# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
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data_s16rlw5-Cpd-1b
_database_code_depnum_ccdc_archive 'CCDC 1849265'
_audit_update_record
;
2018-06-14 deposited with the CCDC.
2018-08-22 downloaded from the CCDC.
;
_audit_creation_date 2018-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number 2014-3
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C29 H28 O2 P2'
_chemical_formula_sum 'C29 H28 O2 P2'
_chemical_formula_weight 470.45
_chemical_melting_point ?
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.8918(3)
_cell_length_b 11.8798(7)
_cell_length_c 12.5977(6)
_cell_angle_alpha 117.242(5)
_cell_angle_beta 103.910(3)
_cell_angle_gamma 98.150(4)
_cell_volume 1222.00(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6731
_cell_measurement_temperature 150.03(10)
_cell_measurement_theta_max 73.2470
_cell_measurement_theta_min 4.2280
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.799
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.27655
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.279
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description rhomboid
_exptl_crystal_F_000 496
_exptl_crystal_size_max 0.666
_exptl_crystal_size_mid 0.271
_exptl_crystal_size_min 0.188
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0292
_diffrn_reflns_av_unetI/netI 0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 10428
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 73.343
_diffrn_reflns_theta_min 4.209
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 150.03(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4456
_reflns_number_total 4843
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 0.526
_refine_diff_density_min -0.333
_refine_diff_density_rms 0.046
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 299
_refine_ls_number_reflns 4843
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0390
_refine_ls_R_factor_gt 0.0360
_refine_ls_restrained_S_all 1.042
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.3590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0965
_refine_ls_wR_factor_ref 0.0989
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C25(H25)
2.b Secondary CH2 refined with riding coordinates:
C26(H26A,H26B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
C22(H22), C23(H23), C24(H24)
2.d Idealised Me refined as rotating group:
C29(H29A,H29B,H29C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
P1 P 0.36241(4) 0.32735(3) 0.56291(3) 0.02271(10) Uani 1 1 d . . . . .
P2 P 0.39220(4) 0.27546(3) 0.77363(3) 0.02173(10) Uani 1 1 d . . . . .
O1 O 0.13855(11) -0.06638(11) 0.52557(11) 0.0302(2) Uani 1 1 d . . . . .
O2 O 0.30534(12) -0.15132(11) 0.44663(11) 0.0314(2) Uani 1 1 d . . . . .
C1 C 0.24058(15) 0.26475(14) 0.39981(14) 0.0232(3) Uani 1 1 d . . . . .
C2 C 0.29283(17) 0.31562(17) 0.33261(16) 0.0316(3) Uani 1 1 d . . . . .
H2 H 0.3824 0.3800 0.3726 0.038 Uiso 1 1 calc R . . . .
C3 C 0.21330(19) 0.27171(19) 0.20701(17) 0.0369(4) Uani 1 1 d . . . . .
H3 H 0.2487 0.3085 0.1643 0.044 Uiso 1 1 calc R . . . .
C4 C 0.08205(18) 0.17384(18) 0.14524(15) 0.0339(4) Uani 1 1 d . . . . .
H4 H 0.0298 0.1430 0.0604 0.041 Uiso 1 1 calc R . . . .
C5 C 0.02860(18) 0.12182(17) 0.21040(16) 0.0338(4) Uani 1 1 d . . . . .
H5 H -0.0600 0.0560 0.1691 0.041 Uiso 1 1 calc R . . . .
C6 C 0.10649(17) 0.16736(16) 0.33728(15) 0.0297(3) Uani 1 1 d . . . . .
H6 H 0.0689 0.1327 0.3806 0.036 Uiso 1 1 calc R . . . .
C7 C 0.29226(16) 0.45800(14) 0.66054(14) 0.0237(3) Uani 1 1 d . . . . .
C8 C 0.14647(17) 0.45613(16) 0.62930(16) 0.0322(3) Uani 1 1 d . . . . .
H8 H 0.0781 0.3867 0.5531 0.039 Uiso 1 1 calc R . . . .
C9 C 0.10304(19) 0.55771(17) 0.71171(18) 0.0385(4) Uani 1 1 d . . . . .
H9 H 0.0059 0.5565 0.6898 0.046 Uiso 1 1 calc R . . . .
C10 C 0.2037(2) 0.66057(16) 0.82612(17) 0.0359(4) Uani 1 1 d . . . . .
H10 H 0.1739 0.7273 0.8819 0.043 Uiso 1 1 calc R . . . .
C11 C 0.34905(19) 0.66399(16) 0.85752(16) 0.0339(4) Uani 1 1 d . . . . .
H11 H 0.4170 0.7332 0.9341 0.041 Uiso 1 1 calc R . . . .
C12 C 0.39281(17) 0.56391(15) 0.77442(15) 0.0285(3) Uani 1 1 d . . . . .
H12 H 0.4908 0.5676 0.7951 0.034 Uiso 1 1 calc R . . . .
C13 C 0.24260(16) 0.29575(14) 0.83570(14) 0.0235(3) Uani 1 1 d . . . . .
C14 C 0.27377(18) 0.40632(16) 0.95561(15) 0.0313(3) Uani 1 1 d . . . . .
H14 H 0.3663 0.4667 0.9982 0.038 Uiso 1 1 calc R . . . .
C15 C 0.1682(2) 0.42711(18) 1.01201(17) 0.0407(4) Uani 1 1 d . . . . .
H15 H 0.1906 0.5008 1.0923 0.049 Uiso 1 1 calc R . . . .
C16 C 0.0297(2) 0.3388(2) 0.94936(18) 0.0394(4) Uani 1 1 d . . . . .
H16 H -0.0410 0.3530 0.9872 0.047 Uiso 1 1 calc R . . . .
C17 C -0.00285(18) 0.22943(19) 0.83032(17) 0.0357(4) Uani 1 1 d . . . . .
H17 H -0.0958 0.1700 0.7881 0.043 Uiso 1 1 calc R . . . .
C18 C 0.10209(16) 0.20744(16) 0.77305(15) 0.0289(3) Uani 1 1 d . . . . .
H18 H 0.0788 0.1337 0.6927 0.035 Uiso 1 1 calc R . . . .
C19 C 0.44153(15) 0.14138(14) 0.79411(13) 0.0228(3) Uani 1 1 d . . . . .
C20 C 0.57969(17) 0.12838(17) 0.79413(16) 0.0316(3) Uani 1 1 d . . . . .
H20 H 0.6392 0.1826 0.7785 0.038 Uiso 1 1 calc R . . . .
C21 C 0.62915(19) 0.03510(19) 0.81738(16) 0.0371(4) Uani 1 1 d . . . . .
H21 H 0.7205 0.0261 0.8154 0.045 Uiso 1 1 calc R . . . .
C22 C 0.5441(2) -0.04368(18) 0.84324(16) 0.0372(4) Uani 1 1 d . . . . .
H22 H 0.5777 -0.1056 0.8592 0.045 Uiso 1 1 calc R . . . .
C23 C 0.40768(19) -0.03064(17) 0.84555(17) 0.0369(4) Uani 1 1 d . . . . .
H23 H 0.3500 -0.0834 0.8639 0.044 Uiso 1 1 calc R . . . .
C24 C 0.35690(16) 0.06082(16) 0.82063(15) 0.0300(3) Uani 1 1 d . . . . .
H24 H 0.2649 0.0683 0.8217 0.036 Uiso 1 1 calc R . . . .
C25 C 0.29600(15) 0.19679(13) 0.59712(13) 0.0213(3) Uani 1 1 d . . . . .
H25 H 0.1904 0.1774 0.5776 0.026 Uiso 1 1 calc R . . . .
C26 C 0.33374(15) 0.07192(14) 0.51533(14) 0.0239(3) Uani 1 1 d . . . . .
H26A H 0.3177 0.0607 0.4316 0.029 Uiso 1 1 calc R . . . .
H26B H 0.4365 0.0845 0.5532 0.029 Uiso 1 1 calc R . . . .
C27 C 0.24714(15) -0.05323(14) 0.50017(13) 0.0241(3) Uani 1 1 d . . . . .
C28 C 0.22881(19) -0.28354(15) 0.41414(17) 0.0347(4) Uani 1 1 d . . . . .
H28A H 0.2549 -0.3491 0.3474 0.042 Uiso 1 1 calc R . . . .
H28B H 0.1247 -0.2980 0.3817 0.042 Uiso 1 1 calc R . . . .
C29 C 0.2653(2) -0.30112(18) 0.52656(19) 0.0417(4) Uani 1 1 d . . . . .
H29A H 0.3692 -0.2746 0.5662 0.063 Uiso 1 1 calc GR . . . .
H29B H 0.2261 -0.3925 0.4993 0.063 Uiso 1 1 calc GR . . . .
H29C H 0.2241 -0.2476 0.5864 0.063 Uiso 1 1 calc GR . . . .
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
P1 0.02342(18) 0.02182(18) 0.02446(19) 0.01312(15) 0.00901(14) 0.00520(13)
P2 0.02129(17) 0.02059(18) 0.02180(19) 0.01091(14) 0.00613(13) 0.00402(13)
O1 0.0248(5) 0.0270(5) 0.0350(6) 0.0137(5) 0.0106(4) 0.0044(4)
O2 0.0347(6) 0.0213(5) 0.0398(6) 0.0144(5) 0.0178(5) 0.0088(4)
C1 0.0265(7) 0.0229(7) 0.0238(7) 0.0131(6) 0.0111(5) 0.0092(5)
C2 0.0317(8) 0.0338(8) 0.0344(8) 0.0220(7) 0.0118(7) 0.0068(6)
C3 0.0405(9) 0.0467(10) 0.0374(9) 0.0304(8) 0.0169(7) 0.0139(7)
C4 0.0384(8) 0.0410(9) 0.0263(8) 0.0190(7) 0.0109(7) 0.0169(7)
C5 0.0298(8) 0.0343(8) 0.0319(8) 0.0157(7) 0.0071(6) 0.0047(6)
C6 0.0307(7) 0.0313(8) 0.0296(8) 0.0175(7) 0.0118(6) 0.0068(6)
C7 0.0290(7) 0.0193(6) 0.0255(7) 0.0133(6) 0.0109(6) 0.0058(5)
C8 0.0274(7) 0.0250(7) 0.0340(8) 0.0095(7) 0.0082(6) 0.0041(6)
C9 0.0324(8) 0.0312(8) 0.0465(10) 0.0142(8) 0.0157(7) 0.0108(7)
C10 0.0473(9) 0.0235(7) 0.0374(9) 0.0127(7) 0.0205(8) 0.0117(7)
C11 0.0445(9) 0.0219(7) 0.0267(8) 0.0102(6) 0.0066(7) 0.0035(6)
C12 0.0287(7) 0.0237(7) 0.0305(8) 0.0154(6) 0.0056(6) 0.0033(6)
C13 0.0275(7) 0.0239(7) 0.0231(7) 0.0138(6) 0.0096(6) 0.0105(6)
C14 0.0407(8) 0.0258(7) 0.0254(8) 0.0120(6) 0.0096(6) 0.0109(6)
C15 0.0636(12) 0.0364(9) 0.0303(8) 0.0163(7) 0.0246(8) 0.0260(9)
C16 0.0502(10) 0.0519(10) 0.0455(10) 0.0346(9) 0.0331(8) 0.0333(9)
C17 0.0294(8) 0.0476(10) 0.0431(9) 0.0295(8) 0.0175(7) 0.0166(7)
C18 0.0276(7) 0.0307(8) 0.0273(7) 0.0142(6) 0.0093(6) 0.0087(6)
C19 0.0234(6) 0.0237(7) 0.0187(6) 0.0102(5) 0.0049(5) 0.0063(5)
C20 0.0312(8) 0.0416(9) 0.0327(8) 0.0236(7) 0.0159(6) 0.0155(7)
C21 0.0378(9) 0.0501(10) 0.0357(9) 0.0248(8) 0.0182(7) 0.0269(8)
C22 0.0507(10) 0.0374(9) 0.0341(9) 0.0226(7) 0.0160(7) 0.0249(8)
C23 0.0403(9) 0.0343(9) 0.0414(9) 0.0249(8) 0.0121(7) 0.0097(7)
C24 0.0258(7) 0.0301(8) 0.0358(8) 0.0197(7) 0.0084(6) 0.0069(6)
C25 0.0233(6) 0.0205(6) 0.0208(6) 0.0112(5) 0.0077(5) 0.0059(5)
C26 0.0279(7) 0.0224(7) 0.0234(7) 0.0118(6) 0.0115(6) 0.0082(6)
C27 0.0247(7) 0.0221(7) 0.0206(7) 0.0096(6) 0.0041(5) 0.0053(5)
C28 0.0403(9) 0.0204(7) 0.0381(9) 0.0122(7) 0.0128(7) 0.0052(6)
C29 0.0466(10) 0.0326(9) 0.0449(10) 0.0223(8) 0.0113(8) 0.0078(7)
_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
P1 C1 1.8394(15) . ?
P1 C7 1.8361(15) . ?
P1 C25 1.8662(15) . ?
P2 C13 1.8287(15) . ?
P2 C19 1.8379(15) . ?
P2 C25 1.8845(14) . ?
O1 C27 1.2017(19) . ?
O2 C27 1.3422(18) . ?
O2 C28 1.4606(18) . ?
C1 C2 1.392(2) . ?
C1 C6 1.395(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.387(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.379(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.384(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.393(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.395(2) . ?
C7 C12 1.392(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.390(2) . ?
C9 H9 0.9300 . ?
C9 C10 1.384(2) . ?
C10 H10 0.9300 . ?
C10 C11 1.386(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.386(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.395(2) . ?
C13 C18 1.399(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.388(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.384(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.381(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.389(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.397(2) . ?
C19 C24 1.389(2) . ?
C20 H20 0.9300 . ?
C20 C21 1.391(2) . ?
C21 H21 0.9300 . ?
C21 C22 1.371(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.385(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.387(2) . ?
C24 H24 0.9300 . ?
C25 H25 0.9800 . ?
C25 C26 1.5311(19) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.510(2) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.492(3) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
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
C1 P1 C25 103.24(7) . . ?
C7 P1 C1 103.02(7) . . ?
C7 P1 C25 100.02(6) . . ?
C13 P2 C19 102.25(7) . . ?
C13 P2 C25 102.60(6) . . ?
C19 P2 C25 104.90(6) . . ?
C27 O2 C28 117.47(12) . . ?
C2 C1 P1 115.81(11) . . ?
C2 C1 C6 118.33(14) . . ?
C6 C1 P1 125.77(12) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 C1 121.02(15) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.29(16) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.48(15) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.51(15) . . ?
C6 C5 H5 119.7 . . ?
C1 C6 H6 119.8 . . ?
C5 C6 C1 120.35(15) . . ?
C5 C6 H6 119.8 . . ?
C8 C7 P1 124.49(11) . . ?
C12 C7 P1 116.73(11) . . ?
C12 C7 C8 118.76(14) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.24(15) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.29(16) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 119.91(15) . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.82(15) . . ?
C12 C11 H11 120.1 . . ?
C7 C12 H12 119.5 . . ?
C11 C12 C7 120.95(15) . . ?
C11 C12 H12 119.5 . . ?
C14 C13 P2 116.77(12) . . ?
C14 C13 C18 118.49(14) . . ?
C18 C13 P2 124.73(12) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.67(16) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.33(16) . . ?
C16 C15 H15 119.8 . . ?
C15 C16 H16 120.2 . . ?
C17 C16 C15 119.58(16) . . ?
C17 C16 H16 120.2 . . ?
C16 C17 H17 119.7 . . ?
C16 C17 C18 120.60(16) . . ?
C18 C17 H17 119.7 . . ?
C13 C18 H18 119.8 . . ?
C17 C18 C13 120.32(15) . . ?
C17 C18 H18 119.8 . . ?
C20 C19 P2 117.01(12) . . ?
C24 C19 P2 124.58(11) . . ?
C24 C19 C20 118.15(14) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.63(16) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 119.8 . . ?
C22 C21 C20 120.41(15) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 120.2 . . ?
C21 C22 C23 119.69(15) . . ?
C23 C22 H22 120.2 . . ?
C22 C23 H23 119.9 . . ?
C22 C23 C24 120.17(16) . . ?
C24 C23 H23 119.9 . . ?
C19 C24 H24 119.5 . . ?
C23 C24 C19 120.94(15) . . ?
C23 C24 H24 119.5 . . ?
P1 C25 P2 103.60(7) . . ?
P1 C25 H25 110.0 . . ?
P2 C25 H25 110.0 . . ?
C26 C25 P1 108.68(10) . . ?
C26 C25 P2 114.24(9) . . ?
C26 C25 H25 110.0 . . ?
C25 C26 H26A 108.7 . . ?
C25 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
C27 C26 C25 114.40(12) . . ?
C27 C26 H26A 108.7 . . ?
C27 C26 H26B 108.7 . . ?
O1 C27 O2 124.48(14) . . ?
O1 C27 C26 125.99(13) . . ?
O2 C27 C26 109.44(12) . . ?
O2 C28 H28A 109.3 . . ?
O2 C28 H28B 109.3 . . ?
O2 C28 C29 111.70(14) . . ?
H28A C28 H28B 107.9 . . ?
C29 C28 H28A 109.3 . . ?
C29 C28 H28B 109.3 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 C3 177.27(13) . . . . ?
P1 C1 C6 C5 -175.60(12) . . . . ?
P1 C7 C8 C9 177.76(14) . . . . ?
P1 C7 C12 C11 -176.75(12) . . . . ?
P1 C25 C26 C27 -161.30(10) . . . . ?
P2 C13 C14 C15 -177.75(12) . . . . ?
P2 C13 C18 C17 177.78(12) . . . . ?
P2 C19 C20 C21 175.78(13) . . . . ?
P2 C19 C24 C23 -174.38(13) . . . . ?
P2 C25 C26 C27 83.59(13) . . . . ?
C1 P1 C7 C8 31.67(15) . . . . ?
C1 P1 C7 C12 -149.74(12) . . . . ?
C1 P1 C25 P2 -168.49(6) . . . . ?
C1 P1 C25 C26 69.66(10) . . . . ?
C1 C2 C3 C4 -1.7(3) . . . . ?
C2 C1 C6 C5 0.7(2) . . . . ?
C2 C3 C4 C5 1.5(3) . . . . ?
C3 C4 C5 C6 -0.2(3) . . . . ?
C4 C5 C6 C1 -0.9(2) . . . . ?
C6 C1 C2 C3 0.6(2) . . . . ?
C7 P1 C1 C2 97.64(12) . . . . ?
C7 P1 C1 C6 -85.95(14) . . . . ?
C7 P1 C25 P2 -62.43(8) . . . . ?
C7 P1 C25 C26 175.72(9) . . . . ?
C7 C8 C9 C10 -0.9(3) . . . . ?
C8 C7 C12 C11 1.9(2) . . . . ?
C8 C9 C10 C11 1.4(3) . . . . ?
C9 C10 C11 C12 -0.3(3) . . . . ?
C10 C11 C12 C7 -1.4(2) . . . . ?
C12 C7 C8 C9 -0.8(2) . . . . ?
C13 P2 C19 C20 -160.29(12) . . . . ?
C13 P2 C19 C24 13.70(14) . . . . ?
C13 P2 C25 P1 112.56(7) . . . . ?
C13 P2 C25 C26 -129.38(11) . . . . ?
C13 C14 C15 C16 -0.6(3) . . . . ?
C14 C13 C18 C17 -0.7(2) . . . . ?
C14 C15 C16 C17 0.2(3) . . . . ?
C15 C16 C17 C18 0.0(3) . . . . ?
C16 C17 C18 C13 0.3(2) . . . . ?
C18 C13 C14 C15 0.8(2) . . . . ?
C19 P2 C13 C14 104.98(12) . . . . ?
C19 P2 C13 C18 -73.52(14) . . . . ?
C19 P2 C25 P1 -140.91(7) . . . . ?
C19 P2 C25 C26 -22.85(12) . . . . ?
C19 C20 C21 C22 -1.4(3) . . . . ?
C20 C19 C24 C23 -0.5(2) . . . . ?
C20 C21 C22 C23 0.3(3) . . . . ?
C21 C22 C23 C24 0.6(3) . . . . ?
C22 C23 C24 C19 -0.5(3) . . . . ?
C24 C19 C20 C21 1.4(2) . . . . ?
C25 P1 C1 C2 -158.59(12) . . . . ?
C25 P1 C1 C6 17.82(15) . . . . ?
C25 P1 C7 C8 -74.57(14) . . . . ?
C25 P1 C7 C12 104.02(12) . . . . ?
C25 P2 C13 C14 -146.47(12) . . . . ?
C25 P2 C13 C18 35.03(14) . . . . ?
C25 P2 C19 C20 92.93(12) . . . . ?
C25 P2 C19 C24 -93.09(14) . . . . ?
C25 C26 C27 O1 14.2(2) . . . . ?
C25 C26 C27 O2 -169.32(12) . . . . ?
C27 O2 C28 C29 -82.50(18) . . . . ?
C28 O2 C27 O1 1.7(2) . . . . ?
C28 O2 C27 C26 -174.85(12) . . . . ?
_iucr_refine_instructions_details
;
TITL s16rlw5
CELL 1.54184 9.891803 11.879769 12.597675 117.2419 103.9095 98.1497
ZERR 2 0.000333 0.000704 0.000556 0.0051 0.0033 0.0037
LATT 1
SFAC C H O P
UNIT 58 56 4 4
L.S. 10
PLAN 2
MORE -1
BOND $H
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.052000 0.359000
FVAR 9.20879
P1 4 0.362414 0.327353 0.562907 11.00000 0.02342 0.02182 =
0.02446 0.01312 0.00901 0.00520
P2 4 0.392197 0.275458 0.773627 11.00000 0.02129 0.02059 =
0.02180 0.01091 0.00613 0.00402
O1 3 0.138550 -0.066379 0.525573 11.00000 0.02476 0.02696 =
0.03503 0.01372 0.01061 0.00439
O2 3 0.305342 -0.151318 0.446629 11.00000 0.03473 0.02133 =
0.03985 0.01443 0.01775 0.00883
C1 1 0.240582 0.264750 0.399810 11.00000 0.02653 0.02290 =
0.02383 0.01306 0.01112 0.00922
C2 1 0.292826 0.315615 0.332609 11.00000 0.03167 0.03385 =
0.03441 0.02197 0.01178 0.00683
AFIX 43
H2 2 0.382423 0.380014 0.372551 11.00000 -1.20000
AFIX 0
C3 1 0.213295 0.271713 0.207011 11.00000 0.04053 0.04668 =
0.03743 0.03044 0.01689 0.01386
AFIX 43
H3 2 0.248659 0.308458 0.164288 11.00000 -1.20000
AFIX 0
C4 1 0.082051 0.173843 0.145235 11.00000 0.03837 0.04101 =
0.02626 0.01901 0.01087 0.01689
AFIX 43
H4 2 0.029842 0.143016 0.060441 11.00000 -1.20000
AFIX 0
C5 1 0.028599 0.121824 0.210400 11.00000 0.02981 0.03432 =
0.03187 0.01568 0.00714 0.00468
AFIX 43
H5 2 -0.060014 0.055959 0.169135 11.00000 -1.20000
AFIX 0
C6 1 0.106493 0.167358 0.337280 11.00000 0.03073 0.03135 =
0.02959 0.01746 0.01178 0.00678
AFIX 43
H6 2 0.068935 0.132665 0.380562 11.00000 -1.20000
AFIX 0
C7 1 0.292261 0.458003 0.660538 11.00000 0.02900 0.01928 =
0.02551 0.01327 0.01091 0.00580
C8 1 0.146470 0.456126 0.629300 11.00000 0.02738 0.02500 =
0.03405 0.00946 0.00825 0.00409
AFIX 43
H8 2 0.078050 0.386668 0.553068 11.00000 -1.20000
AFIX 0
C9 1 0.103041 0.557709 0.711705 11.00000 0.03243 0.03117 =
0.04646 0.01424 0.01569 0.01084
AFIX 43
H9 2 0.005894 0.556528 0.689836 11.00000 -1.20000
AFIX 0
C10 1 0.203729 0.660567 0.826120 11.00000 0.04731 0.02351 =
0.03741 0.01274 0.02046 0.01172
AFIX 43
H10 2 0.173899 0.727301 0.881857 11.00000 -1.20000
AFIX 0
C11 1 0.349054 0.663988 0.857524 11.00000 0.04451 0.02193 =
0.02665 0.01021 0.00661 0.00352
AFIX 43
H11 2 0.417044 0.733242 0.934147 11.00000 -1.20000
AFIX 0
C12 1 0.392815 0.563907 0.774420 11.00000 0.02874 0.02367 =
0.03049 0.01536 0.00559 0.00330
AFIX 43
H12 2 0.490769 0.567574 0.795052 11.00000 -1.20000
AFIX 0
C13 1 0.242602 0.295746 0.835704 11.00000 0.02745 0.02394 =
0.02314 0.01382 0.00960 0.01050
C14 1 0.273770 0.406317 0.955612 11.00000 0.04069 0.02576 =
0.02536 0.01201 0.00964 0.01092
AFIX 43
H14 2 0.366251 0.466697 0.998178 11.00000 -1.20000
AFIX 0
C15 1 0.168157 0.427106 1.012005 11.00000 0.06362 0.03644 =
0.03031 0.01626 0.02459 0.02595
AFIX 43
H15 2 0.190569 0.500769 1.092298 11.00000 -1.20000
AFIX 0
C16 1 0.029689 0.338778 0.949356 11.00000 0.05022 0.05192 =
0.04550 0.03458 0.03313 0.03330
AFIX 43
H16 2 -0.041007 0.352983 0.987200 11.00000 -1.20000
AFIX 0
C17 1 -0.002849 0.229434 0.830319 11.00000 0.02945 0.04760 =
0.04312 0.02952 0.01754 0.01658
AFIX 43
H17 2 -0.095850 0.169950 0.788077 11.00000 -1.20000
AFIX 0
C18 1 0.102089 0.207444 0.773047 11.00000 0.02763 0.03066 =
0.02734 0.01418 0.00925 0.00874
AFIX 43
H18 2 0.078785 0.133651 0.692660 11.00000 -1.20000
AFIX 0
C19 1 0.441534 0.141379 0.794105 11.00000 0.02335 0.02373 =
0.01875 0.01019 0.00494 0.00631
C20 1 0.579694 0.128379 0.794131 11.00000 0.03122 0.04156 =
0.03269 0.02356 0.01591 0.01547
AFIX 43
H20 2 0.639173 0.182600 0.778457 11.00000 -1.20000
AFIX 0
C21 1 0.629153 0.035105 0.817376 11.00000 0.03777 0.05010 =
0.03565 0.02476 0.01818 0.02691
AFIX 43
H21 2 0.720533 0.026146 0.815353 11.00000 -1.20000
AFIX 0
C22 1 0.544061 -0.043676 0.843243 11.00000 0.05074 0.03737 =
0.03411 0.02257 0.01602 0.02488
AFIX 43
H22 2 0.577728 -0.105603 0.859174 11.00000 -1.20000
AFIX 0
C23 1 0.407678 -0.030637 0.845547 11.00000 0.04032 0.03427 =
0.04145 0.02493 0.01213 0.00966
AFIX 43
H23 2 0.350027 -0.083359 0.863855 11.00000 -1.20000
AFIX 0
C24 1 0.356898 0.060825 0.820627 11.00000 0.02580 0.03015 =
0.03576 0.01970 0.00841 0.00695
AFIX 43
H24 2 0.264852 0.068327 0.821689 11.00000 -1.20000
AFIX 0
C25 1 0.295999 0.196786 0.597118 11.00000 0.02328 0.02050 =
0.02080 0.01118 0.00772 0.00595
AFIX 13
H25 2 0.190431 0.177374 0.577574 11.00000 -1.20000
AFIX 0
C26 1 0.333744 0.071919 0.515335 11.00000 0.02788 0.02243 =
0.02338 0.01177 0.01148 0.00818
AFIX 23
H26A 2 0.317737 0.060725 0.431596 11.00000 -1.20000
H26B 2 0.436460 0.084497 0.553202 11.00000 -1.20000
AFIX 0
C27 1 0.247144 -0.053235 0.500172 11.00000 0.02471 0.02215 =
0.02064 0.00956 0.00413 0.00525
C28 1 0.228811 -0.283538 0.414145 11.00000 0.04032 0.02043 =
0.03809 0.01224 0.01281 0.00524
AFIX 23
H28A 2 0.254852 -0.349072 0.347419 11.00000 -1.20000
H28B 2 0.124663 -0.298030 0.381692 11.00000 -1.20000
AFIX 0
C29 1 0.265302 -0.301115 0.526565 11.00000 0.04663 0.03259 =
0.04485 0.02229 0.01133 0.00778
AFIX 137
H29A 2 0.369155 -0.274566 0.566248 11.00000 -1.50000
H29B 2 0.226144 -0.392469 0.499333 11.00000 -1.50000
H29C 2 0.224087 -0.247622 0.586449 11.00000 -1.50000
AFIX 0
HKLF 4
REM
REM R1 = 0.0360 for 4456 Fo > 4sig(Fo) and 0.0390 for all 4843 data
REM 299 parameters refined using 0 restraints
END
WGHT 0.0517 0.3595
REM Highest difference peak 0.526, deepest hole -0.333, 1-sigma level 0.046
Q1 1 0.4193 0.1999 0.7856 11.00000 0.05 0.53
Q2 1 0.4814 0.3679 0.5779 11.00000 0.05 0.32
REM The information below was added by Olex2.
REM
REM R1 = 0.0360 for 4456 Fo > 4sig(Fo) and 0.0390 for all 10428 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.53, deepest hole -0.33
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0390
REM R1_gt = 0.0360
REM wR_ref = 0.0989
REM GOOF = 1.042
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 10428
REM Reflections_gt = 4456
REM Parameters = n/a
REM Hole = -0.33
REM Peak = 0.53
REM Flack = n/a
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_e17rlw30-Cpd-1h
_database_code_depnum_ccdc_archive 'CCDC 1849267'
_audit_update_record
;
2018-06-14 deposited with the CCDC.
2018-08-22 downloaded from the CCDC.
;
_audit_creation_date 2017-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number 2014-3
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C33 H28 O P2'
_chemical_formula_sum 'C33 H28 O P2'
_chemical_formula_weight 502.49
_chemical_melting_point ?
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 6.2505(2)
_cell_length_b 22.1889(9)
_cell_length_c 18.8017(6)
_cell_angle_alpha 90
_cell_angle_beta 93.871(3)
_cell_angle_gamma 90
_cell_volume 2601.69(16)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 7829
_cell_measurement_temperature 150.00(10)
_cell_measurement_theta_max 28.3840
_cell_measurement_theta_min 3.7100
_shelx_estimated_absorpt_T_max 0.956
_shelx_estimated_absorpt_T_min 0.897
_exptl_absorpt_coefficient_mu 0.192
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.96015
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.283
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1056
_exptl_crystal_size_max 0.577
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.234
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0329
_diffrn_reflns_av_unetI/netI 0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -28
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 22176
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.479
_diffrn_reflns_theta_min 3.385
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 150.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'New Xcalibur, EosS2'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4773
_reflns_number_total 5808
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 0.507
_refine_diff_density_min -0.259
_refine_diff_density_rms 0.050
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.029
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 325
_refine_ls_number_reflns 5808
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0577
_refine_ls_R_factor_gt 0.0441
_refine_ls_restrained_S_all 1.029
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+1.6232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1000
_refine_ls_wR_factor_ref 0.1075
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
C1(H1)
2.b Secondary CH2 refined with riding coordinates:
C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31),
C32(H32), C33(H33)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary iterative
_atom_sites_solution_secondary ?
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
P1 P 0.50737(7) 0.64357(2) 0.78112(2) 0.02018(11) Uani 1 1 d . . . . .
P2 P 0.63302(7) 0.51696(2) 0.81595(2) 0.02337(12) Uani 1 1 d . . . . .
O1 O 0.8343(2) 0.60233(8) 0.61680(8) 0.0418(4) Uani 1 1 d . . . . .
C1 C 0.6627(3) 0.57787(8) 0.74917(9) 0.0195(3) Uani 1 1 d . . . . .
H1 H 0.8138 0.5884 0.7455 0.023 Uiso 1 1 calc R . . . .
C2 C 0.5614(3) 0.55444(8) 0.67766(9) 0.0213(4) Uani 1 1 d . . . . .
H2A H 0.5820 0.5112 0.6756 0.026 Uiso 1 1 calc R . . . .
H2B H 0.4083 0.5620 0.6757 0.026 Uiso 1 1 calc R . . . .
C3 C 0.6525(3) 0.58277(8) 0.61296(9) 0.0238(4) Uani 1 1 d . . . . .
C4 C 0.5201(3) 0.58341(8) 0.54362(9) 0.0229(4) Uani 1 1 d . . . . .
C5 C 0.6084(3) 0.61003(9) 0.48529(10) 0.0323(4) Uani 1 1 d . . . . .
H5 H 0.7468 0.6255 0.4902 0.039 Uiso 1 1 calc R . . . .
C6 C 0.4926(4) 0.61367(10) 0.42035(11) 0.0399(5) Uani 1 1 d . . . . .
H6 H 0.5526 0.6321 0.3820 0.048 Uiso 1 1 calc R . . . .
C7 C 0.2888(4) 0.59018(10) 0.41211(11) 0.0390(5) Uani 1 1 d . . . . .
H7 H 0.2112 0.5926 0.3682 0.047 Uiso 1 1 calc R . . . .
C8 C 0.2001(3) 0.56306(10) 0.46910(11) 0.0368(5) Uani 1 1 d . . . . .
H8 H 0.0628 0.5469 0.4634 0.044 Uiso 1 1 calc R . . . .
C9 C 0.3144(3) 0.55975(9) 0.53493(10) 0.0299(4) Uani 1 1 d . . . . .
H9 H 0.2530 0.5417 0.5733 0.036 Uiso 1 1 calc R . . . .
C10 C 0.4569(3) 0.69011(8) 0.70020(9) 0.0213(4) Uani 1 1 d . . . . .
C11 C 0.5907(3) 0.73493(9) 0.67666(10) 0.0301(4) Uani 1 1 d . . . . .
H11 H 0.7230 0.7417 0.7010 0.036 Uiso 1 1 calc R . . . .
C12 C 0.5298(4) 0.76961(9) 0.61740(11) 0.0361(5) Uani 1 1 d . . . . .
H12 H 0.6209 0.7995 0.6026 0.043 Uiso 1 1 calc R . . . .
C13 C 0.3346(3) 0.75999(10) 0.58022(10) 0.0351(5) Uani 1 1 d . . . . .
H13 H 0.2937 0.7835 0.5407 0.042 Uiso 1 1 calc R . . . .
C14 C 0.2006(3) 0.71515(9) 0.60230(10) 0.0308(4) Uani 1 1 d . . . . .
H14 H 0.0699 0.7080 0.5771 0.037 Uiso 1 1 calc R . . . .
C15 C 0.2609(3) 0.68087(9) 0.66188(9) 0.0246(4) Uani 1 1 d . . . . .
H15 H 0.1689 0.6511 0.6766 0.030 Uiso 1 1 calc R . . . .
C16 C 0.7110(3) 0.68744(8) 0.83334(9) 0.0214(4) Uani 1 1 d . . . . .
C17 C 0.9166(3) 0.69914(8) 0.81280(10) 0.0266(4) Uani 1 1 d . . . . .
H17 H 0.9610 0.6821 0.7711 0.032 Uiso 1 1 calc R . . . .
C18 C 1.0557(3) 0.73573(9) 0.85347(11) 0.0296(4) Uani 1 1 d . . . . .
H18 H 1.1916 0.7438 0.8385 0.035 Uiso 1 1 calc R . . . .
C19 C 0.9930(3) 0.76032(9) 0.91625(10) 0.0319(4) Uani 1 1 d . . . . .
H19 H 1.0853 0.7857 0.9431 0.038 Uiso 1 1 calc R . . . .
C20 C 0.7933(3) 0.74710(9) 0.93897(10) 0.0327(4) Uani 1 1 d . . . . .
H20 H 0.7530 0.7623 0.9822 0.039 Uiso 1 1 calc R . . . .
C21 C 0.6521(3) 0.71117(8) 0.89760(9) 0.0252(4) Uani 1 1 d . . . . .
H21 H 0.5169 0.7029 0.9130 0.030 Uiso 1 1 calc R . . . .
C22 C 0.7641(3) 0.54853(8) 0.89766(10) 0.0257(4) Uani 1 1 d . . . . .
C23 C 0.9757(3) 0.56815(10) 0.90663(12) 0.0372(5) Uani 1 1 d . . . . .
H23 H 1.0653 0.5648 0.8693 0.045 Uiso 1 1 calc R . . . .
C24 C 1.0533(4) 0.59271(11) 0.97115(13) 0.0476(6) Uani 1 1 d . . . . .
H24 H 1.1943 0.6062 0.9767 0.057 Uiso 1 1 calc R . . . .
C25 C 0.9221(4) 0.59714(11) 1.02723(12) 0.0490(6) Uani 1 1 d . . . . .
H25 H 0.9754 0.6133 1.0705 0.059 Uiso 1 1 calc R . . . .
C26 C 0.7145(5) 0.57790(11) 1.01919(12) 0.0487(6) Uani 1 1 d . . . . .
H26 H 0.6261 0.5810 1.0569 0.058 Uiso 1 1 calc R . . . .
C27 C 0.6357(4) 0.55367(9) 0.95459(11) 0.0354(5) Uani 1 1 d . . . . .
H27 H 0.4941 0.5406 0.9494 0.042 Uiso 1 1 calc R . . . .
C28 C 0.8258(3) 0.46091(8) 0.78754(9) 0.0244(4) Uani 1 1 d . . . . .
C29 C 1.0194(3) 0.47319(9) 0.75838(12) 0.0356(5) Uani 1 1 d . . . . .
H29 H 1.0612 0.5130 0.7524 0.043 Uiso 1 1 calc R . . . .
C30 C 1.1512(3) 0.42695(10) 0.73801(13) 0.0415(5) Uani 1 1 d . . . . .
H30 H 1.2803 0.4360 0.7186 0.050 Uiso 1 1 calc R . . . .
C31 C 1.0922(4) 0.36760(10) 0.74636(11) 0.0379(5) Uani 1 1 d . . . . .
H31 H 1.1807 0.3367 0.7324 0.045 Uiso 1 1 calc R . . . .
C32 C 0.9022(4) 0.35441(9) 0.77538(11) 0.0390(5) Uani 1 1 d . . . . .
H32 H 0.8628 0.3145 0.7817 0.047 Uiso 1 1 calc R . . . .
C33 C 0.7682(3) 0.40059(9) 0.79541(10) 0.0318(4) Uani 1 1 d . . . . .
H33 H 0.6387 0.3912 0.8143 0.038 Uiso 1 1 calc R . . . .
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
P1 0.0197(2) 0.0225(2) 0.0179(2) -0.00147(17) -0.00143(16) -0.00016(17)
P2 0.0255(2) 0.0227(2) 0.0215(2) 0.00132(18) -0.00152(18) -0.00216(18)
O1 0.0290(7) 0.0671(11) 0.0294(8) -0.0033(7) 0.0032(6) -0.0196(7)
C1 0.0203(8) 0.0195(9) 0.0184(8) -0.0017(7) -0.0012(6) -0.0014(6)
C2 0.0227(8) 0.0214(9) 0.0195(9) -0.0021(7) -0.0012(7) -0.0027(7)
C3 0.0243(9) 0.0250(10) 0.0222(9) -0.0043(7) 0.0027(7) -0.0023(7)
C4 0.0298(9) 0.0191(9) 0.0200(9) -0.0035(7) 0.0025(7) 0.0030(7)
C5 0.0384(11) 0.0317(11) 0.0273(10) -0.0004(8) 0.0055(8) -0.0019(8)
C6 0.0615(14) 0.0370(12) 0.0217(10) 0.0040(9) 0.0073(9) 0.0027(10)
C7 0.0569(13) 0.0356(12) 0.0226(10) -0.0050(9) -0.0105(9) 0.0127(10)
C8 0.0344(11) 0.0424(13) 0.0320(11) -0.0067(9) -0.0089(9) 0.0010(9)
C9 0.0325(10) 0.0357(11) 0.0212(9) -0.0021(8) -0.0008(8) -0.0022(8)
C10 0.0257(9) 0.0201(9) 0.0177(8) -0.0018(7) -0.0009(7) 0.0031(7)
C11 0.0319(10) 0.0277(10) 0.0299(10) -0.0002(8) -0.0044(8) -0.0062(8)
C12 0.0505(12) 0.0271(11) 0.0308(11) 0.0054(8) 0.0027(9) -0.0086(9)
C13 0.0497(12) 0.0331(11) 0.0220(10) 0.0043(8) -0.0025(9) 0.0068(9)
C14 0.0300(10) 0.0399(12) 0.0216(9) -0.0007(8) -0.0055(7) 0.0057(8)
C15 0.0232(9) 0.0296(10) 0.0211(9) -0.0027(7) 0.0008(7) 0.0010(7)
C16 0.0236(8) 0.0199(9) 0.0197(8) -0.0016(7) -0.0054(7) 0.0032(7)
C17 0.0256(9) 0.0273(10) 0.0265(10) -0.0041(8) -0.0002(7) 0.0023(7)
C18 0.0252(9) 0.0272(10) 0.0350(11) 0.0044(8) -0.0074(8) -0.0013(7)
C19 0.0415(11) 0.0249(10) 0.0269(10) -0.0002(8) -0.0151(8) -0.0049(8)
C20 0.0492(12) 0.0290(11) 0.0192(9) -0.0062(8) -0.0031(8) 0.0021(9)
C21 0.0288(9) 0.0267(10) 0.0197(9) 0.0000(7) -0.0018(7) 0.0052(7)
C22 0.0345(10) 0.0201(9) 0.0217(9) 0.0024(7) -0.0036(7) 0.0043(7)
C23 0.0324(10) 0.0408(13) 0.0372(12) -0.0103(10) -0.0076(9) 0.0063(9)
C24 0.0410(12) 0.0460(14) 0.0524(15) -0.0171(11) -0.0227(11) 0.0111(10)
C25 0.0809(18) 0.0350(13) 0.0278(12) -0.0056(9) -0.0207(12) 0.0091(12)
C26 0.0857(19) 0.0353(13) 0.0259(11) -0.0019(9) 0.0096(11) -0.0063(12)
C27 0.0507(12) 0.0265(11) 0.0293(11) 0.0012(8) 0.0066(9) -0.0039(9)
C28 0.0304(9) 0.0201(9) 0.0216(9) -0.0022(7) -0.0075(7) 0.0000(7)
C29 0.0311(10) 0.0210(10) 0.0545(14) -0.0090(9) 0.0001(9) -0.0033(8)
C30 0.0295(10) 0.0343(12) 0.0600(15) -0.0158(11) -0.0028(10) 0.0003(8)
C31 0.0487(12) 0.0281(11) 0.0349(11) -0.0079(9) -0.0113(9) 0.0121(9)
C32 0.0715(15) 0.0194(10) 0.0254(10) 0.0006(8) -0.0012(10) 0.0005(9)
C33 0.0497(12) 0.0245(10) 0.0209(9) 0.0012(8) 0.0003(8) -0.0052(8)
_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
P1 C1 1.8726(17) . ?
P1 C10 1.8481(18) . ?
P1 C16 1.8339(17) . ?
P2 C1 1.8624(18) . ?
P2 C22 1.8309(19) . ?
P2 C28 1.8361(19) . ?
O1 C3 1.214(2) . ?
C1 H1 0.9800 . ?
C1 C2 1.537(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.514(2) . ?
C3 C4 1.496(2) . ?
C4 C5 1.392(3) . ?
C4 C9 1.388(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.379(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.375(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.378(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.389(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.391(3) . ?
C10 C15 1.394(2) . ?
C11 H11 0.9300 . ?
C11 C12 1.386(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.381(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.382(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.385(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.391(3) . ?
C16 C21 1.390(2) . ?
C17 H17 0.9300 . ?
C17 C18 1.382(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.381(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.378(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.388(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.392(3) . ?
C22 C27 1.385(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.387(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.383(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.364(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.388(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.389(3) . ?
C28 C33 1.396(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.386(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.379(3) . ?
C31 H31 0.9300 . ?
C31 C32 1.372(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.391(3) . ?
C33 H33 0.9300 . ?
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
C10 P1 C1 103.55(8) . . ?
C16 P1 C1 103.23(8) . . ?
C16 P1 C10 102.58(8) . . ?
C22 P2 C1 103.22(8) . . ?
C22 P2 C28 103.77(8) . . ?
C28 P2 C1 101.44(8) . . ?
P1 C1 H1 111.1 . . ?
P2 C1 P1 105.74(8) . . ?
P2 C1 H1 111.1 . . ?
C2 C1 P1 110.61(11) . . ?
C2 C1 P2 106.88(11) . . ?
C2 C1 H1 111.1 . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C3 C2 C1 114.04(14) . . ?
C3 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
O1 C3 C2 120.11(16) . . ?
O1 C3 C4 120.58(17) . . ?
C4 C3 C2 119.23(15) . . ?
C5 C4 C3 117.74(16) . . ?
C9 C4 C3 123.52(16) . . ?
C9 C4 C5 118.74(17) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.69(19) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.3(2) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 120.1 . . ?
C6 C7 C8 119.75(19) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 H8 119.8 . . ?
C7 C8 C9 120.4(2) . . ?
C9 C8 H8 119.8 . . ?
C4 C9 C8 120.11(19) . . ?
C4 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 P1 126.06(13) . . ?
C11 C10 C15 117.85(17) . . ?
C15 C10 P1 116.01(13) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 C10 120.94(18) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.44(19) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C14 119.44(18) . . ?
C14 C13 H13 120.3 . . ?
C13 C14 H14 120.0 . . ?
C13 C14 C15 120.06(18) . . ?
C15 C14 H14 120.0 . . ?
C10 C15 H15 119.4 . . ?
C14 C15 C10 121.26(18) . . ?
C14 C15 H15 119.4 . . ?
C17 C16 P1 124.83(13) . . ?
C21 C16 P1 116.84(13) . . ?
C21 C16 C17 118.33(16) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 C16 120.96(17) . . ?
C18 C17 H17 119.5 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 120.06(18) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.74(18) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.23(18) . . ?
C21 C20 H20 119.9 . . ?
C16 C21 H21 119.7 . . ?
C20 C21 C16 120.58(18) . . ?
C20 C21 H21 119.7 . . ?
C23 C22 P2 126.08(15) . . ?
C27 C22 P2 115.48(15) . . ?
C27 C22 C23 118.43(19) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.1(2) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.3(2) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.1(2) . . ?
C26 C25 H25 119.9 . . ?
C25 C26 H26 120.1 . . ?
C25 C26 C27 119.8(2) . . ?
C27 C26 H26 120.1 . . ?
C22 C27 C26 121.2(2) . . ?
C22 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C29 C28 P2 126.04(15) . . ?
C29 C28 C33 117.87(18) . . ?
C33 C28 P2 116.08(15) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 C28 120.93(19) . . ?
C30 C29 H29 119.5 . . ?
C29 C30 H30 119.8 . . ?
C31 C30 C29 120.4(2) . . ?
C31 C30 H30 119.8 . . ?
C30 C31 H31 120.2 . . ?
C32 C31 C30 119.62(19) . . ?
C32 C31 H31 120.2 . . ?
C31 C32 H32 119.9 . . ?
C31 C32 C33 120.2(2) . . ?
C33 C32 H32 119.9 . . ?
C28 C33 H33 119.6 . . ?
C32 C33 C28 120.9(2) . . ?
C32 C33 H33 119.6 . . ?
_iucr_refine_instructions_details
;
TITL e17rlw30
CELL 0.71073 6.2505 22.1889 18.8017 90 93.871 90
ZERR 4 0.0002 0.0009 0.0006 0 0.003 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H O P
UNIT 132 112 4 8
L.S. 10
PLAN 2
SIZE 0.234 0.3 0.577
BOND $H
list 4
fmap 2
acta
SHEL 999 0.77
REM
REM
REM
WGHT 0.042700 1.623200
FVAR 0.47621
P1 4 0.507369 0.643566 0.781115 11.00000 0.01975 0.02250 =
0.01793 -0.00147 -0.00143 -0.00016
P2 4 0.633019 0.516963 0.815949 11.00000 0.02548 0.02269 =
0.02153 0.00132 -0.00152 -0.00216
O1 3 0.834282 0.602329 0.616801 11.00000 0.02904 0.06707 =
0.02939 -0.00331 0.00324 -0.01963
C1 1 0.662686 0.577871 0.749175 11.00000 0.02032 0.01947 =
0.01837 -0.00170 -0.00124 -0.00144
AFIX 13
H1 2 0.813824 0.588377 0.745495 11.00000 -1.20000
AFIX 0
C2 1 0.561437 0.554440 0.677661 11.00000 0.02274 0.02138 =
0.01952 -0.00210 -0.00122 -0.00265
AFIX 23
H2A 2 0.582041 0.511161 0.675629 11.00000 -1.20000
H2B 2 0.408306 0.562003 0.675717 11.00000 -1.20000
AFIX 0
C3 1 0.652475 0.582772 0.612959 11.00000 0.02434 0.02498 =
0.02224 -0.00432 0.00275 -0.00228
C4 1 0.520137 0.583409 0.543623 11.00000 0.02979 0.01914 =
0.01997 -0.00351 0.00251 0.00303
C5 1 0.608351 0.610035 0.485295 11.00000 0.03840 0.03175 =
0.02731 -0.00040 0.00550 -0.00192
AFIX 43
H5 2 0.746799 0.625538 0.490172 11.00000 -1.20000
AFIX 0
C6 1 0.492594 0.613665 0.420348 11.00000 0.06154 0.03702 =
0.02168 0.00404 0.00735 0.00274
AFIX 43
H6 2 0.552597 0.632069 0.381960 11.00000 -1.20000
AFIX 0
C7 1 0.288789 0.590184 0.412106 11.00000 0.05694 0.03564 =
0.02257 -0.00497 -0.01054 0.01272
AFIX 43
H7 2 0.211154 0.592609 0.368228 11.00000 -1.20000
AFIX 0
C8 1 0.200073 0.563056 0.469097 11.00000 0.03442 0.04237 =
0.03198 -0.00667 -0.00891 0.00095
AFIX 43
H8 2 0.062756 0.546855 0.463444 11.00000 -1.20000
AFIX 0
C9 1 0.314386 0.559751 0.534930 11.00000 0.03252 0.03567 =
0.02115 -0.00210 -0.00084 -0.00221
AFIX 43
H9 2 0.253021 0.541661 0.573259 11.00000 -1.20000
AFIX 0
C10 1 0.456920 0.690111 0.700204 11.00000 0.02574 0.02009 =
0.01766 -0.00183 -0.00091 0.00314
C11 1 0.590749 0.734928 0.676664 11.00000 0.03195 0.02770 =
0.02986 -0.00022 -0.00441 -0.00617
AFIX 43
H11 2 0.723008 0.741724 0.701030 11.00000 -1.20000
AFIX 0
C12 1 0.529798 0.769606 0.617403 11.00000 0.05050 0.02708 =
0.03077 0.00539 0.00269 -0.00864
AFIX 43
H12 2 0.620935 0.799546 0.602586 11.00000 -1.20000
AFIX 0
C13 1 0.334634 0.759991 0.580219 11.00000 0.04968 0.03308 =
0.02197 0.00433 -0.00245 0.00681
AFIX 43
H13 2 0.293707 0.783486 0.540654 11.00000 -1.20000
AFIX 0
C14 1 0.200635 0.715151 0.602301 11.00000 0.03003 0.03986 =
0.02160 -0.00070 -0.00545 0.00573
AFIX 43
H14 2 0.069875 0.707996 0.577133 11.00000 -1.20000
AFIX 0
C15 1 0.260945 0.680866 0.661881 11.00000 0.02317 0.02960 =
0.02107 -0.00266 0.00076 0.00103
AFIX 43
H15 2 0.168908 0.651110 0.676593 11.00000 -1.20000
AFIX 0
C16 1 0.710995 0.687442 0.833344 11.00000 0.02360 0.01991 =
0.01969 -0.00159 -0.00541 0.00317
C17 1 0.916551 0.699136 0.812802 11.00000 0.02563 0.02728 =
0.02651 -0.00414 -0.00023 0.00234
AFIX 43
H17 2 0.961035 0.682087 0.771090 11.00000 -1.20000
AFIX 0
C18 1 1.055691 0.735726 0.853475 11.00000 0.02525 0.02716 =
0.03504 0.00445 -0.00735 -0.00132
AFIX 43
H18 2 1.191624 0.743790 0.838547 11.00000 -1.20000
AFIX 0
C19 1 0.993035 0.760316 0.916253 11.00000 0.04146 0.02493 =
0.02687 -0.00019 -0.01511 -0.00485
AFIX 43
H19 2 1.085266 0.785696 0.943095 11.00000 -1.20000
AFIX 0
C20 1 0.793307 0.747102 0.938974 11.00000 0.04923 0.02903 =
0.01917 -0.00618 -0.00314 0.00210
AFIX 43
H20 2 0.752973 0.762312 0.982176 11.00000 -1.20000
AFIX 0
C21 1 0.652091 0.711165 0.897602 11.00000 0.02876 0.02668 =
0.01973 0.00004 -0.00176 0.00518
AFIX 43
H21 2 0.516889 0.702890 0.913013 11.00000 -1.20000
AFIX 0
C22 1 0.764085 0.548532 0.897662 11.00000 0.03448 0.02008 =
0.02174 0.00238 -0.00362 0.00426
C23 1 0.975735 0.568151 0.906627 11.00000 0.03238 0.04079 =
0.03716 -0.01027 -0.00761 0.00631
AFIX 43
H23 2 1.065285 0.564789 0.869283 11.00000 -1.20000
AFIX 0
C24 1 1.053345 0.592706 0.971151 11.00000 0.04096 0.04600 =
0.05240 -0.01708 -0.02269 0.01113
AFIX 43
H24 2 1.194293 0.606246 0.976708 11.00000 -1.20000
AFIX 0
C25 1 0.922076 0.597138 1.027229 11.00000 0.08085 0.03500 =
0.02779 -0.00564 -0.02069 0.00908
AFIX 43
H25 2 0.975356 0.613264 1.070522 11.00000 -1.20000
AFIX 0
C26 1 0.714519 0.577901 1.019189 11.00000 0.08570 0.03525 =
0.02592 -0.00194 0.00964 -0.00631
AFIX 43
H26 2 0.626143 0.581014 1.056878 11.00000 -1.20000
AFIX 0
C27 1 0.635695 0.553672 0.954587 11.00000 0.05075 0.02652 =
0.02932 0.00124 0.00663 -0.00388
AFIX 43
H27 2 0.494074 0.540649 0.949426 11.00000 -1.20000
AFIX 0
C28 1 0.825801 0.460910 0.787536 11.00000 0.03037 0.02009 =
0.02162 -0.00217 -0.00749 -0.00004
C29 1 1.019380 0.473190 0.758378 11.00000 0.03109 0.02097 =
0.05451 -0.00905 0.00011 -0.00327
AFIX 43
H29 2 1.061152 0.513000 0.752435 11.00000 -1.20000
AFIX 0
C30 1 1.151202 0.426952 0.738010 11.00000 0.02950 0.03426 =
0.05998 -0.01582 -0.00281 0.00026
AFIX 43
H30 2 1.280322 0.436000 0.718582 11.00000 -1.20000
AFIX 0
C31 1 1.092192 0.367601 0.746359 11.00000 0.04874 0.02807 =
0.03491 -0.00786 -0.01129 0.01205
AFIX 43
H31 2 1.180736 0.336705 0.732390 11.00000 -1.20000
AFIX 0
C32 1 0.902199 0.354414 0.775378 11.00000 0.07154 0.01936 =
0.02543 0.00056 -0.00122 0.00055
AFIX 43
H32 2 0.862768 0.314454 0.781685 11.00000 -1.20000
AFIX 0
C33 1 0.768249 0.400594 0.795413 11.00000 0.04966 0.02453 =
0.02094 0.00121 0.00026 -0.00515
AFIX 43
H33 2 0.638655 0.391167 0.814304 11.00000 -1.20000
AFIX 0
HKLF 4
REM e17rlw30
REM R1 = 0.0441 for 4773 Fo > 4sig(Fo) and 0.0577 for all 5808 data
REM 325 parameters refined using 0 restraints
END
WGHT 0.0427 1.6219
REM Highest difference peak 0.507, deepest hole -0.259, 1-sigma level 0.050
Q1 1 0.4614 0.4995 0.8280 11.00000 0.05 0.51
Q2 1 0.3498 0.6267 0.8050 11.00000 0.05 0.48
REM The information below was added by Olex2.
REM
REM R1 = 0.0441 for 4773 Fo > 4sig(Fo) and 0.0577 for all 23149 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.51, deepest hole -0.26
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0577
REM R1_gt = 0.0441
REM wR_ref = 0.1075
REM GOOF = 1.029
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 23149
REM Reflections_gt = 4773
REM Parameters = n/a
REM Hole = -0.26
REM Peak = 0.51
REM Flack = n/a
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_s17rlw8-Cpd-1f
_database_code_depnum_ccdc_archive 'CCDC 1849266'
_audit_update_record
;
2018-06-14 deposited with the CCDC.
2018-08-22 downloaded from the CCDC.
;
_audit_creation_date 2017-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C34 H31 N O P2'
_chemical_formula_sum 'C34 H31 N O P2'
_chemical_formula_weight 531.54
_chemical_absolute_configuration ?
_chemical_melting_point ?
_chemical_oxdiff_usercomment 'Colourless block'
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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 9
_space_group_name_H-M_alt 'C 1 c 1'
_space_group_name_Hall 'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
_cell_length_a 17.0617(3)
_cell_length_b 10.74210(10)
_cell_length_c 17.4615(3)
_cell_angle_alpha 90
_cell_angle_beta 117.433(2)
_cell_angle_gamma 90
_cell_volume 2840.44(9)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 12722
_cell_measurement_temperature 150.00(10)
_cell_measurement_theta_max 73.3380
_cell_measurement_theta_min 5.0470
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.593
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.88151
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.243
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1120
_exptl_crystal_size_max 0.248
_exptl_crystal_size_mid 0.182
_exptl_crystal_size_min 0.081
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0223
_diffrn_reflns_av_unetI/netI 0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 15029
_diffrn_reflns_point_group_measured_fraction_full 0.752
_diffrn_reflns_point_group_measured_fraction_max 0.739
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 73.414
_diffrn_reflns_theta_min 5.048
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 150.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.478
_reflns_Friedel_fraction_full 0.503
_reflns_Friedel_fraction_max 0.479
_reflns_number_gt 4207
_reflns_number_total 4234
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 0.199
_refine_diff_density_min -0.156
_refine_diff_density_rms 0.031
_refine_ls_abs_structure_details
;
Flack x determined using 1334 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.012(8)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.066
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 344
_refine_ls_number_reflns 4234
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0231
_refine_ls_R_factor_gt 0.0230
_refine_ls_restrained_S_all 1.066
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.6654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0616
_refine_ls_wR_factor_ref 0.0618
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C3(H3)
2.b Secondary CH2 refined with riding coordinates:
C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
C24(H24), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32),
C33(H33), C34(H34)
2.d Idealised Me refined as rotating group:
C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary iterative
_atom_sites_solution_secondary ?
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
P1 P 0.61498(3) 0.45398(4) 0.54988(3) 0.02066(10) Uani 1 1 d . . . . .
P2 P 0.55820(3) 0.21070(4) 0.47877(3) 0.02010(10) Uani 1 1 d . . . . .
O1 O 0.38645(10) 0.55643(13) 0.38669(9) 0.0274(3) Uani 1 1 d . . . . .
N1 N 0.32119(12) 0.54337(15) 0.47287(11) 0.0260(4) Uani 1 1 d . . . . .
C1 C 0.37864(12) 0.50300(17) 0.44503(12) 0.0204(4) Uani 1 1 d . . . . .
C2 C 0.43071(12) 0.38478(16) 0.48700(12) 0.0202(3) Uani 1 1 d . . . . .
H2A H 0.3925 0.3130 0.4636 0.024 Uiso 1 1 calc R . . . .
H2B H 0.4496 0.3875 0.5486 0.024 Uiso 1 1 calc R . . . .
C3 C 0.51166(12) 0.36993(16) 0.47184(11) 0.0187(3) Uani 1 1 d . . . . .
H3 H 0.4958 0.4021 0.4140 0.022 Uiso 1 1 calc R . . . .
C4 C 0.57893(13) 0.57801(18) 0.60022(13) 0.0230(4) Uani 1 1 d . . . . .
C5 C 0.53495(16) 0.68825(18) 0.56310(14) 0.0309(4) Uani 1 1 d . . . . .
H5 H 0.5164 0.7038 0.5049 0.037 Uiso 1 1 calc R . . . .
C6 C 0.51873(19) 0.7751(2) 0.61313(17) 0.0395(6) Uani 1 1 d . . . . .
H6 H 0.4900 0.8491 0.5883 0.047 Uiso 1 1 calc R . . . .
C7 C 0.54517(18) 0.7521(2) 0.69983(16) 0.0388(5) Uani 1 1 d . . . . .
H7 H 0.5341 0.8106 0.7329 0.047 Uiso 1 1 calc R . . . .
C8 C 0.58776(17) 0.6430(2) 0.73678(14) 0.0373(5) Uani 1 1 d . . . . .
H8 H 0.6051 0.6269 0.7947 0.045 Uiso 1 1 calc R . . . .
C9 C 0.60460(15) 0.5571(2) 0.68687(14) 0.0316(5) Uani 1 1 d . . . . .
H9 H 0.6339 0.4836 0.7122 0.038 Uiso 1 1 calc R . . . .
C10 C 0.64409(13) 0.53430(17) 0.47379(13) 0.0222(4) Uani 1 1 d . . . . .
C11 C 0.73047(14) 0.5204(2) 0.48618(14) 0.0293(4) Uani 1 1 d . . . . .
H11 H 0.7709 0.4740 0.5325 0.035 Uiso 1 1 calc R . . . .
C12 C 0.75655(16) 0.5762(2) 0.42910(16) 0.0360(5) Uani 1 1 d . . . . .
H12 H 0.8140 0.5657 0.4373 0.043 Uiso 1 1 calc R . . . .
C13 C 0.69781(16) 0.6461(2) 0.36122(15) 0.0354(5) Uani 1 1 d . . . . .
H13 H 0.7160 0.6845 0.3243 0.043 Uiso 1 1 calc R . . . .
C14 C 0.61122(16) 0.65982(19) 0.34724(14) 0.0316(5) Uani 1 1 d . . . . .
H14 H 0.5714 0.7068 0.3009 0.038 Uiso 1 1 calc R . . . .
C15 C 0.58430(14) 0.60320(18) 0.40269(13) 0.0252(4) Uani 1 1 d . . . . .
H15 H 0.5260 0.6111 0.3925 0.030 Uiso 1 1 calc R . . . .
C16 C 0.56853(13) 0.15058(16) 0.58143(12) 0.0232(4) Uani 1 1 d . . . . .
C17 C 0.49803(15) 0.13183(18) 0.60010(14) 0.0270(4) Uani 1 1 d . . . . .
H17 H 0.4407 0.1484 0.5582 0.032 Uiso 1 1 calc R . . . .
C18 C 0.51279(17) 0.08873(19) 0.68059(14) 0.0342(5) Uani 1 1 d . . . . .
H18 H 0.4655 0.0777 0.6926 0.041 Uiso 1 1 calc R . . . .
C19 C 0.5974(2) 0.06222(19) 0.74286(15) 0.0400(6) Uani 1 1 d . . . . .
H19 H 0.6070 0.0336 0.7968 0.048 Uiso 1 1 calc R . . . .
C20 C 0.66792(17) 0.0780(2) 0.72537(15) 0.0389(5) Uani 1 1 d . . . . .
H20 H 0.7248 0.0589 0.7672 0.047 Uiso 1 1 calc R . . . .
C21 C 0.65374(15) 0.12263(18) 0.64504(13) 0.0303(4) Uani 1 1 d . . . . .
H21 H 0.7015 0.1339 0.6337 0.036 Uiso 1 1 calc R . . . .
C22 C 0.46639(13) 0.11932(17) 0.39840(13) 0.0224(4) Uani 1 1 d . . . . .
C23 C 0.46877(15) -0.01075(19) 0.40721(14) 0.0292(4) Uani 1 1 d . . . . .
H23 H 0.5123 -0.0476 0.4568 0.035 Uiso 1 1 calc R . . . .
C24 C 0.40672(16) -0.0849(2) 0.34263(16) 0.0354(5) Uani 1 1 d . . . . .
H24 H 0.4084 -0.1708 0.3495 0.043 Uiso 1 1 calc R . . . .
C25 C 0.34250(15) -0.0312(2) 0.26819(15) 0.0354(5) Uani 1 1 d . . . . .
H25 H 0.3013 -0.0812 0.2248 0.043 Uiso 1 1 calc R . . . .
C26 C 0.33946(14) 0.0971(2) 0.25814(14) 0.0328(5) Uani 1 1 d . . . . .
H26 H 0.2962 0.1332 0.2081 0.039 Uiso 1 1 calc R . . . .
C27 C 0.40130(14) 0.17170(19) 0.32305(13) 0.0271(4) Uani 1 1 d . . . . .
H27 H 0.3991 0.2576 0.3159 0.033 Uiso 1 1 calc R . . . .
C28 C 0.27136(17) 0.6584(2) 0.43576(17) 0.0399(5) Uani 1 1 d . . . . .
H28A H 0.2233 0.6645 0.4498 0.060 Uiso 1 1 calc GR . . . .
H28B H 0.2486 0.6569 0.3742 0.060 Uiso 1 1 calc GR . . . .
H28C H 0.3097 0.7289 0.4591 0.060 Uiso 1 1 calc GR . . . .
C29 C 0.31196(13) 0.48507(18) 0.54218(12) 0.0226(4) Uani 1 1 d . . . . .
C30 C 0.36600(14) 0.5222(2) 0.62637(14) 0.0299(4) Uani 1 1 d . . . . .
H30 H 0.4067 0.5860 0.6374 0.036 Uiso 1 1 calc R . . . .
C31 C 0.35944(17) 0.4643(2) 0.69417(15) 0.0365(5) Uani 1 1 d . . . . .
H31 H 0.3960 0.4889 0.7507 0.044 Uiso 1 1 calc R . . . .
C32 C 0.29918(19) 0.3711(2) 0.67806(17) 0.0408(6) Uani 1 1 d . . . . .
H32 H 0.2952 0.3318 0.7236 0.049 Uiso 1 1 calc R . . . .
C33 C 0.2443(2) 0.3354(2) 0.59432(19) 0.0477(7) Uani 1 1 d . . . . .
H33 H 0.2029 0.2728 0.5836 0.057 Uiso 1 1 calc R . . . .
C34 C 0.25061(17) 0.3926(2) 0.52562(16) 0.0368(5) Uani 1 1 d . . . . .
H34 H 0.2136 0.3683 0.4692 0.044 Uiso 1 1 calc R . . . .
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
P1 0.0184(2) 0.0212(2) 0.0188(2) 0.00215(17) 0.00549(17) -0.00005(18)
P2 0.0173(2) 0.0206(2) 0.0226(2) -0.00092(16) 0.00944(17) 0.00171(18)
O1 0.0266(7) 0.0357(7) 0.0215(7) 0.0074(5) 0.0125(6) 0.0098(6)
N1 0.0270(9) 0.0298(8) 0.0253(9) 0.0061(6) 0.0154(7) 0.0104(7)
C1 0.0189(9) 0.0241(9) 0.0162(8) -0.0006(7) 0.0064(7) 0.0012(7)
C2 0.0180(8) 0.0217(8) 0.0210(9) -0.0006(7) 0.0090(7) 0.0001(7)
C3 0.0176(9) 0.0181(8) 0.0195(8) -0.0001(6) 0.0079(7) 0.0006(7)
C4 0.0233(9) 0.0238(8) 0.0210(9) -0.0035(7) 0.0096(7) -0.0070(8)
C5 0.0454(13) 0.0236(9) 0.0256(10) -0.0012(8) 0.0181(10) -0.0026(9)
C6 0.0633(17) 0.0208(9) 0.0446(14) -0.0029(9) 0.0336(13) -0.0032(10)
C7 0.0548(15) 0.0338(11) 0.0384(12) -0.0180(9) 0.0306(12) -0.0201(11)
C8 0.0414(13) 0.0495(13) 0.0226(10) -0.0067(9) 0.0161(9) -0.0130(11)
C9 0.0296(11) 0.0396(11) 0.0223(10) 0.0024(8) 0.0093(9) -0.0022(9)
C10 0.0223(9) 0.0212(9) 0.0237(10) -0.0045(7) 0.0111(8) -0.0050(7)
C11 0.0224(10) 0.0329(10) 0.0319(11) -0.0071(8) 0.0119(9) -0.0039(8)
C12 0.0283(11) 0.0436(12) 0.0435(13) -0.0149(10) 0.0229(10) -0.0122(10)
C13 0.0466(13) 0.0339(11) 0.0380(12) -0.0089(9) 0.0301(11) -0.0157(10)
C14 0.0398(12) 0.0272(9) 0.0297(11) 0.0002(8) 0.0178(10) -0.0048(9)
C15 0.0268(10) 0.0248(9) 0.0251(10) -0.0002(7) 0.0129(8) -0.0013(8)
C16 0.0267(10) 0.0164(7) 0.0243(9) -0.0018(7) 0.0099(8) 0.0021(7)
C17 0.0304(10) 0.0222(9) 0.0277(10) -0.0013(7) 0.0127(8) -0.0003(8)
C18 0.0512(14) 0.0251(10) 0.0341(12) -0.0036(8) 0.0263(11) -0.0021(9)
C19 0.0669(17) 0.0251(10) 0.0237(11) 0.0000(8) 0.0171(11) 0.0013(11)
C20 0.0428(14) 0.0309(11) 0.0279(11) 0.0018(9) 0.0034(10) 0.0049(10)
C21 0.0289(11) 0.0251(9) 0.0286(11) 0.0002(8) 0.0060(9) 0.0046(8)
C22 0.0222(9) 0.0243(9) 0.0241(9) -0.0039(7) 0.0136(7) -0.0004(7)
C23 0.0313(11) 0.0249(9) 0.0305(11) -0.0030(8) 0.0134(9) 0.0015(8)
C24 0.0393(12) 0.0247(10) 0.0420(13) -0.0084(8) 0.0184(10) -0.0021(9)
C25 0.0294(12) 0.0379(11) 0.0356(12) -0.0169(9) 0.0120(10) -0.0062(9)
C26 0.0255(10) 0.0415(12) 0.0255(10) -0.0048(9) 0.0067(8) 0.0007(9)
C27 0.0269(10) 0.0282(9) 0.0254(10) -0.0025(8) 0.0114(8) 0.0008(8)
C28 0.0425(13) 0.0411(12) 0.0443(14) 0.0168(10) 0.0271(11) 0.0227(11)
C29 0.0224(10) 0.0245(9) 0.0235(9) 0.0020(7) 0.0127(8) 0.0059(7)
C30 0.0250(10) 0.0377(11) 0.0272(10) -0.0026(8) 0.0123(8) -0.0043(9)
C31 0.0361(12) 0.0496(13) 0.0242(11) 0.0036(9) 0.0143(9) 0.0074(10)
C32 0.0628(16) 0.0313(11) 0.0447(13) 0.0115(10) 0.0390(13) 0.0139(11)
C33 0.0656(18) 0.0287(11) 0.0669(19) -0.0094(11) 0.0462(16) -0.0175(11)
C34 0.0419(13) 0.0365(11) 0.0355(12) -0.0151(9) 0.0209(10) -0.0126(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
P1 C3 1.8885(18) . ?
P1 C4 1.850(2) . ?
P1 C10 1.834(2) . ?
P2 C3 1.8660(17) . ?
P2 C16 1.8359(19) . ?
P2 C22 1.833(2) . ?
O1 C1 1.229(2) . ?
N1 C1 1.351(2) . ?
N1 C28 1.470(3) . ?
N1 C29 1.434(2) . ?
C1 C2 1.529(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.530(2) . ?
C3 H3 0.9800 . ?
C4 C5 1.392(3) . ?
C4 C9 1.386(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.390(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.388(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.373(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.387(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.396(3) . ?
C10 C15 1.401(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.399(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.371(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.390(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.388(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.398(3) . ?
C16 C21 1.396(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.388(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.379(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.381(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.394(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.404(3) . ?
C22 C27 1.391(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.388(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.382(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.387(3) . ?
C26 H26 0.9300 . ?
C26 C27 1.392(3) . ?
C27 H27 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.386(3) . ?
C29 C34 1.374(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.387(3) . ?
C31 H31 0.9300 . ?
C31 C32 1.368(4) . ?
C32 H32 0.9300 . ?
C32 C33 1.378(4) . ?
C33 H33 0.9300 . ?
C33 C34 1.395(3) . ?
C34 H34 0.9300 . ?
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
C4 P1 C3 106.44(8) . . ?
C10 P1 C3 100.16(8) . . ?
C10 P1 C4 105.40(9) . . ?
C16 P2 C3 103.44(8) . . ?
C22 P2 C3 104.67(8) . . ?
C22 P2 C16 102.88(9) . . ?
C1 N1 C28 118.64(16) . . ?
C1 N1 C29 122.93(15) . . ?
C29 N1 C28 118.21(16) . . ?
O1 C1 N1 121.48(17) . . ?
O1 C1 C2 121.61(16) . . ?
N1 C1 C2 116.86(16) . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
C1 C2 C3 112.03(15) . . ?
H2A C2 H2B 107.9 . . ?
C3 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
P1 C3 H3 107.3 . . ?
P2 C3 P1 99.42(8) . . ?
P2 C3 H3 107.3 . . ?
C2 C3 P1 116.25(12) . . ?
C2 C3 P2 118.40(12) . . ?
C2 C3 H3 107.3 . . ?
C5 C4 P1 128.11(15) . . ?
C9 C4 P1 113.26(16) . . ?
C9 C4 C5 118.54(19) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 119.9(2) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.5(2) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0(2) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 120.3 . . ?
C7 C8 C9 119.4(2) . . ?
C9 C8 H8 120.3 . . ?
C4 C9 C8 121.7(2) . . ?
C4 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C11 C10 P1 117.17(16) . . ?
C11 C10 C15 118.66(19) . . ?
C15 C10 P1 124.11(15) . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.2(2) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.3(2) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.9 . . ?
C12 C13 C14 120.3(2) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.8(2) . . ?
C15 C14 H14 120.1 . . ?
C10 C15 H15 119.7 . . ?
C14 C15 C10 120.6(2) . . ?
C14 C15 H15 119.7 . . ?
C17 C16 P2 124.92(16) . . ?
C21 C16 P2 116.67(16) . . ?
C21 C16 C17 118.41(19) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.7(2) . . ?
C18 C17 H17 119.7 . . ?
C17 C18 H18 119.9 . . ?
C19 C18 C17 120.2(2) . . ?
C19 C18 H18 119.9 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.2(2) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 120.0 . . ?
C19 C20 C21 120.0(2) . . ?
C21 C20 H20 120.0 . . ?
C16 C21 H21 119.7 . . ?
C20 C21 C16 120.6(2) . . ?
C20 C21 H21 119.7 . . ?
C23 C22 P2 118.52(16) . . ?
C27 C22 P2 122.39(15) . . ?
C27 C22 C23 118.45(18) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 C22 120.6(2) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.2(2) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.0(2) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 120.0 . . ?
C25 C26 C27 119.9(2) . . ?
C27 C26 H26 120.0 . . ?
C22 C27 C26 120.83(19) . . ?
C22 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
N1 C28 H28A 109.5 . . ?
N1 C28 H28B 109.5 . . ?
N1 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N1 119.43(18) . . ?
C34 C29 N1 120.49(19) . . ?
C34 C29 C30 120.08(19) . . ?
C29 C30 H30 120.0 . . ?
C29 C30 C31 120.0(2) . . ?
C31 C30 H30 120.0 . . ?
C30 C31 H31 120.0 . . ?
C32 C31 C30 120.1(2) . . ?
C32 C31 H31 120.0 . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120.0(2) . . ?
C33 C32 H32 120.0 . . ?
C32 C33 H33 119.8 . . ?
C32 C33 C34 120.4(2) . . ?
C34 C33 H33 119.8 . . ?
C29 C34 C33 119.4(2) . . ?
C29 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
_iucr_refine_instructions_details
;
s17rlw8.res created by SHELXL-2014/7
TITL s17rlw8
CELL 1.54184 17.0617 10.7421 17.4615 90 117.433 90
ZERR 4 0.0003 0.0001 0.0003 0 0.002 0
LATT -7
SYMM +X,-Y,0.5+Z
SFAC C H N O P
UNIT 136 124 4 4 8
L.S. 10
PLAN 2
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.039500 0.665400
FVAR 0.43616
P1 5 0.614982 0.453984 0.549881 11.00000 0.01838 0.02116 =
0.01884 0.00215 0.00549 -0.00005
P2 5 0.558199 0.210704 0.478770 11.00000 0.01730 0.02065 =
0.02263 -0.00092 0.00944 0.00171
O1 4 0.386446 0.556435 0.386689 11.00000 0.02658 0.03569 =
0.02150 0.00743 0.01248 0.00979
N1 3 0.321192 0.543368 0.472866 11.00000 0.02697 0.02976 =
0.02530 0.00611 0.01542 0.01041
C1 1 0.378640 0.503004 0.445027 11.00000 0.01893 0.02405 =
0.01616 -0.00065 0.00637 0.00115
C2 1 0.430711 0.384783 0.486998 11.00000 0.01802 0.02165 =
0.02101 -0.00060 0.00900 0.00007
AFIX 23
H2A 2 0.392515 0.313002 0.463583 11.00000 -1.20000
H2B 2 0.449633 0.387543 0.548561 11.00000 -1.20000
AFIX 0
C3 1 0.511659 0.369926 0.471837 11.00000 0.01763 0.01814 =
0.01947 -0.00013 0.00794 0.00060
AFIX 13
H3 2 0.495755 0.402134 0.414012 11.00000 -1.20000
AFIX 0
C4 1 0.578929 0.578014 0.600219 11.00000 0.02333 0.02380 =
0.02104 -0.00350 0.00960 -0.00697
C5 1 0.534948 0.688248 0.563099 11.00000 0.04542 0.02357 =
0.02562 -0.00119 0.01809 -0.00255
AFIX 43
H5 2 0.516428 0.703787 0.504889 11.00000 -1.20000
AFIX 0
C6 1 0.518728 0.775118 0.613131 11.00000 0.06332 0.02085 =
0.04461 -0.00295 0.03360 -0.00320
AFIX 43
H6 2 0.489961 0.849146 0.588338 11.00000 -1.20000
AFIX 0
C7 1 0.545173 0.752118 0.699831 11.00000 0.05480 0.03379 =
0.03843 -0.01803 0.03060 -0.02008
AFIX 43
H7 2 0.534051 0.810602 0.732892 11.00000 -1.20000
AFIX 0
C8 1 0.587761 0.643001 0.736784 11.00000 0.04139 0.04950 =
0.02260 -0.00673 0.01609 -0.01303
AFIX 43
H8 2 0.605147 0.626859 0.794717 11.00000 -1.20000
AFIX 0
C9 1 0.604596 0.557094 0.686873 11.00000 0.02965 0.03960 =
0.02233 0.00237 0.00926 -0.00220
AFIX 43
H9 2 0.633852 0.483584 0.712200 11.00000 -1.20000
AFIX 0
C10 1 0.644089 0.534297 0.473785 11.00000 0.02227 0.02123 =
0.02368 -0.00445 0.01112 -0.00497
C11 1 0.730474 0.520435 0.486179 11.00000 0.02243 0.03289 =
0.03185 -0.00706 0.01190 -0.00392
AFIX 43
H11 2 0.770855 0.473990 0.532532 11.00000 -1.20000
AFIX 0
C12 1 0.756551 0.576175 0.429105 11.00000 0.02828 0.04364 =
0.04349 -0.01486 0.02295 -0.01216
AFIX 43
H12 2 0.814001 0.565738 0.437271 11.00000 -1.20000
AFIX 0
C13 1 0.697811 0.646086 0.361220 11.00000 0.04664 0.03395 =
0.03804 -0.00892 0.03008 -0.01566
AFIX 43
H13 2 0.715980 0.684506 0.324346 11.00000 -1.20000
AFIX 0
C14 1 0.611219 0.659816 0.347244 11.00000 0.03976 0.02724 =
0.02973 0.00022 0.01776 -0.00476
AFIX 43
H14 2 0.571413 0.706806 0.300876 11.00000 -1.20000
AFIX 0
C15 1 0.584298 0.603197 0.402685 11.00000 0.02681 0.02479 =
0.02513 -0.00017 0.01293 -0.00130
AFIX 43
H15 2 0.526017 0.611086 0.392526 11.00000 -1.20000
AFIX 0
C16 1 0.568529 0.150578 0.581429 11.00000 0.02675 0.01645 =
0.02431 -0.00184 0.00989 0.00207
C17 1 0.498035 0.131829 0.600097 11.00000 0.03036 0.02223 =
0.02773 -0.00127 0.01274 -0.00027
AFIX 43
H17 2 0.440688 0.148395 0.558175 11.00000 -1.20000
AFIX 0
C18 1 0.512790 0.088729 0.680594 11.00000 0.05119 0.02512 =
0.03405 -0.00356 0.02635 -0.00209
AFIX 43
H18 2 0.465466 0.077707 0.692552 11.00000 -1.20000
AFIX 0
C19 1 0.597402 0.062216 0.742864 11.00000 0.06688 0.02512 =
0.02370 0.00002 0.01707 0.00132
AFIX 43
H19 2 0.607020 0.033639 0.796772 11.00000 -1.20000
AFIX 0
C20 1 0.667917 0.077997 0.725375 11.00000 0.04282 0.03093 =
0.02795 0.00184 0.00338 0.00492
AFIX 43
H20 2 0.724830 0.058854 0.767176 11.00000 -1.20000
AFIX 0
C21 1 0.653740 0.122629 0.645044 11.00000 0.02887 0.02509 =
0.02857 0.00021 0.00598 0.00456
AFIX 43
H21 2 0.701459 0.133888 0.633722 11.00000 -1.20000
AFIX 0
C22 1 0.466391 0.119317 0.398401 11.00000 0.02219 0.02433 =
0.02411 -0.00389 0.01361 -0.00038
C23 1 0.468769 -0.010748 0.407215 11.00000 0.03133 0.02488 =
0.03052 -0.00302 0.01344 0.00149
AFIX 43
H23 2 0.512313 -0.047568 0.456776 11.00000 -1.20000
AFIX 0
C24 1 0.406719 -0.084851 0.342626 11.00000 0.03930 0.02466 =
0.04198 -0.00840 0.01843 -0.00212
AFIX 43
H24 2 0.408362 -0.170827 0.349461 11.00000 -1.20000
AFIX 0
C25 1 0.342501 -0.031221 0.268189 11.00000 0.02936 0.03789 =
0.03561 -0.01685 0.01199 -0.00617
AFIX 43
H25 2 0.301305 -0.081157 0.224814 11.00000 -1.20000
AFIX 0
C26 1 0.339460 0.097068 0.258140 11.00000 0.02552 0.04151 =
0.02547 -0.00484 0.00666 0.00073
AFIX 43
H26 2 0.296167 0.133188 0.208102 11.00000 -1.20000
AFIX 0
C27 1 0.401297 0.171696 0.323050 11.00000 0.02687 0.02819 =
0.02542 -0.00250 0.01136 0.00079
AFIX 43
H27 2 0.399051 0.257643 0.315938 11.00000 -1.20000
AFIX 0
C28 1 0.271364 0.658392 0.435760 11.00000 0.04250 0.04107 =
0.04426 0.01681 0.02706 0.02274
AFIX 137
H28A 2 0.223302 0.664484 0.449779 11.00000 -1.50000
H28B 2 0.248553 0.656913 0.374204 11.00000 -1.50000
H28C 2 0.309703 0.728883 0.459070 11.00000 -1.50000
AFIX 0
C29 1 0.311965 0.485074 0.542180 11.00000 0.02236 0.02448 =
0.02347 0.00198 0.01271 0.00586
C30 1 0.366001 0.522192 0.626365 11.00000 0.02499 0.03770 =
0.02720 -0.00261 0.01230 -0.00434
AFIX 43
H30 2 0.406680 0.585960 0.637387 11.00000 -1.20000
AFIX 0
C31 1 0.359445 0.464298 0.694169 11.00000 0.03608 0.04964 =
0.02417 0.00361 0.01432 0.00738
AFIX 43
H31 2 0.396047 0.488854 0.750656 11.00000 -1.20000
AFIX 0
C32 1 0.299184 0.371086 0.678056 11.00000 0.06284 0.03133 =
0.04473 0.01149 0.03897 0.01390
AFIX 43
H32 2 0.295238 0.331807 0.723619 11.00000 -1.20000
AFIX 0
C33 1 0.244326 0.335381 0.594321 11.00000 0.06564 0.02874 =
0.06691 -0.00939 0.04616 -0.01755
AFIX 43
H33 2 0.202875 0.272803 0.583558 11.00000 -1.20000
AFIX 0
C34 1 0.250613 0.392554 0.525624 11.00000 0.04189 0.03649 =
0.03550 -0.01505 0.02093 -0.01260
AFIX 43
H34 2 0.213636 0.368282 0.469162 11.00000 -1.20000
AFIX 0
HKLF 4
REM s17rlw8
REM R1 = 0.0230 for 4207 Fo > 4sig(Fo) and 0.0231 for all 4234 data
REM 344 parameters refined using 2 restraints
END
WGHT 0.0395 0.6654
REM Highest difference peak 0.199, deepest hole -0.156, 1-sigma level 0.031
Q1 1 0.5213 0.2872 0.4718 11.00000 0.05 0.20
Q2 1 0.6589 0.3963 0.5834 11.00000 0.05 0.19
REM The information below was added by Olex2.
REM
REM R1 = 0.0230 for 4207 Fo > 4sig(Fo) and 0.0231 for all 15484 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.20, deepest hole -0.16
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0231
REM R1_gt = 0.0230
REM wR_ref = 0.0618
REM GOOF = 1.066
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 15484
REM Reflections_gt = 4207
REM Parameters = n/a
REM Hole = -0.16
REM Peak = 0.20
REM Flack = 0.012(8)
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_p18prr20-Cpd-1j
_database_code_depnum_ccdc_archive 'CCDC 1849268'
_audit_update_record
;
2018-06-14 deposited with the CCDC.
2018-08-22 downloaded from the CCDC.
;
_audit_creation_date 2018-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number 2014-3
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C39 H33 N P2, C2 H3 N'
_chemical_formula_sum 'C41 H36 N2 P2'
_chemical_formula_weight 618.66
_chemical_melting_point ?
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_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 10.1534(3)
_cell_length_b 18.1256(4)
_cell_length_c 18.7968(5)
_cell_angle_alpha 90
_cell_angle_beta 99.266(3)
_cell_angle_gamma 90
_cell_volume 3414.16(16)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 13041
_cell_measurement_temperature 150.00(10)
_cell_measurement_theta_max 28.8590
_cell_measurement_theta_min 3.3230
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.159
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.92932
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour pale-yellow
_exptl_crystal_density_diffrn 1.204
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description tablet
_exptl_crystal_F_000 1304
_exptl_crystal_size_max 0.442
_exptl_crystal_size_mid 0.321
_exptl_crystal_size_min 0.139
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0383
_diffrn_reflns_av_unetI/netI 0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 42670
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.484
_diffrn_reflns_theta_min 2.963
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 150.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6133
_reflns_number_total 7735
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 0.594
_refine_diff_density_min -0.309
_refine_diff_density_rms 0.045
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 411
_refine_ls_number_reflns 7735
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0610
_refine_ls_R_factor_gt 0.0437
_refine_ls_restrained_S_all 1.045
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+1.4568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1033
_refine_ls_wR_factor_ref 0.1127
_refine_special_details
;
The asymmetric unit in this structure houses one molecule of
the phosphine and one molecule of acetonitrile. H1 was
located and refined subject to being a distance of 0.98\%A from N1.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
N1-H1
0.98 with sigma of 0.005
3.a Ternary CH refined with riding coordinates:
C1(H1A)
3.b Aromatic/amide H refined with riding coordinates:
C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31),
C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
3.c Idealised Me refined as rotating group:
C41(H41A,H41B,H41C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary iterative
_atom_sites_solution_secondary ?
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
P1 P 0.91773(4) 0.23599(2) 0.44085(2) 0.02911(11) Uani 1 1 d . . . . .
P2 P 0.67216(4) 0.32484(2) 0.37784(2) 0.02645(11) Uani 1 1 d . . . . .
N1 N 0.69354(14) 0.21261(7) 0.59710(7) 0.0269(3) Uani 1 1 d D . . . .
H1 H 0.734(2) 0.1735(8) 0.5726(10) 0.050(6) Uiso 1 1 d D . . . .
C1 C 0.75065(16) 0.26886(9) 0.45756(8) 0.0249(3) Uani 1 1 d . . . . .
H1A H 0.6942 0.2257 0.4618 0.030 Uiso 1 1 calc R . . . .
C2 C 0.76980(16) 0.30960(8) 0.52761(8) 0.0249(3) Uani 1 1 d . . . . .
H2 H 0.8068 0.3566 0.5279 0.030 Uiso 1 1 calc R . . . .
C3 C 0.73872(15) 0.28496(8) 0.59011(8) 0.0240(3) Uani 1 1 d . . . . .
C4 C 0.76839(16) 0.33037(8) 0.65676(8) 0.0248(3) Uani 1 1 d . . . . .
C5 C 0.75443(17) 0.40685(9) 0.65439(9) 0.0301(4) Uani 1 1 d . . . . .
H5 H 0.7209 0.4301 0.6111 0.036 Uiso 1 1 calc R . . . .
C6 C 0.7903(2) 0.44828(10) 0.71621(10) 0.0380(4) Uani 1 1 d . . . . .
H6 H 0.7818 0.4994 0.7141 0.046 Uiso 1 1 calc R . . . .
C7 C 0.83893(19) 0.41445(10) 0.78113(10) 0.0383(4) Uani 1 1 d . . . . .
H7 H 0.8629 0.4426 0.8226 0.046 Uiso 1 1 calc R . . . .
C8 C 0.85151(19) 0.33880(10) 0.78395(9) 0.0355(4) Uani 1 1 d . . . . .
H8 H 0.8836 0.3158 0.8275 0.043 Uiso 1 1 calc R . . . .
C9 C 0.81676(17) 0.29713(9) 0.72244(9) 0.0303(4) Uani 1 1 d . . . . .
H9 H 0.8258 0.2461 0.7249 0.036 Uiso 1 1 calc R . . . .
C10 C 0.59336(16) 0.19084(9) 0.63575(8) 0.0259(3) Uani 1 1 d . . . . .
C11 C 0.50351(17) 0.24072(10) 0.65762(9) 0.0327(4) Uani 1 1 d . . . . .
H11 H 0.5088 0.2905 0.6465 0.039 Uiso 1 1 calc R . . . .
C12 C 0.40631(19) 0.21620(11) 0.69585(10) 0.0397(4) Uani 1 1 d . . . . .
H12 H 0.3479 0.2500 0.7112 0.048 Uiso 1 1 calc R . . . .
C13 C 0.39490(18) 0.14225(12) 0.71145(10) 0.0404(4) Uani 1 1 d . . . . .
H13 H 0.3291 0.1261 0.7370 0.048 Uiso 1 1 calc R . . . .
C14 C 0.48214(18) 0.09276(11) 0.68871(10) 0.0400(4) Uani 1 1 d . . . . .
H14 H 0.4742 0.0428 0.6984 0.048 Uiso 1 1 calc R . . . .
C15 C 0.58164(17) 0.11640(9) 0.65153(9) 0.0316(4) Uani 1 1 d . . . . .
H15 H 0.6407 0.0824 0.6371 0.038 Uiso 1 1 calc R . . . .
C16 C 0.95983(16) 0.17475(9) 0.51912(9) 0.0302(4) Uani 1 1 d . . . . .
C17 C 1.02591(17) 0.20633(11) 0.58289(10) 0.0372(4) Uani 1 1 d . . . . .
H17 H 1.0511 0.2557 0.5832 0.045 Uiso 1 1 calc R . . . .
C18 C 1.05427(19) 0.16526(12) 0.64541(11) 0.0458(5) Uani 1 1 d . . . . .
H18 H 1.0958 0.1874 0.6878 0.055 Uiso 1 1 calc R . . . .
C19 C 1.0210(2) 0.09161(12) 0.64497(11) 0.0493(5) Uani 1 1 d . . . . .
H19 H 1.0407 0.0638 0.6869 0.059 Uiso 1 1 calc R . . . .
C20 C 0.9582(2) 0.05923(11) 0.58206(11) 0.0479(5) Uani 1 1 d . . . . .
H20 H 0.9372 0.0093 0.5817 0.057 Uiso 1 1 calc R . . . .
C21 C 0.92595(19) 0.10033(10) 0.51944(10) 0.0379(4) Uani 1 1 d . . . . .
H21 H 0.8817 0.0782 0.4777 0.045 Uiso 1 1 calc R . . . .
C22 C 0.87895(18) 0.17059(9) 0.36602(9) 0.0300(4) Uani 1 1 d . . . . .
C23 C 0.75279(19) 0.14359(10) 0.33853(10) 0.0396(4) Uani 1 1 d . . . . .
H23 H 0.6801 0.1569 0.3602 0.047 Uiso 1 1 calc R . . . .
C24 C 0.7343(2) 0.09713(11) 0.27930(11) 0.0447(5) Uani 1 1 d . . . . .
H24 H 0.6492 0.0800 0.2610 0.054 Uiso 1 1 calc R . . . .
C25 C 0.8417(2) 0.07605(10) 0.24728(10) 0.0443(5) Uani 1 1 d . . . . .
H25 H 0.8292 0.0446 0.2076 0.053 Uiso 1 1 calc R . . . .
C26 C 0.9674(2) 0.10191(11) 0.27446(10) 0.0423(5) Uani 1 1 d . . . . .
H26 H 1.0402 0.0873 0.2535 0.051 Uiso 1 1 calc R . . . .
C27 C 0.98592(19) 0.14946(10) 0.33281(9) 0.0357(4) Uani 1 1 d . . . . .
H27 H 1.0708 0.1675 0.3500 0.043 Uiso 1 1 calc R . . . .
C28 C 0.72719(17) 0.41844(9) 0.40507(8) 0.0277(3) Uani 1 1 d . . . . .
C29 C 0.85275(18) 0.44053(10) 0.39206(9) 0.0342(4) Uani 1 1 d . . . . .
H29 H 0.9040 0.4083 0.3694 0.041 Uiso 1 1 calc R . . . .
C30 C 0.9020(2) 0.51000(11) 0.41261(11) 0.0444(5) Uani 1 1 d . . . . .
H30 H 0.9863 0.5239 0.4041 0.053 Uiso 1 1 calc R . . . .
C31 C 0.8266(2) 0.55846(11) 0.44554(11) 0.0473(5) Uani 1 1 d . . . . .
H31 H 0.8598 0.6050 0.4594 0.057 Uiso 1 1 calc R . . . .
C32 C 0.7020(2) 0.53772(11) 0.45790(11) 0.0461(5) Uani 1 1 d . . . . .
H32 H 0.6508 0.5706 0.4799 0.055 Uiso 1 1 calc R . . . .
C33 C 0.65223(19) 0.46843(10) 0.43795(10) 0.0362(4) Uani 1 1 d . . . . .
H33 H 0.5678 0.4551 0.4466 0.043 Uiso 1 1 calc R . . . .
C34 C 0.49743(17) 0.32548(8) 0.39076(9) 0.0274(3) Uani 1 1 d . . . . .
C35 C 0.40615(19) 0.35607(9) 0.33506(10) 0.0354(4) Uani 1 1 d . . . . .
H35 H 0.4371 0.3782 0.2962 0.042 Uiso 1 1 calc R . . . .
C36 C 0.27038(19) 0.35403(10) 0.33668(11) 0.0408(4) Uani 1 1 d . . . . .
H36 H 0.2110 0.3745 0.2990 0.049 Uiso 1 1 calc R . . . .
C37 C 0.22309(18) 0.32180(10) 0.39376(11) 0.0402(4) Uani 1 1 d . . . . .
H37 H 0.1318 0.3204 0.3947 0.048 Uiso 1 1 calc R . . . .
C38 C 0.31117(18) 0.29159(10) 0.44948(10) 0.0368(4) Uani 1 1 d . . . . .
H38 H 0.2791 0.2698 0.4881 0.044 Uiso 1 1 calc R . . . .
C39 C 0.44754(17) 0.29339(9) 0.44849(9) 0.0291(3) Uani 1 1 d . . . . .
H39 H 0.5061 0.2731 0.4866 0.035 Uiso 1 1 calc R . . . .
N2 N 0.5371(3) 0.09509(13) 0.46402(11) 0.0725(6) Uani 1 1 d . . . A 1
C40 C 0.4367(3) 0.09170(13) 0.48373(12) 0.0542(6) Uani 1 1 d . . . A 1
C41 C 0.3115(3) 0.08634(16) 0.50935(15) 0.0695(7) Uani 1 1 d . . . A 1
H41A H 0.2403 0.0987 0.4711 0.104 Uiso 1 1 calc GR . . A 1
H41B H 0.3108 0.1199 0.5488 0.104 Uiso 1 1 calc GR . . A 1
H41C H 0.2993 0.0368 0.5253 0.104 Uiso 1 1 calc GR . . A 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_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0283(2) 0.0275(2) 0.0339(2) -0.00314(18) 0.01230(18) -0.00256(17)
P2 0.0327(2) 0.0254(2) 0.0227(2) -0.00097(16) 0.00891(17) -0.00182(17)
N1 0.0339(8) 0.0202(6) 0.0291(7) -0.0014(5) 0.0128(6) -0.0019(5)
C1 0.0287(8) 0.0224(7) 0.0256(7) 0.0004(6) 0.0105(6) -0.0005(6)
C2 0.0269(8) 0.0213(7) 0.0271(8) -0.0004(6) 0.0067(6) -0.0010(6)
C3 0.0252(8) 0.0199(7) 0.0273(8) 0.0004(6) 0.0056(6) 0.0007(6)
C4 0.0260(8) 0.0232(7) 0.0259(8) 0.0005(6) 0.0064(6) -0.0018(6)
C5 0.0383(9) 0.0246(8) 0.0275(8) 0.0038(7) 0.0054(7) -0.0006(7)
C6 0.0542(12) 0.0222(8) 0.0372(9) -0.0026(7) 0.0061(9) -0.0041(8)
C7 0.0486(11) 0.0348(10) 0.0303(9) -0.0073(8) 0.0021(8) -0.0084(8)
C8 0.0418(10) 0.0351(9) 0.0275(8) 0.0040(7) -0.0007(7) -0.0020(8)
C9 0.0374(9) 0.0232(8) 0.0299(8) 0.0027(7) 0.0039(7) -0.0009(7)
C10 0.0279(8) 0.0276(8) 0.0215(7) -0.0006(6) 0.0026(6) -0.0046(6)
C11 0.0335(9) 0.0293(9) 0.0367(9) -0.0047(7) 0.0099(7) -0.0039(7)
C12 0.0318(9) 0.0487(11) 0.0407(10) -0.0114(9) 0.0127(8) -0.0055(8)
C13 0.0294(9) 0.0589(12) 0.0335(9) 0.0077(9) 0.0067(8) -0.0104(9)
C14 0.0342(10) 0.0396(10) 0.0443(10) 0.0161(8) 0.0010(8) -0.0079(8)
C15 0.0297(9) 0.0282(8) 0.0363(9) 0.0047(7) 0.0036(7) -0.0009(7)
C16 0.0227(8) 0.0322(9) 0.0367(9) -0.0016(7) 0.0081(7) 0.0051(7)
C17 0.0252(9) 0.0400(10) 0.0450(10) -0.0046(8) 0.0020(8) 0.0015(7)
C18 0.0347(10) 0.0558(13) 0.0436(11) -0.0039(9) -0.0035(8) 0.0098(9)
C19 0.0533(13) 0.0481(12) 0.0448(11) 0.0087(9) 0.0025(10) 0.0209(10)
C20 0.0615(14) 0.0319(10) 0.0508(12) 0.0019(9) 0.0106(10) 0.0115(9)
C21 0.0431(10) 0.0314(9) 0.0396(10) -0.0035(8) 0.0079(8) 0.0052(8)
C22 0.0383(9) 0.0246(8) 0.0300(8) 0.0007(7) 0.0145(7) 0.0008(7)
C23 0.0391(10) 0.0392(10) 0.0444(10) -0.0097(8) 0.0186(9) -0.0056(8)
C24 0.0510(12) 0.0389(10) 0.0460(11) -0.0108(9) 0.0134(9) -0.0104(9)
C25 0.0683(14) 0.0331(10) 0.0339(9) -0.0054(8) 0.0154(10) 0.0049(9)
C26 0.0536(12) 0.0405(10) 0.0370(10) 0.0002(8) 0.0207(9) 0.0147(9)
C27 0.0378(10) 0.0361(9) 0.0360(9) 0.0029(8) 0.0143(8) 0.0059(8)
C28 0.0355(9) 0.0258(8) 0.0224(7) 0.0040(6) 0.0062(7) -0.0044(7)
C29 0.0328(9) 0.0378(10) 0.0326(9) 0.0040(7) 0.0068(7) -0.0022(7)
C30 0.0378(11) 0.0479(11) 0.0467(11) 0.0053(9) 0.0049(9) -0.0160(9)
C31 0.0580(13) 0.0347(10) 0.0485(11) -0.0038(9) 0.0066(10) -0.0164(9)
C32 0.0603(13) 0.0307(9) 0.0506(11) -0.0077(9) 0.0192(10) -0.0068(9)
C33 0.0437(10) 0.0285(9) 0.0398(10) -0.0042(8) 0.0175(8) -0.0072(8)
C34 0.0317(9) 0.0216(7) 0.0288(8) -0.0044(6) 0.0050(7) -0.0031(6)
C35 0.0431(10) 0.0253(8) 0.0365(9) 0.0013(7) 0.0025(8) -0.0030(7)
C36 0.0371(10) 0.0270(9) 0.0536(11) -0.0009(8) -0.0074(9) 0.0020(8)
C37 0.0280(9) 0.0287(9) 0.0633(12) -0.0088(9) 0.0054(9) -0.0020(7)
C38 0.0357(10) 0.0306(9) 0.0472(10) -0.0052(8) 0.0159(8) -0.0043(7)
C39 0.0311(9) 0.0257(8) 0.0311(8) -0.0035(7) 0.0068(7) -0.0012(7)
N2 0.0829(17) 0.0817(16) 0.0555(12) 0.0011(11) 0.0190(12) -0.0107(13)
C40 0.0659(16) 0.0471(12) 0.0453(12) -0.0018(10) -0.0038(11) -0.0054(11)
C41 0.0532(15) 0.0808(19) 0.0711(16) -0.0046(14) -0.0004(12) -0.0062(13)
_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
P1 C1 1.8717(16) . ?
P1 C16 1.8378(18) . ?
P1 C22 1.8331(17) . ?
P2 C1 1.8776(16) . ?
P2 C28 1.8332(17) . ?
P2 C34 1.8290(17) . ?
N1 H1 0.973(5) . ?
N1 C3 1.4024(19) . ?
N1 C10 1.399(2) . ?
C1 H1A 0.9800 . ?
C1 C2 1.495(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.341(2) . ?
C3 C4 1.489(2) . ?
C4 C5 1.393(2) . ?
C4 C9 1.390(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.382(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.384(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.377(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.379(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.393(2) . ?
C10 C15 1.391(2) . ?
C11 H11 0.9300 . ?
C11 C12 1.384(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.381(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.376(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.386(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.398(2) . ?
C16 C21 1.392(2) . ?
C17 H17 0.9300 . ?
C17 C18 1.382(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.377(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.381(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.387(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.391(3) . ?
C22 C27 1.391(2) . ?
C23 H23 0.9300 . ?
C23 C24 1.384(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.382(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.379(3) . ?
C26 H26 0.9300 . ?
C26 C27 1.384(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.395(2) . ?
C28 C33 1.391(2) . ?
C29 H29 0.9300 . ?
C29 C30 1.387(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.376(3) . ?
C31 H31 0.9300 . ?
C31 C32 1.375(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.383(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.396(2) . ?
C34 C39 1.396(2) . ?
C35 H35 0.9300 . ?
C35 C36 1.384(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.374(3) . ?
C37 H37 0.9300 . ?
C37 C38 1.377(3) . ?
C38 H38 0.9300 . ?
C38 C39 1.388(2) . ?
C39 H39 0.9300 . ?
N2 C40 1.141(3) . ?
C40 C41 1.434(4) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
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
C16 P1 C1 99.10(7) . . ?
C22 P1 C1 104.24(8) . . ?
C22 P1 C16 102.54(8) . . ?
C28 P2 C1 101.90(7) . . ?
C34 P2 C1 101.16(7) . . ?
C34 P2 C28 102.45(7) . . ?
C3 N1 H1 117.9(13) . . ?
C10 N1 H1 116.0(13) . . ?
C10 N1 C3 126.07(13) . . ?
P1 C1 P2 108.53(7) . . ?
P1 C1 H1A 108.5 . . ?
P2 C1 H1A 108.5 . . ?
C2 C1 P1 108.19(11) . . ?
C2 C1 P2 114.48(11) . . ?
C2 C1 H1A 108.5 . . ?
C1 C2 H2 116.9 . . ?
C3 C2 C1 126.26(14) . . ?
C3 C2 H2 116.9 . . ?
N1 C3 C4 117.59(13) . . ?
C2 C3 N1 121.35(14) . . ?
C2 C3 C4 120.58(14) . . ?
C5 C4 C3 121.16(14) . . ?
C9 C4 C3 120.16(14) . . ?
C9 C4 C5 118.61(15) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.13(15) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.59(16) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 120.2 . . ?
C8 C7 C6 119.52(16) . . ?
C8 C7 H7 120.2 . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.24(16) . . ?
C9 C8 H8 119.9 . . ?
C4 C9 H9 119.6 . . ?
C8 C9 C4 120.89(15) . . ?
C8 C9 H9 119.6 . . ?
C11 C10 N1 122.41(15) . . ?
C15 C10 N1 118.62(15) . . ?
C15 C10 C11 118.96(15) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.04(17) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.86(17) . . ?
C13 C12 H12 119.6 . . ?
C12 C13 H13 120.4 . . ?
C14 C13 C12 119.11(16) . . ?
C14 C13 H13 120.4 . . ?
C13 C14 H14 119.6 . . ?
C13 C14 C15 120.87(17) . . ?
C15 C14 H14 119.6 . . ?
C10 C15 H15 119.9 . . ?
C14 C15 C10 120.14(17) . . ?
C14 C15 H15 119.9 . . ?
C17 C16 P1 117.17(13) . . ?
C21 C16 P1 124.26(14) . . ?
C21 C16 C17 118.53(17) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 C16 120.93(18) . . ?
C18 C17 H17 119.5 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 119.99(19) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 120.1 . . ?
C18 C19 C20 119.76(19) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.79(19) . . ?
C21 C20 H20 119.6 . . ?
C16 C21 H21 120.0 . . ?
C20 C21 C16 119.96(18) . . ?
C20 C21 H21 120.0 . . ?
C23 C22 P1 125.73(13) . . ?
C23 C22 C27 118.39(16) . . ?
C27 C22 P1 115.82(14) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 C22 120.69(17) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.29(19) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 120.2 . . ?
C26 C25 C24 119.54(18) . . ?
C26 C25 H25 120.2 . . ?
C25 C26 H26 119.8 . . ?
C25 C26 C27 120.34(17) . . ?
C27 C26 H26 119.8 . . ?
C22 C27 H27 119.6 . . ?
C26 C27 C22 120.73(18) . . ?
C26 C27 H27 119.6 . . ?
C29 C28 P2 117.56(13) . . ?
C33 C28 P2 124.27(13) . . ?
C33 C28 C29 118.17(16) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 C28 120.70(17) . . ?
C30 C29 H29 119.6 . . ?
C29 C30 H30 119.9 . . ?
C31 C30 C29 120.22(18) . . ?
C31 C30 H30 119.9 . . ?
C30 C31 H31 120.2 . . ?
C32 C31 C30 119.68(18) . . ?
C32 C31 H31 120.2 . . ?
C31 C32 H32 119.7 . . ?
C31 C32 C33 120.57(19) . . ?
C33 C32 H32 119.7 . . ?
C28 C33 H33 119.7 . . ?
C32 C33 C28 120.66(17) . . ?
C32 C33 H33 119.7 . . ?
C35 C34 P2 116.35(13) . . ?
C39 C34 P2 125.56(13) . . ?
C39 C34 C35 117.91(16) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 C34 121.06(17) . . ?
C36 C35 H35 119.5 . . ?
C35 C36 H36 119.9 . . ?
C37 C36 C35 120.19(18) . . ?
C37 C36 H36 119.9 . . ?
C36 C37 H37 120.1 . . ?
C36 C37 C38 119.81(17) . . ?
C38 C37 H37 120.1 . . ?
C37 C38 H38 119.7 . . ?
C37 C38 C39 120.51(17) . . ?
C39 C38 H38 119.7 . . ?
C34 C39 H39 119.7 . . ?
C38 C39 C34 120.51(17) . . ?
C38 C39 H39 119.7 . . ?
N2 C40 C41 178.9(3) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
_iucr_refine_instructions_details
;
TITL p18prr20
CELL 0.71073 10.1534 18.1256 18.7968 90 99.266 90
ZERR 4 0.0003 0.0004 0.0005 0 0.003 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N P
UNIT 164 144 8 8
DFIX 0.98 0.005 N1 H1
L.S. 20
PLAN 20
BOND $H
list 4
more -3
fmap 2 53
acta
SHEL 999 0.77
OMIT 2 5 5
REM
REM
REM
WGHT 0.047700 1.456800
FVAR 0.46478
P1 4 0.917733 0.235995 0.440845 11.00000 0.02831 0.02753 =
0.03390 -0.00314 0.01230 -0.00256
P2 4 0.672158 0.324839 0.377838 11.00000 0.03271 0.02543 =
0.02266 -0.00097 0.00891 -0.00182
N1 3 0.693537 0.212612 0.597098 11.00000 0.03386 0.02025 =
0.02909 -0.00145 0.01280 -0.00191
H1 2 0.734159 0.173459 0.572618 11.00000 0.04960
C1 1 0.750648 0.268857 0.457556 11.00000 0.02870 0.02243 =
0.02557 0.00037 0.01048 -0.00047
AFIX 13
H1A 2 0.694219 0.225729 0.461791 11.00000 -1.20000
AFIX 0
C2 1 0.769800 0.309602 0.527614 11.00000 0.02692 0.02131 =
0.02713 -0.00038 0.00672 -0.00099
AFIX 43
H2 2 0.806824 0.356551 0.527882 11.00000 -1.20000
AFIX 0
C3 1 0.738722 0.284957 0.590109 11.00000 0.02523 0.01992 =
0.02733 0.00039 0.00561 0.00066
C4 1 0.768387 0.330368 0.656756 11.00000 0.02597 0.02324 =
0.02588 0.00050 0.00636 -0.00178
C5 1 0.754426 0.406847 0.654392 11.00000 0.03831 0.02461 =
0.02753 0.00384 0.00540 -0.00062
AFIX 43
H5 2 0.720872 0.430058 0.611138 11.00000 -1.20000
AFIX 0
C6 1 0.790345 0.448284 0.716205 11.00000 0.05421 0.02224 =
0.03723 -0.00257 0.00611 -0.00410
AFIX 43
H6 2 0.781784 0.499355 0.714141 11.00000 -1.20000
AFIX 0
C7 1 0.838926 0.414454 0.781131 11.00000 0.04859 0.03478 =
0.03027 -0.00725 0.00210 -0.00844
AFIX 43
H7 2 0.862905 0.442593 0.822564 11.00000 -1.20000
AFIX 0
C8 1 0.851514 0.338805 0.783949 11.00000 0.04184 0.03508 =
0.02745 0.00405 -0.00068 -0.00196
AFIX 43
H8 2 0.883572 0.315756 0.827503 11.00000 -1.20000
AFIX 0
C9 1 0.816763 0.297132 0.722439 11.00000 0.03738 0.02316 =
0.02990 0.00272 0.00394 -0.00089
AFIX 43
H9 2 0.825799 0.246097 0.724911 11.00000 -1.20000
AFIX 0
C10 1 0.593364 0.190842 0.635746 11.00000 0.02793 0.02765 =
0.02155 -0.00058 0.00261 -0.00455
C11 1 0.503506 0.240718 0.657624 11.00000 0.03355 0.02929 =
0.03673 -0.00468 0.00993 -0.00388
AFIX 43
H11 2 0.508806 0.290524 0.646543 11.00000 -1.20000
AFIX 0
C12 1 0.406308 0.216200 0.695853 11.00000 0.03183 0.04874 =
0.04069 -0.01143 0.01266 -0.00547
AFIX 43
H12 2 0.347927 0.249973 0.711235 11.00000 -1.20000
AFIX 0
C13 1 0.394899 0.142245 0.711449 11.00000 0.02942 0.05885 =
0.03352 0.00772 0.00674 -0.01041
AFIX 43
H13 2 0.329138 0.126100 0.736978 11.00000 -1.20000
AFIX 0
C14 1 0.482144 0.092761 0.688708 11.00000 0.03421 0.03960 =
0.04433 0.01610 0.00097 -0.00793
AFIX 43
H14 2 0.474215 0.042791 0.698420 11.00000 -1.20000
AFIX 0
C15 1 0.581645 0.116404 0.651532 11.00000 0.02968 0.02820 =
0.03634 0.00468 0.00362 -0.00093
AFIX 43
H15 2 0.640711 0.082423 0.637108 11.00000 -1.20000
AFIX 0
C16 1 0.959829 0.174746 0.519121 11.00000 0.02272 0.03219 =
0.03672 -0.00162 0.00813 0.00509
C17 1 1.025913 0.206328 0.582889 11.00000 0.02520 0.03999 =
0.04505 -0.00455 0.00197 0.00152
AFIX 43
H17 2 1.051132 0.255668 0.583218 11.00000 -1.20000
AFIX 0
C18 1 1.054268 0.165264 0.645411 11.00000 0.03469 0.05577 =
0.04359 -0.00392 -0.00350 0.00983
AFIX 43
H18 2 1.095832 0.187372 0.687787 11.00000 -1.20000
AFIX 0
C19 1 1.020980 0.091606 0.644968 11.00000 0.05334 0.04805 =
0.04484 0.00867 0.00253 0.02087
AFIX 43
H19 2 1.040736 0.063761 0.686887 11.00000 -1.20000
AFIX 0
C20 1 0.958156 0.059235 0.582057 11.00000 0.06154 0.03188 =
0.05077 0.00191 0.01064 0.01149
AFIX 43
H20 2 0.937192 0.009275 0.581671 11.00000 -1.20000
AFIX 0
C21 1 0.925949 0.100334 0.519442 11.00000 0.04307 0.03140 =
0.03958 -0.00354 0.00790 0.00522
AFIX 43
H21 2 0.881743 0.078200 0.477690 11.00000 -1.20000
AFIX 0
C22 1 0.878946 0.170592 0.366020 11.00000 0.03826 0.02464 =
0.02999 0.00071 0.01449 0.00076
C23 1 0.752791 0.143586 0.338527 11.00000 0.03906 0.03919 =
0.04437 -0.00971 0.01863 -0.00556
AFIX 43
H23 2 0.680090 0.156879 0.360158 11.00000 -1.20000
AFIX 0
C24 1 0.734299 0.097127 0.279304 11.00000 0.05096 0.03887 =
0.04602 -0.01076 0.01340 -0.01036
AFIX 43
H24 2 0.649220 0.080032 0.260999 11.00000 -1.20000
AFIX 0
C25 1 0.841680 0.076047 0.247275 11.00000 0.06827 0.03313 =
0.03385 -0.00537 0.01538 0.00489
AFIX 43
H25 2 0.829238 0.044623 0.207648 11.00000 -1.20000
AFIX 0
C26 1 0.967406 0.101915 0.274463 11.00000 0.05365 0.04055 =
0.03701 0.00025 0.02071 0.01473
AFIX 43
H26 2 1.040156 0.087334 0.253477 11.00000 -1.20000
AFIX 0
C27 1 0.985916 0.149462 0.332813 11.00000 0.03775 0.03606 =
0.03601 0.00294 0.01429 0.00590
AFIX 43
H27 2 1.070831 0.167490 0.350017 11.00000 -1.20000
AFIX 0
C28 1 0.727190 0.418443 0.405072 11.00000 0.03547 0.02582 =
0.02241 0.00404 0.00623 -0.00444
C29 1 0.852748 0.440532 0.392057 11.00000 0.03284 0.03781 =
0.03256 0.00398 0.00675 -0.00220
AFIX 43
H29 2 0.903969 0.408322 0.369354 11.00000 -1.20000
AFIX 0
C30 1 0.901996 0.509998 0.412606 11.00000 0.03784 0.04794 =
0.04667 0.00529 0.00493 -0.01596
AFIX 43
H30 2 0.986261 0.523882 0.404105 11.00000 -1.20000
AFIX 0
C31 1 0.826607 0.558464 0.445538 11.00000 0.05802 0.03472 =
0.04850 -0.00376 0.00657 -0.01636
AFIX 43
H31 2 0.859769 0.605022 0.459365 11.00000 -1.20000
AFIX 0
C32 1 0.702020 0.537724 0.457901 11.00000 0.06033 0.03067 =
0.05057 -0.00768 0.01923 -0.00679
AFIX 43
H32 2 0.650781 0.570577 0.479866 11.00000 -1.20000
AFIX 0
C33 1 0.652230 0.468426 0.437954 11.00000 0.04373 0.02853 =
0.03982 -0.00417 0.01747 -0.00724
AFIX 43
H33 2 0.567777 0.455126 0.446619 11.00000 -1.20000
AFIX 0
C34 1 0.497433 0.325478 0.390758 11.00000 0.03172 0.02165 =
0.02878 -0.00439 0.00502 -0.00313
C35 1 0.406152 0.356069 0.335057 11.00000 0.04311 0.02534 =
0.03650 0.00130 0.00255 -0.00301
AFIX 43
H35 2 0.437074 0.378163 0.296247 11.00000 -1.20000
AFIX 0
C36 1 0.270383 0.354035 0.336683 11.00000 0.03707 0.02697 =
0.05360 -0.00087 -0.00744 0.00197
AFIX 43
H36 2 0.210997 0.374539 0.299042 11.00000 -1.20000
AFIX 0
C37 1 0.223090 0.321804 0.393758 11.00000 0.02798 0.02870 =
0.06329 -0.00880 0.00539 -0.00195
AFIX 43
H37 2 0.131838 0.320411 0.394736 11.00000 -1.20000
AFIX 0
C38 1 0.311169 0.291590 0.449476 11.00000 0.03569 0.03055 =
0.04722 -0.00522 0.01592 -0.00431
AFIX 43
H38 2 0.279060 0.269803 0.488078 11.00000 -1.20000
AFIX 0
C39 1 0.447541 0.293388 0.448490 11.00000 0.03108 0.02575 =
0.03109 -0.00349 0.00684 -0.00116
AFIX 43
H39 2 0.506125 0.273063 0.486575 11.00000 -1.20000
AFIX 0
PART 1
N2 3 0.537087 0.095095 0.464023 11.00000 0.08287 0.08167 =
0.05555 0.00107 0.01899 -0.01075
C40 1 0.436676 0.091701 0.483726 11.00000 0.06586 0.04709 =
0.04531 -0.00178 -0.00381 -0.00544
C41 1 0.311457 0.086344 0.509352 11.00000 0.05315 0.08084 =
0.07106 -0.00460 -0.00038 -0.00618
AFIX 137
H41A 2 0.240336 0.098715 0.471096 11.00000 -1.50000
H41B 2 0.310840 0.119879 0.548828 11.00000 -1.50000
H41C 2 0.299340 0.036849 0.525292 11.00000 -1.50000
AFIX 0
HKLF 4
REM p18prr20
REM R1 = 0.0437 for 6133 Fo > 4sig(Fo) and 0.0610 for all 7735 data
REM 411 parameters refined using 1 restraints
END
WGHT 0.0479 1.4518
REM Highest difference peak 0.594, deepest hole -0.309, 1-sigma level 0.045
Q1 1 0.5697 0.0358 0.4612 11.00000 0.05 0.59
Q2 1 0.3657 -0.0011 0.5398 11.00000 0.05 0.46
Q3 1 0.4144 0.0341 0.4990 11.00000 0.05 0.34
Q4 1 0.5695 0.3205 0.3794 11.00000 0.05 0.30
Q5 1 0.6978 0.3808 0.3933 11.00000 0.05 0.27
Q6 1 0.9413 0.2001 0.4826 11.00000 0.05 0.27
Q7 1 0.8200 0.2562 0.4405 11.00000 0.05 0.26
Q8 1 0.8823 0.2015 0.3956 11.00000 0.05 0.25
Q9 1 0.7378 0.2967 0.4185 11.00000 0.05 0.23
Q10 1 0.3773 0.2831 0.4420 11.00000 0.05 0.23
Q11 1 0.4623 0.3263 0.3564 11.00000 0.05 0.23
Q12 1 0.7613 0.3141 0.6942 11.00000 0.05 0.23
Q13 1 0.4236 0.1800 0.7120 11.00000 0.05 0.22
Q14 1 0.8024 0.4203 0.4170 11.00000 0.05 0.22
Q15 1 0.7588 0.3063 0.6241 11.00000 0.05 0.22
Q16 1 0.9972 0.2667 0.4454 11.00000 0.05 0.21
Q17 1 0.4767 0.3167 0.4202 11.00000 0.05 0.21
Q18 1 0.6461 0.2028 0.6204 11.00000 0.05 0.21
Q19 1 0.7452 0.3598 0.6602 11.00000 0.05 0.20
Q20 1 0.7189 0.3196 0.3362 11.00000 0.05 0.20
REM The information below was added by Olex2.
REM
REM R1 = 0.0437 for 6133 Fo > 4sig(Fo) and 0.0610 for all 44817 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.59, deepest hole -0.31
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0610
REM R1_gt = 0.0437
REM wR_ref = 0.1127
REM GOOF = 1.045
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 44817
REM Reflections_gt = 6133
REM Parameters = n/a
REM Hole = -0.31
REM Peak = 0.59
REM Flack = n/a
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_e17rlw8-Cpd-2a
_database_code_depnum_ccdc_archive 'CCDC 1849269'
_audit_update_record
;
2018-06-14 deposited with the CCDC.
2018-08-22 downloaded from the CCDC.
;
_audit_creation_date 2017-02-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C22 H19 P'
_chemical_formula_sum 'C22 H19 P'
_chemical_formula_weight 314.34
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 33
_space_group_name_H-M_alt 'P n a 21'
_space_group_name_Hall 'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'
_cell_length_a 15.9327(2)
_cell_length_b 17.7483(3)
_cell_length_c 6.06371(11)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1714.68(5)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9977
_cell_measurement_temperature 150.00(10)
_cell_measurement_theta_max 29.2090
_cell_measurement_theta_min 3.7700
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.157
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.90109
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.218
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 664
_exptl_crystal_size_max 0.307
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.104
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0374
_diffrn_reflns_av_unetI/netI 0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 7
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_number 28027
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.483
_diffrn_reflns_theta_min 3.437
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 150.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.1468
_diffrn_detector_type EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'New Xcalibur, EosS2'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.824
_reflns_Friedel_fraction_full 1.000
_reflns_Friedel_fraction_max 0.994
_reflns_number_gt 3573
_reflns_number_total 3895
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 0.340
_refine_diff_density_min -0.207
_refine_diff_density_rms 0.035
_refine_ls_abs_structure_details
;
Flack x determined using 1473 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.08(3)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 208
_refine_ls_number_reflns 3895
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0393
_refine_ls_R_factor_gt 0.0338
_refine_ls_restrained_S_all 1.033
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.4146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0767
_refine_ls_wR_factor_ref 0.0795
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11),
C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20),
C21(H21), C22(H22)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary iterative
_atom_sites_solution_secondary ?
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
P1 P 0.07071(3) 0.65090(3) 0.46370(11) 0.02313(13) Uani 1 1 d . . . . .
C1 C -0.04454(13) 0.64895(12) 0.4846(4) 0.0237(4) Uani 1 1 d . . . . .
C2 C -0.08789(14) 0.67614(14) 0.6677(4) 0.0269(5) Uani 1 1 d . . . . .
H2 H -0.0584 0.6928 0.7908 0.032 Uiso 1 1 calc R . . . .
C3 C -0.17545(15) 0.67842(14) 0.6667(4) 0.0313(5) Uani 1 1 d . . . . .
H3 H -0.2041 0.6966 0.7893 0.038 Uiso 1 1 calc R . . . .
C4 C -0.21974(13) 0.65392(14) 0.4850(5) 0.0343(6) Uani 1 1 d . . . . .
H4 H -0.2781 0.6554 0.4855 0.041 Uiso 1 1 calc R . . . .
C5 C -0.17740(15) 0.62715(15) 0.3022(5) 0.0350(6) Uani 1 1 d . . . . .
H5 H -0.2072 0.6102 0.1800 0.042 Uiso 1 1 calc R . . . .
C6 C -0.08996(14) 0.62558(15) 0.3013(4) 0.0301(5) Uani 1 1 d . . . . .
H6 H -0.0617 0.6087 0.1766 0.036 Uiso 1 1 calc R . . . .
C7 C 0.10237(14) 0.65030(14) 0.7510(4) 0.0279(5) Uani 1 1 d . . . . .
H7 H 0.1131 0.6032 0.8118 0.033 Uiso 1 1 calc R . . . .
C8 C 0.11207(13) 0.70869(15) 0.8852(4) 0.0308(5) Uani 1 1 d . . . . .
H8 H 0.1320 0.6962 1.0246 0.037 Uiso 1 1 calc R . . . .
C9 C 0.09692(13) 0.78985(14) 0.8528(4) 0.0277(5) Uani 1 1 d . . . . .
C10 C 0.12244(16) 0.83812(17) 1.0202(5) 0.0402(7) Uani 1 1 d . . . . .
H10 H 0.1458 0.8179 1.1476 0.048 Uiso 1 1 calc R . . . .
C11 C 0.11403(18) 0.91514(18) 1.0028(6) 0.0503(8) Uani 1 1 d . . . . .
H11 H 0.1316 0.9461 1.1174 0.060 Uiso 1 1 calc R . . . .
C12 C 0.07928(16) 0.94644(17) 0.8140(6) 0.0469(8) Uani 1 1 d . . . . .
H12 H 0.0749 0.9985 0.7993 0.056 Uiso 1 1 calc R . . . .
C13 C 0.05124(16) 0.89940(15) 0.6480(5) 0.0375(6) Uani 1 1 d . . . . .
H13 H 0.0267 0.9200 0.5226 0.045 Uiso 1 1 calc R . . . .
C14 C 0.05924(14) 0.82209(14) 0.6662(4) 0.0293(5) Uani 1 1 d . . . . .
H14 H 0.0395 0.7912 0.5538 0.035 Uiso 1 1 calc R . . . .
C15 C 0.08980(14) 0.55397(13) 0.3804(4) 0.0300(5) Uani 1 1 d . . . . .
H15 H 0.0488 0.5187 0.4159 0.036 Uiso 1 1 calc R . . . .
C16 C 0.15739(14) 0.52906(13) 0.2728(4) 0.0300(5) Uani 1 1 d . . . . .
H16 H 0.1561 0.4787 0.2302 0.036 Uiso 1 1 calc R . . . .
C17 C 0.23410(13) 0.57123(13) 0.2126(4) 0.0258(5) Uani 1 1 d . . . . .
C18 C 0.27048(13) 0.62466(14) 0.3494(4) 0.0290(5) Uani 1 1 d . . . . .
H18 H 0.2467 0.6347 0.4863 0.035 Uiso 1 1 calc R . . . .
C19 C 0.34204(15) 0.66325(15) 0.2840(5) 0.0366(6) Uani 1 1 d . . . . .
H19 H 0.3660 0.6989 0.3770 0.044 Uiso 1 1 calc R . . . .
C20 C 0.37791(16) 0.64859(14) 0.0799(5) 0.0364(6) Uani 1 1 d . . . . .
H20 H 0.4254 0.6749 0.0349 0.044 Uiso 1 1 calc R . . . .
C21 C 0.34302(14) 0.59496(14) -0.0557(5) 0.0356(6) Uani 1 1 d . . . . .
H21 H 0.3670 0.5851 -0.1924 0.043 Uiso 1 1 calc R . . . .
C22 C 0.27261(14) 0.55573(13) 0.0101(4) 0.0304(5) Uani 1 1 d . . . . .
H22 H 0.2505 0.5186 -0.0810 0.037 Uiso 1 1 calc R . . . .
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
P1 0.0186(2) 0.0266(3) 0.0241(3) 0.0024(3) 0.0037(3) 0.0021(2)
C1 0.0208(9) 0.0239(9) 0.0265(12) 0.0049(10) 0.0011(10) 0.0027(8)
C2 0.0246(11) 0.0283(11) 0.0277(12) 0.0035(10) 0.0047(9) 0.0003(9)
C3 0.0239(12) 0.0351(13) 0.0350(13) 0.0069(11) 0.0084(10) 0.0033(10)
C4 0.0186(10) 0.0404(13) 0.0440(16) 0.0145(12) 0.0019(12) 0.0002(9)
C5 0.0285(12) 0.0411(14) 0.0355(14) 0.0062(12) -0.0077(11) -0.0040(11)
C6 0.0276(11) 0.0348(14) 0.0278(13) 0.0026(11) 0.0027(10) 0.0031(10)
C7 0.0231(11) 0.0354(14) 0.0252(12) 0.0093(11) 0.0003(9) 0.0057(9)
C8 0.0202(10) 0.0484(15) 0.0238(11) 0.0053(11) -0.0004(9) 0.0028(10)
C9 0.0145(9) 0.0401(14) 0.0286(12) -0.0016(11) 0.0052(9) -0.0030(9)
C10 0.0262(12) 0.0551(18) 0.0392(16) -0.0097(13) -0.0012(10) -0.0056(11)
C11 0.0393(15) 0.0543(18) 0.057(2) -0.0233(16) 0.0052(14) -0.0133(13)
C12 0.0348(14) 0.0352(15) 0.071(2) -0.0085(15) 0.0210(15) -0.0038(11)
C13 0.0296(13) 0.0379(14) 0.0451(16) 0.0034(13) 0.0125(12) 0.0048(11)
C14 0.0233(11) 0.0349(13) 0.0299(12) 0.0002(11) 0.0040(9) 0.0008(9)
C15 0.0241(11) 0.0266(12) 0.0393(13) 0.0032(11) 0.0055(10) -0.0012(9)
C16 0.0268(11) 0.0230(11) 0.0401(14) -0.0032(11) 0.0031(10) 0.0012(9)
C17 0.0184(10) 0.0254(11) 0.0337(13) 0.0005(10) 0.0009(9) 0.0060(9)
C18 0.0223(11) 0.0331(12) 0.0315(13) -0.0040(10) 0.0026(10) 0.0046(10)
C19 0.0232(11) 0.0361(13) 0.0506(17) -0.0113(13) -0.0006(11) -0.0006(10)
C20 0.0225(12) 0.0371(14) 0.0495(17) 0.0043(12) 0.0078(11) -0.0009(10)
C21 0.0266(11) 0.0475(14) 0.0327(13) -0.0005(13) 0.0075(11) 0.0073(10)
C22 0.0238(11) 0.0333(12) 0.0342(15) -0.0076(10) -0.0012(9) 0.0059(9)
_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
P1 C1 1.841(2) . ?
P1 C7 1.813(2) . ?
P1 C15 1.819(3) . ?
C1 C2 1.394(3) . ?
C1 C6 1.390(3) . ?
C2 C3 1.396(3) . ?
C3 C4 1.379(4) . ?
C4 C5 1.382(4) . ?
C5 C6 1.393(3) . ?
C7 C8 1.327(4) . ?
C8 C9 1.474(3) . ?
C9 C10 1.389(4) . ?
C9 C14 1.403(3) . ?
C10 C11 1.378(4) . ?
C11 C12 1.388(5) . ?
C12 C13 1.382(4) . ?
C13 C14 1.382(4) . ?
C15 C16 1.335(3) . ?
C16 C17 1.479(3) . ?
C17 C18 1.387(3) . ?
C17 C22 1.400(3) . ?
C18 C19 1.388(3) . ?
C19 C20 1.388(4) . ?
C20 C21 1.375(4) . ?
C21 C22 1.379(3) . ?
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
C7 P1 C1 102.18(11) . . ?
C7 P1 C15 102.40(12) . . ?
C15 P1 C1 99.68(10) . . ?
C2 C1 P1 122.87(18) . . ?
C6 C1 P1 118.02(18) . . ?
C6 C1 C2 118.9(2) . . ?
C1 C2 C3 120.1(2) . . ?
C4 C3 C2 120.4(2) . . ?
C3 C4 C5 120.0(2) . . ?
C4 C5 C6 119.9(2) . . ?
C1 C6 C5 120.8(2) . . ?
C8 C7 P1 128.10(19) . . ?
C7 C8 C9 131.5(2) . . ?
C10 C9 C8 117.2(2) . . ?
C10 C9 C14 117.6(2) . . ?
C14 C9 C8 125.2(2) . . ?
C11 C10 C9 121.8(3) . . ?
C10 C11 C12 120.0(3) . . ?
C13 C12 C11 119.2(3) . . ?
C12 C13 C14 120.8(3) . . ?
C13 C14 C9 120.6(2) . . ?
C16 C15 P1 125.74(19) . . ?
C15 C16 C17 128.3(2) . . ?
C18 C17 C16 123.0(2) . . ?
C18 C17 C22 118.4(2) . . ?
C22 C17 C16 118.6(2) . . ?
C17 C18 C19 120.7(2) . . ?
C20 C19 C18 120.0(2) . . ?
C21 C20 C19 119.8(2) . . ?
C20 C21 C22 120.4(3) . . ?
C21 C22 C17 120.7(2) . . ?
_iucr_refine_instructions_details
;
e17rlw8.res created by SHELXL-2014/7
TITL e17rlw8
CELL 0.71073 15.932698 17.748261 6.063711 90 90 90
ZERR 4 0.000215 0.000292 0.000113 0 0 0
LATT -1
SYMM -X,-Y,0.5+Z
SYMM 0.5-X,0.5+Y,0.5+Z
SYMM 0.5+X,0.5-Y,+Z
SFAC C H P
UNIT 88 76 4
L.S. 18
PLAN 2
BOND
fmap 2
ACTA
more -3
SHEL 999 0.77
REM
REM
REM
WGHT 0.036000 0.414600
FVAR 5.21460
P1 3 0.070715 0.650897 0.463699 11.00000 0.01865 0.02659 =
0.02414 0.00243 0.00372 0.00206
C1 1 -0.044543 0.648950 0.484641 11.00000 0.02075 0.02393 =
0.02650 0.00495 0.00106 0.00265
C2 1 -0.087893 0.676144 0.667746 11.00000 0.02457 0.02830 =
0.02774 0.00351 0.00473 0.00035
AFIX 43
H2 2 -0.058421 0.692802 0.790827 11.00000 -1.20000
AFIX 0
C3 1 -0.175449 0.678418 0.666696 11.00000 0.02388 0.03515 =
0.03497 0.00691 0.00835 0.00329
AFIX 43
H3 2 -0.204093 0.696572 0.789311 11.00000 -1.20000
AFIX 0
C4 1 -0.219740 0.653920 0.485033 11.00000 0.01858 0.04040 =
0.04396 0.01452 0.00191 0.00019
AFIX 43
H4 2 -0.278087 0.655404 0.485522 11.00000 -1.20000
AFIX 0
C5 1 -0.177397 0.627153 0.302177 11.00000 0.02851 0.04109 =
0.03554 0.00620 -0.00770 -0.00396
AFIX 43
H5 2 -0.207203 0.610227 0.179969 11.00000 -1.20000
AFIX 0
C6 1 -0.089959 0.625578 0.301295 11.00000 0.02762 0.03484 =
0.02782 0.00255 0.00268 0.00310
AFIX 43
H6 2 -0.061664 0.608693 0.176584 11.00000 -1.20000
AFIX 0
C7 1 0.102365 0.650299 0.750966 11.00000 0.02308 0.03542 =
0.02522 0.00927 0.00035 0.00567
AFIX 43
H7 2 0.113136 0.603180 0.811806 11.00000 -1.20000
AFIX 0
C8 1 0.112071 0.708685 0.885153 11.00000 0.02020 0.04843 =
0.02384 0.00529 -0.00044 0.00278
AFIX 43
H8 2 0.131996 0.696161 1.024574 11.00000 -1.20000
AFIX 0
C9 1 0.096921 0.789845 0.852768 11.00000 0.01449 0.04006 =
0.02861 -0.00155 0.00518 -0.00297
C10 1 0.122438 0.838122 1.020189 11.00000 0.02616 0.05513 =
0.03924 -0.00969 -0.00120 -0.00559
AFIX 43
H10 2 0.145845 0.817880 1.147586 11.00000 -1.20000
AFIX 0
C11 1 0.114035 0.915139 1.002751 11.00000 0.03926 0.05429 =
0.05747 -0.02327 0.00521 -0.01329
AFIX 43
H11 2 0.131639 0.946136 1.117430 11.00000 -1.20000
AFIX 0
C12 1 0.079284 0.946444 0.813963 11.00000 0.03481 0.03521 =
0.07056 -0.00846 0.02104 -0.00377
AFIX 43
H12 2 0.074921 0.998457 0.799322 11.00000 -1.20000
AFIX 0
C13 1 0.051241 0.899404 0.647984 11.00000 0.02963 0.03791 =
0.04511 0.00341 0.01248 0.00478
AFIX 43
H13 2 0.026700 0.919995 0.522556 11.00000 -1.20000
AFIX 0
C14 1 0.059240 0.822094 0.666202 11.00000 0.02327 0.03486 =
0.02991 0.00020 0.00404 0.00085
AFIX 43
H14 2 0.039463 0.791191 0.553771 11.00000 -1.20000
AFIX 0
C15 1 0.089797 0.553971 0.380384 11.00000 0.02409 0.02662 =
0.03926 0.00318 0.00546 -0.00120
AFIX 43
H15 2 0.048849 0.518652 0.415879 11.00000 -1.20000
AFIX 0
C16 1 0.157392 0.529065 0.272791 11.00000 0.02680 0.02303 =
0.04015 -0.00318 0.00305 0.00117
AFIX 43
H16 2 0.156091 0.478741 0.230192 11.00000 -1.20000
AFIX 0
C17 1 0.234100 0.571231 0.212619 11.00000 0.01840 0.02543 =
0.03371 0.00048 0.00091 0.00601
C18 1 0.270482 0.624662 0.349360 11.00000 0.02232 0.03305 =
0.03152 -0.00395 0.00257 0.00460
AFIX 43
H18 2 0.246691 0.634743 0.486271 11.00000 -1.20000
AFIX 0
C19 1 0.342044 0.663248 0.283955 11.00000 0.02323 0.03611 =
0.05059 -0.01131 -0.00064 -0.00062
AFIX 43
H19 2 0.365975 0.698948 0.376962 11.00000 -1.20000
AFIX 0
C20 1 0.377908 0.648591 0.079859 11.00000 0.02247 0.03709 =
0.04954 0.00430 0.00775 -0.00094
AFIX 43
H20 2 0.425368 0.674949 0.034914 11.00000 -1.20000
AFIX 0
C21 1 0.343018 0.594956 -0.055663 11.00000 0.02656 0.04753 =
0.03275 -0.00052 0.00748 0.00728
AFIX 43
H21 2 0.367024 0.585075 -0.192438 11.00000 -1.20000
AFIX 0
C22 1 0.272607 0.555728 0.010137 11.00000 0.02379 0.03329 =
0.03419 -0.00764 -0.00122 0.00585
AFIX 43
H22 2 0.250471 0.518569 -0.081023 11.00000 -1.20000
AFIX 0
HKLF 4
REM e17rlw8 in Pna21 #33
REM R1 = 0.0338 for 3573 Fo > 4sig(Fo) and 0.0393 for all 3895 data
REM 208 parameters refined using 1 restraints
END
WGHT 0.0359 0.4156
REM Highest difference peak 0.340, deepest hole -0.207, 1-sigma level 0.035
Q1 1 0.0800 0.5976 0.4518 11.00000 0.05 0.34
Q2 1 0.0726 0.7064 0.4916 11.00000 0.05 0.20
REM The information below was added by Olex2.
REM
REM R1 = 0.0338 for 3573 Fo > 4sig(Fo) and 0.0393 for all 29803 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.34, deepest hole -0.21
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0393
REM R1_gt = 0.0338
REM wR_ref = 0.0795
REM GOOF = 1.033
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 29803
REM Reflections_gt = 3573
REM Parameters = n/a
REM Hole = -0.21
REM Peak = 0.34
REM Flack = -0.08(3)
;
#===end