# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016
#######################################################################
#
# 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.
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data_p1
_database_code_depnum_ccdc_archive 'CCDC 1449923'
_audit_update_record
;
2016-04-05 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_audit_creation_date 2016-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'Co2 O114 P4 W32, 8(O), 6(C10 H16 N4)'
_chemical_formula_sum 'C60 H96 Co2 N24 O122 P4 W32'
_chemical_formula_weight 9230.54
_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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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 15.082(2)
_cell_length_b 15.392(2)
_cell_length_c 20.427(3)
_cell_angle_alpha 78.8374(13)
_cell_angle_beta 82.5853(13)
_cell_angle_gamma 75.4572(12)
_cell_volume 4487.0(11)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 9974
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 2.5
_shelx_estimated_absorpt_T_max 0.424
_shelx_estimated_absorpt_T_min 0.288
_exptl_absorpt_coefficient_mu 20.727
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.3239
_exptl_absorpt_correction_type MULTI-SCAN
_exptl_absorpt_process_details sadabs
_exptl_absorpt_special_details ?
_exptl_crystal_colour purple
_exptl_crystal_density_diffrn 3.416
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description blcok
_exptl_crystal_F_000 4082
_exptl_crystal_size_max 0.08
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0565
_diffrn_reflns_av_unetI/netI 0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 78602
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.214
_diffrn_reflns_theta_max 26.000
_diffrn_reflns_theta_min 2.568
_diffrn_ambient_temperature 298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker Apex-II'
_diffrn_measurement_method ?
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 12885
_reflns_number_total 17648
_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_data_collection 'APEX2 (Bruker,2005)'
_computing_cell_refinement 'APEX2 (Bruker,2005)'
_computing_data_reduction 'SAINT (Bruker, 2005)'
_computing_molecular_graphics 'DIAMOND (Brandenburg, 2008)'
_computing_publication_material 'publCIF (Westrip, 2010)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_refine_diff_density_max 3.309
_refine_diff_density_min -3.668
_refine_diff_density_rms 0.310
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.078
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1096
_refine_ls_number_reflns 17648
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0610
_refine_ls_R_factor_gt 0.0399
_refine_ls_restrained_S_all 1.078
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+1.4111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1006
_refine_ls_wR_factor_ref 0.1084
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Fixed Sof: O1W(0.2) O3W(0.3) O3WA(0.7) O4W(0.5) O4WA(0.5) O1WA(0.8)
3.a Me refined with riding coordinates:
C15(H15A,H15B,H15C), C20(H20A,H20B,H20C)
3.b Aromatic/amide H refined with riding coordinates:
N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), N9(H9),
N10(H10), N11(H11), N12(H12)
3.c Idealised Me refined as rotating group:
C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C25(H25A,H25B,
H25C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C)
;
_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
W1 W 0.40116(4) 0.07791(4) 0.34178(3) 0.03222(14) Uani 1 1 d . . . . .
W2 W 0.19098(4) 0.04794(4) 0.41203(3) 0.03121(13) Uani 1 1 d . . . . .
W3 W 0.26221(4) 0.23194(4) 0.43059(2) 0.02952(13) Uani 1 1 d . . . . .
W4 W 0.13775(3) 0.01937(3) 0.24730(2) 0.02562(12) Uani 1 1 d . . . . .
W5 W 0.34464(3) 0.05146(3) 0.17796(3) 0.02740(12) Uani 1 1 d . . . . .
W6 W 0.41185(3) 0.26069(3) 0.19137(3) 0.02646(12) Uani 1 1 d . . . . .
W7 W 0.27718(3) 0.41113(3) 0.28257(2) 0.02282(11) Uani 1 1 d . . . . .
W8 W 0.05151(3) 0.37610(3) 0.35917(2) 0.02219(11) Uani 1 1 d . . . . .
W9 W -0.01871(3) 0.19510(3) 0.33283(2) 0.02206(11) Uani 1 1 d . . . . .
W10 W -0.12904(3) 0.32331(3) 0.17453(2) 0.02169(11) Uani 1 1 d . . . . .
W11 W -0.05525(3) 0.50127(3) 0.20078(2) 0.01584(10) Uani 1 1 d . . . . .
W12 W 0.17219(3) 0.53737(3) 0.12486(2) 0.01597(10) Uani 1 1 d . . . . .
W13 W 0.30637(3) 0.39108(3) 0.03071(3) 0.02777(13) Uani 1 1 d . . . . .
W14 W 0.23758(3) 0.18054(3) 0.02000(2) 0.01908(11) Uani 1 1 d . . . . .
W15 W 0.03223(3) 0.14854(3) 0.08899(2) 0.01823(11) Uani 1 1 d . . . . .
W16 W 0.03344(3) 0.33397(3) -0.05515(2) 0.01975(11) Uani 1 1 d . . . . .
Co1 Co -0.09997(9) 0.48498(9) 0.03315(7) 0.0114(3) Uani 1 1 d . . . . .
P1 P 0.20335(17) 0.21523(17) 0.26946(12) 0.0107(5) Uani 1 1 d . . . . .
P2 P 0.08704(17) 0.35535(16) 0.09847(12) 0.0079(5) Uani 1 1 d . . . . .
O1 O 0.1664(6) -0.0384(5) 0.4748(4) 0.034(2) Uani 1 1 d . . . . .
O1W O 0.715(7) 0.337(7) 0.396(5) 0.15(3) Uiso 0.2 1 d . . P A 2
O2 O 0.2812(6) 0.2642(6) 0.5025(4) 0.041(2) Uani 1 1 d . . . . .
O2W O 0.6764(11) 1.1542(11) 0.4520(8) 0.119(5) Uiso 1 1 d . . . . .
O3 O 0.5068(6) 0.0105(7) 0.3616(5) 0.048(3) Uani 1 1 d . . . . .
O3W O 0.523(3) 0.089(3) 0.496(2) 0.084(14) Uiso 0.3 1 d . . P B 1
O3WA O 0.5093(17) 0.1353(18) 0.5149(13) 0.117(9) Uiso 0.7 1 d . . P C 2
O4 O 0.2095(6) 0.1295(6) 0.4625(4) 0.040(2) Uani 1 1 d . . . . .
O4W O 0.3911(11) 0.3205(11) 0.7872(8) 0.034(4) Uiso 0.5 1 d . . P D 2
O4WA O 0.3025(10) 0.3538(10) 0.8432(7) 0.021(3) Uiso 0.5 1 d . . P E 1
O5 O 0.3208(6) 0.0055(5) 0.3953(5) 0.040(2) Uani 1 1 d . . . . .
O6 O 0.3783(6) 0.1511(6) 0.4102(5) 0.040(2) Uani 1 1 d . . . . .
O7 O 0.1853(6) 0.0005(5) 0.3307(4) 0.037(2) Uani 1 1 d . . . . .
O8 O 0.0770(5) 0.1224(5) 0.3957(4) 0.0265(19) Uani 1 1 d . . . . .
O9 O 0.3787(6) 0.0286(5) 0.2672(4) 0.034(2) Uani 1 1 d . . . . .
O10 O 0.2485(5) 0.1630(5) 0.3370(3) 0.0249(19) Uani 1 1 d . . . . .
O11 O 0.4278(5) 0.1747(6) 0.2798(4) 0.031(2) Uani 1 1 d . . . . .
O12 O 0.1405(5) 0.2978(6) 0.4159(4) 0.032(2) Uani 1 1 d . . . . .
O13 O 0.2992(5) 0.3204(6) 0.3632(4) 0.029(2) Uani 1 1 d . . . . .
O14 O -0.1060(5) 0.1519(6) 0.3772(4) 0.030(2) Uani 1 1 d . . . . .
O15 O 0.0972(6) -0.0755(5) 0.2571(4) 0.036(2) Uani 1 1 d . . . . .
O16 O 0.4307(6) -0.0239(6) 0.1450(4) 0.041(2) Uani 1 1 d . . . . .
O17 O 0.5266(6) 0.2492(6) 0.1693(4) 0.041(2) Uani 1 1 d . . . . .
O18 O 0.3050(6) 0.4980(6) 0.3106(4) 0.036(2) Uani 1 1 d . . . . .
O19 O 0.0017(6) 0.4525(6) 0.4111(4) 0.036(2) Uani 1 1 d . . . . .
O20 O 0.2557(5) -0.0215(5) 0.2038(4) 0.0286(19) Uani 1 1 d . . . . .
O21 O 0.0355(5) 0.1050(5) 0.2793(4) 0.0244(18) Uani 1 1 d . . . . .
O22 O -0.0256(5) 0.2944(5) 0.3798(4) 0.0269(19) Uani 1 1 d . . . . .
O23 O 0.1496(5) 0.4246(5) 0.3137(4) 0.0270(19) Uani 1 1 d . . . . .
O24 O 0.3951(5) 0.3563(5) 0.2428(4) 0.0275(19) Uani 1 1 d . . . . .
O25 O 0.3880(5) 0.1578(5) 0.1634(4) 0.030(2) Uani 1 1 d . . . . .
O26 O 0.2095(5) 0.1439(5) 0.2259(3) 0.0197(17) Uani 1 1 d . . . . .
O27 O 0.2588(5) 0.2841(5) 0.2389(4) 0.0241(18) Uani 1 1 d . . . . .
O28 O 0.1049(5) 0.2609(5) 0.2889(4) 0.0203(17) Uani 1 1 d . . . . .
O29 O 0.3618(5) 0.3374(5) 0.1190(4) 0.0219(18) Uani 1 1 d . . . . .
O30 O 0.2416(5) 0.4715(5) 0.1981(4) 0.0216(17) Uani 1 1 d . . . . .
O31 O 0.2837(5) 0.1041(5) 0.0954(4) 0.0257(19) Uani 1 1 d . . . . .
O32 O -0.0190(5) 0.4334(5) 0.2844(4) 0.0205(17) Uani 1 1 d . . . . .
O33 O 0.0940(5) 0.0745(5) 0.1589(4) 0.028(2) Uani 1 1 d . . . . .
O34 O -0.0780(5) 0.2716(5) 0.2634(3) 0.0233(18) Uani 1 1 d . . . . .
O35 O 0.4066(5) 0.3969(5) -0.0151(4) 0.0255(19) Uani 1 1 d . . . . .
O36 O 0.2756(5) 0.5051(5) 0.0656(4) 0.0180(16) Uani 1 1 d . . . . .
O37 O 0.1776(5) 0.6437(5) 0.1346(4) 0.0229(18) Uani 1 1 d . . . . .
O38 O 0.0636(4) 0.5248(5) 0.1821(4) 0.0184(17) Uani 1 1 d . . . . .
O39 O -0.1172(5) 0.5988(5) 0.2300(4) 0.0191(17) Uani 1 1 d . . . . .
O40 O -0.1505(5) 0.4405(5) 0.2052(4) 0.0184(17) Uani 1 1 d . . . . .
O41 O -0.2337(5) 0.2962(5) 0.1969(4) 0.0279(19) Uani 1 1 d . . . . .
O42 O -0.0556(5) 0.2154(5) 0.1468(3) 0.0182(17) Uani 1 1 d . . . . .
O43 O -0.0299(5) 0.0803(5) 0.0690(4) 0.0275(19) Uani 1 1 d . . . . .
O44 O 0.1386(5) 0.1211(5) 0.0277(4) 0.0219(17) Uani 1 1 d . . . . .
O45 O 0.3093(5) 0.1317(5) -0.0421(4) 0.0280(19) Uani 1 1 d . . . . .
O46 O 0.2968(5) 0.2694(5) 0.0289(4) 0.0216(17) Uani 1 1 d . . . . .
O47 O 0.1665(5) 0.3967(5) 0.1034(3) 0.0178(16) Uani 1 1 d . . . . .
O48 O 0.1201(4) 0.2524(5) 0.0944(3) 0.0161(16) Uani 1 1 d . . . . .
O49 O 0.0122(4) 0.3729(4) 0.1551(3) 0.0140(15) Uani 1 1 d . . . . .
O50 O 0.2274(5) 0.4382(5) -0.0320(4) 0.0203(17) Uani 1 1 d . . . . .
O51 O 0.0908(4) 0.5783(4) 0.0510(3) 0.0163(16) Uani 1 1 d . . . . .
O52 O 0.0429(4) 0.4061(4) 0.0300(3) 0.0136(15) Uani 1 1 d . . . . .
O53 O 0.1563(4) 0.2775(5) -0.0430(3) 0.0163(16) Uani 1 1 d . . . . .
O54 O -0.1437(5) 0.3796(5) 0.0899(4) 0.0193(17) Uani 1 1 d . . . . .
O55 O -0.0097(5) 0.2514(4) 0.0128(3) 0.0157(16) Uani 1 1 d . . . . .
O56 O 0.0714(5) 0.4471(5) -0.1045(4) 0.0170(16) Uani 1 1 d . . . . .
O57 O 0.0186(5) 0.2912(5) -0.1240(4) 0.0228(18) Uani 1 1 d . . . . .
N1 N 0.4711(8) 0.1953(9) 0.9297(7) 0.047(3) Uani 1 1 d . . . . .
H1 H 0.4277 0.1668 0.9355 0.056 Uiso 1 1 calc R . . . .
N2 N 0.4777(7) 0.2685(10) 0.8845(7) 0.061(4) Uani 1 1 d . . . . .
H2 H 0.4394 0.2937 0.8548 0.074 Uiso 1 1 calc R . . . .
N3 N 0.8213(7) 0.2219(8) 0.9919(6) 0.042(3) Uani 1 1 d . . . . .
H3 H 0.8796 0.2005 0.9930 0.051 Uiso 1 1 calc R . . . .
N4 N 0.7748(9) 0.2896(8) 1.0207(5) 0.045(3) Uani 1 1 d . . . . .
H4 H 0.7971 0.3199 1.0431 0.053 Uiso 1 1 calc R . . . .
N5 N 0.9328(11) 0.3131(10) 0.7462(8) 0.074(5) Uani 1 1 d . . . . .
H5 H 0.9185 0.3156 0.7881 0.089 Uiso 1 1 calc R . . . .
N6 N 1.0107(11) 0.3231(9) 0.7125(9) 0.075(5) Uani 1 1 d . . . . .
H6 H 1.0551 0.3326 0.7304 0.090 Uiso 1 1 calc R . . . .
N7 N 0.8749(10) 0.2171(10) 0.5002(6) 0.057(4) Uani 1 1 d . . . . .
H7 H 0.8761 0.1771 0.4758 0.069 Uiso 1 1 calc R . . . .
N8 N 0.8290(10) 0.3003(12) 0.4903(7) 0.074(4) Uani 1 1 d . . . . .
H8 H 0.7951 0.3248 0.4577 0.088 Uiso 1 1 calc R . . . .
N9 N 0.7003(10) 1.0946(11) 0.3294(7) 0.071(4) Uani 1 1 d . . . . .
H9 H 0.6946 1.1175 0.3654 0.085 Uiso 1 1 calc R . . . .
N10 N 0.6995(12) 1.1424(10) 0.2653(7) 0.085(5) Uani 1 1 d . . . . .
H10 H 0.6892 1.2006 0.2542 0.102 Uiso 1 1 calc R . . . .
N11 N 0.7421(11) 0.7921(10) 0.1965(9) 0.080(5) Uani 1 1 d . . . . .
H11 H 0.7224 0.7495 0.1856 0.095 Uiso 1 1 calc R . . . .
N12 N 0.8242(12) 0.8051(11) 0.1840(9) 0.094(6) Uani 1 1 d . . . . .
H12 H 0.8699 0.7678 0.1672 0.113 Uiso 1 1 calc R . . . .
C1 C 0.5520(12) 0.0936(11) 1.0179(11) 0.083(6) Uani 1 1 d . . . . .
H1A H 0.5566 0.1115 1.0596 0.125 Uiso 1 1 calc GR . . . .
H1B H 0.6061 0.0485 1.0076 0.125 Uiso 1 1 calc GR . . . .
H1C H 0.4989 0.0688 1.0215 0.125 Uiso 1 1 calc GR . . . .
C2 C 0.5432(9) 0.1750(11) 0.9634(8) 0.045(4) Uani 1 1 d . . . . .
C3 C 0.5957(8) 0.2376(8) 0.9423(6) 0.027(3) Uani 1 1 d . . . . .
C4 C 0.5527(9) 0.2986(11) 0.8913(7) 0.046(4) Uani 1 1 d . . . . .
C5 C 0.5769(11) 0.3860(12) 0.8518(9) 0.074(6) Uani 1 1 d . . . . .
H5A H 0.5525 0.3999 0.8088 0.110 Uiso 1 1 calc GR . . . .
H5B H 0.6425 0.3777 0.8456 0.110 Uiso 1 1 calc GR . . . .
H5C H 0.5510 0.4353 0.8760 0.110 Uiso 1 1 calc GR . . . .
C6 C 0.6135(10) 0.3735(9) 1.0409(7) 0.042(4) Uani 1 1 d . . . . .
H6A H 0.6420 0.4010 1.0683 0.063 Uiso 1 1 calc GR . . . .
H6B H 0.5687 0.3447 1.0681 0.063 Uiso 1 1 calc GR . . . .
H6C H 0.5840 0.4195 1.0066 0.063 Uiso 1 1 calc GR . . . .
C7 C 0.6847(8) 0.3043(8) 1.0095(6) 0.024(3) Uani 1 1 d . . . . .
C8 C 0.6794(8) 0.2415(8) 0.9701(6) 0.025(3) Uani 1 1 d . . . . .
C9 C 0.7678(8) 0.1899(8) 0.9609(7) 0.031(3) Uani 1 1 d . . . . .
C10 C 0.8037(11) 0.1142(11) 0.9221(9) 0.068(5) Uani 1 1 d . . . . .
H10A H 0.8638 0.1176 0.9012 0.101 Uiso 1 1 calc GR . . . .
H10B H 0.7631 0.1192 0.8883 0.101 Uiso 1 1 calc GR . . . .
H10C H 0.8073 0.0570 0.9516 0.101 Uiso 1 1 calc GR . . . .
C11 C 1.0912(13) 0.3317(15) 0.5963(11) 0.098(8) Uani 1 1 d . . . . .
H11A H 1.1320 0.3581 0.6142 0.147 Uiso 1 1 calc GR . . . .
H11B H 1.0667 0.3720 0.5574 0.147 Uiso 1 1 calc GR . . . .
H11C H 1.1243 0.2744 0.5840 0.147 Uiso 1 1 calc GR . . . .
C12 C 1.0149(13) 0.3171(11) 0.6474(10) 0.070(5) Uani 1 1 d . . . . .
C13 C 0.9302(10) 0.2991(11) 0.6403(7) 0.048(4) Uani 1 1 d . . . . .
C14 C 0.8778(12) 0.2977(10) 0.7026(8) 0.053(4) Uani 1 1 d . . . . .
C15 C 0.7869(11) 0.2825(10) 0.7236(8) 0.058(5) Uani 1 1 d . . . . .
H15A H 0.7603 0.2732 0.6860 0.087 Uiso 1 1 calc R . . . .
H15B H 0.7910 0.2296 0.7579 0.087 Uiso 1 1 calc R . . . .
H15C H 0.7490 0.3346 0.7409 0.087 Uiso 1 1 calc R . . . .
C16 C 0.8029(17) 0.4441(14) 0.5369(10) 0.110(8) Uani 1 1 d . . . . .
H16A H 0.7816 0.4717 0.4937 0.165 Uiso 1 1 calc GR . . . .
H16B H 0.8499 0.4715 0.5454 0.165 Uiso 1 1 calc GR . . . .
H16C H 0.7526 0.4532 0.5707 0.165 Uiso 1 1 calc GR . . . .
C17 C 0.8418(13) 0.3433(14) 0.5382(9) 0.068(5) Uani 1 1 d . . . . .
C18 C 0.9005(11) 0.2840(12) 0.5789(7) 0.050(4) Uani 1 1 d . . . . .
C19 C 0.9204(11) 0.2027(13) 0.5548(7) 0.055(5) Uani 1 1 d . . . . .
C20 C 0.9900(13) 0.1167(12) 0.5763(8) 0.074(6) Uani 1 1 d . . . . .
H20A H 1.0140 0.1210 0.6166 0.110 Uiso 1 1 calc R . . . .
H20B H 0.9613 0.0661 0.5846 0.110 Uiso 1 1 calc R . . . .
H20C H 1.0391 0.1080 0.5416 0.110 Uiso 1 1 calc R . . . .
C21 C 0.7105(15) 0.9426(14) 0.3899(9) 0.096(7) Uani 1 1 d . . . . .
H21A H 0.7296 0.8814 0.3809 0.144 Uiso 1 1 calc GR . . . .
H21B H 0.6494 0.9522 0.4118 0.144 Uiso 1 1 calc GR . . . .
H21C H 0.7519 0.9521 0.4184 0.144 Uiso 1 1 calc GR . . . .
C22 C 0.7115(11) 1.0070(10) 0.3266(8) 0.055(4) Uani 1 1 d . . . . .
C23 C 0.7243(9) 0.9980(10) 0.2615(7) 0.047(4) Uani 1 1 d . . . . .
C24 C 0.7168(11) 1.0851(11) 0.2251(8) 0.054(4) Uani 1 1 d . . . . .
C25 C 0.7289(12) 1.1174(10) 0.1495(7) 0.064(5) Uani 1 1 d . . . . .
H25A H 0.6805 1.1697 0.1367 0.096 Uiso 1 1 calc GR . . . .
H25B H 0.7266 1.0695 0.1263 0.096 Uiso 1 1 calc GR . . . .
H25C H 0.7872 1.1333 0.1379 0.096 Uiso 1 1 calc GR . . . .
C26 C 0.9185(18) 0.9105(18) 0.1886(14) 0.139(10) Uiso 1 1 d . . . . .
H26A H 0.9685 0.8576 0.1901 0.209 Uiso 1 1 calc GR . . . .
H26B H 0.9224 0.9439 0.2228 0.209 Uiso 1 1 calc GR . . . .
H26C H 0.9218 0.9484 0.1455 0.209 Uiso 1 1 calc GR . . . .
C27 C 0.8300(13) 0.8821(12) 0.2000(14) 0.107(9) Uani 1 1 d . . . . .
C28 C 0.7436(11) 0.9187(10) 0.2327(8) 0.053(4) Uani 1 1 d . . . . .
C29 C 0.6915(11) 0.8608(12) 0.2313(7) 0.055(5) Uani 1 1 d . . . . .
C30 C 0.5900(13) 0.8615(15) 0.2571(14) 0.122(9) Uani 1 1 d . . . . .
H30A H 0.5500 0.9018 0.2255 0.182 Uiso 1 1 calc GR . . . .
H30B H 0.5766 0.8821 0.2995 0.182 Uiso 1 1 calc GR . . . .
H30C H 0.5805 0.8011 0.2622 0.182 Uiso 1 1 calc GR . . . .
O1WA O 0.7614(17) 0.3899(17) 0.3648(12) 0.144(8) Uiso 0.8 1 d . . P F 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
W1 0.0308(3) 0.0317(3) 0.0284(3) 0.0044(2) -0.0109(2) 0.0003(2)
W2 0.0394(3) 0.0285(3) 0.0228(3) 0.0076(2) -0.0095(2) -0.0081(2)
W3 0.0358(3) 0.0321(3) 0.0196(3) 0.0012(2) -0.0111(2) -0.0059(2)
W4 0.0354(3) 0.0172(2) 0.0223(3) 0.0021(2) -0.0058(2) -0.0050(2)
W5 0.0278(3) 0.0224(3) 0.0269(3) -0.0017(2) -0.0053(2) 0.0030(2)
W6 0.0193(3) 0.0298(3) 0.0274(3) 0.0010(2) -0.0045(2) -0.0036(2)
W7 0.0253(3) 0.0252(3) 0.0199(3) -0.0007(2) -0.0078(2) -0.0090(2)
W8 0.0264(3) 0.0247(3) 0.0158(2) -0.0033(2) -0.00323(19) -0.0057(2)
W9 0.0274(3) 0.0242(3) 0.0142(2) 0.0014(2) -0.00095(19) -0.0092(2)
W10 0.0227(3) 0.0243(3) 0.0192(3) -0.0008(2) -0.00076(19) -0.0101(2)
W11 0.0162(2) 0.0176(2) 0.0140(2) -0.00250(18) -0.00052(17) -0.00501(18)
W12 0.0165(2) 0.0174(2) 0.0157(2) -0.00258(18) -0.00226(18) -0.00665(18)
W13 0.0227(3) 0.0292(3) 0.0309(3) -0.0051(2) 0.0006(2) -0.0066(2)
W14 0.0173(2) 0.0171(2) 0.0218(3) -0.00372(19) -0.00151(19) -0.00185(18)
W15 0.0205(2) 0.0148(2) 0.0195(2) 0.00030(19) -0.00297(19) -0.00612(18)
W16 0.0224(2) 0.0183(2) 0.0187(2) -0.00230(19) -0.00377(19) -0.00480(19)
Co1 0.0112(7) 0.0144(7) 0.0104(7) -0.0025(6) -0.0014(6) -0.0056(6)
P1 0.0129(13) 0.0133(13) 0.0069(13) -0.0012(11) -0.0028(10) -0.0041(11)
P2 0.0088(12) 0.0082(12) 0.0073(13) -0.0021(10) 0.0011(10) -0.0033(10)
O1 0.048(6) 0.030(5) 0.023(5) 0.013(4) -0.014(4) -0.012(4)
O2 0.047(6) 0.049(6) 0.025(5) 0.005(4) -0.018(4) -0.008(5)
O3 0.047(6) 0.050(6) 0.043(6) 0.001(5) -0.019(5) 0.000(5)
O4 0.046(6) 0.027(5) 0.047(6) -0.013(4) 0.028(5) -0.019(4)
O5 0.034(5) 0.015(4) 0.056(6) 0.016(4) -0.012(4) 0.005(4)
O6 0.028(5) 0.028(5) 0.067(7) -0.011(5) -0.029(5) 0.001(4)
O7 0.057(6) 0.021(5) 0.030(5) 0.009(4) -0.016(4) -0.007(4)
O8 0.035(5) 0.025(4) 0.016(4) 0.005(3) 0.002(4) -0.010(4)
O9 0.045(5) 0.026(5) 0.023(5) 0.001(4) -0.011(4) 0.007(4)
O10 0.031(5) 0.029(5) 0.009(4) 0.009(3) -0.009(3) -0.003(4)
O11 0.029(5) 0.042(5) 0.021(5) 0.004(4) -0.015(4) -0.009(4)
O12 0.032(5) 0.035(5) 0.025(5) 0.004(4) -0.009(4) -0.006(4)
O13 0.034(5) 0.035(5) 0.020(4) 0.005(4) -0.011(4) -0.013(4)
O14 0.037(5) 0.040(5) 0.016(4) 0.004(4) -0.005(4) -0.018(4)
O15 0.053(6) 0.024(5) 0.032(5) 0.001(4) -0.008(4) -0.014(4)
O16 0.047(6) 0.026(5) 0.041(6) -0.005(4) -0.019(5) 0.014(4)
O17 0.024(5) 0.046(6) 0.043(6) 0.009(5) -0.009(4) 0.001(4)
O18 0.042(5) 0.042(5) 0.032(5) -0.005(4) -0.014(4) -0.017(4)
O19 0.038(5) 0.047(6) 0.021(5) -0.007(4) -0.003(4) -0.001(4)
O20 0.036(5) 0.012(4) 0.033(5) 0.002(4) -0.001(4) 0.000(4)
O21 0.032(5) 0.022(4) 0.015(4) -0.001(3) -0.002(3) -0.001(4)
O22 0.026(4) 0.038(5) 0.018(4) -0.002(4) -0.002(3) -0.011(4)
O23 0.032(5) 0.024(4) 0.027(5) -0.004(4) -0.005(4) -0.009(4)
O24 0.017(4) 0.027(5) 0.038(5) -0.002(4) -0.005(4) -0.004(3)
O25 0.029(5) 0.028(5) 0.027(5) 0.002(4) -0.007(4) 0.000(4)
O26 0.026(4) 0.019(4) 0.014(4) 0.004(3) -0.007(3) -0.009(3)
O27 0.022(4) 0.022(4) 0.027(5) 0.001(4) -0.004(3) -0.004(3)
O28 0.020(4) 0.024(4) 0.016(4) 0.000(3) -0.002(3) -0.007(3)
O29 0.010(4) 0.029(4) 0.026(4) 0.001(4) -0.008(3) -0.003(3)
O30 0.019(4) 0.026(4) 0.021(4) -0.001(3) -0.007(3) -0.006(3)
O31 0.026(4) 0.025(4) 0.027(5) -0.009(4) -0.002(4) -0.004(4)
O32 0.022(4) 0.019(4) 0.021(4) -0.002(3) -0.004(3) -0.007(3)
O33 0.042(5) 0.018(4) 0.021(4) 0.005(3) -0.004(4) -0.005(4)
O34 0.032(5) 0.025(4) 0.011(4) -0.001(3) -0.001(3) -0.007(4)
O35 0.019(4) 0.023(4) 0.033(5) -0.011(4) 0.007(4) -0.003(3)
O36 0.012(4) 0.014(4) 0.027(4) -0.001(3) 0.003(3) -0.005(3)
O37 0.022(4) 0.019(4) 0.027(5) -0.004(3) 0.000(3) -0.004(3)
O38 0.008(4) 0.014(4) 0.029(4) 0.007(3) -0.003(3) -0.002(3)
O39 0.016(4) 0.017(4) 0.028(4) -0.009(3) -0.001(3) -0.004(3)
O40 0.019(4) 0.012(4) 0.025(4) -0.005(3) 0.001(3) -0.006(3)
O41 0.024(4) 0.026(5) 0.035(5) -0.005(4) -0.003(4) -0.009(4)
O42 0.023(4) 0.015(4) 0.015(4) 0.004(3) 0.005(3) -0.010(3)
O43 0.037(5) 0.021(4) 0.026(5) 0.002(4) 0.002(4) -0.016(4)
O44 0.025(4) 0.023(4) 0.020(4) -0.007(3) -0.006(3) -0.005(3)
O45 0.027(5) 0.030(5) 0.032(5) -0.017(4) -0.005(4) -0.004(4)
O46 0.024(4) 0.011(4) 0.029(5) -0.006(3) -0.004(3) 0.000(3)
O47 0.018(4) 0.018(4) 0.018(4) -0.005(3) -0.002(3) -0.003(3)
O48 0.012(4) 0.034(4) 0.007(4) -0.004(3) 0.001(3) -0.015(3)
O49 0.014(4) 0.010(4) 0.019(4) 0.000(3) -0.004(3) -0.005(3)
O50 0.014(4) 0.023(4) 0.023(4) -0.001(3) -0.005(3) -0.003(3)
O51 0.012(4) 0.010(4) 0.022(4) 0.004(3) -0.003(3) 0.002(3)
O52 0.016(4) 0.012(4) 0.011(4) 0.004(3) -0.005(3) -0.003(3)
O53 0.008(4) 0.019(4) 0.020(4) 0.002(3) -0.004(3) -0.003(3)
O54 0.028(4) 0.012(4) 0.018(4) 0.003(3) -0.001(3) -0.009(3)
O55 0.018(4) 0.011(4) 0.015(4) 0.003(3) -0.005(3) 0.000(3)
O56 0.012(4) 0.019(4) 0.023(4) -0.003(3) -0.005(3) -0.007(3)
O57 0.025(4) 0.027(4) 0.019(4) -0.002(3) -0.005(3) -0.011(4)
N1 0.033(7) 0.056(8) 0.062(9) -0.014(7) 0.001(6) -0.029(6)
N2 0.022(6) 0.086(11) 0.090(11) -0.051(9) -0.030(7) 0.003(7)
N3 0.020(6) 0.043(7) 0.063(8) 0.010(6) -0.021(6) -0.010(5)
N4 0.073(9) 0.033(7) 0.032(7) 0.009(5) -0.020(6) -0.024(7)
N5 0.078(11) 0.088(12) 0.064(10) -0.052(9) 0.002(9) -0.010(9)
N6 0.078(11) 0.064(10) 0.094(13) -0.049(9) -0.038(10) 0.004(9)
N7 0.091(11) 0.068(10) 0.026(7) -0.011(7) 0.005(7) -0.045(9)
N8 0.078(11) 0.092(13) 0.045(9) -0.019(9) -0.005(8) -0.005(10)
N9 0.077(11) 0.085(12) 0.057(10) -0.019(9) -0.013(8) -0.022(9)
N10 0.166(17) 0.047(9) 0.046(9) 0.003(8) -0.017(10) -0.035(10)
N11 0.071(11) 0.059(10) 0.110(14) -0.026(9) -0.036(10) 0.006(9)
N12 0.073(12) 0.063(11) 0.125(16) -0.018(11) 0.045(11) 0.000(9)
C1 0.075(13) 0.052(11) 0.134(19) -0.014(12) -0.011(13) -0.037(10)
C2 0.034(8) 0.060(10) 0.053(10) -0.033(8) -0.009(7) -0.011(7)
C3 0.028(7) 0.017(6) 0.042(8) -0.011(6) -0.004(6) -0.010(5)
C4 0.030(8) 0.068(11) 0.039(9) -0.018(8) -0.006(6) -0.002(7)
C5 0.046(10) 0.073(13) 0.088(14) 0.017(11) -0.026(10) -0.001(9)
C6 0.065(10) 0.030(7) 0.045(9) -0.015(7) 0.009(7) -0.034(7)
C7 0.020(6) 0.035(7) 0.021(6) -0.001(5) -0.004(5) -0.012(5)
C8 0.028(7) 0.024(6) 0.024(7) 0.001(5) -0.011(5) -0.009(5)
C9 0.026(7) 0.018(6) 0.049(9) 0.000(6) -0.005(6) -0.007(5)
C10 0.052(10) 0.048(10) 0.096(14) -0.004(10) -0.012(10) -0.002(8)
C11 0.067(13) 0.114(18) 0.124(19) -0.056(15) 0.046(13) -0.043(13)
C12 0.083(14) 0.047(10) 0.089(15) -0.037(10) 0.003(12) -0.016(10)
C13 0.050(9) 0.059(10) 0.039(9) -0.022(8) -0.007(7) -0.008(8)
C14 0.068(11) 0.040(9) 0.061(11) -0.030(8) -0.015(9) -0.006(8)
C15 0.079(12) 0.037(9) 0.049(10) -0.009(8) 0.016(9) -0.007(8)
C16 0.17(2) 0.087(17) 0.071(15) -0.023(13) 0.002(15) -0.019(16)
C17 0.072(13) 0.085(14) 0.054(12) -0.024(11) 0.013(10) -0.030(11)
C18 0.057(10) 0.062(11) 0.032(9) -0.007(8) -0.003(7) -0.017(9)
C19 0.059(11) 0.091(14) 0.027(9) -0.010(9) 0.017(8) -0.049(10)
C20 0.114(16) 0.082(14) 0.032(9) -0.020(9) -0.005(10) -0.029(13)
C21 0.111(17) 0.105(17) 0.060(13) 0.035(12) -0.017(12) -0.037(14)
C22 0.075(12) 0.033(9) 0.053(11) 0.013(8) -0.029(9) -0.010(8)
C23 0.039(8) 0.049(9) 0.035(9) 0.021(7) -0.008(7) 0.004(7)
C24 0.065(11) 0.051(10) 0.035(9) 0.005(8) 0.007(8) -0.009(8)
C25 0.099(14) 0.044(10) 0.031(9) 0.005(7) 0.004(9) 0.001(9)
C27 0.055(12) 0.032(10) 0.22(3) -0.015(14) 0.021(14) 0.002(9)
C28 0.057(10) 0.029(8) 0.065(11) -0.005(8) 0.003(9) -0.001(8)
C29 0.054(10) 0.070(12) 0.028(8) -0.020(8) -0.010(7) 0.024(9)
C30 0.061(14) 0.089(17) 0.22(3) -0.049(18) 0.003(16) -0.019(12)
_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
W1 O3 1.718(9) . ?
W1 O5 1.942(8) . ?
W1 O6 1.906(9) . ?
W1 O9 1.930(8) . ?
W1 O10 2.349(7) . ?
W1 O11 1.850(8) . ?
W2 O1 1.737(8) . ?
W2 O4 1.863(9) . ?
W2 O5 1.910(8) . ?
W2 O7 1.959(9) . ?
W2 O8 1.841(8) . ?
W2 O10 2.370(7) . ?
W3 O2 1.717(9) . ?
W3 O4 1.908(8) . ?
W3 O6 1.925(8) . ?
W3 O10 2.413(8) . ?
W3 O12 1.892(8) . ?
W3 O13 1.876(8) . ?
W4 O7 1.876(8) . ?
W4 O15 1.688(8) . ?
W4 O20 1.896(8) . ?
W4 O21 1.896(7) . ?
W4 O26 2.373(7) . ?
W4 O33 1.963(7) . ?
W5 O9 1.900(8) . ?
W5 O16 1.674(8) . ?
W5 O20 1.919(8) . ?
W5 O25 1.869(8) . ?
W5 O26 2.388(7) . ?
W5 O31 1.959(8) . ?
W6 O11 2.025(8) . ?
W6 O17 1.704(8) . ?
W6 O24 1.917(8) . ?
W6 O25 1.911(8) . ?
W6 O27 2.354(7) . ?
W6 O29 1.821(7) . ?
W7 O13 1.947(7) . ?
W7 O18 1.711(8) . ?
W7 O23 1.920(8) . ?
W7 O24 1.916(7) . ?
W7 O27 2.389(8) . ?
W7 O30 1.870(7) . ?
W8 O12 1.908(8) . ?
W8 O19 1.704(8) . ?
W8 O22 1.875(8) . ?
W8 O23 1.882(8) . ?
W8 O28 2.412(7) . ?
W8 O32 1.916(7) . ?
W9 O8 2.025(8) . ?
W9 O14 1.702(8) . ?
W9 O21 1.892(7) . ?
W9 O22 1.931(8) . ?
W9 O28 2.339(7) . ?
W9 O34 1.831(7) . ?
W10 O34 2.003(7) . ?
W10 O40 1.961(7) . ?
W10 O41 1.715(8) . ?
W10 O42 1.894(7) . ?
W10 O49 2.399(6) . ?
W10 O54 1.792(7) . ?
W11 O32 1.889(7) . ?
W11 O38 1.894(7) . ?
W11 O39 1.727(7) . ?
W11 O40 1.885(7) . ?
W11 O49 2.295(7) . ?
W11 O56 1.995(7) 2_565 ?
W12 O30 1.909(7) . ?
W12 O36 1.871(7) . ?
W12 O37 1.710(7) . ?
W12 O38 1.914(7) . ?
W12 O47 2.315(7) . ?
W12 O51 1.975(7) . ?
W13 O29 2.024(7) . ?
W13 O35 1.684(7) . ?
W13 O36 1.948(7) . ?
W13 O46 1.922(7) . ?
W13 O47 2.410(7) . ?
W13 O50 1.785(7) . ?
W14 O31 1.846(8) . ?
W14 O44 1.913(7) . ?
W14 O45 1.718(8) . ?
W14 O46 1.858(7) . ?
W14 O48 2.376(7) . ?
W14 O53 2.032(7) . ?
W15 O33 1.839(7) . ?
W15 O42 1.894(7) . ?
W15 O43 1.705(8) . ?
W15 O44 1.914(7) . ?
W15 O48 2.345(7) . ?
W15 O55 2.031(6) . ?
W16 O51 2.019(6) 2_565 ?
W16 O52 2.274(7) . ?
W16 O53 1.865(6) . ?
W16 O55 1.862(7) . ?
W16 O56 2.012(7) . ?
W16 O57 1.724(7) . ?
Co1 O50 1.988(7) 2_565 ?
Co1 O51 2.108(7) 2_565 ?
Co1 O52 2.191(7) . ?
Co1 O52 2.195(7) 2_565 ?
Co1 O54 2.005(7) . ?
Co1 O56 2.093(7) 2_565 ?
P1 O10 1.597(7) . ?
P1 O26 1.520(8) . ?
P1 O27 1.505(8) . ?
P1 O28 1.514(7) . ?
P2 O47 1.514(7) . ?
P2 O48 1.552(8) . ?
P2 O49 1.522(7) . ?
P2 O52 1.601(7) . ?
O50 Co1 1.988(7) 2_565 ?
O51 W16 2.019(6) 2_565 ?
O51 Co1 2.108(7) 2_565 ?
O52 Co1 2.195(7) 2_565 ?
O56 W11 1.995(7) 2_565 ?
O56 Co1 2.092(7) 2_565 ?
N1 N2 1.327(17) . ?
N1 C2 1.301(17) . ?
N2 C4 1.356(18) . ?
N3 N4 1.299(15) . ?
N3 C9 1.322(15) . ?
N4 C7 1.363(15) . ?
N5 N6 1.312(19) . ?
N5 C14 1.382(19) . ?
N6 C12 1.34(2) . ?
N7 N8 1.285(18) . ?
N7 C19 1.337(19) . ?
N8 C17 1.34(2) . ?
N9 N10 1.372(17) . ?
N9 C22 1.328(19) . ?
N10 C24 1.277(19) . ?
N11 N12 1.290(19) . ?
N11 C29 1.398(19) . ?
N12 C27 1.31(2) . ?
C1 C2 1.50(2) . ?
C2 C3 1.369(18) . ?
C3 C4 1.371(18) . ?
C3 C8 1.466(16) . ?
C4 C5 1.53(2) . ?
C6 C7 1.487(17) . ?
C7 C8 1.396(16) . ?
C8 C9 1.380(16) . ?
C9 C10 1.486(19) . ?
C11 C12 1.48(2) . ?
C12 C13 1.40(2) . ?
C13 C14 1.41(2) . ?
C13 C18 1.46(2) . ?
C14 C15 1.45(2) . ?
C16 C17 1.51(3) . ?
C17 C18 1.34(2) . ?
C18 C19 1.38(2) . ?
C19 C20 1.50(2) . ?
C21 C22 1.47(2) . ?
C22 C23 1.35(2) . ?
C23 C24 1.387(19) . ?
C23 C28 1.41(2) . ?
C24 C25 1.531(19) . ?
C26 C27 1.48(3) . ?
C27 C28 1.42(2) . ?
C28 C29 1.33(2) . ?
C29 C30 1.55(2) . ?
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
O3 W1 O5 100.5(4) . . ?
O3 W1 O6 99.4(4) . . ?
O3 W1 O9 101.6(4) . . ?
O3 W1 O10 168.9(4) . . ?
O3 W1 O11 104.5(4) . . ?
O5 W1 O10 71.4(3) . . ?
O6 W1 O5 88.2(4) . . ?
O6 W1 O9 158.9(3) . . ?
O6 W1 O10 73.3(3) . . ?
O9 W1 O5 85.8(4) . . ?
O9 W1 O10 85.6(3) . . ?
O11 W1 O5 154.9(3) . . ?
O11 W1 O6 89.8(4) . . ?
O11 W1 O9 87.1(4) . . ?
O11 W1 O10 84.2(3) . . ?
O1 W2 O4 101.0(4) . . ?
O1 W2 O5 100.8(4) . . ?
O1 W2 O7 102.2(4) . . ?
O1 W2 O8 103.5(4) . . ?
O1 W2 O10 169.5(3) . . ?
O4 W2 O5 90.3(4) . . ?
O4 W2 O7 156.8(3) . . ?
O4 W2 O10 72.6(3) . . ?
O5 W2 O7 84.3(4) . . ?
O5 W2 O10 71.4(3) . . ?
O7 W2 O10 84.3(3) . . ?
O8 W2 O4 89.0(4) . . ?
O8 W2 O5 155.4(3) . . ?
O8 W2 O7 86.7(3) . . ?
O8 W2 O10 85.0(3) . . ?
O2 W3 O4 103.7(4) . . ?
O2 W3 O6 101.8(4) . . ?
O2 W3 O10 171.0(3) . . ?
O2 W3 O12 102.8(4) . . ?
O2 W3 O13 102.7(4) . . ?
O4 W3 O6 89.8(4) . . ?
O4 W3 O10 70.8(3) . . ?
O6 W3 O10 71.4(3) . . ?
O12 W3 O4 85.5(4) . . ?
O12 W3 O6 155.4(4) . . ?
O12 W3 O10 84.2(3) . . ?
O13 W3 O4 153.4(4) . . ?
O13 W3 O6 87.5(4) . . ?
O13 W3 O10 83.3(3) . . ?
O13 W3 O12 86.1(3) . . ?
O7 W4 O20 92.4(4) . . ?
O7 W4 O21 88.5(3) . . ?
O7 W4 O26 82.3(3) . . ?
O7 W4 O33 163.3(3) . . ?
O15 W4 O7 99.0(4) . . ?
O15 W4 O20 100.1(4) . . ?
O15 W4 O21 102.8(4) . . ?
O15 W4 O26 173.4(3) . . ?
O15 W4 O33 97.2(4) . . ?
O20 W4 O26 73.3(3) . . ?
O20 W4 O33 88.3(3) . . ?
O21 W4 O20 156.6(3) . . ?
O21 W4 O26 83.7(3) . . ?
O21 W4 O33 84.4(3) . . ?
O33 W4 O26 81.9(3) . . ?
O9 W5 O20 91.1(4) . . ?
O9 W5 O26 82.1(3) . . ?
O9 W5 O31 163.5(3) . . ?
O16 W5 O9 99.3(4) . . ?
O16 W5 O20 99.6(4) . . ?
O16 W5 O25 104.0(4) . . ?
O16 W5 O26 172.1(4) . . ?
O16 W5 O31 97.0(4) . . ?
O20 W5 O26 72.6(3) . . ?
O20 W5 O31 88.5(3) . . ?
O25 W5 O9 88.3(4) . . ?
O25 W5 O20 156.1(3) . . ?
O25 W5 O26 83.7(3) . . ?
O25 W5 O31 85.4(3) . . ?
O31 W5 O26 82.1(3) . . ?
O11 W6 O27 79.3(3) . . ?
O17 W6 O11 95.1(4) . . ?
O17 W6 O24 97.7(4) . . ?
O17 W6 O25 102.5(4) . . ?
O17 W6 O27 169.9(4) . . ?
O17 W6 O29 101.9(4) . . ?
O24 W6 O11 85.8(3) . . ?
O24 W6 O27 73.7(3) . . ?
O25 W6 O11 82.7(3) . . ?
O25 W6 O24 157.5(3) . . ?
O25 W6 O27 85.2(3) . . ?
O29 W6 O11 162.9(3) . . ?
O29 W6 O24 93.5(3) . . ?
O29 W6 O25 91.9(3) . . ?
O29 W6 O27 84.1(3) . . ?
O13 W7 O27 82.3(3) . . ?
O18 W7 O13 97.5(4) . . ?
O18 W7 O23 102.5(4) . . ?
O18 W7 O24 99.8(4) . . ?
O18 W7 O27 172.7(3) . . ?
O18 W7 O30 99.5(4) . . ?
O23 W7 O13 85.1(3) . . ?
O23 W7 O27 84.8(3) . . ?
O24 W7 O13 89.5(3) . . ?
O24 W7 O23 157.6(3) . . ?
O24 W7 O27 72.9(3) . . ?
O30 W7 O13 162.8(3) . . ?
O30 W7 O23 88.7(3) . . ?
O30 W7 O24 90.2(3) . . ?
O30 W7 O27 81.2(3) . . ?
O12 W8 O28 83.5(3) . . ?
O12 W8 O32 163.7(3) . . ?
O19 W8 O12 98.6(4) . . ?
O19 W8 O22 101.3(4) . . ?
O19 W8 O23 102.4(4) . . ?
O19 W8 O28 172.9(3) . . ?
O19 W8 O32 97.5(4) . . ?
O22 W8 O12 91.8(3) . . ?
O22 W8 O23 156.2(3) . . ?
O22 W8 O28 71.7(3) . . ?
O22 W8 O32 87.2(3) . . ?
O23 W8 O12 85.9(3) . . ?
O23 W8 O28 84.5(3) . . ?
O23 W8 O32 88.6(3) . . ?
O32 W8 O28 80.8(3) . . ?
O8 W9 O28 79.8(3) . . ?
O14 W9 O8 94.5(3) . . ?
O14 W9 O21 101.6(4) . . ?
O14 W9 O22 99.2(4) . . ?
O14 W9 O28 170.3(3) . . ?
O14 W9 O34 101.2(4) . . ?
O21 W9 O8 83.7(3) . . ?
O21 W9 O22 157.4(3) . . ?
O21 W9 O28 85.8(3) . . ?
O22 W9 O8 85.8(3) . . ?
O22 W9 O28 72.6(3) . . ?
O34 W9 O8 164.2(3) . . ?
O34 W9 O21 92.5(3) . . ?
O34 W9 O22 92.2(3) . . ?
O34 W9 O28 84.6(3) . . ?
O34 W10 O49 80.2(3) . . ?
O40 W10 O34 84.3(3) . . ?
O40 W10 O49 71.6(3) . . ?
O41 W10 O34 96.0(3) . . ?
O41 W10 O40 101.6(3) . . ?
O41 W10 O42 102.3(3) . . ?
O41 W10 O49 172.4(3) . . ?
O41 W10 O54 100.6(3) . . ?
O42 W10 O34 85.3(3) . . ?
O42 W10 O40 154.8(3) . . ?
O42 W10 O49 84.0(3) . . ?
O54 W10 O34 163.3(3) . . ?
O54 W10 O40 91.0(3) . . ?
O54 W10 O42 92.4(3) . . ?
O54 W10 O49 83.2(3) . . ?
O32 W11 O38 88.5(3) . . ?
O32 W11 O49 87.6(3) . . ?
O32 W11 O56 167.6(3) . 2_565 ?
O38 W11 O49 83.7(3) . . ?
O38 W11 O56 85.5(3) . 2_565 ?
O39 W11 O32 97.0(3) . . ?
O39 W11 O38 101.5(3) . . ?
O39 W11 O40 99.4(3) . . ?
O39 W11 O49 173.2(3) . . ?
O39 W11 O56 94.9(3) . 2_565 ?
O40 W11 O32 90.7(3) . . ?
O40 W11 O38 159.0(3) . . ?
O40 W11 O49 75.3(3) . . ?
O40 W11 O56 91.0(3) . 2_565 ?
O56 W11 O49 80.9(3) 2_565 . ?
O30 W12 O38 87.6(3) . . ?
O30 W12 O47 86.3(3) . . ?
O30 W12 O51 166.4(3) . . ?
O36 W12 O30 89.5(3) . . ?
O36 W12 O38 158.0(3) . . ?
O36 W12 O47 75.1(3) . . ?
O36 W12 O51 91.8(3) . . ?
O37 W12 O30 96.8(3) . . ?
O37 W12 O36 102.1(3) . . ?
O37 W12 O38 99.8(3) . . ?
O37 W12 O47 175.9(3) . . ?
O37 W12 O51 96.2(3) . . ?
O38 W12 O47 82.9(3) . . ?
O38 W12 O51 86.1(3) . . ?
O51 W12 O47 80.9(3) . . ?
O29 W13 O47 81.0(3) . . ?
O35 W13 O29 96.1(3) . . ?
O35 W13 O36 101.7(3) . . ?
O35 W13 O46 102.8(3) . . ?
O35 W13 O47 172.9(3) . . ?
O35 W13 O50 100.5(4) . . ?
O36 W13 O29 84.4(3) . . ?
O36 W13 O47 71.6(3) . . ?
O46 W13 O29 85.4(3) . . ?
O46 W13 O36 154.3(3) . . ?
O46 W13 O47 83.5(3) . . ?
O50 W13 O29 163.4(3) . . ?
O50 W13 O36 91.1(3) . . ?
O50 W13 O46 92.0(3) . . ?
O50 W13 O47 82.4(3) . . ?
O31 W14 O44 90.5(3) . . ?
O31 W14 O46 92.9(3) . . ?
O31 W14 O48 86.2(3) . . ?
O31 W14 O53 163.1(3) . . ?
O44 W14 O48 73.4(3) . . ?
O44 W14 O53 82.9(3) . . ?
O45 W14 O31 100.9(4) . . ?
O45 W14 O44 101.0(3) . . ?
O45 W14 O46 100.4(3) . . ?
O45 W14 O48 171.1(3) . . ?
O45 W14 O53 95.5(3) . . ?
O46 W14 O44 157.4(3) . . ?
O46 W14 O48 84.5(3) . . ?
O46 W14 O53 87.6(3) . . ?
O53 W14 O48 77.1(3) . . ?
O33 W15 O42 92.9(3) . . ?
O33 W15 O44 91.1(3) . . ?
O33 W15 O48 86.8(3) . . ?
O33 W15 O55 163.7(3) . . ?
O42 W15 O44 158.3(3) . . ?
O42 W15 O48 84.8(3) . . ?
O42 W15 O55 87.6(3) . . ?
O43 W15 O33 102.1(4) . . ?
O43 W15 O42 100.9(3) . . ?
O43 W15 O44 99.1(3) . . ?
O43 W15 O48 169.1(3) . . ?
O43 W15 O55 93.8(3) . . ?
O44 W15 O48 74.1(3) . . ?
O44 W15 O55 82.7(3) . . ?
O55 W15 O48 77.0(3) . . ?
O51 W16 O52 78.0(3) 2_565 . ?
O53 W16 O51 161.9(3) . 2_565 ?
O53 W16 O52 84.6(3) . . ?
O53 W16 O56 89.8(3) . . ?
O55 W16 O51 90.0(3) . 2_565 ?
O55 W16 O52 84.1(3) . . ?
O55 W16 O53 93.1(3) . . ?
O55 W16 O56 161.3(3) . . ?
O56 W16 O51 81.7(3) . 2_565 ?
O56 W16 O52 77.8(3) . . ?
O57 W16 O51 96.5(3) . 2_565 ?
O57 W16 O52 173.3(3) . . ?
O57 W16 O53 100.5(3) . . ?
O57 W16 O55 99.8(3) . . ?
O57 W16 O56 97.8(3) . . ?
O50 Co1 O51 101.4(3) 2_565 2_565 ?
O50 Co1 O52 92.4(3) 2_565 2_565 ?
O50 Co1 O52 176.8(3) 2_565 . ?
O50 Co1 O54 91.5(3) 2_565 . ?
O50 Co1 O56 90.5(3) 2_565 2_565 ?
O51 Co1 O52 89.7(3) 2_565 2_565 ?
O51 Co1 O52 78.0(3) 2_565 . ?
O52 Co1 O52 84.5(3) . 2_565 ?
O54 Co1 O51 88.8(3) . 2_565 ?
O54 Co1 O52 176.0(3) . 2_565 ?
O54 Co1 O52 91.6(3) . . ?
O54 Co1 O56 102.7(3) . 2_565 ?
O56 Co1 O51 163.3(3) 2_565 2_565 ?
O56 Co1 O52 78.0(3) 2_565 2_565 ?
O56 Co1 O52 89.4(3) 2_565 . ?
O26 P1 O10 106.8(4) . . ?
O27 P1 O10 105.8(4) . . ?
O27 P1 O26 112.9(4) . . ?
O27 P1 O28 111.4(4) . . ?
O28 P1 O10 107.1(4) . . ?
O28 P1 O26 112.2(4) . . ?
O47 P2 O48 111.6(4) . . ?
O47 P2 O49 111.7(4) . . ?
O47 P2 O52 106.6(4) . . ?
O48 P2 O52 107.8(4) . . ?
O49 P2 O48 111.8(4) . . ?
O49 P2 O52 107.1(4) . . ?
W2 O4 W3 126.8(5) . . ?
W2 O5 W1 124.5(4) . . ?
W1 O6 W3 124.5(4) . . ?
W4 O7 W2 148.2(5) . . ?
W2 O8 W9 151.8(4) . . ?
W5 O9 W1 147.6(5) . . ?
W1 O10 W2 92.5(2) . . ?
W1 O10 W3 90.7(2) . . ?
W2 O10 W3 89.6(2) . . ?
P1 O10 W1 124.4(4) . . ?
P1 O10 W2 123.5(4) . . ?
P1 O10 W3 125.8(4) . . ?
W1 O11 W6 152.0(4) . . ?
W3 O12 W8 151.3(5) . . ?
W3 O13 W7 151.2(4) . . ?
W4 O20 W5 124.0(4) . . ?
W9 O21 W4 151.9(4) . . ?
W8 O22 W9 124.9(4) . . ?
W8 O23 W7 151.0(4) . . ?
W7 O24 W6 122.4(4) . . ?
W5 O25 W6 153.2(5) . . ?
W4 O26 W5 90.1(2) . . ?
P1 O26 W4 128.3(4) . . ?
P1 O26 W5 128.0(4) . . ?
W6 O27 W7 90.2(3) . . ?
P1 O27 W6 129.3(4) . . ?
P1 O27 W7 128.8(4) . . ?
W9 O28 W8 90.5(2) . . ?
P1 O28 W8 127.5(4) . . ?
P1 O28 W9 129.2(4) . . ?
W6 O29 W13 164.7(5) . . ?
W7 O30 W12 164.1(4) . . ?
W14 O31 W5 164.5(5) . . ?
W11 O32 W8 162.6(4) . . ?
W15 O33 W4 164.5(5) . . ?
W9 O34 W10 163.3(4) . . ?
W12 O36 W13 122.9(4) . . ?
W11 O38 W12 153.4(4) . . ?
W11 O40 W10 121.7(4) . . ?
W10 O42 W15 154.3(4) . . ?
W14 O44 W15 121.8(4) . . ?
W14 O46 W13 155.5(4) . . ?
W12 O47 W13 90.4(2) . . ?
P2 O47 W12 132.2(4) . . ?
P2 O47 W13 128.0(4) . . ?
W15 O48 W14 90.2(2) . . ?
P2 O48 W14 128.3(4) . . ?
P2 O48 W15 128.7(4) . . ?
W11 O49 W10 91.3(2) . . ?
P2 O49 W10 127.1(4) . . ?
P2 O49 W11 131.9(4) . . ?
W13 O50 Co1 134.8(4) . 2_565 ?
W12 O51 W16 124.9(4) . 2_565 ?
W12 O51 Co1 126.1(3) . 2_565 ?
W16 O51 Co1 107.2(3) 2_565 2_565 ?
Co1 O52 W16 96.2(3) . . ?
Co1 O52 W16 95.7(3) 2_565 . ?
Co1 O52 Co1 95.5(3) . 2_565 ?
P2 O52 W16 123.9(4) . . ?
P2 O52 Co1 119.6(4) . 2_565 ?
P2 O52 Co1 119.6(4) . . ?
W16 O53 W14 142.0(4) . . ?
W10 O54 Co1 133.3(4) . . ?
W16 O55 W15 142.3(4) . . ?
W11 O56 W16 125.0(3) 2_565 . ?
W11 O56 Co1 125.9(3) 2_565 2_565 ?
W16 O56 Co1 107.6(3) . 2_565 ?
C2 N1 N2 106.6(12) . . ?
N1 N2 C4 111.3(12) . . ?
N4 N3 C9 111.6(11) . . ?
N3 N4 C7 108.3(11) . . ?
N6 N5 C14 107.8(14) . . ?
N5 N6 C12 114.1(15) . . ?
N8 N7 C19 109.0(15) . . ?
N7 N8 C17 109.9(16) . . ?
C22 N9 N10 108.5(14) . . ?
C24 N10 N9 107.9(14) . . ?
N12 N11 C29 106.3(16) . . ?
N11 N12 C27 112.2(16) . . ?
N1 C2 C1 117.0(14) . . ?
N1 C2 C3 110.7(14) . . ?
C3 C2 C1 132.2(13) . . ?
C2 C3 C4 106.2(12) . . ?
C2 C3 C8 127.4(12) . . ?
C4 C3 C8 126.4(12) . . ?
N2 C4 C3 105.1(14) . . ?
N2 C4 C5 125.3(14) . . ?
C3 C4 C5 129.5(13) . . ?
N4 C7 C6 120.5(11) . . ?
N4 C7 C8 106.9(11) . . ?
C8 C7 C6 132.6(11) . . ?
C7 C8 C3 125.1(11) . . ?
C9 C8 C3 129.0(11) . . ?
C9 C8 C7 105.9(10) . . ?
N3 C9 C8 107.4(11) . . ?
N3 C9 C10 122.8(12) . . ?
C8 C9 C10 129.8(12) . . ?
N6 C12 C11 126.2(19) . . ?
N6 C12 C13 103.9(16) . . ?
C13 C12 C11 129.8(18) . . ?
C12 C13 C14 108.6(14) . . ?
C12 C13 C18 126.3(15) . . ?
C14 C13 C18 125.1(14) . . ?
N5 C14 C13 105.6(15) . . ?
N5 C14 C15 122.4(16) . . ?
C13 C14 C15 132.0(15) . . ?
N8 C17 C16 122.3(19) . . ?
C18 C17 N8 107.8(17) . . ?
C18 C17 C16 129.5(18) . . ?
C17 C18 C13 127.1(16) . . ?
C17 C18 C19 106.1(16) . . ?
C19 C18 C13 126.5(15) . . ?
N7 C19 C18 107.2(16) . . ?
N7 C19 C20 123.5(16) . . ?
C18 C19 C20 128.7(15) . . ?
N9 C22 C21 118.3(17) . . ?
N9 C22 C23 107.7(14) . . ?
C23 C22 C21 134.0(16) . . ?
C22 C23 C24 106.3(15) . . ?
C22 C23 C28 129.4(14) . . ?
C24 C23 C28 124.3(15) . . ?
N10 C24 C23 109.4(14) . . ?
N10 C24 C25 120.2(14) . . ?
C23 C24 C25 130.3(15) . . ?
N12 C27 C26 120.6(19) . . ?
N12 C27 C28 106.7(17) . . ?
C28 C27 C26 132(2) . . ?
C23 C28 C27 124.0(17) . . ?
C29 C28 C23 130.6(15) . . ?
C29 C28 C27 105.4(15) . . ?
N11 C29 C30 119.3(18) . . ?
C28 C29 N11 108.8(15) . . ?
C28 C29 C30 131.8(15) . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
p.res created by SHELXL-2014/7
TITL Integration of 150529c
CELL 0.71 15.0824 15.392 20.4265 78.8374 82.5853 75.4572
ZERR 1 0.0021 0.0021 0.0028 0.0013 0.0013 0.0012
LATT 1
SFAC C H Co N O P W
UNIT 60 96 2 24 122 4 32
L.S. 8 0 0
PLAN 10
SIZE 0.05 0.06 0.08
TEMP 25
fmap 2 53
acta
OMIT -3 52
OMIT -3 0 2
OMIT 4 1 4
OMIT 4 -2 2
OMIT 1 -1 1
OMIT 0 0 4
OMIT 1 -3 2
OMIT -2 -2 1
OMIT 4 2 1
OMIT 2 1 0
OMIT 2 -1 1
OMIT 7 17 15
OMIT 3 1 3
OMIT -2 3 1
OMIT 3 14 2
OMIT -12 -6 4
OMIT 3 1 2
OMIT 4 3 2
REM
REM
REM
WGHT 0.053900 1.411100
FVAR 5.33595
W1 7 0.401162 0.077907 0.341783 11.00000 0.03082 0.03175 =
0.02836 0.00439 -0.01094 0.00025
W2 7 0.190978 0.047936 0.412029 11.00000 0.03939 0.02847 =
0.02283 0.00758 -0.00952 -0.00805
W3 7 0.262210 0.231938 0.430586 11.00000 0.03585 0.03211 =
0.01964 0.00118 -0.01115 -0.00590
W4 7 0.137753 0.019366 0.247296 11.00000 0.03542 0.01719 =
0.02232 0.00209 -0.00582 -0.00499
W5 7 0.344637 0.051463 0.177961 11.00000 0.02781 0.02241 =
0.02694 -0.00166 -0.00532 0.00302
W6 7 0.411850 0.260693 0.191367 11.00000 0.01931 0.02982 =
0.02739 0.00099 -0.00450 -0.00364
W7 7 0.277182 0.411132 0.282574 11.00000 0.02535 0.02522 =
0.01991 -0.00074 -0.00784 -0.00896
W8 7 0.051510 0.376100 0.359166 11.00000 0.02638 0.02465 =
0.01577 -0.00326 -0.00323 -0.00575
W9 7 -0.018712 0.195104 0.332834 11.00000 0.02740 0.02422 =
0.01417 0.00140 -0.00095 -0.00920
W10 7 -0.129042 0.323309 0.174529 11.00000 0.02268 0.02426 =
0.01919 -0.00080 -0.00076 -0.01010
W11 7 -0.055254 0.501266 0.200778 11.00000 0.01623 0.01758 =
0.01404 -0.00250 -0.00052 -0.00501
W12 7 0.172188 0.537372 0.124862 11.00000 0.01649 0.01736 =
0.01570 -0.00258 -0.00226 -0.00665
W13 7 0.306366 0.391081 0.030710 11.00000 0.02273 0.02921 =
0.03091 -0.00514 0.00056 -0.00656
W14 7 0.237577 0.180544 0.020002 11.00000 0.01735 0.01712 =
0.02176 -0.00372 -0.00151 -0.00185
W15 7 0.032235 0.148536 0.088987 11.00000 0.02054 0.01481 =
0.01947 0.00030 -0.00297 -0.00612
W16 7 0.033441 0.333969 -0.055147 11.00000 0.02244 0.01835 =
0.01871 -0.00230 -0.00377 -0.00480
CO1 3 -0.099966 0.484984 0.033149 11.00000 0.01115 0.01442 =
0.01044 -0.00249 -0.00143 -0.00558
P1 6 0.203349 0.215231 0.269456 11.00000 0.01288 0.01325 =
0.00691 -0.00125 -0.00283 -0.00408
P2 6 0.087042 0.355351 0.098466 11.00000 0.00877 0.00819 =
0.00730 -0.00208 0.00113 -0.00330
O1 5 0.166382 -0.038427 0.474845 11.00000 0.04839 0.02971 =
0.02275 0.01252 -0.01419 -0.01186
PART 2
O1W 5 0.715340 0.336993 0.396341 10.20000 0.14931
PART 0
O2 5 0.281232 0.264173 0.502494 11.00000 0.04702 0.04905 =
0.02527 0.00486 -0.01785 -0.00825
O2W 5 0.676402 1.154178 0.451983 11.00000 0.11894
O3 5 0.506844 0.010550 0.361577 11.00000 0.04699 0.05019 =
0.04262 0.00068 -0.01898 0.00025
PART 1
O3W 5 0.523035 0.088891 0.496072 10.30000 0.08413
PART 0
PART 2
O3WA 5 0.509261 0.135318 0.514888 10.70000 0.11731
PART 0
O4 5 0.209521 0.129495 0.462530 11.00000 0.04554 0.02702 =
0.04742 -0.01305 0.02769 -0.01873
PART 2
O4W 5 0.391073 0.320549 0.787163 10.50000 0.03357
PART 0
PART 1
O4WA 5 0.302544 0.353779 0.843150 10.50000 0.02090
PART 0
O5 5 0.320795 0.005512 0.395343 11.00000 0.03415 0.01524 =
0.05649 0.01573 -0.01247 0.00522
O6 5 0.378319 0.151058 0.410220 11.00000 0.02815 0.02840 =
0.06727 -0.01125 -0.02919 0.00139
O7 5 0.185274 0.000481 0.330696 11.00000 0.05729 0.02134 =
0.02957 0.00919 -0.01552 -0.00746
O8 5 0.077025 0.122367 0.395729 11.00000 0.03501 0.02517 =
0.01607 0.00525 0.00239 -0.00987
O9 5 0.378701 0.028593 0.267180 11.00000 0.04508 0.02636 =
0.02306 0.00054 -0.01085 0.00652
O10 5 0.248516 0.162957 0.336968 11.00000 0.03125 0.02873 =
0.00947 0.00910 -0.00866 -0.00326
O11 5 0.427777 0.174670 0.279813 11.00000 0.02859 0.04209 =
0.02112 0.00367 -0.01539 -0.00866
O12 5 0.140460 0.297833 0.415856 11.00000 0.03220 0.03490 =
0.02464 0.00400 -0.00916 -0.00551
O13 5 0.299182 0.320418 0.363182 11.00000 0.03426 0.03513 =
0.02030 0.00492 -0.01080 -0.01335
O14 5 -0.105995 0.151907 0.377241 11.00000 0.03676 0.04017 =
0.01633 0.00428 -0.00545 -0.01786
O15 5 0.097204 -0.075462 0.257146 11.00000 0.05323 0.02360 =
0.03178 0.00141 -0.00750 -0.01442
O16 5 0.430730 -0.023895 0.145046 11.00000 0.04734 0.02586 =
0.04149 -0.00476 -0.01922 0.01375
O17 5 0.526579 0.249207 0.169322 11.00000 0.02382 0.04566 =
0.04254 0.00857 -0.00917 0.00053
O18 5 0.304956 0.497975 0.310557 11.00000 0.04157 0.04198 =
0.03151 -0.00459 -0.01444 -0.01742
O19 5 0.001704 0.452476 0.411073 11.00000 0.03758 0.04697 =
0.02060 -0.00738 -0.00316 -0.00140
O20 5 0.255705 -0.021511 0.203838 11.00000 0.03570 0.01196 =
0.03282 0.00173 -0.00139 -0.00046
O21 5 0.035455 0.104959 0.279262 11.00000 0.03201 0.02190 =
0.01548 -0.00117 -0.00241 -0.00062
O22 5 -0.025586 0.294355 0.379800 11.00000 0.02596 0.03792 =
0.01757 -0.00166 -0.00178 -0.01086
O23 5 0.149577 0.424601 0.313652 11.00000 0.03234 0.02366 =
0.02720 -0.00364 -0.00533 -0.00936
O24 5 0.395068 0.356264 0.242835 11.00000 0.01666 0.02700 =
0.03779 -0.00222 -0.00496 -0.00445
O25 5 0.388048 0.157773 0.163400 11.00000 0.02898 0.02761 =
0.02732 0.00241 -0.00734 0.00028
O26 5 0.209534 0.143866 0.225942 11.00000 0.02644 0.01859 =
0.01446 0.00396 -0.00676 -0.00873
O27 5 0.258769 0.284086 0.238942 11.00000 0.02190 0.02189 =
0.02656 0.00096 -0.00352 -0.00433
O28 5 0.104858 0.260921 0.288937 11.00000 0.02008 0.02415 =
0.01632 0.00020 -0.00196 -0.00696
O29 5 0.361775 0.337421 0.118964 11.00000 0.00959 0.02871 =
0.02602 0.00080 -0.00769 -0.00264
O30 5 0.241616 0.471502 0.198093 11.00000 0.01859 0.02581 =
0.02139 -0.00145 -0.00688 -0.00632
O31 5 0.283717 0.104075 0.095442 11.00000 0.02648 0.02457 =
0.02681 -0.00919 -0.00163 -0.00386
O32 5 -0.019023 0.433434 0.284360 11.00000 0.02229 0.01935 =
0.02123 -0.00201 -0.00447 -0.00680
O33 5 0.093960 0.074464 0.158853 11.00000 0.04161 0.01839 =
0.02080 0.00549 -0.00400 -0.00491
O34 5 -0.078030 0.271631 0.263381 11.00000 0.03242 0.02494 =
0.01138 -0.00093 -0.00090 -0.00653
O35 5 0.406562 0.396861 -0.015088 11.00000 0.01878 0.02346 =
0.03327 -0.01150 0.00690 -0.00250
O36 5 0.275638 0.505068 0.065642 11.00000 0.01213 0.01376 =
0.02668 -0.00099 0.00294 -0.00460
O37 5 0.177558 0.643716 0.134633 11.00000 0.02192 0.01916 =
0.02693 -0.00426 -0.00036 -0.00430
O38 5 0.063630 0.524822 0.182094 11.00000 0.00809 0.01443 =
0.02878 0.00670 -0.00340 -0.00218
O39 5 -0.117176 0.598843 0.230036 11.00000 0.01562 0.01657 =
0.02752 -0.00945 -0.00094 -0.00435
O40 5 -0.150499 0.440536 0.205185 11.00000 0.01927 0.01243 =
0.02462 -0.00516 0.00130 -0.00592
O41 5 -0.233659 0.296241 0.196869 11.00000 0.02421 0.02625 =
0.03463 -0.00492 -0.00286 -0.00862
O42 5 -0.055554 0.215351 0.146800 11.00000 0.02296 0.01537 =
0.01458 0.00415 0.00451 -0.00975
O43 5 -0.029895 0.080301 0.069004 11.00000 0.03693 0.02129 =
0.02601 0.00192 0.00172 -0.01648
O44 5 0.138554 0.121133 0.027661 11.00000 0.02489 0.02268 =
0.02029 -0.00659 -0.00625 -0.00513
O45 5 0.309311 0.131685 -0.042118 11.00000 0.02721 0.02964 =
0.03168 -0.01699 -0.00550 -0.00416
O46 5 0.296796 0.269390 0.028942 11.00000 0.02377 0.01103 =
0.02929 -0.00581 -0.00438 0.00019
O47 5 0.166529 0.396713 0.103379 11.00000 0.01826 0.01782 =
0.01751 -0.00452 -0.00221 -0.00320
O48 5 0.120103 0.252430 0.094421 11.00000 0.01234 0.03388 =
0.00671 -0.00353 0.00103 -0.01463
O49 5 0.012168 0.372894 0.155101 11.00000 0.01384 0.01014 =
0.01885 0.00035 -0.00439 -0.00485
O50 5 0.227382 0.438186 -0.031988 11.00000 0.01357 0.02312 =
0.02336 -0.00103 -0.00481 -0.00305
O51 5 0.090817 0.578302 0.051023 11.00000 0.01219 0.00999 =
0.02190 0.00373 -0.00268 0.00187
O52 5 0.042904 0.406103 0.030024 11.00000 0.01611 0.01220 =
0.01133 0.00368 -0.00519 -0.00332
O53 5 0.156304 0.277472 -0.043001 11.00000 0.00842 0.01856 =
0.02048 0.00167 -0.00411 -0.00281
O54 5 -0.143652 0.379574 0.089851 11.00000 0.02808 0.01189 =
0.01766 0.00287 -0.00139 -0.00877
O55 5 -0.009735 0.251433 0.012832 11.00000 0.01785 0.01095 =
0.01518 0.00304 -0.00505 0.00003
O56 5 0.071407 0.447132 -0.104493 11.00000 0.01159 0.01853 =
0.02332 -0.00278 -0.00514 -0.00680
O57 5 0.018628 0.291227 -0.123969 11.00000 0.02509 0.02664 =
0.01934 -0.00208 -0.00470 -0.01090
N1 4 0.471126 0.195305 0.929693 11.00000 0.03280 0.05576 =
0.06225 -0.01428 0.00103 -0.02863
AFIX 43
H1 2 0.427683 0.166821 0.935543 11.00000 -1.20000
AFIX 0
N2 4 0.477733 0.268528 0.884521 11.00000 0.02235 0.08561 =
0.09009 -0.05125 -0.03031 0.00257
AFIX 43
H2 2 0.439416 0.293673 0.854800 11.00000 -1.20000
AFIX 0
N3 4 0.821268 0.221874 0.991943 11.00000 0.02013 0.04287 =
0.06293 0.01013 -0.02102 -0.01047
AFIX 43
H3 2 0.879606 0.200486 0.992965 11.00000 -1.20000
AFIX 0
N4 4 0.774786 0.289604 1.020736 11.00000 0.07278 0.03333 =
0.03215 0.00879 -0.02040 -0.02376
AFIX 43
H4 2 0.797062 0.319945 1.043056 11.00000 -1.20000
AFIX 0
N5 4 0.932775 0.313079 0.746215 11.00000 0.07847 0.08795 =
0.06387 -0.05152 0.00214 -0.00978
AFIX 43
H5 2 0.918457 0.315642 0.788051 11.00000 -1.20000
AFIX 0
N6 4 1.010673 0.323078 0.712463 11.00000 0.07848 0.06368 =
0.09414 -0.04859 -0.03801 0.00376
AFIX 43
H6 2 1.055118 0.332611 0.730443 11.00000 -1.20000
AFIX 0
N7 4 0.874869 0.217094 0.500247 11.00000 0.09073 0.06815 =
0.02615 -0.01057 0.00530 -0.04530
AFIX 43
H7 2 0.876076 0.177124 0.475783 11.00000 -1.20000
AFIX 0
N8 4 0.828974 0.300334 0.490283 11.00000 0.07840 0.09229 =
0.04519 -0.01872 -0.00543 -0.00543
AFIX 43
H8 2 0.795099 0.324814 0.457713 11.00000 -1.20000
AFIX 0
N9 4 0.700311 1.094602 0.329437 11.00000 0.07683 0.08456 =
0.05688 -0.01926 -0.01257 -0.02176
AFIX 43
H9 2 0.694567 1.117521 0.365383 11.00000 -1.20000
AFIX 0
N10 4 0.699492 1.142395 0.265317 11.00000 0.16631 0.04659 =
0.04611 0.00299 -0.01746 -0.03521
AFIX 43
H10 2 0.689159 1.200634 0.254192 11.00000 -1.20000
AFIX 0
N11 4 0.742099 0.792055 0.196502 11.00000 0.07136 0.05873 =
0.10974 -0.02594 -0.03641 0.00616
AFIX 43
H11 2 0.722381 0.749467 0.185577 11.00000 -1.20000
AFIX 0
N12 4 0.824241 0.805147 0.184047 11.00000 0.07306 0.06325 =
0.12483 -0.01813 0.04463 -0.00040
AFIX 43
H12 2 0.869936 0.767813 0.167232 11.00000 -1.20000
AFIX 0
C1 1 0.551987 0.093648 1.017902 11.00000 0.07514 0.05243 =
0.13405 -0.01415 -0.01128 -0.03732
AFIX 137
H1A 2 0.556582 0.111464 1.059625 11.00000 -1.50000
H1B 2 0.606149 0.048514 1.007584 11.00000 -1.50000
H1C 2 0.498879 0.068778 1.021455 11.00000 -1.50000
AFIX 0
C2 1 0.543174 0.175041 0.963382 11.00000 0.03418 0.05983 =
0.05303 -0.03299 -0.00913 -0.01056
C3 1 0.595744 0.237571 0.942328 11.00000 0.02763 0.01663 =
0.04199 -0.01087 -0.00400 -0.00979
C4 1 0.552693 0.298577 0.891280 11.00000 0.03044 0.06817 =
0.03948 -0.01783 -0.00590 -0.00220
C5 1 0.576940 0.386049 0.851758 11.00000 0.04630 0.07256 =
0.08762 0.01686 -0.02608 -0.00068
AFIX 137
H5A 2 0.552461 0.399934 0.808848 11.00000 -1.50000
H5B 2 0.642546 0.377660 0.845621 11.00000 -1.50000
H5C 2 0.551001 0.435350 0.876046 11.00000 -1.50000
AFIX 0
C6 1 0.613539 0.373518 1.040900 11.00000 0.06451 0.02975 =
0.04509 -0.01524 0.00944 -0.03387
AFIX 137
H6A 2 0.642022 0.401013 1.068286 11.00000 -1.50000
H6B 2 0.568674 0.344730 1.068130 11.00000 -1.50000
H6C 2 0.583989 0.419500 1.006561 11.00000 -1.50000
AFIX 0
C7 1 0.684671 0.304307 1.009496 11.00000 0.02019 0.03491 =
0.02068 -0.00103 -0.00406 -0.01224
C8 1 0.679353 0.241482 0.970061 11.00000 0.02835 0.02444 =
0.02376 0.00061 -0.01056 -0.00879
C9 1 0.767776 0.189901 0.960875 11.00000 0.02615 0.01774 =
0.04922 -0.00008 -0.00546 -0.00714
C10 1 0.803663 0.114247 0.922051 11.00000 0.05168 0.04809 =
0.09579 -0.00438 -0.01184 -0.00157
AFIX 137
H10A 2 0.863770 0.117632 0.901187 11.00000 -1.50000
H10B 2 0.763122 0.119184 0.888252 11.00000 -1.50000
H10C 2 0.807280 0.057048 0.951632 11.00000 -1.50000
AFIX 0
C11 1 1.091196 0.331670 0.596273 11.00000 0.06703 0.11445 =
0.12367 -0.05604 0.04636 -0.04276
AFIX 137
H11A 2 1.132036 0.358109 0.614231 11.00000 -1.50000
H11B 2 1.066714 0.371970 0.557398 11.00000 -1.50000
H11C 2 1.124283 0.274361 0.584044 11.00000 -1.50000
AFIX 0
C12 1 1.014929 0.317124 0.647396 11.00000 0.08347 0.04675 =
0.08888 -0.03711 0.00255 -0.01559
C13 1 0.930211 0.299100 0.640281 11.00000 0.04965 0.05900 =
0.03916 -0.02242 -0.00747 -0.00800
C14 1 0.877810 0.297692 0.702565 11.00000 0.06784 0.03992 =
0.06061 -0.03002 -0.01519 -0.00640
C15 1 0.786862 0.282492 0.723621 11.00000 0.07887 0.03709 =
0.04939 -0.00932 0.01568 -0.00710
AFIX 33
H15A 2 0.760257 0.273233 0.686028 11.00000 -1.50000
H15B 2 0.790997 0.229596 0.757878 11.00000 -1.50000
H15C 2 0.748957 0.334558 0.740934 11.00000 -1.50000
AFIX 0
C16 1 0.802925 0.444107 0.536893 11.00000 0.16629 0.08706 =
0.07063 -0.02270 0.00194 -0.01889
AFIX 137
H16A 2 0.781560 0.471675 0.493713 11.00000 -1.50000
H16B 2 0.849928 0.471529 0.545415 11.00000 -1.50000
H16C 2 0.752605 0.453168 0.570717 11.00000 -1.50000
AFIX 0
C17 1 0.841767 0.343307 0.538205 11.00000 0.07231 0.08454 =
0.05414 -0.02439 0.01338 -0.03007
C18 1 0.900462 0.283973 0.578900 11.00000 0.05702 0.06205 =
0.03233 -0.00741 -0.00322 -0.01663
C19 1 0.920425 0.202678 0.554778 11.00000 0.05891 0.09140 =
0.02735 -0.00971 0.01676 -0.04867
C20 1 0.989953 0.116748 0.576326 11.00000 0.11424 0.08211 =
0.03199 -0.02024 -0.00510 -0.02927
AFIX 33
H20A 2 1.013996 0.121025 0.616574 11.00000 -1.50000
H20B 2 0.961315 0.066120 0.584581 11.00000 -1.50000
H20C 2 1.039145 0.107981 0.541645 11.00000 -1.50000
AFIX 0
C21 1 0.710519 0.942584 0.389911 11.00000 0.11131 0.10476 =
0.05976 0.03519 -0.01679 -0.03703
AFIX 137
H21A 2 0.729615 0.881391 0.380867 11.00000 -1.50000
H21B 2 0.649436 0.952208 0.411813 11.00000 -1.50000
H21C 2 0.751881 0.952094 0.418393 11.00000 -1.50000
AFIX 0
C22 1 0.711474 1.006973 0.326618 11.00000 0.07503 0.03252 =
0.05299 0.01330 -0.02898 -0.00993
C23 1 0.724326 0.997955 0.261461 11.00000 0.03876 0.04904 =
0.03528 0.02132 -0.00818 0.00376
C24 1 0.716779 1.085118 0.225104 11.00000 0.06545 0.05125 =
0.03461 0.00494 0.00678 -0.00907
C25 1 0.728889 1.117427 0.149455 11.00000 0.09925 0.04440 =
0.03100 0.00534 0.00402 0.00112
AFIX 137
H25A 2 0.680490 1.169714 0.136664 11.00000 -1.50000
H25B 2 0.726559 1.069483 0.126314 11.00000 -1.50000
H25C 2 0.787211 1.133344 0.137949 11.00000 -1.50000
AFIX 0
C26 1 0.918489 0.910501 0.188600 11.00000 0.13926
AFIX 137
H26A 2 0.968497 0.857553 0.190089 11.00000 -1.50000
H26B 2 0.922414 0.943944 0.222797 11.00000 -1.50000
H26C 2 0.921826 0.948398 0.145523 11.00000 -1.50000
AFIX 0
C27 1 0.830012 0.882085 0.200018 11.00000 0.05522 0.03240 =
0.21564 -0.01482 0.02057 0.00202
C28 1 0.743585 0.918652 0.232713 11.00000 0.05705 0.02919 =
0.06484 -0.00465 0.00345 -0.00100
C29 1 0.691533 0.860843 0.231275 11.00000 0.05372 0.06962 =
0.02826 -0.02035 -0.01004 0.02367
C30 1 0.589972 0.861498 0.257104 11.00000 0.06095 0.08925 =
0.22091 -0.04941 0.00275 -0.01884
AFIX 137
H30A 2 0.550044 0.901767 0.225498 11.00000 -1.50000
H30B 2 0.576571 0.882064 0.299548 11.00000 -1.50000
H30C 2 0.580504 0.801069 0.262238 11.00000 -1.50000
AFIX 0
PART 1
O1WA 5 0.761365 0.389872 0.364839 10.80000 0.14433
HKLF 4
REM Integration of 150529c
REM R1 = 0.0399 for 12885 Fo > 4sig(Fo) and 0.0610 for all 17648 data
REM 1096 parameters refined using 0 restraints
END
WGHT 0.0536 1.7976
REM Highest difference peak 3.309, deepest hole -3.668, 1-sigma level 0.310
Q1 1 0.3249 -0.0178 0.3462 11.00000 0.05 3.31
Q2 1 0.2572 0.3592 0.8743 11.00000 0.05 2.92
Q3 1 0.3952 0.1781 0.3613 11.00000 0.05 2.78
Q4 1 0.0807 0.1749 0.2533 11.00000 0.05 2.58
Q5 1 0.1438 0.2013 0.1039 11.00000 0.05 2.43
Q6 1 0.2985 0.2053 0.1813 11.00000 0.05 2.38
Q7 1 0.1534 0.3543 0.2736 11.00000 0.05 2.14
Q8 1 0.0711 0.5384 0.2165 11.00000 0.05 1.98
Q9 1 0.1621 0.5775 0.1547 11.00000 0.05 1.90
Q10 1 0.1031 0.3551 0.3594 11.00000 0.05 1.89
REM The information below was added by Olex2.
REM
REM R1 = 0.0399 for 12885 Fo > 4sig(Fo) and 0.0610 for all 78648 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 3.31, deepest hole -3.67
REM Mean Shift 0, Max Shift -0.002.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0610
REM R1_gt = 0.0399
REM wR_ref = 0.1084
REM GOOF = 1.078
REM Shift_max = -0.002
REM Shift_mean = 0
REM Reflections_all = 78648
REM Reflections_gt = 12885
REM Parameters = n/a
REM Hole = -3.67
REM Peak = 3.31
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.500 628 174 ' '
_platon_squeeze_details ?
# start Validation Reply Form
_vrf_PLAT201_p
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 1 Report
RESPONSE: Structure contain highly disordered CH3 group, so we didn't anisotropically refine C26 atom in this case.
;
_vrf_PLAT306_p
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O2W Check
RESPONSE: We have tried to theoretically add the H-atoms for water molecules in the crystal structure, but this is unsuccessful. Due to the highly disordered water solvents in the void, we have used PLATON/SQUEEZE program to substract the contributions from these solvents, thus it is impossible to find the reasonable H-bonding directions and H-bonding donors around the cluster for the H atoms on water, which will bring some of B alerts in the checkcif relating to the missed H-bonding donor or acceptor. Anyway, this issues will not influence us to recognize the main body of cluster as well as their properties in this work.
;
_vrf_PLAT342_p
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02374 Ang.
RESPONSE:Moderate crystal quality in context with many disordered solvents,
hence only small amount of reflections have I>2sigma(I)
;
_vrf_PLAT430_p
;
PROBLEM: Short Inter D...A Contact O3WA .. O2W .. 2.73 Ang.
RESPONSE: There are H-bonding between them, but adding H atoms for them is not possible due to the large disorder water which has been removed by PLATON/SQUEEZE program.
;
#######################################################################
#
# 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_p2
_database_code_depnum_ccdc_archive 'CCDC 1449924'
_audit_update_record
;
2016-04-05 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_audit_creation_date 2016-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'Co3 O114 P4 W31, 6(C10 H16 N4), 12(O)'
_chemical_formula_sum 'C60 H96 Co3 N24 O126 P4 W31'
_chemical_formula_weight 9169.62
_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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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 24.592(3)
_cell_length_b 14.2596(17)
_cell_length_c 24.846(3)
_cell_angle_alpha 90
_cell_angle_beta 111.4003(10)
_cell_angle_gamma 90
_cell_volume 8112.0(17)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 5428
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.279
_cell_measurement_theta_min 2.454
_shelx_estimated_absorpt_T_max 0.401
_shelx_estimated_absorpt_T_min 0.214
_exptl_absorpt_coefficient_mu 22.327
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6009
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0733 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.8059.
The \l/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour purple
_exptl_crystal_density_diffrn 3.754
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 8134
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max 0.7456
_exptl_transmission_factor_min 0.6009
_diffrn_reflns_av_R_equivalents 0.0581
_diffrn_reflns_av_unetI/netI 0.0716
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 45258
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.214
_diffrn_reflns_theta_max 26.000
_diffrn_reflns_theta_min 2.451
_diffrn_ambient_temperature 298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker Apex II'
_diffrn_measurement_method ?
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.710
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 10803
_reflns_number_total 15970
_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_data_collection 'APEX2 (Bruker,2005)'
_computing_cell_refinement 'APEX2 (Bruker,2005)'
_computing_data_reduction 'SAINT (Bruker, 2005)'
_computing_molecular_graphics 'DIAMOND (Brandenburg, 2008)'
_computing_publication_material 'publCIF (Westrip, 2010)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_refine_diff_density_max 2.514
_refine_diff_density_min -2.903
_refine_diff_density_rms 0.324
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.020
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1136
_refine_ls_number_reflns 15970
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0760
_refine_ls_R_factor_gt 0.0411
_refine_ls_restrained_S_all 1.020
_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^)+(0.0381P)^2^+7.8885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0848
_refine_ls_wR_factor_ref 0.0987
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Shared sites
{Co1, W1}
3. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
Uanis(Co1) = Uanis(W1)
4. Others
Fixed Sof: W1(0.5) Co1(0.5) O6W(0.5) O6WA(0.5)
5.a Me refined with riding coordinates:
C20(H20A,H20B,H20C), C6(H6A,H6B,H6C)
5.b Aromatic/amide H refined with riding coordinates:
N5(H5), N6(H6), N7(H7), N8(H8), N1(H1), N2(H2), N3(H3), N4(H4), N9(H9),
N10(H10), N11(H11), N12(H12)
5.c Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C1(H1A,H1B,
H1C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C21(H21A,H21B,H21C), C25(H25A,H25B,
H25C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C)
;
_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
W1 W -0.02237(3) 0.65098(5) 0.41485(4) 0.01422(18) Uani 0.5 1 d . . P . .
W2 W 0.13034(3) 0.66882(4) 0.48855(3) 0.02185(14) Uani 1 1 d . . . . .
W3 W 0.06686(2) 0.49571(4) 0.37243(2) 0.02016(13) Uani 1 1 d . . . . .
W4 W 0.05621(3) 0.27000(4) 0.40387(3) 0.03119(16) Uani 1 1 d . . . . .
W5 W 0.12566(3) 0.19016(4) 0.55490(3) 0.02273(14) Uani 1 1 d . . . . .
W6 W 0.18063(3) 0.34778(4) 0.66106(3) 0.02347(14) Uani 1 1 d . . . . .
W7 W 0.17797(3) 0.59901(4) 0.62746(3) 0.02877(15) Uani 1 1 d . . . . .
W8 W 0.32923(3) 0.31401(4) 0.65199(3) 0.02606(15) Uani 1 1 d . . . . .
W9 W 0.32691(3) 0.56557(4) 0.61707(3) 0.02706(15) Uani 1 1 d . . . . .
W10 W 0.27760(3) 0.63531(4) 0.47861(3) 0.02602(15) Uani 1 1 d . . . . .
W11 W 0.21352(3) 0.46186(4) 0.36207(3) 0.02404(14) Uani 1 1 d . . . . .
W12 W 0.20788(3) 0.23715(4) 0.39582(3) 0.02539(14) Uani 1 1 d . . . . .
W13 W 0.27436(3) 0.15506(4) 0.54637(3) 0.02705(15) Uani 1 1 d . . . . .
W14 W 0.37304(3) 0.46878(4) 0.44152(3) 0.02474(14) Uani 1 1 d . . . . .
W15 W 0.37149(3) 0.23749(4) 0.47417(3) 0.02587(15) Uani 1 1 d . . . . .
W16 W 0.42784(3) 0.40179(4) 0.58206(3) 0.02593(14) Uani 1 1 d . . . . .
Co1 Co -0.02237(3) 0.65098(5) 0.41485(4) 0.01422(18) Uani 0.5 1 d . . P . .
Co2 Co -0.02795(8) 0.42596(12) 0.44914(8) 0.0170(4) Uani 1 1 d . . . . .
P1 P 0.11434(14) 0.4298(2) 0.51853(15) 0.0135(7) Uani 1 1 d . . . . .
P2 P 0.27698(15) 0.3930(2) 0.50869(15) 0.0160(7) Uani 1 1 d . . . . .
O1 O 0.4058(4) 0.1455(7) 0.4549(4) 0.032(3) Uani 1 1 d . . . . .
O2 O 0.4976(4) 0.4077(7) 0.6305(4) 0.029(2) Uani 1 1 d . . . . .
O3 O 0.4345(4) 0.2856(6) 0.5429(4) 0.026(2) Uani 1 1 d . . . . .
O4 O 0.3930(4) 0.3379(6) 0.4343(4) 0.025(2) Uani 1 1 d . . . . .
O5 O 0.4369(4) 0.4654(6) 0.5176(4) 0.023(2) Uani 1 1 d . . . . .
O6 O 0.4077(4) 0.5203(6) 0.4007(4) 0.029(2) Uani 1 1 d . . . . .
O7 O 0.2979(4) 0.2358(6) 0.4196(4) 0.022(2) Uani 1 1 d . . . . .
O8 O 0.3409(4) 0.1790(6) 0.5272(4) 0.021(2) Uani 1 1 d . . . . .
O9 O 0.2986(4) 0.4472(6) 0.3871(4) 0.021(2) Uani 1 1 d . . . . .
O10 O 0.3386(4) 0.3798(6) 0.5041(4) 0.021(2) Uani 1 1 d . . . . .
O11 O 0.3919(4) 0.3270(6) 0.6248(4) 0.022(2) Uani 1 1 d . . . . .
O12 O 0.3437(4) 0.5720(6) 0.4691(4) 0.023(2) Uani 1 1 d . . . . .
O13 O 0.3927(4) 0.5032(6) 0.6003(4) 0.024(2) Uani 1 1 d . . . . .
O14 O 0.1995(4) 0.1383(7) 0.3529(4) 0.029(2) Uani 1 1 d . . . . .
O15 O 0.2775(4) 0.0365(6) 0.5500(4) 0.033(3) Uani 1 1 d . . . . .
O16 O 0.3696(4) 0.2907(7) 0.7225(4) 0.031(2) Uani 1 1 d . . . . .
O17 O 0.3697(4) 0.6263(7) 0.6767(4) 0.032(3) Uani 1 1 d . . . . .
O18 O 0.2868(5) 0.7397(7) 0.4506(4) 0.034(3) Uani 1 1 d . . . . .
O19 O 0.2022(4) 0.5094(7) 0.2960(4) 0.029(2) Uani 1 1 d . . . . .
O20 O 0.3156(4) 0.1880(6) 0.6243(4) 0.022(2) Uani 1 1 d . . . . .
O21 O 0.3235(4) 0.4463(6) 0.6503(4) 0.022(2) Uani 1 1 d . . . . .
O22 O 0.3243(4) 0.6538(6) 0.5571(4) 0.024(2) Uani 1 1 d . . . . .
O23 O 0.2324(4) 0.5670(6) 0.4115(4) 0.024(2) Uani 1 1 d . . . . .
O24 O 0.2092(4) 0.3311(6) 0.3424(4) 0.017(2) Uani 1 1 d . . . . .
O25 O 0.2284(4) 0.1776(6) 0.4702(4) 0.020(2) Uani 1 1 d . . . . .
O26 O 0.2739(4) 0.3216(6) 0.5528(4) 0.016(2) Uani 1 1 d . . . . .
O27 O 0.2740(4) 0.4932(6) 0.5272(4) 0.022(2) Uani 1 1 d . . . . .
O28 O 0.2313(4) 0.3743(6) 0.4493(4) 0.022(2) Uani 1 1 d . . . . .
O29 O 0.2011(4) 0.1672(6) 0.5613(4) 0.024(2) Uani 1 1 d . . . . .
O30 O 0.2537(4) 0.3132(6) 0.6583(4) 0.023(2) Uani 1 1 d . . . . .
O31 O 0.1335(4) 0.2588(6) 0.3896(4) 0.018(2) Uani 1 1 d . . . . .
O32 O 0.1401(4) 0.4614(6) 0.3632(4) 0.023(2) Uani 1 1 d . . . . .
O33 O 0.2549(4) 0.5954(6) 0.6142(4) 0.019(2) Uani 1 1 d . . . . .
O34 O 0.2096(4) 0.6593(6) 0.4939(4) 0.024(2) Uani 1 1 d . . . . .
O35 O 0.1161(4) 0.7785(6) 0.4610(4) 0.027(2) Uani 1 1 d . . . . .
O36 O 0.1565(4) 0.6968(6) 0.5686(4) 0.020(2) Uani 1 1 d . . . . .
O37 O 0.2028(4) 0.6635(7) 0.6898(4) 0.030(2) Uani 1 1 d . . . . .
O38 O 0.1969(4) 0.4749(6) 0.6568(4) 0.022(2) Uani 1 1 d . . . . .
O39 O 0.1961(4) 0.3340(7) 0.7329(4) 0.028(2) Uani 1 1 d . . . . .
O40 O 0.1529(4) 0.2237(6) 0.6351(4) 0.019(2) Uani 1 1 d . . . . .
O41 O 0.1013(4) 0.0785(6) 0.5589(4) 0.021(2) Uani 1 1 d . . . . .
O42 O 0.0990(4) 0.2076(6) 0.4757(4) 0.021(2) Uani 1 1 d . . . . .
O43 O 0.0227(4) 0.1786(6) 0.3613(4) 0.025(2) Uani 1 1 d . . . . .
O44 O 0.0397(4) 0.3716(6) 0.3497(4) 0.021(2) Uani 1 1 d . . . . .
O45 O 0.0388(4) 0.5523(6) 0.3080(4) 0.022(2) Uani 1 1 d . . . . .
O46 O 0.1102(4) 0.5915(6) 0.4220(4) 0.019(2) Uani 1 1 d . . . . .
O47 O 0.1469(4) 0.3517(6) 0.5588(4) 0.021(2) Uani 1 1 d . . . . .
O48 O 0.1467(4) 0.5229(6) 0.5358(4) 0.019(2) Uani 1 1 d . . . . .
O49 O 0.1034(4) 0.4046(6) 0.4554(4) 0.019(2) Uani 1 1 d . . . . .
O50 O 0.0003(4) 0.3047(6) 0.4291(4) 0.020(2) Uani 1 1 d . . . . .
O51 O 0.0526(4) 0.4403(6) 0.5242(4) 0.020(2) Uani 1 1 d . . . . .
O52 O 0.0045(4) 0.5200(6) 0.4015(4) 0.017(2) Uani 1 1 d . . . . .
O53 O 0.1029(4) 0.5856(6) 0.6182(4) 0.021(2) Uani 1 1 d . . . . .
O54 O 0.0498(4) 0.6431(6) 0.4850(4) 0.019(2) Uani 1 1 d . . . . .
O55 O -0.0973(4) 0.6191(6) 0.3609(4) 0.022(2) Uani 1 1 d . . . . .
O56 O -0.0516(4) 0.7480(6) 0.4454(4) 0.021(2) Uani 1 1 d . . . . .
O57 O 0.0037(4) 0.7108(7) 0.3705(4) 0.027(2) Uani 1 1 d . . . . .
N5 N 0.4794(7) 0.7461(10) 0.6561(8) 0.056(4) Uani 1 1 d . . . . .
H5 H 0.5066 0.7048 0.6685 0.067 Uiso 1 1 calc R . . . .
N6 N 0.4545(6) 0.7746(11) 0.6011(7) 0.049(4) Uani 1 1 d . . . . .
H6 H 0.4641 0.7552 0.5730 0.058 Uiso 1 1 calc R . . . .
N7 N 0.3416(11) 1.0248(13) 0.7051(10) 0.092(7) Uani 1 1 d . . . . .
H7 H 0.3400 1.0737 0.7247 0.111 Uiso 1 1 calc R . . . .
N8 N 0.2967(9) 0.9689(13) 0.6782(9) 0.076(6) Uani 1 1 d . . . . .
H8 H 0.2615 0.9762 0.6768 0.091 Uiso 1 1 calc R . . . .
C11 C 0.4724(9) 0.7762(14) 0.7506(9) 0.067(6) Uani 1 1 d . . . . .
H11A H 0.4571 0.7173 0.7573 0.101 Uiso 1 1 calc GR . . . .
H11B H 0.4568 0.8260 0.7666 0.101 Uiso 1 1 calc GR . . . .
H11C H 0.5142 0.7757 0.7688 0.101 Uiso 1 1 calc GR . . . .
C12 C 0.4558(8) 0.7911(13) 0.6878(9) 0.049(5) Uani 1 1 d . . . . .
C13 C 0.4129(8) 0.8498(12) 0.6505(8) 0.042(4) Uani 1 1 d . . . . .
C14 C 0.4132(7) 0.8364(12) 0.5962(9) 0.044(5) Uani 1 1 d . . . . .
C15 C 0.3801(10) 0.8785(14) 0.5422(10) 0.076(7) Uani 1 1 d . . . . .
H15A H 0.3958 0.9393 0.5399 0.115 Uiso 1 1 calc GR . . . .
H15B H 0.3401 0.8849 0.5391 0.115 Uiso 1 1 calc GR . . . .
H15C H 0.3819 0.8398 0.5113 0.115 Uiso 1 1 calc GR . . . .
C16 C 0.2742(10) 0.8264(18) 0.6205(11) 0.099(9) Uani 1 1 d . . . . .
H16A H 0.2806 0.7701 0.6432 0.148 Uiso 1 1 calc GR . . . .
H16B H 0.2809 0.8140 0.5855 0.148 Uiso 1 1 calc GR . . . .
H16C H 0.2347 0.8471 0.6113 0.148 Uiso 1 1 calc GR . . . .
C17 C 0.3152(10) 0.9007(13) 0.6540(10) 0.063(6) Uani 1 1 d . . . . .
C18 C 0.3748(9) 0.9138(12) 0.6683(9) 0.055(6) Uani 1 1 d . . . . .
C19 C 0.3897(12) 0.9948(15) 0.6975(12) 0.082(8) Uani 1 1 d . . . . .
C20 C 0.4437(15) 1.041(2) 0.7204(18) 0.19(2) Uani 1 1 d . . . . .
H20A H 0.4723 1.0080 0.7099 0.292 Uiso 1 1 calc R . . . .
H20B H 0.4397 1.1039 0.7053 0.292 Uiso 1 1 calc R . . . .
H20C H 0.4561 1.0438 0.7618 0.292 Uiso 1 1 calc R . . . .
N1 N 0.6749(7) -0.0814(9) 0.6983(7) 0.049(4) Uani 1 1 d . . . . .
H1 H 0.6726 -0.1352 0.7129 0.059 Uiso 1 1 calc R . . . .
N2 N 0.7181(6) -0.0555(9) 0.6834(6) 0.044(4) Uani 1 1 d . U . . .
H2 H 0.7486 -0.0886 0.6876 0.052 Uiso 1 1 calc R . . . .
N3 N 0.5500(7) 0.2355(10) 0.5909(6) 0.050(4) Uani 1 1 d . . . . .
H3 H 0.5168 0.2554 0.5675 0.060 Uiso 1 1 calc R . . . .
N4 N 0.5917(6) 0.2903(9) 0.6225(7) 0.042(4) Uani 1 1 d . . . . .
H4 H 0.5909 0.3506 0.6238 0.051 Uiso 1 1 calc R . . . .
C1 C 0.7469(11) 0.0809(19) 0.6384(14) 0.134(14) Uani 1 1 d . . . . .
H1A H 0.7758 0.1137 0.6695 0.201 Uiso 1 1 calc GR . . . .
H1B H 0.7245 0.1250 0.6097 0.201 Uiso 1 1 calc GR . . . .
H1C H 0.7658 0.0374 0.6214 0.201 Uiso 1 1 calc GR . . . .
C2 C 0.7080(8) 0.0298(12) 0.6607(8) 0.050(5) Uani 1 1 d . . . . .
C3 C 0.6545(7) 0.0573(11) 0.6629(7) 0.035(4) Uani 1 1 d . . . . .
C4 C 0.6361(8) -0.0167(12) 0.6885(8) 0.043(4) Uani 1 1 d . . . . .
C5 C 0.5844(9) -0.0234(13) 0.7032(10) 0.069(7) Uani 1 1 d . . . . .
H5A H 0.5637 -0.0802 0.6873 0.104 Uiso 1 1 calc GR . . . .
H5B H 0.5595 0.0295 0.6875 0.104 Uiso 1 1 calc GR . . . .
H5C H 0.5956 -0.0240 0.7444 0.104 Uiso 1 1 calc GR . . . .
C6 C 0.5247(9) 0.0689(12) 0.5671(9) 0.081(8) Uani 1 1 d . . . . .
H6A H 0.5434 0.0094 0.5792 0.121 Uiso 1 1 calc R . . . .
H6B H 0.4894 0.0713 0.5752 0.121 Uiso 1 1 calc R . . . .
H6C H 0.5155 0.0767 0.5264 0.121 Uiso 1 1 calc R . . . .
C7 C 0.5643(7) 0.1450(13) 0.5988(7) 0.042(4) Uani 1 1 d . . . . .
C8 C 0.6205(7) 0.1428(11) 0.6391(7) 0.034(4) Uani 1 1 d . . . . .
C9 C 0.6365(7) 0.2341(12) 0.6529(8) 0.040(4) Uani 1 1 d . . . . .
C10 C 0.6904(9) 0.2796(16) 0.6938(11) 0.096(9) Uani 1 1 d . . . . .
H10A H 0.7198 0.2328 0.7105 0.144 Uiso 1 1 calc GR . . . .
H10B H 0.6816 0.3108 0.7239 0.144 Uiso 1 1 calc GR . . . .
H10C H 0.7046 0.3246 0.6733 0.144 Uiso 1 1 calc GR . . . .
N9 N 0.0445(7) 0.9703(10) 0.4323(6) 0.043(4) Uani 1 1 d . . . . .
H9 H 0.0533 0.9840 0.4682 0.052 Uiso 1 1 calc R . . . .
N10 N -0.0072(7) 0.9461(11) 0.3959(7) 0.053(4) Uani 1 1 d . . . . .
H10 H -0.0375 0.9404 0.4051 0.063 Uiso 1 1 calc R . . . .
N11 N 0.1011(6) 0.8782(11) 0.2345(6) 0.046(4) Uani 1 1 d . . . . .
H11 H 0.1109 0.8390 0.2134 0.056 Uiso 1 1 calc R . . . .
N12 N 0.0980(6) 0.9694(11) 0.2264(6) 0.042(4) Uani 1 1 d . . . . .
H12 H 0.1062 0.9985 0.2000 0.051 Uiso 1 1 calc R . . . .
C21 C 0.1448(9) 0.9860(12) 0.4364(8) 0.058(6) Uani 1 1 d . . . . .
H21A H 0.1501 1.0210 0.4710 0.087 Uiso 1 1 calc GR . . . .
H21B H 0.1607 1.0206 0.4125 0.087 Uiso 1 1 calc GR . . . .
H21C H 0.1644 0.9267 0.4465 0.087 Uiso 1 1 calc GR . . . .
C22 C 0.0807(7) 0.9699(11) 0.4041(8) 0.036(4) Uani 1 1 d . . . . .
C23 C 0.0503(8) 0.9495(11) 0.3484(7) 0.037(4) Uani 1 1 d . . . . .
C24 C -0.0072(8) 0.9313(13) 0.3432(8) 0.044(5) Uani 1 1 d . . . . .
C25 C -0.0584(9) 0.9063(15) 0.2939(9) 0.070(6) Uani 1 1 d . . . . .
H25A H -0.0810 0.8610 0.3053 0.105 Uiso 1 1 calc GR . . . .
H25B H -0.0466 0.8800 0.2643 0.105 Uiso 1 1 calc GR . . . .
H25C H -0.0816 0.9613 0.2793 0.105 Uiso 1 1 calc GR . . . .
C26 C 0.0895(12) 0.7563(13) 0.3000(12) 0.108(11) Uani 1 1 d . . . . .
H26A H 0.1144 0.7531 0.3400 0.162 Uiso 1 1 calc GR . . . .
H26B H 0.1046 0.7163 0.2777 0.162 Uiso 1 1 calc GR . . . .
H26C H 0.0508 0.7361 0.2956 0.162 Uiso 1 1 calc GR . . . .
C27 C 0.0872(8) 0.8538(12) 0.2793(8) 0.047(5) Uani 1 1 d . . . . .
C28 C 0.0734(8) 0.9388(12) 0.3002(7) 0.040(4) Uani 1 1 d . . . . .
C29 C 0.0801(6) 1.0099(10) 0.2658(6) 0.027(3) Uani 1 1 d . . . . .
C30 C 0.0751(8) 1.1136(11) 0.2685(7) 0.046(5) Uani 1 1 d . . . . .
H30A H 0.0368 1.1298 0.2672 0.069 Uiso 1 1 calc GR . . . .
H30B H 0.0815 1.1415 0.2361 0.069 Uiso 1 1 calc GR . . . .
H30C H 0.1038 1.1365 0.3038 0.069 Uiso 1 1 calc GR . . . .
O6W O -0.1031(10) 0.1949(15) 0.3323(12) 0.055(7) Uani 0.5 1 d . . P . .
O2W O 0.6848(6) 0.7208(9) 0.6941(6) 0.067(4) Uani 1 1 d . . . . .
O1W O 0.5761(6) 0.6362(10) 0.6754(6) 0.076(5) Uani 1 1 d . . . . .
O3W O 0.7613(7) 0.6100(11) 0.7815(6) 0.082(5) Uani 1 1 d . . . . .
O4W O 0.4799(5) 0.6574(8) 0.5285(5) 0.047(3) Uani 1 1 d . . . . .
O5W O 0.0430(8) 0.8798(10) 0.5364(7) 0.095(6) Uani 1 1 d . . . . .
O6WA O -0.1726(10) 0.047(2) 0.3433(14) 0.077(9) Uani 0.5 1 d . . P . .
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
W1 0.0124(4) 0.0171(4) 0.0161(4) 0.0023(3) 0.0087(4) 0.0017(3)
W2 0.0221(3) 0.0207(3) 0.0240(3) 0.0000(3) 0.0098(3) -0.0005(2)
W3 0.0193(3) 0.0232(3) 0.0191(3) 0.0007(3) 0.0083(3) 0.0019(2)
W4 0.0316(4) 0.0315(4) 0.0310(4) -0.0021(3) 0.0120(3) -0.0003(3)
W5 0.0237(3) 0.0227(3) 0.0231(3) 0.0010(3) 0.0100(3) -0.0004(3)
W6 0.0215(3) 0.0299(3) 0.0193(3) 0.0015(3) 0.0077(3) 0.0015(3)
W7 0.0249(3) 0.0364(4) 0.0267(4) -0.0041(3) 0.0112(3) -0.0034(3)
W8 0.0222(3) 0.0325(3) 0.0239(4) 0.0040(3) 0.0090(3) 0.0024(3)
W9 0.0207(3) 0.0308(3) 0.0301(4) -0.0015(3) 0.0097(3) -0.0023(3)
W10 0.0250(3) 0.0249(3) 0.0312(4) 0.0020(3) 0.0139(3) -0.0001(3)
W11 0.0219(3) 0.0294(3) 0.0238(3) 0.0028(3) 0.0117(3) 0.0027(3)
W12 0.0232(3) 0.0284(3) 0.0258(4) -0.0010(3) 0.0104(3) 0.0014(3)
W13 0.0266(3) 0.0260(3) 0.0291(4) 0.0038(3) 0.0108(3) 0.0025(3)
W14 0.0191(3) 0.0288(3) 0.0309(4) 0.0054(3) 0.0145(3) 0.0020(3)
W15 0.0186(3) 0.0272(3) 0.0335(4) 0.0023(3) 0.0115(3) 0.0041(3)
W16 0.0163(3) 0.0333(3) 0.0291(4) 0.0039(3) 0.0094(3) 0.0030(3)
Co1 0.0124(4) 0.0171(4) 0.0161(4) 0.0023(3) 0.0087(4) 0.0017(3)
Co2 0.0152(9) 0.0210(10) 0.0166(10) -0.0013(8) 0.0078(8) 0.0004(8)
P1 0.0124(17) 0.0137(17) 0.0144(19) 0.0007(14) 0.0050(15) 0.0024(14)
P2 0.0129(17) 0.0194(18) 0.0175(19) 0.0007(15) 0.0078(15) 0.0012(15)
O1 0.031(6) 0.029(6) 0.038(7) 0.004(5) 0.015(5) 0.016(5)
O2 0.026(6) 0.031(6) 0.031(6) 0.004(5) 0.010(5) -0.007(5)
O3 0.013(5) 0.027(5) 0.040(7) 0.001(5) 0.014(5) 0.005(4)
O4 0.029(6) 0.021(5) 0.031(6) 0.007(4) 0.020(5) 0.009(4)
O5 0.017(5) 0.019(5) 0.027(6) -0.002(4) 0.000(4) 0.001(4)
O6 0.028(6) 0.020(5) 0.045(7) 0.009(5) 0.020(5) 0.002(4)
O7 0.023(5) 0.023(5) 0.025(6) 0.006(4) 0.016(5) 0.006(4)
O8 0.010(5) 0.018(5) 0.033(6) 0.007(4) 0.006(4) 0.001(4)
O9 0.018(5) 0.033(6) 0.012(5) 0.002(4) 0.006(4) 0.002(4)
O10 0.014(5) 0.025(5) 0.028(6) 0.000(4) 0.013(4) -0.002(4)
O11 0.019(5) 0.031(5) 0.018(5) 0.000(4) 0.010(4) 0.004(4)
O12 0.019(5) 0.027(5) 0.028(6) 0.006(4) 0.013(5) 0.002(4)
O13 0.008(5) 0.031(5) 0.028(6) -0.004(5) 0.003(4) -0.003(4)
O14 0.034(6) 0.027(6) 0.027(6) 0.000(5) 0.012(5) 0.006(5)
O15 0.037(6) 0.019(5) 0.041(7) 0.007(5) 0.013(6) 0.004(5)
O16 0.026(6) 0.040(6) 0.028(6) 0.012(5) 0.011(5) 0.009(5)
O17 0.026(6) 0.032(6) 0.041(7) -0.005(5) 0.017(5) -0.007(5)
O18 0.039(7) 0.032(6) 0.035(7) 0.003(5) 0.016(6) -0.008(5)
O19 0.029(6) 0.033(6) 0.024(6) 0.008(5) 0.010(5) 0.005(5)
O20 0.023(5) 0.021(5) 0.024(6) 0.007(4) 0.011(5) 0.008(4)
O21 0.019(5) 0.020(5) 0.026(6) 0.011(4) 0.008(5) 0.006(4)
O22 0.017(5) 0.020(5) 0.037(6) -0.002(4) 0.013(5) -0.001(4)
O23 0.016(5) 0.031(6) 0.023(6) 0.006(4) 0.006(4) 0.010(4)
O24 0.014(5) 0.022(5) 0.015(5) -0.001(4) 0.004(4) 0.001(4)
O25 0.015(5) 0.025(5) 0.021(5) 0.004(4) 0.007(4) -0.002(4)
O26 0.018(5) 0.017(5) 0.011(5) 0.004(4) 0.004(4) 0.002(4)
O27 0.024(5) 0.026(5) 0.022(6) -0.002(4) 0.015(5) 0.001(4)
O28 0.019(5) 0.028(5) 0.022(6) 0.002(4) 0.012(4) 0.004(4)
O29 0.020(5) 0.030(5) 0.023(6) 0.000(4) 0.009(5) 0.000(4)
O30 0.015(5) 0.023(5) 0.034(6) -0.002(4) 0.013(5) 0.000(4)
O31 0.013(5) 0.029(5) 0.012(5) 0.000(4) 0.005(4) 0.001(4)
O32 0.022(5) 0.029(5) 0.022(6) -0.001(4) 0.014(5) 0.005(4)
O33 0.006(4) 0.021(5) 0.032(6) -0.001(4) 0.010(4) -0.005(4)
O34 0.022(5) 0.023(5) 0.032(6) -0.001(4) 0.014(5) 0.003(4)
O35 0.027(6) 0.025(5) 0.034(6) 0.005(5) 0.019(5) 0.004(5)
O36 0.021(5) 0.021(5) 0.019(5) 0.000(4) 0.008(4) 0.004(4)
O37 0.032(6) 0.037(6) 0.019(6) -0.004(5) 0.007(5) -0.004(5)
O38 0.016(5) 0.030(5) 0.016(5) 0.002(4) 0.003(4) 0.011(4)
O39 0.027(6) 0.046(6) 0.005(5) 0.001(4) -0.001(4) -0.004(5)
O40 0.016(5) 0.017(5) 0.027(6) 0.000(4) 0.012(4) -0.006(4)
O41 0.014(5) 0.026(5) 0.023(6) 0.007(4) 0.006(4) 0.000(4)
O42 0.015(5) 0.023(5) 0.025(6) 0.000(4) 0.008(4) 0.004(4)
O43 0.026(6) 0.021(5) 0.030(6) -0.006(4) 0.013(5) -0.002(4)
O44 0.021(5) 0.021(5) 0.027(6) 0.006(4) 0.016(5) 0.001(4)
O45 0.019(5) 0.032(6) 0.018(5) 0.004(4) 0.010(4) 0.000(4)
O46 0.014(5) 0.025(5) 0.021(5) 0.002(4) 0.009(4) 0.005(4)
O47 0.019(5) 0.028(5) 0.020(5) -0.005(4) 0.011(4) 0.000(4)
O48 0.018(5) 0.023(5) 0.019(5) 0.000(4) 0.010(4) 0.003(4)
O49 0.022(5) 0.022(5) 0.017(5) 0.003(4) 0.012(4) 0.003(4)
O50 0.013(5) 0.027(5) 0.022(5) -0.002(4) 0.009(4) 0.000(4)
O51 0.018(5) 0.025(5) 0.020(5) -0.004(4) 0.009(4) -0.004(4)
O52 0.023(5) 0.012(5) 0.019(5) 0.006(4) 0.012(4) 0.001(4)
O53 0.021(5) 0.024(5) 0.021(6) 0.003(4) 0.013(5) -0.002(4)
O54 0.015(5) 0.022(5) 0.026(6) -0.002(4) 0.014(4) 0.002(4)
O55 0.022(5) 0.020(5) 0.028(6) 0.006(4) 0.015(5) 0.006(4)
O56 0.012(5) 0.029(5) 0.022(6) -0.005(4) 0.005(4) 0.001(4)
O57 0.030(6) 0.036(6) 0.025(6) 0.005(5) 0.022(5) 0.006(5)
N5 0.039(9) 0.051(10) 0.082(14) -0.015(9) 0.027(10) 0.004(8)
N6 0.027(8) 0.071(11) 0.053(11) -0.009(9) 0.021(8) 0.007(8)
N7 0.14(2) 0.057(12) 0.13(2) -0.014(12) 0.101(18) -0.004(13)
N8 0.096(16) 0.065(12) 0.100(16) 0.040(11) 0.076(14) 0.043(12)
C11 0.067(15) 0.066(14) 0.080(17) -0.014(12) 0.040(14) -0.002(12)
C12 0.036(11) 0.059(12) 0.057(14) -0.021(11) 0.022(10) -0.018(10)
C13 0.038(10) 0.044(10) 0.044(12) 0.008(9) 0.016(9) -0.001(9)
C14 0.028(9) 0.044(11) 0.072(15) 0.003(10) 0.030(10) -0.001(8)
C15 0.10(2) 0.065(15) 0.078(18) 0.000(13) 0.048(16) 0.012(14)
C16 0.055(16) 0.12(2) 0.11(2) -0.043(18) 0.014(15) -0.004(16)
C17 0.080(16) 0.044(12) 0.092(18) 0.024(11) 0.065(15) 0.026(12)
C18 0.058(13) 0.039(11) 0.095(17) 0.000(11) 0.058(13) 0.007(10)
C19 0.10(2) 0.046(13) 0.14(2) -0.016(14) 0.09(2) -0.006(13)
C20 0.17(3) 0.17(3) 0.33(6) -0.17(4) 0.19(4) -0.10(3)
N1 0.056(10) 0.028(8) 0.068(11) 0.017(7) 0.030(9) 0.016(7)
N2 0.039(5) 0.043(5) 0.049(5) 0.004(4) 0.017(4) 0.011(4)
N3 0.048(10) 0.038(9) 0.051(10) 0.010(8) 0.004(8) 0.027(8)
N4 0.037(9) 0.018(7) 0.071(11) 0.002(7) 0.019(8) 0.005(6)
C1 0.10(2) 0.14(3) 0.21(4) 0.11(2) 0.10(2) 0.041(19)
C2 0.068(13) 0.042(10) 0.057(13) 0.024(9) 0.044(11) 0.042(10)
C3 0.039(10) 0.030(9) 0.036(10) 0.001(8) 0.013(8) 0.014(8)
C4 0.038(10) 0.042(10) 0.053(12) 0.005(9) 0.021(9) 0.010(9)
C5 0.065(14) 0.042(12) 0.12(2) 0.043(12) 0.049(15) 0.025(10)
C6 0.078(16) 0.035(11) 0.076(16) -0.008(11) -0.034(13) 0.018(11)
C7 0.032(10) 0.059(12) 0.025(10) -0.006(9) -0.003(8) -0.002(9)
C8 0.034(9) 0.031(9) 0.038(10) -0.004(8) 0.013(8) 0.006(8)
C9 0.019(8) 0.048(11) 0.049(12) -0.002(9) 0.009(8) 0.011(8)
C10 0.047(14) 0.081(18) 0.13(2) -0.014(16) -0.006(15) 0.003(13)
N9 0.061(11) 0.058(10) 0.022(8) 0.004(7) 0.028(8) 0.011(8)
N10 0.050(10) 0.078(12) 0.042(10) 0.004(9) 0.032(9) 0.011(9)
N11 0.051(10) 0.056(10) 0.048(10) -0.019(8) 0.038(8) -0.016(8)
N12 0.039(9) 0.063(10) 0.031(9) -0.002(7) 0.020(7) -0.014(8)
C21 0.099(18) 0.033(10) 0.054(13) -0.014(9) 0.044(13) -0.017(11)
C22 0.039(10) 0.030(9) 0.052(12) -0.005(8) 0.032(10) 0.000(8)
C23 0.046(11) 0.036(9) 0.036(11) 0.010(8) 0.024(9) 0.001(8)
C24 0.047(11) 0.063(12) 0.029(10) 0.006(9) 0.023(9) 0.003(10)
C25 0.056(14) 0.097(17) 0.064(15) 0.020(13) 0.031(13) 0.001(13)
C26 0.16(3) 0.042(13) 0.20(3) 0.022(15) 0.15(3) 0.000(14)
C27 0.053(12) 0.044(11) 0.060(13) -0.008(9) 0.040(11) -0.008(9)
C28 0.054(11) 0.044(10) 0.031(10) 0.003(8) 0.028(9) 0.004(9)
C29 0.028(8) 0.031(9) 0.021(8) -0.002(7) 0.006(7) -0.004(7)
C30 0.050(12) 0.048(11) 0.039(11) -0.006(9) 0.015(9) 0.003(9)
O6W 0.030(14) 0.037(14) 0.08(2) 0.004(13) 0.005(14) 0.017(11)
O2W 0.084(11) 0.065(9) 0.065(10) -0.017(7) 0.045(9) 0.003(8)
O1W 0.071(10) 0.110(12) 0.051(9) -0.003(8) 0.027(8) 0.037(9)
O3W 0.094(12) 0.104(12) 0.074(11) -0.037(9) 0.059(10) -0.053(10)
O4W 0.041(7) 0.048(7) 0.057(9) -0.010(6) 0.025(7) -0.009(6)
O5W 0.157(17) 0.083(11) 0.081(12) -0.039(9) 0.085(12) -0.064(11)
O6WA 0.022(14) 0.09(2) 0.13(3) 0.028(19) 0.040(17) -0.003(14)
_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
W1 O51 2.316(8) 3_566 ?
W1 O52 2.047(8) . ?
W1 O54 1.987(9) . ?
W1 O55 1.896(9) . ?
W1 O56 1.846(8) . ?
W1 O57 1.694(9) . ?
W2 O34 1.909(9) . ?
W2 O35 1.692(9) . ?
W2 O36 1.896(9) . ?
W2 O46 1.897(9) . ?
W2 O48 2.351(9) . ?
W2 O54 1.983(8) . ?
W3 O32 1.959(8) . ?
W3 O44 1.903(9) . ?
W3 O45 1.697(9) . ?
W3 O46 1.886(9) . ?
W3 O49 2.323(9) . ?
W3 O52 1.951(8) . ?
W4 O31 2.063(8) . ?
W4 O42 1.927(9) . ?
W4 O43 1.691(9) . ?
W4 O44 1.917(9) . ?
W4 O49 2.364(9) . ?
W4 O50 1.778(8) . ?
W5 O29 1.831(9) . ?
W5 O40 1.918(9) . ?
W5 O41 1.716(9) . ?
W5 O42 1.850(9) . ?
W5 O47 2.356(9) . ?
W5 O56 2.021(8) 3_566 ?
W6 O30 1.888(8) . ?
W6 O38 1.867(9) . ?
W6 O39 1.696(9) . ?
W6 O40 1.921(8) . ?
W6 O47 2.369(9) . ?
W6 O55 1.976(9) 3_566 ?
W7 O33 2.036(8) . ?
W7 O36 1.949(9) . ?
W7 O37 1.711(9) . ?
W7 O38 1.906(9) . ?
W7 O48 2.383(9) . ?
W7 O53 1.786(9) . ?
W8 O11 1.903(8) . ?
W8 O16 1.702(10) . ?
W8 O20 1.909(9) . ?
W8 O21 1.891(9) . ?
W8 O26 2.343(8) . ?
W8 O30 1.921(8) . ?
W9 O13 2.018(9) . ?
W9 O17 1.707(10) . ?
W9 O21 1.905(8) . ?
W9 O22 1.935(9) . ?
W9 O27 2.371(9) . ?
W9 O33 1.797(8) . ?
W10 O12 1.948(9) . ?
W10 O18 1.693(9) . ?
W10 O22 1.885(10) . ?
W10 O23 1.900(10) . ?
W10 O27 2.378(9) . ?
W10 O34 1.877(9) . ?
W11 O9 1.965(9) . ?
W11 O19 1.702(9) . ?
W11 O23 1.886(9) . ?
W11 O24 1.920(8) . ?
W11 O28 2.398(9) . ?
W11 O32 1.815(9) . ?
W12 O7 2.073(9) . ?
W12 O14 1.733(9) . ?
W12 O24 1.895(8) . ?
W12 O25 1.925(9) . ?
W12 O28 2.315(9) . ?
W12 O31 1.805(8) . ?
W13 O8 1.895(8) . ?
W13 O15 1.694(9) . ?
W13 O20 1.888(9) . ?
W13 O25 1.846(9) . ?
W13 O26 2.380(8) . ?
W13 O29 1.977(9) . ?
W14 O4 1.954(9) . ?
W14 O5 1.969(9) . ?
W14 O6 1.710(9) . ?
W14 O9 1.862(9) . ?
W14 O10 2.389(8) . ?
W14 O12 1.876(9) . ?
W15 O1 1.719(9) . ?
W15 O3 1.964(10) . ?
W15 O4 1.922(9) . ?
W15 O7 1.823(9) . ?
W15 O8 1.928(9) . ?
W15 O10 2.402(9) . ?
W16 O2 1.701(10) . ?
W16 O3 1.958(9) . ?
W16 O5 1.922(9) . ?
W16 O10 2.358(9) . ?
W16 O11 1.933(9) . ?
W16 O13 1.825(9) . ?
Co2 O50 1.993(9) . ?
Co2 O51 2.178(9) . ?
Co2 O51 2.176(9) 3_566 ?
Co2 O52 2.126(8) . ?
Co2 O53 1.994(9) 3_566 ?
Co2 O54 2.140(9) 3_566 ?
P1 O47 1.515(10) . ?
P1 O48 1.527(9) . ?
P1 O49 1.533(9) . ?
P1 O51 1.583(9) . ?
P2 O10 1.572(9) . ?
P2 O26 1.517(9) . ?
P2 O27 1.510(9) . ?
P2 O28 1.518(10) . ?
O51 W1 2.316(8) 3_566 ?
O51 Co1 2.316(8) 3_566 ?
O51 Co2 2.176(9) 3_566 ?
O53 Co2 1.994(9) 3_566 ?
O54 Co2 2.140(9) 3_566 ?
O55 W6 1.976(9) 3_566 ?
O56 W5 2.021(8) 3_566 ?
N5 N6 1.34(2) . ?
N5 C12 1.30(2) . ?
N6 C14 1.32(2) . ?
N7 N8 1.33(3) . ?
N7 C19 1.33(3) . ?
N8 C17 1.31(2) . ?
C11 C12 1.48(3) . ?
C12 C13 1.40(2) . ?
C13 C14 1.36(2) . ?
C13 C18 1.48(2) . ?
C14 C15 1.42(3) . ?
C16 C17 1.49(3) . ?
C17 C18 1.39(3) . ?
C18 C19 1.34(3) . ?
C19 C20 1.41(3) . ?
N1 N2 1.300(17) . ?
N1 C4 1.285(19) . ?
N2 C2 1.325(19) . ?
N3 N4 1.301(19) . ?
N3 C7 1.33(2) . ?
N4 C9 1.350(19) . ?
C1 C2 1.46(3) . ?
C2 C3 1.39(2) . ?
C3 C4 1.39(2) . ?
C3 C8 1.47(2) . ?
C4 C5 1.45(2) . ?
C6 C7 1.48(2) . ?
C7 C8 1.38(2) . ?
C8 C9 1.37(2) . ?
C9 C10 1.49(3) . ?
N9 N10 1.309(19) . ?
N9 C22 1.320(18) . ?
N10 C24 1.33(2) . ?
N11 N12 1.314(18) . ?
N11 C27 1.32(2) . ?
N12 C29 1.343(18) . ?
C21 C22 1.50(2) . ?
C22 C23 1.34(2) . ?
C23 C24 1.40(2) . ?
C23 C28 1.51(2) . ?
C24 C25 1.44(3) . ?
C26 C27 1.48(2) . ?
C27 C28 1.41(2) . ?
C28 C29 1.38(2) . ?
C29 C30 1.49(2) . ?
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
O52 W1 O51 78.0(3) . 3_566 ?
O54 W1 O51 78.0(3) . 3_566 ?
O54 W1 O52 81.5(3) . . ?
O55 W1 O51 82.3(3) . 3_566 ?
O55 W1 O52 87.4(4) . . ?
O55 W1 O54 159.0(4) . . ?
O56 W1 O51 83.5(3) . 3_566 ?
O56 W1 O52 161.3(4) . . ?
O56 W1 O54 92.2(4) . . ?
O56 W1 O55 92.7(4) . . ?
O57 W1 O51 175.3(4) . 3_566 ?
O57 W1 O52 97.7(4) . . ?
O57 W1 O54 99.8(4) . . ?
O57 W1 O55 99.3(4) . . ?
O57 W1 O56 100.8(4) . . ?
O34 W2 O48 85.3(3) . . ?
O34 W2 O54 165.2(4) . . ?
O35 W2 O34 98.6(4) . . ?
O35 W2 O36 99.8(4) . . ?
O35 W2 O46 103.6(4) . . ?
O35 W2 O48 173.1(4) . . ?
O35 W2 O54 95.5(4) . . ?
O36 W2 O34 89.7(4) . . ?
O36 W2 O46 156.6(4) . . ?
O36 W2 O48 74.4(3) . . ?
O36 W2 O54 92.1(4) . . ?
O46 W2 O34 87.4(4) . . ?
O46 W2 O48 82.2(3) . . ?
O46 W2 O54 85.1(4) . . ?
O54 W2 O48 81.1(3) . . ?
O32 W3 O49 83.7(3) . . ?
O44 W3 O32 88.4(4) . . ?
O44 W3 O49 73.9(4) . . ?
O44 W3 O52 92.1(3) . . ?
O45 W3 O32 94.8(4) . . ?
O45 W3 O44 100.6(4) . . ?
O45 W3 O46 102.1(4) . . ?
O45 W3 O49 174.4(4) . . ?
O45 W3 O52 99.3(4) . . ?
O46 W3 O32 86.2(4) . . ?
O46 W3 O44 157.0(4) . . ?
O46 W3 O49 83.3(3) . . ?
O46 W3 O52 87.9(3) . . ?
O52 W3 O32 165.6(4) . . ?
O52 W3 O49 82.6(3) . . ?
O31 W4 O49 81.7(3) . . ?
O42 W4 O31 84.2(3) . . ?
O42 W4 O49 83.0(3) . . ?
O43 W4 O31 95.8(4) . . ?
O43 W4 O42 101.6(4) . . ?
O43 W4 O44 102.3(4) . . ?
O43 W4 O49 174.6(4) . . ?
O43 W4 O50 99.9(4) . . ?
O44 W4 O31 84.9(3) . . ?
O44 W4 O42 154.6(4) . . ?
O44 W4 O49 72.7(4) . . ?
O50 W4 O31 164.2(4) . . ?
O50 W4 O42 91.9(4) . . ?
O50 W4 O44 92.5(4) . . ?
O50 W4 O49 82.7(3) . . ?
O29 W5 O40 89.7(4) . . ?
O29 W5 O42 94.1(4) . . ?
O29 W5 O47 88.2(4) . . ?
O29 W5 O56 163.9(4) . 3_566 ?
O40 W5 O47 74.1(3) . . ?
O40 W5 O56 82.4(4) . 3_566 ?
O41 W5 O29 101.1(4) . . ?
O41 W5 O40 99.6(4) . . ?
O41 W5 O42 101.0(4) . . ?
O41 W5 O47 168.8(3) . . ?
O41 W5 O56 94.1(4) . 3_566 ?
O42 W5 O40 157.8(4) . . ?
O42 W5 O47 84.2(3) . . ?
O42 W5 O56 88.1(4) . 3_566 ?
O56 W5 O47 76.1(3) 3_566 . ?
O30 W6 O40 88.5(4) . . ?
O30 W6 O47 86.1(4) . . ?
O30 W6 O55 163.1(4) . 3_566 ?
O38 W6 O30 91.4(4) . . ?
O38 W6 O40 158.8(4) . . ?
O38 W6 O47 85.1(3) . . ?
O38 W6 O55 88.6(4) . 3_566 ?
O39 W6 O30 99.0(4) . . ?
O39 W6 O38 101.6(4) . . ?
O39 W6 O40 99.3(4) . . ?
O39 W6 O47 171.3(4) . . ?
O39 W6 O55 97.5(4) . 3_566 ?
O40 W6 O47 73.7(3) . . ?
O40 W6 O55 85.5(4) . 3_566 ?
O55 W6 O47 77.0(3) 3_566 . ?
O33 W7 O48 80.1(3) . . ?
O36 W7 O33 84.8(4) . . ?
O36 W7 O48 72.8(3) . . ?
O37 W7 O33 96.5(4) . . ?
O37 W7 O36 101.8(4) . . ?
O37 W7 O38 101.3(4) . . ?
O37 W7 O48 173.8(4) . . ?
O37 W7 O53 100.7(4) . . ?
O38 W7 O33 85.8(4) . . ?
O38 W7 O36 155.9(4) . . ?
O38 W7 O48 83.7(3) . . ?
O53 W7 O33 162.7(4) . . ?
O53 W7 O36 89.8(4) . . ?
O53 W7 O38 92.7(4) . . ?
O53 W7 O48 82.6(3) . . ?
O11 W8 O20 91.2(4) . . ?
O11 W8 O26 81.8(3) . . ?
O11 W8 O30 164.1(4) . . ?
O16 W8 O11 98.0(4) . . ?
O16 W8 O20 98.4(4) . . ?
O16 W8 O21 103.2(4) . . ?
O16 W8 O26 171.3(4) . . ?
O16 W8 O30 97.7(4) . . ?
O20 W8 O26 72.9(3) . . ?
O20 W8 O30 88.7(4) . . ?
O21 W8 O11 87.6(4) . . ?
O21 W8 O20 158.3(4) . . ?
O21 W8 O26 85.5(3) . . ?
O21 W8 O30 86.6(4) . . ?
O30 W8 O26 83.0(3) . . ?
O13 W9 O27 79.6(3) . . ?
O17 W9 O13 96.6(4) . . ?
O17 W9 O21 100.8(4) . . ?
O17 W9 O22 100.1(4) . . ?
O17 W9 O27 172.1(4) . . ?
O17 W9 O33 101.6(4) . . ?
O21 W9 O13 82.0(4) . . ?
O21 W9 O22 157.0(4) . . ?
O21 W9 O27 85.6(4) . . ?
O22 W9 O13 86.1(4) . . ?
O22 W9 O27 72.9(3) . . ?
O33 W9 O13 161.5(4) . . ?
O33 W9 O21 91.7(4) . . ?
O33 W9 O22 93.5(4) . . ?
O33 W9 O27 82.6(4) . . ?
O12 W10 O27 81.6(3) . . ?
O18 W10 O12 96.6(4) . . ?
O18 W10 O22 100.3(4) . . ?
O18 W10 O23 102.3(4) . . ?
O18 W10 O27 173.6(4) . . ?
O18 W10 O34 100.8(4) . . ?
O22 W10 O12 88.2(4) . . ?
O22 W10 O23 156.9(4) . . ?
O22 W10 O27 73.5(3) . . ?
O23 W10 O12 84.4(4) . . ?
O23 W10 O27 83.7(4) . . ?
O34 W10 O12 162.5(4) . . ?
O34 W10 O22 91.0(4) . . ?
O34 W10 O23 89.5(4) . . ?
O34 W10 O27 81.4(3) . . ?
O9 W11 O28 80.6(3) . . ?
O19 W11 O9 97.3(4) . . ?
O19 W11 O23 103.1(4) . . ?
O19 W11 O24 99.6(4) . . ?
O19 W11 O28 171.9(4) . . ?
O19 W11 O32 101.7(4) . . ?
O23 W11 O9 84.1(4) . . ?
O23 W11 O24 156.2(4) . . ?
O23 W11 O28 84.6(3) . . ?
O24 W11 O9 86.0(4) . . ?
O24 W11 O28 72.5(3) . . ?
O32 W11 O9 160.9(4) . . ?
O32 W11 O23 90.2(4) . . ?
O32 W11 O24 92.1(4) . . ?
O32 W11 O28 80.7(3) . . ?
O7 W12 O28 80.1(3) . . ?
O14 W12 O7 92.4(4) . . ?
O14 W12 O24 99.9(4) . . ?
O14 W12 O25 99.4(4) . . ?
O14 W12 O28 171.2(4) . . ?
O14 W12 O31 101.4(4) . . ?
O24 W12 O7 85.2(3) . . ?
O24 W12 O25 156.7(4) . . ?
O24 W12 O28 74.9(3) . . ?
O25 W12 O7 81.0(3) . . ?
O25 W12 O28 84.2(3) . . ?
O31 W12 O7 165.8(4) . . ?
O31 W12 O24 95.4(4) . . ?
O31 W12 O25 93.5(4) . . ?
O31 W12 O28 86.4(3) . . ?
O8 W13 O26 82.1(3) . . ?
O8 W13 O29 164.2(4) . . ?
O15 W13 O8 99.6(4) . . ?
O15 W13 O20 101.3(4) . . ?
O15 W13 O25 103.2(4) . . ?
O15 W13 O26 173.6(4) . . ?
O15 W13 O29 96.0(4) . . ?
O20 W13 O8 91.3(4) . . ?
O20 W13 O26 72.4(3) . . ?
O20 W13 O29 88.4(4) . . ?
O25 W13 O8 88.4(4) . . ?
O25 W13 O20 155.2(4) . . ?
O25 W13 O26 83.0(3) . . ?
O25 W13 O29 85.3(4) . . ?
O29 W13 O26 82.7(3) . . ?
O4 W14 O5 85.7(4) . . ?
O4 W14 O10 73.3(3) . . ?
O5 W14 O10 73.1(3) . . ?
O6 W14 O4 99.2(4) . . ?
O6 W14 O5 100.6(4) . . ?
O6 W14 O9 102.2(4) . . ?
O6 W14 O10 170.3(4) . . ?
O6 W14 O12 102.8(4) . . ?
O9 W14 O4 89.4(4) . . ?
O9 W14 O5 157.1(4) . . ?
O9 W14 O10 84.1(3) . . ?
O9 W14 O12 89.3(4) . . ?
O12 W14 O4 157.8(4) . . ?
O12 W14 O5 86.9(4) . . ?
O12 W14 O10 84.5(3) . . ?
O1 W15 O3 101.3(4) . . ?
O1 W15 O4 99.8(4) . . ?
O1 W15 O7 103.7(4) . . ?
O1 W15 O8 102.3(4) . . ?
O1 W15 O10 170.4(4) . . ?
O3 W15 O10 71.5(3) . . ?
O4 W15 O3 84.8(4) . . ?
O4 W15 O8 157.4(4) . . ?
O4 W15 O10 73.5(3) . . ?
O7 W15 O3 154.9(4) . . ?
O7 W15 O4 90.7(4) . . ?
O7 W15 O8 88.5(4) . . ?
O7 W15 O10 83.5(3) . . ?
O8 W15 O3 86.5(4) . . ?
O8 W15 O10 83.9(3) . . ?
O2 W16 O3 98.5(4) . . ?
O2 W16 O5 99.9(4) . . ?
O2 W16 O10 169.7(4) . . ?
O2 W16 O11 100.6(4) . . ?
O2 W16 O13 103.4(4) . . ?
O3 W16 O10 72.6(3) . . ?
O5 W16 O3 85.9(4) . . ?
O5 W16 O10 74.6(3) . . ?
O5 W16 O11 159.0(4) . . ?
O11 W16 O3 86.8(4) . . ?
O11 W16 O10 84.4(3) . . ?
O13 W16 O3 158.0(4) . . ?
O13 W16 O5 92.4(4) . . ?
O13 W16 O10 85.8(3) . . ?
O13 W16 O11 87.0(4) . . ?
O50 Co2 O51 90.3(3) . . ?
O50 Co2 O51 175.9(4) . 3_566 ?
O50 Co2 O52 100.0(3) . . ?
O50 Co2 O53 91.0(4) . 3_566 ?
O50 Co2 O54 89.9(3) . 3_566 ?
O51 Co2 O51 85.6(3) 3_566 . ?
O52 Co2 O51 79.6(3) . 3_566 ?
O52 Co2 O51 90.5(3) . . ?
O52 Co2 O54 164.9(3) . 3_566 ?
O53 Co2 O51 93.1(3) 3_566 3_566 ?
O53 Co2 O51 178.4(3) 3_566 . ?
O53 Co2 O52 90.3(3) 3_566 . ?
O53 Co2 O54 101.0(3) 3_566 3_566 ?
O54 Co2 O51 89.7(3) 3_566 3_566 ?
O54 Co2 O51 78.0(3) 3_566 . ?
O47 P1 O48 111.0(5) . . ?
O47 P1 O49 110.8(5) . . ?
O47 P1 O51 107.7(5) . . ?
O48 P1 O49 111.7(5) . . ?
O48 P1 O51 108.1(5) . . ?
O49 P1 O51 107.2(5) . . ?
O26 P2 O10 105.9(5) . . ?
O26 P2 O28 111.7(5) . . ?
O27 P2 O10 106.9(5) . . ?
O27 P2 O26 113.2(5) . . ?
O27 P2 O28 111.2(5) . . ?
O28 P2 O10 107.4(5) . . ?
W16 O3 W15 123.0(5) . . ?
W15 O4 W14 122.6(4) . . ?
W16 O5 W14 121.2(5) . . ?
W15 O7 W12 151.5(5) . . ?
W13 O8 W15 146.9(5) . . ?
W14 O9 W11 149.7(5) . . ?
W14 O10 W15 90.4(3) . . ?
W16 O10 W14 91.1(3) . . ?
W16 O10 W15 92.8(3) . . ?
P2 O10 W14 124.3(5) . . ?
P2 O10 W15 124.5(5) . . ?
P2 O10 W16 123.9(5) . . ?
W8 O11 W16 147.2(5) . . ?
W14 O12 W10 149.0(5) . . ?
W16 O13 W9 152.7(5) . . ?
W13 O20 W8 124.2(5) . . ?
W8 O21 W9 152.3(5) . . ?
W10 O22 W9 122.8(5) . . ?
W11 O23 W10 154.9(5) . . ?
W12 O24 W11 121.5(4) . . ?
W13 O25 W12 155.4(5) . . ?
W8 O26 W13 90.5(3) . . ?
P2 O26 W8 128.9(5) . . ?
P2 O26 W13 128.2(5) . . ?
W9 O27 W10 89.9(3) . . ?
P2 O27 W9 128.9(5) . . ?
P2 O27 W10 129.5(5) . . ?
W12 O28 W11 89.8(3) . . ?
P2 O28 W11 127.8(5) . . ?
P2 O28 W12 130.4(5) . . ?
W5 O29 W13 164.4(6) . . ?
W6 O30 W8 164.4(5) . . ?
W12 O31 W4 165.2(5) . . ?
W11 O32 W3 164.3(5) . . ?
W9 O33 W7 163.7(5) . . ?
W10 O34 W2 164.0(6) . . ?
W2 O36 W7 122.2(4) . . ?
W6 O38 W7 153.5(5) . . ?
W5 O40 W6 121.6(4) . . ?
W5 O42 W4 155.4(5) . . ?
W3 O44 W4 122.2(5) . . ?
W3 O46 W2 153.6(5) . . ?
W5 O47 W6 90.4(3) . . ?
P1 O47 W5 129.5(5) . . ?
P1 O47 W6 128.3(5) . . ?
W2 O48 W7 90.6(3) . . ?
P1 O48 W2 130.7(5) . . ?
P1 O48 W7 128.2(5) . . ?
W3 O49 W4 91.1(3) . . ?
P1 O49 W3 130.0(5) . . ?
P1 O49 W4 127.8(5) . . ?
W4 O50 Co2 135.6(5) . . ?
W1 O51 Co1 0.00(5) 3_566 3_566 ?
Co2 O51 W1 95.9(3) 3_566 3_566 ?
Co2 O51 W1 95.7(3) . 3_566 ?
Co2 O51 Co1 95.7(3) . 3_566 ?
Co2 O51 Co1 95.9(3) 3_566 3_566 ?
Co2 O51 Co2 94.4(3) 3_566 . ?
P1 O51 W1 123.5(5) . 3_566 ?
P1 O51 Co1 123.5(5) . 3_566 ?
P1 O51 Co2 121.2(5) . . ?
P1 O51 Co2 119.6(5) . 3_566 ?
W1 O52 Co2 106.1(4) . . ?
W3 O52 W1 124.4(4) . . ?
W3 O52 Co2 126.8(4) . . ?
W7 O53 Co2 135.4(5) . 3_566 ?
W1 O54 Co2 107.6(4) . 3_566 ?
W2 O54 W1 125.9(4) . . ?
W2 O54 Co2 125.2(5) . 3_566 ?
W1 O55 W6 141.3(5) . 3_566 ?
W1 O56 W5 144.2(5) . 3_566 ?
C12 N5 N6 109.1(17) . . ?
C14 N6 N5 110.3(15) . . ?
N8 N7 C19 110.7(19) . . ?
C17 N8 N7 108.2(19) . . ?
N5 C12 C11 124(2) . . ?
N5 C12 C13 106.8(18) . . ?
C13 C12 C11 129.4(17) . . ?
C12 C13 C18 125.2(17) . . ?
C14 C13 C12 107.1(16) . . ?
C14 C13 C18 127.7(17) . . ?
N6 C14 C13 106.6(17) . . ?
N6 C14 C15 121.7(18) . . ?
C13 C14 C15 131.6(17) . . ?
N8 C17 C16 121(2) . . ?
N8 C17 C18 107(2) . . ?
C18 C17 C16 132.3(18) . . ?
C17 C18 C13 124.2(18) . . ?
C19 C18 C13 127.8(19) . . ?
C19 C18 C17 107.9(18) . . ?
N7 C19 C18 106(2) . . ?
N7 C19 C20 123(2) . . ?
C18 C19 C20 131(2) . . ?
C4 N1 N2 111.7(14) . . ?
N1 N2 C2 109.7(14) . . ?
N4 N3 C7 112.6(14) . . ?
N3 N4 C9 106.5(13) . . ?
N2 C2 C1 124.9(17) . . ?
N2 C2 C3 106.0(15) . . ?
C3 C2 C1 129.2(17) . . ?
C2 C3 C8 128.6(15) . . ?
C4 C3 C2 105.9(14) . . ?
C4 C3 C8 125.3(15) . . ?
N1 C4 C3 106.8(14) . . ?
N1 C4 C5 124.3(16) . . ?
C3 C4 C5 128.9(15) . . ?
N3 C7 C6 123.0(16) . . ?
N3 C7 C8 105.7(15) . . ?
C8 C7 C6 131.3(17) . . ?
C7 C8 C3 125.6(16) . . ?
C9 C8 C3 128.1(16) . . ?
C9 C8 C7 106.4(15) . . ?
N4 C9 C8 108.9(15) . . ?
N4 C9 C10 117.6(17) . . ?
C8 C9 C10 133.5(17) . . ?
N10 N9 C22 107.8(14) . . ?
N9 N10 C24 112.1(14) . . ?
N12 N11 C27 111.8(14) . . ?
N11 N12 C29 109.2(13) . . ?
N9 C22 C21 119.6(17) . . ?
N9 C22 C23 108.6(16) . . ?
C23 C22 C21 131.7(15) . . ?
C22 C23 C24 107.4(14) . . ?
C22 C23 C28 127.5(16) . . ?
C24 C23 C28 124.8(16) . . ?
N10 C24 C23 104.1(16) . . ?
N10 C24 C25 124.3(17) . . ?
C23 C24 C25 131.5(16) . . ?
N11 C27 C26 123.4(16) . . ?
N11 C27 C28 104.8(15) . . ?
C28 C27 C26 131.8(16) . . ?
C27 C28 C23 126.2(14) . . ?
C29 C28 C23 125.7(14) . . ?
C29 C28 C27 107.8(14) . . ?
N12 C29 C28 106.4(14) . . ?
N12 C29 C30 121.0(14) . . ?
C28 C29 C30 132.5(14) . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
p.res created by SHELXL-2014/7
TITL Integration of 150521d
CELL 0.71 24.5917 14.2596 24.8461 90 111.4003 90
ZERR 2 0.0029 0.0017 0.0029 0 0.001 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Co N O P W
UNIT 120 192 6 48 252 8 62
ISOR 0.005 0.2 N2
EADP Co1 W1
EXYZ Co1 W1
L.S. 7 0 0
PLAN 30
SIZE 0.05 0.1 0.08
TEMP 25
fmap 2 53
acta
OMIT -3 52
OMIT 1 2 7
OMIT -5 1 4
OMIT 1 3 2
OMIT -3 2 3
OMIT -9 0 10
OMIT 1 5 2
OMIT -3 0 4
OMIT 4 1 0
OMIT -1 0 6
OMIT 3 1 1
OMIT 0 1 4
OMIT -3 1 1
OMIT -5 2 2
OMIT -7 3 8
OMIT -5 5 6
OMIT -6 0 8
OMIT -3 3 7
REM
REM
REM
WGHT 0.038100 7.888500
FVAR 0.04179
W1 7 -0.022373 0.650980 0.414853 10.50000 0.01243 0.01709 =
0.01607 0.00234 0.00870 0.00165
W2 7 0.130337 0.668815 0.488552 11.00000 0.02209 0.02069 =
0.02397 0.00001 0.00983 -0.00053
W3 7 0.066863 0.495713 0.372433 11.00000 0.01931 0.02317 =
0.01908 0.00068 0.00828 0.00186
W4 7 0.056212 0.269995 0.403866 11.00000 0.03156 0.03152 =
0.03099 -0.00205 0.01201 -0.00028
W5 7 0.125660 0.190157 0.554901 11.00000 0.02371 0.02267 =
0.02307 0.00102 0.01004 -0.00040
W6 7 0.180631 0.347775 0.661056 11.00000 0.02150 0.02986 =
0.01929 0.00149 0.00771 0.00145
W7 7 0.177970 0.599010 0.627464 11.00000 0.02486 0.03635 =
0.02666 -0.00407 0.01125 -0.00344
W8 7 0.329225 0.314012 0.651988 11.00000 0.02220 0.03251 =
0.02393 0.00395 0.00896 0.00242
W9 7 0.326912 0.565571 0.617075 11.00000 0.02071 0.03077 =
0.03008 -0.00151 0.00974 -0.00232
W10 7 0.277601 0.635310 0.478615 11.00000 0.02502 0.02486 =
0.03123 0.00198 0.01391 -0.00011
W11 7 0.213519 0.461862 0.362071 11.00000 0.02187 0.02937 =
0.02377 0.00285 0.01175 0.00273
W12 7 0.207876 0.237145 0.395821 11.00000 0.02320 0.02841 =
0.02583 -0.00096 0.01045 0.00143
W13 7 0.274360 0.155065 0.546374 11.00000 0.02662 0.02596 =
0.02908 0.00377 0.01076 0.00248
W14 7 0.373039 0.468781 0.441515 11.00000 0.01910 0.02875 =
0.03088 0.00536 0.01446 0.00202
W15 7 0.371490 0.237490 0.474166 11.00000 0.01859 0.02723 =
0.03350 0.00232 0.01154 0.00406
W16 7 0.427841 0.401789 0.582058 11.00000 0.01630 0.03333 =
0.02908 0.00393 0.00936 0.00299
CO1 3 -0.022373 0.650980 0.414853 10.50000 0.01243 0.01709 =
0.01607 0.00234 0.00870 0.00165
CO2 3 -0.027953 0.425962 0.449140 11.00000 0.01521 0.02097 =
0.01660 -0.00130 0.00779 0.00042
P1 6 0.114343 0.429781 0.518531 11.00000 0.01244 0.01369 =
0.01436 0.00071 0.00497 0.00238
P2 6 0.276976 0.393019 0.508691 11.00000 0.01286 0.01943 =
0.01748 0.00072 0.00778 0.00116
O1 5 0.405799 0.145481 0.454931 11.00000 0.03135 0.02899 =
0.03849 0.00438 0.01493 0.01617
O2 5 0.497636 0.407721 0.630491 11.00000 0.02557 0.03092 =
0.03076 0.00434 0.01023 -0.00677
O3 5 0.434528 0.285634 0.542901 11.00000 0.01304 0.02680 =
0.04016 0.00111 0.01363 0.00482
O4 5 0.392999 0.337945 0.434336 11.00000 0.02858 0.02134 =
0.03096 0.00680 0.01952 0.00867
O5 5 0.436855 0.465403 0.517629 11.00000 0.01732 0.01888 =
0.02697 -0.00167 0.00009 0.00144
O6 5 0.407733 0.520278 0.400749 11.00000 0.02839 0.01970 =
0.04502 0.00877 0.01985 0.00179
O7 5 0.297931 0.235771 0.419588 11.00000 0.02273 0.02312 =
0.02515 0.00635 0.01562 0.00557
O8 5 0.340866 0.179035 0.527152 11.00000 0.01048 0.01773 =
0.03265 0.00745 0.00572 0.00111
O9 5 0.298606 0.447214 0.387062 11.00000 0.01762 0.03263 =
0.01215 0.00175 0.00633 0.00232
O10 5 0.338613 0.379845 0.504125 11.00000 0.01360 0.02458 =
0.02790 -0.00029 0.01274 -0.00167
O11 5 0.391876 0.326991 0.624836 11.00000 0.01950 0.03061 =
0.01805 0.00022 0.01041 0.00376
O12 5 0.343727 0.572008 0.469137 11.00000 0.01933 0.02697 =
0.02792 0.00582 0.01343 0.00201
O13 5 0.392682 0.503171 0.600318 11.00000 0.00818 0.03132 =
0.02844 -0.00357 0.00251 -0.00334
O14 5 0.199511 0.138336 0.352905 11.00000 0.03367 0.02706 =
0.02669 -0.00029 0.01202 0.00568
O15 5 0.277495 0.036454 0.550018 11.00000 0.03712 0.01918 =
0.04057 0.00736 0.01259 0.00383
O16 5 0.369623 0.290665 0.722489 11.00000 0.02557 0.03957 =
0.02788 0.01235 0.01054 0.00890
O17 5 0.369716 0.626301 0.676673 11.00000 0.02612 0.03226 =
0.04070 -0.00466 0.01677 -0.00671
O18 5 0.286842 0.739679 0.450565 11.00000 0.03890 0.03183 =
0.03478 0.00322 0.01590 -0.00835
O19 5 0.202233 0.509350 0.296001 11.00000 0.02950 0.03305 =
0.02426 0.00847 0.00976 0.00475
O20 5 0.315623 0.188016 0.624276 11.00000 0.02274 0.02091 =
0.02402 0.00699 0.01051 0.00788
O21 5 0.323532 0.446329 0.650302 11.00000 0.01934 0.01994 =
0.02647 0.01111 0.00765 0.00573
O22 5 0.324330 0.653836 0.557051 11.00000 0.01672 0.02042 =
0.03661 -0.00152 0.01305 -0.00054
O23 5 0.232435 0.567044 0.411530 11.00000 0.01624 0.03072 =
0.02338 0.00573 0.00590 0.00994
O24 5 0.209201 0.331130 0.342408 11.00000 0.01400 0.02167 =
0.01499 -0.00051 0.00356 0.00083
O25 5 0.228352 0.177648 0.470160 11.00000 0.01526 0.02532 =
0.02140 0.00417 0.00728 -0.00237
O26 5 0.273937 0.321608 0.552778 11.00000 0.01800 0.01731 =
0.01096 0.00375 0.00354 0.00214
O27 5 0.273985 0.493159 0.527233 11.00000 0.02417 0.02641 =
0.02193 -0.00196 0.01478 0.00112
O28 5 0.231302 0.374267 0.449256 11.00000 0.01893 0.02752 =
0.02232 0.00234 0.01242 0.00383
O29 5 0.201056 0.167199 0.561337 11.00000 0.01980 0.02975 =
0.02280 0.00019 0.00857 -0.00012
O30 5 0.253668 0.313246 0.658290 11.00000 0.01518 0.02316 =
0.03392 -0.00215 0.01298 -0.00040
O31 5 0.133499 0.258850 0.389567 11.00000 0.01328 0.02877 =
0.01161 0.00033 0.00479 0.00062
O32 5 0.140129 0.461393 0.363215 11.00000 0.02220 0.02853 =
0.02211 -0.00107 0.01436 0.00487
O33 5 0.254908 0.595358 0.614184 11.00000 0.00602 0.02143 =
0.03195 -0.00055 0.01002 -0.00451
O34 5 0.209573 0.659271 0.493905 11.00000 0.02177 0.02273 =
0.03178 -0.00059 0.01351 0.00253
O35 5 0.116088 0.778518 0.461042 11.00000 0.02657 0.02541 =
0.03434 0.00479 0.01863 0.00381
O36 5 0.156532 0.696762 0.568609 11.00000 0.02057 0.02057 =
0.01917 0.00025 0.00848 0.00435
O37 5 0.202840 0.663542 0.689786 11.00000 0.03166 0.03723 =
0.01914 -0.00426 0.00663 -0.00412
O38 5 0.196928 0.474856 0.656788 11.00000 0.01622 0.03047 =
0.01639 0.00157 0.00283 0.01085
O39 5 0.196114 0.334019 0.732918 11.00000 0.02680 0.04572 =
0.00529 0.00134 -0.00053 -0.00433
O40 5 0.152922 0.223672 0.635145 11.00000 0.01568 0.01731 =
0.02658 0.00042 0.01196 -0.00645
O41 5 0.101312 0.078541 0.558945 11.00000 0.01351 0.02641 =
0.02323 0.00740 0.00574 0.00035
O42 5 0.098971 0.207630 0.475709 11.00000 0.01455 0.02266 =
0.02493 -0.00026 0.00768 0.00398
O43 5 0.022737 0.178600 0.361292 11.00000 0.02636 0.02100 =
0.02996 -0.00587 0.01325 -0.00232
O44 5 0.039658 0.371600 0.349747 11.00000 0.02148 0.02114 =
0.02673 0.00579 0.01579 0.00123
O45 5 0.038813 0.552269 0.308037 11.00000 0.01914 0.03210 =
0.01805 0.00362 0.01034 -0.00026
O46 5 0.110153 0.591535 0.421963 11.00000 0.01413 0.02500 =
0.02062 0.00193 0.00931 0.00535
O47 5 0.146895 0.351693 0.558773 11.00000 0.01944 0.02828 =
0.01998 -0.00508 0.01125 -0.00040
O48 5 0.146723 0.522882 0.535806 11.00000 0.01787 0.02339 =
0.01861 0.00030 0.01049 0.00331
O49 5 0.103382 0.404587 0.455447 11.00000 0.02159 0.02180 =
0.01731 0.00267 0.01164 0.00285
O50 5 0.000259 0.304668 0.429125 11.00000 0.01283 0.02685 =
0.02152 -0.00167 0.00923 0.00005
O51 5 0.052571 0.440348 0.524173 11.00000 0.01780 0.02488 =
0.01986 -0.00377 0.00944 -0.00413
O52 5 0.004452 0.520022 0.401531 11.00000 0.02273 0.01205 =
0.01898 0.00560 0.01214 0.00108
O53 5 0.102897 0.585620 0.618228 11.00000 0.02075 0.02391 =
0.02143 0.00255 0.01294 -0.00224
O54 5 0.049840 0.643119 0.485020 11.00000 0.01483 0.02245 =
0.02601 -0.00211 0.01382 0.00180
O55 5 -0.097298 0.619114 0.360926 11.00000 0.02230 0.01980 =
0.02769 0.00602 0.01506 0.00557
O56 5 -0.051599 0.748003 0.445431 11.00000 0.01225 0.02913 =
0.02203 -0.00538 0.00531 0.00135
O57 5 0.003681 0.710776 0.370482 11.00000 0.03015 0.03637 =
0.02546 0.00528 0.02179 0.00557
N5 4 0.479412 0.746133 0.656088 11.00000 0.03869 0.05113 =
0.08180 -0.01500 0.02710 0.00441
AFIX 43
H5 2 0.506616 0.704793 0.668497 11.00000 -1.20000
AFIX 0
N6 4 0.454505 0.774587 0.601138 11.00000 0.02701 0.07148 =
0.05302 -0.00878 0.02088 0.00653
AFIX 43
H6 2 0.464124 0.755242 0.573049 11.00000 -1.20000
AFIX 0
N7 4 0.341618 1.024812 0.705111 11.00000 0.13634 0.05689 =
0.12845 -0.01423 0.10141 -0.00355
AFIX 43
H7 2 0.339952 1.073673 0.724742 11.00000 -1.20000
AFIX 0
N8 4 0.296656 0.968880 0.678174 11.00000 0.09579 0.06468 =
0.09969 0.04027 0.07556 0.04256
AFIX 43
H8 2 0.261476 0.976249 0.676835 11.00000 -1.20000
AFIX 0
C11 1 0.472442 0.776247 0.750614 11.00000 0.06705 0.06584 =
0.08030 -0.01358 0.04008 -0.00233
AFIX 137
H11A 2 0.457081 0.717331 0.757281 11.00000 -1.50000
H11B 2 0.456793 0.826034 0.766607 11.00000 -1.50000
H11C 2 0.514237 0.775724 0.768774 11.00000 -1.50000
AFIX 0
C12 1 0.455838 0.791105 0.687769 11.00000 0.03561 0.05937 =
0.05700 -0.02107 0.02212 -0.01841
C13 1 0.412870 0.849838 0.650516 11.00000 0.03768 0.04388 =
0.04439 0.00786 0.01644 -0.00149
C14 1 0.413181 0.836419 0.596245 11.00000 0.02778 0.04356 =
0.07162 0.00255 0.02995 -0.00073
C15 1 0.380057 0.878531 0.542240 11.00000 0.10007 0.06472 =
0.07798 -0.00047 0.04839 0.01172
AFIX 137
H15A 2 0.395828 0.939311 0.539883 11.00000 -1.50000
H15B 2 0.340143 0.884902 0.539078 11.00000 -1.50000
H15C 2 0.381865 0.839774 0.511343 11.00000 -1.50000
AFIX 0
C16 1 0.274223 0.826372 0.620508 11.00000 0.05471 0.11761 =
0.10950 -0.04311 0.01367 -0.00385
AFIX 137
H16A 2 0.280638 0.770096 0.643191 11.00000 -1.50000
H16B 2 0.280920 0.814009 0.585450 11.00000 -1.50000
H16C 2 0.234712 0.847131 0.611266 11.00000 -1.50000
AFIX 0
C17 1 0.315177 0.900651 0.654042 11.00000 0.08010 0.04385 =
0.09183 0.02406 0.06469 0.02631
C18 1 0.374806 0.913757 0.668327 11.00000 0.05785 0.03878 =
0.09454 0.00020 0.05763 0.00715
C19 1 0.389665 0.994757 0.697513 11.00000 0.10294 0.04584 =
0.13803 -0.01637 0.09224 -0.00550
C20 1 0.443726 1.041325 0.720436 11.00000 0.16674 0.17082 =
0.32903 -0.16847 0.18743 -0.09881
AFIX 33
H20A 2 0.472282 1.008037 0.709882 11.00000 -1.50000
H20B 2 0.439712 1.103934 0.705273 11.00000 -1.50000
H20C 2 0.456065 1.043773 0.761793 11.00000 -1.50000
AFIX 0
N1 4 0.674918 -0.081396 0.698294 11.00000 0.05648 0.02814 =
0.06781 0.01731 0.03001 0.01631
AFIX 43
H1 2 0.672582 -0.135222 0.712914 11.00000 -1.20000
AFIX 0
N2 4 0.718134 -0.055456 0.683382 11.00000 0.03929 0.04270 =
0.04926 0.00403 0.01670 0.01145
AFIX 43
H2 2 0.748638 -0.088600 0.687609 11.00000 -1.20000
AFIX 0
N3 4 0.549977 0.235475 0.590927 11.00000 0.04755 0.03828 =
0.05104 0.01045 0.00382 0.02704
AFIX 43
H3 2 0.516762 0.255405 0.567514 11.00000 -1.20000
AFIX 0
N4 4 0.591697 0.290347 0.622509 11.00000 0.03713 0.01783 =
0.07086 0.00202 0.01898 0.00499
AFIX 43
H4 2 0.590871 0.350582 0.623766 11.00000 -1.20000
AFIX 0
C1 1 0.746860 0.080868 0.638412 11.00000 0.09571 0.13518 =
0.20965 0.10813 0.10151 0.04132
AFIX 137
H1A 2 0.775802 0.113707 0.669513 11.00000 -1.50000
H1B 2 0.724542 0.125036 0.609679 11.00000 -1.50000
H1C 2 0.765756 0.037418 0.621407 11.00000 -1.50000
AFIX 0
C2 1 0.708028 0.029803 0.660684 11.00000 0.06780 0.04180 =
0.05715 0.02436 0.04411 0.04158
C3 1 0.654534 0.057333 0.662868 11.00000 0.03915 0.03002 =
0.03559 0.00068 0.01276 0.01426
C4 1 0.636122 -0.016659 0.688486 11.00000 0.03778 0.04249 =
0.05258 0.00488 0.02135 0.00953
C5 1 0.584352 -0.023403 0.703158 11.00000 0.06451 0.04240 =
0.11551 0.04331 0.04944 0.02470
AFIX 137
H5A 2 0.563738 -0.080164 0.687298 11.00000 -1.50000
H5B 2 0.559485 0.029522 0.687459 11.00000 -1.50000
H5C 2 0.595551 -0.024032 0.744435 11.00000 -1.50000
AFIX 0
C6 1 0.524679 0.068922 0.567113 11.00000 0.07830 0.03511 =
0.07626 -0.00777 -0.03434 0.01828
AFIX 33
H6A 2 0.543447 0.009440 0.579217 11.00000 -1.50000
H6B 2 0.489394 0.071278 0.575197 11.00000 -1.50000
H6C 2 0.515469 0.076653 0.526355 11.00000 -1.50000
AFIX 0
C7 1 0.564327 0.145044 0.598815 11.00000 0.03197 0.05922 =
0.02467 -0.00558 -0.00338 -0.00231
C8 1 0.620458 0.142828 0.639140 11.00000 0.03377 0.03075 =
0.03812 -0.00350 0.01256 0.00571
C9 1 0.636532 0.234078 0.652915 11.00000 0.01912 0.04783 =
0.04927 -0.00220 0.00916 0.01064
C10 1 0.690426 0.279617 0.693789 11.00000 0.04680 0.08064 =
0.12782 -0.01411 -0.00640 0.00345
AFIX 137
H10A 2 0.719811 0.232794 0.710526 11.00000 -1.50000
H10B 2 0.681562 0.310752 0.723858 11.00000 -1.50000
H10C 2 0.704574 0.324599 0.673277 11.00000 -1.50000
AFIX 0
N9 4 0.044512 0.970285 0.432344 11.00000 0.06063 0.05791 =
0.02233 0.00440 0.02844 0.01078
AFIX 43
H9 2 0.053288 0.983988 0.468237 11.00000 -1.20000
AFIX 0
N10 4 -0.007180 0.946080 0.395926 11.00000 0.05011 0.07821 =
0.04220 0.00408 0.03200 0.01147
AFIX 43
H10 2 -0.037521 0.940439 0.405114 11.00000 -1.20000
AFIX 0
N11 4 0.101084 0.878157 0.234535 11.00000 0.05150 0.05615 =
0.04834 -0.01853 0.03797 -0.01646
AFIX 43
H11 2 0.110922 0.839029 0.213358 11.00000 -1.20000
AFIX 0
N12 4 0.098038 0.969363 0.226368 11.00000 0.03920 0.06283 =
0.03091 -0.00238 0.01999 -0.01413
AFIX 43
H12 2 0.106210 0.998465 0.199953 11.00000 -1.20000
AFIX 0
C21 1 0.144771 0.985983 0.436447 11.00000 0.09940 0.03299 =
0.05442 -0.01402 0.04396 -0.01713
AFIX 137
H21A 2 0.150140 1.020955 0.471029 11.00000 -1.50000
H21B 2 0.160745 1.020598 0.412526 11.00000 -1.50000
H21C 2 0.164366 0.926686 0.446467 11.00000 -1.50000
AFIX 0
C22 1 0.080745 0.969891 0.404105 11.00000 0.03855 0.02989 =
0.05219 -0.00469 0.03233 0.00004
C23 1 0.050291 0.949455 0.348352 11.00000 0.04570 0.03618 =
0.03601 0.01041 0.02378 0.00073
C24 1 -0.007245 0.931285 0.343203 11.00000 0.04707 0.06276 =
0.02929 0.00631 0.02287 0.00344
C25 1 -0.058388 0.906325 0.293897 11.00000 0.05582 0.09742 =
0.06363 0.02002 0.03050 0.00146
AFIX 137
H25A 2 -0.080966 0.861032 0.305346 11.00000 -1.50000
H25B 2 -0.046597 0.880027 0.264287 11.00000 -1.50000
H25C 2 -0.081604 0.961323 0.279276 11.00000 -1.50000
AFIX 0
C26 1 0.089454 0.756284 0.299953 11.00000 0.15873 0.04173 =
0.19684 0.02154 0.15301 -0.00023
AFIX 137
H26A 2 0.114389 0.753103 0.339967 11.00000 -1.50000
H26B 2 0.104609 0.716251 0.277678 11.00000 -1.50000
H26C 2 0.050849 0.736078 0.295642 11.00000 -1.50000
AFIX 0
C27 1 0.087174 0.853801 0.279306 11.00000 0.05329 0.04436 =
0.06049 -0.00769 0.04000 -0.00792
C28 1 0.073431 0.938770 0.300249 11.00000 0.05379 0.04436 =
0.03065 0.00324 0.02762 0.00365
C29 1 0.080134 1.009921 0.265829 11.00000 0.02755 0.03094 =
0.02108 -0.00236 0.00644 -0.00389
C30 1 0.075104 1.113620 0.268471 11.00000 0.04960 0.04801 =
0.03857 -0.00647 0.01496 0.00327
AFIX 137
H30A 2 0.036764 1.129751 0.267230 11.00000 -1.50000
H30B 2 0.081521 1.141520 0.236126 11.00000 -1.50000
H30C 2 0.103779 1.136523 0.303764 11.00000 -1.50000
AFIX 0
O6W 5 -0.103124 0.194855 0.332279 10.50000 0.03014 0.03745 =
0.08500 0.00448 0.00493 0.01674
O2W 5 0.684793 0.720780 0.694108 11.00000 0.08398 0.06509 =
0.06531 -0.01666 0.04477 0.00314
O1W 5 0.576059 0.636210 0.675449 11.00000 0.07086 0.10992 =
0.05056 -0.00329 0.02692 0.03667
O3W 5 0.761307 0.609955 0.781451 11.00000 0.09375 0.10376 =
0.07371 -0.03739 0.05919 -0.05288
O4W 5 0.479949 0.657398 0.528507 11.00000 0.04103 0.04826 =
0.05730 -0.00955 0.02468 -0.00871
O5W 5 0.042975 0.879785 0.536411 11.00000 0.15715 0.08263 =
0.08060 -0.03933 0.08490 -0.06450
O6WA 5 -0.172635 0.046918 0.343278 10.50000 0.02232 0.09042 =
0.12968 0.02843 0.04045 -0.00276
HKLF 4
REM Integration of 150521d
REM R1 = 0.0411 for 10803 Fo > 4sig(Fo) and 0.0760 for all 15970 data
REM 1136 parameters refined using 6 restraints
END
WGHT 0.0381 7.5424
REM Highest difference peak 2.514, deepest hole -2.903, 1-sigma level 0.324
Q1 1 -0.0155 0.6415 0.4385 11.00000 0.05 2.36
Q2 1 0.4193 0.4610 0.5414 11.00000 0.05 1.64
Q3 1 0.0401 0.6980 0.4401 11.00000 0.05 1.52
Q4 1 0.4231 0.8646 0.4807 11.00000 0.05 1.38
Q5 1 0.2783 0.7016 0.4785 11.00000 0.05 1.33
Q6 1 -0.1395 0.1180 0.3851 11.00000 0.05 1.29
Q7 1 0.4428 1.1463 0.6246 11.00000 0.05 1.28
Q8 1 0.4198 0.2389 0.5776 11.00000 0.05 1.26
Q9 1 0.1748 0.2867 0.6614 11.00000 0.05 1.25
Q10 1 0.7374 -0.0314 0.7022 11.00000 0.05 1.24
Q11 1 0.0852 0.2959 0.3766 11.00000 0.05 1.19
Q12 1 0.0000 0.5000 0.5000 10.50000 0.05 1.16
Q13 1 -0.0818 0.7402 0.4820 11.00000 0.05 1.16
Q14 1 -0.1196 0.1615 0.3613 11.00000 0.05 1.15
Q15 1 0.0805 0.9250 0.2215 11.00000 0.05 1.13
Q16 1 0.7599 0.0214 0.7196 11.00000 0.05 1.12
Q17 1 0.1596 0.6817 0.5175 11.00000 0.05 1.12
Q18 1 0.7014 0.6647 0.7238 11.00000 0.05 1.11
Q19 1 0.6609 0.0595 0.6365 11.00000 0.05 1.09
Q20 1 0.6328 0.1595 0.7024 11.00000 0.05 1.08
Q21 1 -0.0811 1.0216 0.3594 11.00000 0.05 1.08
Q22 1 0.2425 0.5120 0.3373 11.00000 0.05 1.08
Q23 1 0.2238 0.5033 0.4592 11.00000 0.05 1.07
Q24 1 0.6461 -0.0231 0.6407 11.00000 0.05 1.07
Q25 1 -0.0216 0.4386 0.4794 11.00000 0.05 1.04
Q26 1 0.3393 0.3391 0.5574 11.00000 0.05 1.04
Q27 1 0.1768 0.2438 0.3567 11.00000 0.05 1.03
Q28 1 0.4206 0.4230 0.6787 11.00000 0.05 1.03
Q29 1 0.1984 0.1164 0.4408 11.00000 0.05 1.02
Q30 1 0.4643 0.6718 0.5032 11.00000 0.05 1.02
REM The information below was added by Olex2.
REM
REM R1 = 0.0411 for 10803 Fo > 4sig(Fo) and 0.0760 for all 51546 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 2.51, deepest hole -2.90
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0760
REM R1_gt = 0.0411
REM wR_ref = 0.0987
REM GOOF = 1.020
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 51546
REM Reflections_gt = 10803
REM Parameters = n/a
REM Hole = -2.90
REM Peak = 2.51
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT306_p
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check
RESPONSE: In this case, we have tried to theoretically add the H-atoms for water molecules in the crystal structure, but this is unsuccessful. Due to the some disordered nature of water solvents in the void, it is impossible to find the reasonable H-bonding directions and H-bonding donors around the cluster for the H atoms on water, which will bring some of B alerts in the checkcif relating to the missed H-bonding donor or acceptor. Moreover, X-ray diffraction could not reach such high resolutions to identify H atoms from the E maps. Anyway, this issue will not influence us to recognize the main body of cluster as well as their properties in this work.
;
_vrf_PLAT342_p
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02852 Ang.
RESPONSE: Moderate crystal quality in context with some disordered solvents,
hence only small amount of reflections have I>2sigma(I)
;
_vrf_PLAT430_p
;
PROBLEM: Short Inter D...A Contact O6WA .. O6W .. 2.79 Ang.
RESPONSE: O6WA and O6W are a pair of disordered water molecule.
;
# end Validation Reply Form