3 0.025(3) 0.028(3) 0.022(3) -0.002(2) 0.004(2) 0.005(2)
C4 0.020(2) 0.031(3) 0.034(3) -0.005(2) 0.003(2) 0.011(2)
C5 0.019(2) 0.025(3) 0.034(3) -0.003(2) -0.001(2) 0.011(2)
C6 0.019(2) 0.017(2) 0.026(2) -0.0027(19) 0.0000(19) 0.0073(19)
C7 0.021(2) 0.024(2) 0.025(3) 0.001(2) 0.002(2) 0.011(2)
C8 0.022(2) 0.019(2) 0.027(3) 0.000(2) -0.001(2) 0.007(2)
C9 0.024(3) 0.031(3) 0.036(3) -0.001(2) 0.000(2) 0.014(2)
C10 0.030(3) 0.031(3) 0.036(3) 0.000(2) -0.009(2) 0.016(2)
C11 0.036(3) 0.026(3) 0.025(3) -0.001(2) -0.007(2) 0.014(2)
C12 0.029(3) 0.024(3) 0.024(3) -0.003(2) -0.002(2) 0.013(2)
C13 0.023(2) 0.020(2) 0.022(2) -0.0022(19) -0.002(2) 0.009(2)
C14 0.062(5) 0.041(4) 0.163(9) -0.002(5) -0.007(5) 0.030(4)
C15 0.055(6) 0.055(6) 0.17(2) 0.000 0.000 0.028(3)
Cl1 0.0524(12) 0.0580(13) 0.158(3) 0.0026(15) 0.0066(14) 0.0278(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C6 1.792(5) . ?
S1 C7 1.839(5) . ?
Si1 C1 1.882(5) 3_665 ?
Si1 C1 1.882(5) 2_655 ?
Si1 C1 1.882(5) . ?
Si1 H1A 1.26(10) . ?
Si2 C13 1.876(5) . ?
Si2 C13 1.876(5) 3_665 ?
Si2 C13 1.876(5) 2_655 ?
Si2 H2A 1.28(10) . ?
C1 C2 1.397(7) . ?
C1 C6 1.399(7) . ?
C2 C3 1.389(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(7) . ?
C5 H5 0.9500 . ?
C7 C8 1.526(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C13 1.399(7) . ?
C8 C9 1.402(7) . ?
C9 C10 1.381(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.407(7) . ?
C12 H12 0.9500 . ?
C14 C14 1.391(9) 6_656 ?
C14 C14 1.391(9) 5_566 ?
C14 H14 0.9500 . ?
C15 Cl1 1.749(8) . ?
C15 Cl1 1.749(8) 3_675 ?
C15 Cl1 1.749(8) 2_765 ?
C15 H15 1.0000 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 S1 C7 99.9(2) . . ?
C1 Si1 C1 109.90(16) 3_665 2_655 ?
C1 Si1 C1 109.90(16) 3_665 . ?
C1 Si1 C1 109.90(16) 2_655 . ?
C1 Si1 H1A 109.04(16) 3_665 . ?
C1 Si1 H1A 109.04(16) 2_655 . ?
C1 Si1 H1A 109.04(16) . . ?
C13 Si2 C13 110.69(16) . 3_665 ?
C13 Si2 C13 110.69(16) . 2_655 ?
C13 Si2 C13 110.69(16) 3_665 2_655 ?
C13 Si2 H2A 108.22(17) . . ?
C13 Si2 H2A 108.22(17) 3_665 . ?
C13 Si2 H2A 108.22(17) 2_655 . ?
C2 C1 C6 117.7(5) . . ?
C2 C1 Si1 121.4(4) . . ?
C6 C1 Si1 120.9(4) . . ?
C3 C2 C1 122.0(5) . . ?
C3 C2 H2 119.0 . . ?
C1 C2 H2 119.0 . . ?
C4 C3 C2 119.1(5) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C5 C4 C3 120.6(5) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.3(5) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C5 120.3(5) . . ?
C1 C6 S1 121.8(4) . . ?
C5 C6 S1 117.9(4) . . ?
C8 C7 S1 109.1(3) . . ?
C8 C7 H7A 109.9 . . ?
S1 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
S1 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C13 C8 C9 119.5(5) . . ?
C13 C8 C7 122.9(5) . . ?
C9 C8 C7 117.6(5) . . ?
C10 C9 C8 121.2(5) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 120.2(5) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C12 118.9(5) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C11 C12 C13 122.1(5) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 H12 119.0 . . ?
C8 C13 C12 118.1(5) . . ?
C8 C13 Si2 123.4(4) . . ?
C12 C13 Si2 118.5(4) . . ?
C14 C14 C14 119.83(18) 6_656 5_566 ?
C14 C14 H14 120.1 6_656 . ?
C14 C14 H14 120.1 5_566 . ?
Cl1 C15 Cl1 112.5(8) . 3_675 ?
Cl1 C15 Cl1 112.5(8) . 2_765 ?
Cl1 C15 Cl1 112.5(8) 3_675 2_765 ?
Cl1 C15 H15 106.2 . . ?
Cl1 C15 H15 106.2 3_675 . ?
Cl1 C15 H15 106.2 2_765 . ?
_refine_diff_density_max 1.382
_refine_diff_density_min -1.835
_refine_diff_density_rms 0.157
_shelxl_version_number 2013-2
_shelx_res_file
;
TITL rap059_0m in P-3
CELL 1.54178 14.0183 14.0183 11.3948 90.000 90.000 120.000
ZERR 2.00 0.0005 0.0005 0.0005 0.000 0.000 0.000
LATT 1
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SFAC C H Si S Cl
UNIT 86 72 4 6 6
L.S. 5
ACTA 133.4
SHEL 999 0.839
BOND $H
FMAP 2
PLAN 5
ISOR 0.008 C14
TEMP -173
WGHT 0.141400 4.755300
BASF 0.42465
FVAR 0.38806
S1 4 0.806158 0.236202 0.526994 11.00000 0.02456 0.02031 =
0.02584 0.00222 0.00105 0.01172
SI1 3 0.666667 0.333333 0.384734 10.33333 0.01946 0.01946 =
0.01933 0.00000 0.00000 0.00973
H1A 2 0.666667 0.333333 0.495595 10.33333 -1.20000
SI2 3 0.666667 0.333333 0.773770 10.33333 0.02278 0.02278 =
0.01767 0.00000 0.00000 0.01139
H2A 2 0.666667 0.333333 0.661038 10.33333 -1.20000
C1 1 0.802698 0.354125 0.330849 11.00000 0.02050 0.02000 =
0.02182 -0.00295 -0.00158 0.00869
C2 1 0.851147 0.412937 0.228160 11.00000 0.02674 0.02489 =
0.02409 -0.00340 -0.00223 0.01067
AFIX 43
H2 2 0.816137 0.445915 0.186902 11.00000 -1.20000
AFIX 0
C3 1 0.948958 0.424675 0.184525 11.00000 0.02458 0.02787 =
0.02241 -0.00216 0.00399 0.00534
AFIX 43
H3 2 0.980099 0.464695 0.114203 11.00000 -1.20000
AFIX 0
C4 1 1.000348 0.377350 0.244794 11.00000 0.02044 0.03096 =
0.03401 -0.00537 0.00274 0.01093
AFIX 43
H4 2 1.066630 0.383862 0.214948 11.00000 -1.20000
AFIX 0
C5 1 0.956416 0.320936 0.347547 11.00000 0.01947 0.02517 =
0.03422 -0.00350 -0.00134 0.01125
AFIX 43
H5 2 0.993055 0.289689 0.388882 11.00000 -1.20000
AFIX 0
C6 1 0.857773 0.309284 0.391651 11.00000 0.01860 0.01704 =
0.02639 -0.00266 0.00004 0.00728
C7 1 0.877510 0.350333 0.631599 11.00000 0.02111 0.02358 =
0.02547 0.00108 0.00196 0.01056
AFIX 23
H7A 2 0.957600 0.390248 0.615248 11.00000 -1.20000
H7B 2 0.850105 0.402796 0.623224 11.00000 -1.20000
AFIX 0
C8 1 0.856370 0.304156 0.756115 11.00000 0.02211 0.01875 =
0.02691 -0.00031 -0.00135 0.00729
C9 1 0.927425 0.269728 0.800876 11.00000 0.02355 0.03096 =
0.03605 -0.00069 -0.00027 0.01406
AFIX 43
H9 2 0.985446 0.275157 0.753044 11.00000 -1.20000
AFIX 0
C10 1 0.914615 0.228082 0.913188 11.00000 0.03049 0.03074 =
0.03639 -0.00016 -0.00864 0.01583
AFIX 43
H10 2 0.964828 0.207055 0.942641 11.00000 -1.20000
AFIX 0
C11 1 0.828659 0.216876 0.983085 11.00000 0.03600 0.02636 =
0.02466 -0.00096 -0.00669 0.01404
AFIX 43
H11 2 0.818955 0.187508 1.060118 11.00000 -1.20000
AFIX 0
C12 1 0.757012 0.249241 0.938732 11.00000 0.02917 0.02375 =
0.02360 -0.00345 -0.00199 0.01286
AFIX 43
H12 2 0.697902 0.241255 0.986486 11.00000 -1.20000
AFIX 0
C13 1 0.769134 0.293513 0.825272 11.00000 0.02346 0.01979 =
0.02163 -0.00221 -0.00163 0.00940
C14 1 0.949415 0.885762 0.502521 11.00000 0.06192 0.04149 =
0.16272 -0.00226 -0.00720 0.02951
AFIX 43
H14 2 0.914957 0.807945 0.509387 11.00000 -1.20000
AFIX 0
C15 1 1.000000 1.000000 0.772374 10.33333 0.05518 0.05518 =
0.17065 0.00000 0.00000 0.02759
AFIX 13
H15 2 0.999999 1.000000 0.684615 10.33333 -1.20000
AFIX 0
CL1 5 0.868469 0.971205 0.815280 11.00000 0.05242 0.05796 =
0.15836 0.00262 0.00661 0.02781
HKLF 5
REM rap059_0m in P-3
REM R1 = 0.0822 for 4366 Fo > 4sig(Fo) and 0.0905 for all 4981 data
REM 157 parameters refined using 6 restraints
END
WGHT 0.1415 4.7569
REM Highest difference peak 1.382, deepest hole -1.835, 1-sigma level 0.157
Q1 1 1.0000 1.0000 1.0000 10.16667 0.05 1.38
Q2 1 0.9462 0.8815 0.4130 11.00000 0.05 0.69
Q3 1 0.9283 0.8805 0.5883 11.00000 0.05 0.63
Q4 1 0.6772 0.3859 0.7923 11.00000 0.05 0.62
Q5 1 0.7595 0.3434 0.3402 11.00000 0.05 0.61
;
_shelx_res_checksum 1446
#========================= END DATA_rap059_0m_a ========================
# The following lines are used to test the character set of files sent
# by email or other means. They are not part of the CIF data set.
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./
#=======================================================================
# END of CIF
#=======================================================================