data_2007src1142
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C17.50 H36.50 Cl0.50 N10 O8 P6'
_chemical_formula_weight          718.61
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.6107(3)
_cell_length_b                    13.1064(3)
_cell_length_c                    13.7556(4)
_cell_angle_alpha                 95.945(2)
_cell_angle_beta                  108.6670(10)
_cell_angle_gamma                 103.670(2)
_cell_volume                      1564.51(8)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     58258
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description      plate
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.525
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              748
_exptl_absorpt_coefficient_mu     0.445
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9569
_exptl_absorpt_correction_T_max   0.9956
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   '10cm confocal mirrors'
_diffrn_measurement_device_type   'Bruker-Nonius APEX2 Area Detector'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          none
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         negligible
_diffrn_reflns_number             32713
_diffrn_reflns_av_R_equivalents   0.0519
_diffrn_reflns_av_sigmaI/netI     0.0435
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          3.19
_diffrn_reflns_theta_max          27.50
_reflns_number_total              7129
_reflns_number_gt                 5654
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        'DENZO, COLLECT'
_computing_data_reduction         'DENZO, COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'PLATON (Spek, 2003)'
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0935P)²+11.4711P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          7129
_refine_ls_number_parameters      409
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1308
_refine_ls_R_factor_gt            0.1088
_refine_ls_wR_factor_ref          0.2806
_refine_ls_wR_factor_gt           0.2639
_refine_ls_goodness_of_fit_ref    1.084
_refine_ls_restrained_S_all       1.084
_refine_ls_shift/su_max           0.084
_refine_ls_shift/su_mean          0.004
 
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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.7837(8) 0.4435(6) 0.3636(5) 0.0449(15) Uani 1 1 d . . .
H1A H 0.8884 0.4735 0.4165 0.054 Uiso 1 1 calc R . .
H1B H 0.7109 0.4641 0.3934 0.054 Uiso 1 1 calc R . .
C2 C 0.7742(9) 0.4891(7) 0.2643(6) 0.060(2) Uani 1 1 d . . .
H2A H 0.7956 0.5678 0.2811 0.071 Uiso 1 1 calc R . .
H2B H 0.8533 0.4735 0.2382 0.071 Uiso 1 1 calc R . .
C3 C 0.6188(9) 0.4419(6) 0.1803(6) 0.057(2) Uani 1 1 d . . .
H3A H 0.5404 0.4623 0.2040 0.068 Uiso 1 1 calc R . .
H3B H 0.6174 0.4710 0.1164 0.068 Uiso 1 1 calc R . .
C4 C 0.514(2) -0.1313(12) 0.1987(17) 0.153(7) Uani 1 1 d . . .
H4A H 0.4938 -0.1951 0.2305 0.183 Uiso 1 1 calc R . .
H4B H 0.6256 -0.1069 0.2142 0.183 Uiso 1 1 calc R . .
C5 C 0.4389(18) -0.1657(13) 0.0858(14) 0.135(7) Uani 1 1 d . . .
H5A H 0.3777 -0.2415 0.0715 0.162 Uiso 1 1 calc R . .
H5B H 0.5199 -0.1636 0.0555 0.162 Uiso 1 1 calc R . .
C6 C 0.338(2) -0.1061(10) 0.0285(11) 0.122(5) Uani 1 1 d . . .
H6A H 0.3476 -0.1059 -0.0409 0.146 Uiso 1 1 calc R . .
H6B H 0.2306 -0.1463 0.0165 0.146 Uiso 1 1 calc R . .
C7 C 0.0212(7) 0.1612(6) 0.2635(5) 0.0384(13) Uani 1 1 d . . .
H7A H -0.0158 0.0866 0.2240 0.046 Uiso 1 1 calc R . .
H7B H -0.0622 0.1952 0.2391 0.046 Uiso 1 1 calc R . .
C8 C 0.0589(6) 0.1604(5) 0.3795(5) 0.0326(12) Uani 1 1 d . . .
C9 C 0.1955(7) 0.1137(5) 0.4192(5) 0.0370(13) Uani 1 1 d . . .
H9A H 0.2205 0.1122 0.4946 0.044 Uiso 1 1 calc R . .
H9B H 0.1691 0.0396 0.3806 0.044 Uiso 1 1 calc R . .
C10 C -0.0838(7) 0.0890(5) 0.3925(5) 0.0387(13) Uani 1 1 d . . .
H10A H -0.1736 0.1149 0.3605 0.046 Uiso 1 1 calc R . .
H10B H -0.1059 0.0145 0.3561 0.046 Uiso 1 1 calc R . .
C11 C 0.0967(7) 0.2729(5) 0.4406(5) 0.0361(13) Uani 1 1 d . . .
H11A H 0.1891 0.3188 0.4331 0.043 Uiso 1 1 calc R . .
H11B H 0.0107 0.3033 0.4111 0.043 Uiso 1 1 calc R . .
C12 C -0.4639(11) 0.3417(13) 0.6373(8) 0.100(5) Uani 1 1 d . . .
H12A H -0.4507 0.3369 0.7109 0.120 Uiso 1 1 calc R . .
H12B H -0.5752 0.3211 0.5964 0.120 Uiso 1 1 calc R . .
C13 C -0.391(2) 0.4578(14) 0.6319(12) 0.129(7) Uani 1 1 d . . .
H13A H -0.4109 0.4634 0.5578 0.155 Uiso 1 1 calc R . .
H13B H -0.4413 0.5051 0.6606 0.155 Uiso 1 1 calc R . .
C14 C -0.230(2) 0.4937(10) 0.6887(11) 0.107(5) Uani 1 1 d . . .
H14A H -0.2086 0.4869 0.7627 0.129 Uiso 1 1 calc R . .
H14B H -0.1892 0.5698 0.6865 0.129 Uiso 1 1 calc R . .
C15 C 0.0974(11) 0.1188(7) 0.9234(7) 0.069(2) Uani 1 1 d . . .
H15A H 0.1470 0.0838 0.8823 0.083 Uiso 1 1 calc R . .
H15B H 0.0626 0.0683 0.9653 0.083 Uiso 1 1 calc R . .
C16 C 0.2133(11) 0.2201(7) 0.9964(6) 0.074(3) Uani 1 1 d . . .
H16A H 0.1671 0.2517 1.0424 0.088 Uiso 1 1 calc R . .
H16B H 0.3043 0.2023 1.0412 0.088 Uiso 1 1 calc R . .
C17 C 0.2613(10) 0.3004(7) 0.9329(7) 0.076(3) Uani 1 1 d . . .
H17A H 0.3346 0.3666 0.9809 0.091 Uiso 1 1 calc R . .
H17B H 0.3141 0.2704 0.8910 0.091 Uiso 1 1 calc R . .
N1 N 0.4421(5) 0.2830(4) 0.2849(4) 0.0338(10) Uani 1 1 d . . .
N2 N 0.5690(7) 0.1438(5) 0.2124(5) 0.0537(15) Uani 1 1 d . . .
N3 N 0.2884(6) 0.0713(4) 0.2238(5) 0.0448(13) Uani 1 1 d . . .
N4 N 0.7462(6) 0.3255(5) 0.3386(5) 0.0423(13) Uani 1 1 d . . .
N5 N 0.4747(10) -0.0503(6) 0.2507(7) 0.084(3) Uani 1 1 d . . .
H5 H 0.4776 -0.0509 0.3152 0.100 Uiso 1 1 calc R . .
N6 N -0.1540(7) 0.2521(5) 0.5469(4) 0.0463(14) Uani 1 1 d . . .
N7 N -0.1441(7) 0.2775(6) 0.7465(4) 0.0551(16) Uani 1 1 d . . .
N8 N 0.0531(6) 0.1873(6) 0.6944(5) 0.0549(17) Uani 1 1 d . . .
N9 N -0.3933(7) 0.2645(8) 0.5951(6) 0.072(2) Uani 1 1 d . . .
N10 N -0.0296(7) 0.1421(5) 0.8550(4) 0.0521(15) Uani 1 1 d . . .
O1 O 0.5822(5) 0.3253(4) 0.1560(3) 0.0509(12) Uani 1 1 d . . .
O2 O 0.3604(9) -0.0059(7) 0.0725(5) 0.096(3) Uani 1 1 d . . .
O3 O 0.1539(5) 0.2190(4) 0.2424(3) 0.0368(9) Uani 1 1 d . . .
O4 O 0.3265(4) 0.1813(4) 0.4024(3) 0.0356(9) Uani 1 1 d . . .
O5 O -0.0584(5) 0.0910(4) 0.5028(4) 0.0439(11) Uani 1 1 d . . .
O6 O 0.1235(5) 0.2737(4) 0.5504(3) 0.0407(10) Uani 1 1 d . . .
O7 O -0.1592(9) 0.4275(5) 0.6400(5) 0.0800(19) Uani 1 1 d . . .
O8 O 0.1364(6) 0.3253(5) 0.8666(4) 0.0658(16) Uani 1 1 d . . .
P1 P 0.30916(17) 0.18715(13) 0.28406(12) 0.0322(3) Uani 1 1 d . . .
P2 P 0.57857(17) 0.26352(14) 0.24849(12) 0.0356(4) Uani 1 1 d . . .
P3 P 0.4240(2) 0.04537(16) 0.19287(16) 0.0510(5) Uani 1 1 d . . .
P4 P -0.01288(18) 0.20361(15) 0.57826(13) 0.0399(4) Uani 1 1 d . . .
P5 P -0.20776(19) 0.30175(15) 0.63361(13) 0.0410(4) Uani 1 1 d . . .
P6 P -0.0009(2) 0.23227(16) 0.78420(13) 0.0455(5) Uani 1 1 d . . .
C18 C 0.091(3) 0.540(2) 0.0049(18) 0.062(7) Uani 0.33 1 d P A 1
H18A H 0.0382 0.4658 -0.0342 0.074 Uiso 0.33 1 calc PR A 1
H18B H 0.0485 0.5538 0.0599 0.074 Uiso 0.33 1 calc PR A 1
Cl1 Cl 0.2739(17) 0.5536(9) 0.0593(7) 0.122(4) Uani 0.33 1 d P A 1
Cl2 Cl 0.062(2) 0.6221(11) -0.0737(11) 0.161(6) Uani 0.33 1 d P A 1
H4N H 0.759(11) 0.306(7) 0.386(7) 0.06(3) Uiso 1 1 d . . .
H9N H -0.430(11) 0.240(8) 0.534(8) 0.07(3) Uiso 1 1 d . . .
H10N H -0.132(14) 0.076(10) 0.805(9) 0.12(4) Uiso 1 1 d . . .
 
 
_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
C1 N4 1.479(9) . ?
C1 C2 1.532(9) . ?
C2 C3 1.503(10) . ?
C3 O1 1.461(10) . ?
C4 N5 1.409(16) . ?
C4 C5 1.46(2) . ?
C5 C6 1.47(2) . ?
C6 O2 1.324(13) . ?
C7 O3 1.453(7) . ?
C7 C8 1.520(8) . ?
C8 C11 1.520(9) . ?
C8 C10 1.541(8) . ?
C8 C9 1.544(8) . ?
C9 O4 1.457(7) . ?
C10 O5 1.454(7) . ?
C11 O6 1.447(7) . ?
C12 N9 1.509(13) . ?
C12 C13 1.54(2) . ?
C13 C14 1.43(2) . ?
C14 O7 1.457(13) . ?
C15 N10 1.403(11) . ?
C15 C16 1.524(12) . ?
C16 C17 1.518(11) . ?
C17 O8 1.388(10) . ?
N1 P1 1.562(5) . ?
N1 P2 1.609(5) . ?
N2 P2 1.568(7) . ?
N2 P3 1.587(7) . ?
N3 P1 1.588(6) . ?
N3 P3 1.590(6) . ?
N4 P2 1.639(6) . ?
N5 P3 1.640(8) . ?
N6 P5 1.583(6) . ?
N6 P4 1.587(5) . ?
N7 P5 1.572(6) . ?
N7 P6 1.583(7) . ?
N8 P4 1.577(5) . ?
N8 P6 1.597(7) . ?
N9 P5 1.622(7) . ?
N10 P6 1.636(6) . ?
O1 P2 1.583(5) . ?
O2 P3 1.580(6) . ?
O3 P1 1.589(4) . ?
O4 P1 1.594(4) . ?
O5 P4 1.592(5) . ?
O6 P4 1.592(4) . ?
O7 P5 1.588(7) . ?
O8 P6 1.584(6) . ?
C18 Cl2 1.61(3) . ?
C18 Cl1 1.63(3) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N4 C1 C2 109.8(6) . . ?
C3 C2 C1 111.4(6) . . ?
O1 C3 C2 110.6(6) . . ?
N5 C4 C5 119.1(14) . . ?
C4 C5 C6 118.5(11) . . ?
O2 C6 C5 117.5(13) . . ?
O3 C7 C8 111.6(5) . . ?
C7 C8 C11 110.4(5) . . ?
C7 C8 C10 107.6(5) . . ?
C11 C8 C10 109.1(5) . . ?
C7 C8 C9 109.4(5) . . ?
C11 C8 C9 110.4(5) . . ?
C10 C8 C9 109.9(5) . . ?
O4 C9 C8 108.2(5) . . ?
O5 C10 C8 110.2(5) . . ?
O6 C11 C8 111.6(5) . . ?
N9 C12 C13 112.2(9) . . ?
C14 C13 C12 112.7(10) . . ?
C13 C14 O7 107.8(11) . . ?
N10 C15 C16 111.1(8) . . ?
C17 C16 C15 109.9(7) . . ?
O8 C17 C16 111.7(8) . . ?
P1 N1 P2 121.2(3) . . ?
P2 N2 P3 124.3(4) . . ?
P1 N3 P3 120.5(3) . . ?
C1 N4 P2 115.9(5) . . ?
C4 N5 P3 121.0(10) . . ?
P5 N6 P4 120.7(3) . . ?
P5 N7 P6 122.9(4) . . ?
P4 N8 P6 122.4(4) . . ?
C12 N9 P5 115.6(7) . . ?
C15 N10 P6 118.9(5) . . ?
C3 O1 P2 117.2(4) . . ?
C6 O2 P3 128.1(9) . . ?
C7 O3 P1 119.2(4) . . ?
C9 O4 P1 116.6(4) . . ?
C10 O5 P4 118.5(4) . . ?
C11 O6 P4 116.7(4) . . ?
C14 O7 P5 119.4(7) . . ?
C17 O8 P6 119.4(6) . . ?
N1 P1 N3 119.1(3) . . ?
N1 P1 O3 107.8(3) . . ?
N3 P1 O3 110.0(3) . . ?
N1 P1 O4 108.0(3) . . ?
N3 P1 O4 108.7(3) . . ?
O3 P1 O4 101.9(2) . . ?
N2 P2 O1 109.0(3) . . ?
N2 P2 N1 116.1(3) . . ?
O1 P2 N1 107.7(3) . . ?
N2 P2 N4 110.2(3) . . ?
O1 P2 N4 101.8(3) . . ?
N1 P2 N4 111.0(3) . . ?
O2 P3 N2 106.8(4) . . ?
O2 P3 N3 108.9(4) . . ?
N2 P3 N3 116.4(3) . . ?
O2 P3 N5 103.9(4) . . ?
N2 P3 N5 110.9(4) . . ?
N3 P3 N5 109.1(4) . . ?
N8 P4 N6 118.2(3) . . ?
N8 P4 O6 108.6(3) . . ?
N6 P4 O6 109.7(3) . . ?
N8 P4 O5 107.7(3) . . ?
N6 P4 O5 108.8(3) . . ?
O6 P4 O5 102.7(2) . . ?
N7 P5 N6 117.6(3) . . ?
N7 P5 O7 109.1(4) . . ?
N6 P5 O7 106.0(3) . . ?
N7 P5 N9 107.6(4) . . ?
N6 P5 N9 110.0(4) . . ?
O7 P5 N9 106.1(5) . . ?
N7 P6 O8 107.5(4) . . ?
N7 P6 N8 115.8(3) . . ?
O8 P6 N8 109.4(4) . . ?
N7 P6 N10 110.6(4) . . ?
O8 P6 N10 102.2(3) . . ?
N8 P6 N10 110.3(4) . . ?
Cl2 C18 Cl1 110.9(16) . . ?
 
_diffrn_measured_fraction_theta_max    0.992
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.992
_refine_diff_density_max    1.509
_refine_diff_density_min   -0.737
_refine_diff_density_rms    0.131
