# Copyright The Royal Society of Chemistry, 1998


# MANUSCRIPT 8/01622D 

 data_5

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C60 H66 Cl2 Cu2 N10 O8 P2'
_chemical_formula_weight          1315.15
_chemical_melting_point           ?
_chemical_compound_source         ?

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Cu'  'Cu'   0.3201   1.2651
 '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'
 'P'  'P'   0.1023   0.0942
 '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'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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'

_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    C2/c

loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 'x, -y, z+1/2'
 'x+1/2, y+1/2, z'
 'x+1/2, -y+1/2, z+1/2'
 '-x, -y, -z'
 '-x, y, -z-1/2'
 '-x+1/2, -y+1/2, -z'
 '-x+1/2, y+1/2, -z-1/2'

_cell_length_a                    23.769(3)
_cell_length_b                    14.386(2)
_cell_length_c                    20.284(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  100.61(3)
_cell_angle_gamma                 90.00
_cell_volume                      6817.3(16)
_cell_formula_units_Z             4
_cell_measurement_temperature     298(2)
_cell_measurement_reflns_used     25
_cell_measurement_theta_min       12
_cell_measurement_theta_max       15

_exptl_crystal_description        plate
_exptl_crystal_colour             'faint yellow'
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.1
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.281
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              2728
_exptl_absorpt_coefficient_mu     0.805
_exptl_absorpt_correction_type    'psi scan'
_exptl_absorpt_correction_T_min   0.89
_exptl_absorpt_correction_T_max   0.98

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       298(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        'CAD4 Diffractometer'
_diffrn_measurement_method        'omega twotheta'
_diffrn_standards_number          2
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   'one hour'
_diffrn_standards_decay_%         3
_diffrn_reflns_number             3734
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0121
_diffrn_reflns_limit_h_min        -27
_diffrn_reflns_limit_h_max        27
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_theta_min          2.03
_diffrn_reflns_theta_max          24.97
_reflns_number_total              3734
_reflns_number_observed           3734
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'CAD4 Programs'
_computing_cell_refinement        'CAD4 Programs'
_computing_data_reduction         MolEN
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     ZORTEP
_computing_publication_material   'SHELXL-93 (Sheldrick, 1993)'

_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 0 with very negative 
F^2^
 or flagged by the user for potential systematic errors.  Weighted R-
factors
 wR and all goodnesses of fit S are based on F^2^, conventional R-
factors R
 are based on F, with F set to zero for negative F^2^. The observed 
criterion
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. 
and is
 not relevant to the choice of reflections for refinement.  R-factors 
based
 on F^2^ are statistically about twice as large as those based on F, and 
R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+18.8900P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     ?
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00000(9)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          3734
_refine_ls_number_parameters      380
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0466
_refine_ls_R_factor_obs           0.0466
_refine_ls_wR_factor_all          0.1344
_refine_ls_wR_factor_obs          0.1344
_refine_ls_goodness_of_fit_all    1.122
_refine_ls_goodness_of_fit_obs    1.122
_refine_ls_restrained_S_all       1.122
_refine_ls_restrained_S_obs       1.122
_refine_ls_shift/esd_max          -1.048
_refine_ls_shift/esd_mean         0.003

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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Cu Cu 0.14636(3) 0.07703(4) 0.00084(3) 0.0531(2) Uani 1 d . .
Cl Cl 0.13802(10) -0.40835(15) -0.13006(12) 0.1020(6) Uani 1 d . .
P P 0.19172(5) 0.15516(9) -0.06772(6) 0.0493(3) Uani 1 d . .
O1 O 0.1059(4) -0.3873(7) -0.0829(4) 0.192(3) Uani 1 d . .
O2 O 0.1717(6) -0.3338(10) -0.1337(9) 0.327(8) Uani 1 d . .
O3 O 0.1041(6) -0.4079(10) -0.1946(6) 0.266(6) Uani 1 d . .
O4 O 0.1672(4) -0.4882(6) -0.1197(5) 0.200(4) Uani 1 d . .
N1 N 0.1720(2) -0.0522(3) 0.0459(2) 0.0479(9) Uani 1 d . .
N2 N 0.0825(2) -0.0733(3) -0.0807(2) 0.0543(10) Uani 1 d . .
N3 N 0.0741(2) 0.0121(3) -0.0546(2) 0.0525(10) Uani 1 d . .
N4 N 0.1683(2) 0.1015(3) 0.1494(2) 0.0574(11) Uani 1 d . .
N5 N 0.1424(2) 0.1409(3) 0.0903(2) 0.0609(11) Uani 1 d . .
C1 C 0.1553(2) -0.1304(3) 0.0120(2) 0.0536(12) Uani 1 d . .
C2 C 0.1535(3) -0.2160(4) 0.0425(3) 0.073(2) Uani 1 d . .
H2 H 0.1422(3) -0.2693(4) 0.0176(3) 0.088 Uiso 1 calc R .
C3 C 0.1693(3) -0.2195(4) 0.1121(3) 0.092(2) Uani 1 d . .
H3 H 0.1688(3) -0.2756(4) 0.1348(3) 0.111 Uiso 1 calc R .
C4 C 0.1855(3) -0.1405(4) 0.1462(3) 0.080(2) Uani 1 d . .
H4 H 0.1955(3) -0.1424(4) 0.1927(3) 0.096 Uiso 1 calc R .
C5 C 0.1874(2) -0.0574(4) 0.1137(2) 0.0562(12) Uani 1 d . .
C6 C 0.1379(2) -0.1179(4) -0.0627(2) 0.0570(12) Uani 1 d . .
H6A H 0.1664(2) -0.0806(4) -0.0790(2) 0.068 Uiso 1 calc R .
H6B H 0.1365(2) -0.1782(4) -0.0844(2) 0.068 Uiso 1 calc R .
C7 C 0.0341(2) -0.1050(4) -0.1201(2) 0.0601(13) Uani 1 d . .
C8 C 0.0325(3) -0.1968(4) -0.1560(3) 0.085(2) Uani 1 d . .
H8A H 0.0690(3) -0.2270(4) -0.1440(3) 0.127 Uiso 1 calc R .
H8B H 0.0241(3) -0.1865(4) -0.2035(3) 0.127 Uiso 1 calc R .
H8C H 0.0033(3) -0.2354(4) -0.1433(3) 0.127 Uiso 1 calc R .
C9 C -0.0060(2) -0.0383(4) -0.1205(3) 0.0611(13) Uani 1 d . .
H9 H -0.0436(2) -0.0402(4) -0.1435(3) 0.073 Uiso 1 calc R .
C10 C 0.0195(2) 0.0334(4) -0.0802(2) 0.0549(12) Uani 1 d . .
C11 C -0.0057(3) 0.1240(4) -0.0633(3) 0.073(2) Uani 1 d . .
H11A H 0.0229(3) 0.1592(4) -0.0341(3) 0.110 Uiso 1 calc R .
H11B H -0.0374(3) 0.1121(4) -0.0414(3) 0.110 Uiso 1 calc R .
H11C H -0.0186(3) 0.1585(4) -0.1038(3) 0.110 Uiso 1 calc R .
C12 C 0.2106(2) 0.0296(4) 0.1489(3) 0.0630(13) Uani 1 d . .
H12A H 0.2275(2) 0.0144(4) 0.1948(3) 0.076 Uiso 1 calc R .
H12B H 0.2407(2) 0.0537(4) 0.1273(3) 0.076 Uiso 1 calc R .
C13 C 0.1601(3) 0.1536(4) 0.2027(3) 0.069(2) Uani 1 d . .
C14 C 0.1871(4) 0.1309(5) 0.2734(3) 0.110(3) Uani 1 d . .
H14A H 0.2086(4) 0.0742(5) 0.2741(3) 0.164 Uiso 1 calc R .
H14B H 0.1578(4) 0.1234(5) 0.2998(3) 0.164 Uiso 1 calc R .
H14C H 0.2123(4) 0.1805(5) 0.2916(3) 0.164 Uiso 1 calc R .
C15 C 0.1265(3) 0.2259(4) 0.1775(3) 0.072(2) Uani 1 d . .
H15 H 0.1126(3) 0.2724(4) 0.2020(3) 0.087 Uiso 1 calc R .
C16 C 0.1164(2) 0.2173(4) 0.1072(3) 0.0614(13) Uani 1 d . .
C17 C 0.0846(3) 0.2808(4) 0.0548(3) 0.086(2) Uani 1 d . .
H17A H 0.0852(3) 0.2556(4) 0.0111(3) 0.129 Uiso 1 calc R .
H17B H 0.1026(3) 0.3409(4) 0.0587(3) 0.129 Uiso 1 calc R .
H17C H 0.0457(3) 0.2868(4) 0.0610(3) 0.129 Uiso 1 calc R .
C18 C 0.2481(2) 0.0926(3) -0.0981(2) 0.0572(13) Uani 1 d . .
C19 C 0.2778(3) 0.0254(4) -0.0585(3) 0.0700(15) Uani 1 d . .
H19 H 0.2670(3) 0.0110(4) -0.0178(3) 0.084 Uiso 1 calc R .
C20 C 0.3232(3) -0.0217(5) -0.0765(4) 0.098(2) Uani 1 d . .
H20 H 0.3443(3) -0.0644(5) -0.0475(4) 0.117 Uiso 1 calc R .
C21 C 0.3366(4) -0.0034(6) -0.1399(5) 0.105(3) Uani 1 d . .
H21 H 0.3652(4) -0.0374(6) -0.1547(5) 0.126 Uiso 1 calc R .
C22 C 0.3079(3) 0.0639(5) -0.1797(3) 0.085(2) Uani 1 d . .
H22 H 0.3185(3) 0.0778(5) -0.2206(3) 0.103 Uiso 1 calc R .
C23 C 0.2633(2) 0.1120(4) -0.1604(2) 0.0679(15) Uani 1 d . .
H23 H 0.2434(2) 0.1569(4) -0.1885(2) 0.082 Uiso 1 calc R .
C24 C 0.1456(2) 0.1950(4) -0.1453(2) 0.0557(12) Uani 1 d . .
C25 C 0.1125(2) 0.1310(4) -0.1842(2) 0.0671(15) Uani 1 d . .
H25 H 0.1137(2) 0.0689(4) -0.1711(2) 0.080 Uiso 1 calc R .
C26 C 0.0771(3) 0.1583(6) -0.2432(3) 0.085(2) Uani 1 d . .
H26 H 0.0557(3) 0.1143(6) -0.2706(3) 0.102 Uiso 1 calc R .
C27 C 0.0737(3) 0.2496(6) -0.2609(3) 0.101(2) Uani 1 d . .
H27 H 0.0498(3) 0.2680(6) -0.3004(3) 0.122 Uiso 1 calc R .
C28 C 0.1048(3) 0.3138(5) -0.2214(3) 0.100(2) Uani 1 d . .
H28 H 0.1021(3) 0.3761(5) -0.2337(3) 0.120 Uiso 1 calc R .
C29 C 0.1400(3) 0.2882(4) -0.1643(3) 0.078(2) Uani 1 d . .
H29 H 0.1607(3) 0.3332(4) -0.1372(3) 0.093 Uiso 1 calc R .
C30 C 0.2294(2) 0.2613(3) -0.0334(2) 0.0536(12) Uani 1 d . .
H30A H 0.2511(2) 0.2864(3) -0.0654(2) 0.064 Uiso 1 calc R .
H30B H 0.2019(2) 0.3077(3) -0.0255(2) 0.064 Uiso 1 calc R .

loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Cu 0.0680(4) 0.0502(4) 0.0390(3) -0.0002(3) 0.0041(2) -0.0032(3)
Cl 0.1180(15) 0.0837(13) 0.112(2) -0.0024(11) 0.0404(12) 0.0264(11)
P 0.0663(8) 0.0439(7) 0.0337(6) -0.0036(5) -0.0012(5) -0.0084(6)
O1 0.209(8) 0.223(9) 0.157(7) 0.007(7) 0.070(6) 0.040(7)
O2 0.271(14) 0.215(12) 0.508(26) -0.026(14) 0.107(15) -0.052(11)
O3 0.275(13) 0.315(16) 0.202(11) -0.021(10) 0.023(10) 0.039(12)
O4 0.188(8) 0.136(7) 0.271(11) -0.011(7) 0.032(7) 0.037(6)
N1 0.060(2) 0.045(2) 0.037(2) -0.001(2) 0.002(2) 0.003(2)
N2 0.059(2) 0.064(3) 0.037(2) -0.001(2) 0.001(2) 0.000(2)
N3 0.065(2) 0.048(2) 0.043(2) -0.002(2) 0.005(2) 0.003(2)
N4 0.076(3) 0.060(3) 0.034(2) -0.001(2) 0.005(2) -0.008(2)
N5 0.076(3) 0.058(3) 0.046(2) -0.009(2) 0.005(2) 0.000(2)
C1 0.064(3) 0.048(3) 0.047(3) -0.009(2) 0.006(2) 0.006(2)
C2 0.099(4) 0.041(3) 0.072(4) 0.006(3) -0.002(3) 0.009(3)
C3 0.146(6) 0.056(4) 0.066(4) 0.018(3) -0.004(4) -0.001(4)
C4 0.124(5) 0.069(4) 0.042(3) 0.012(3) -0.002(3) 0.012(4)
C5 0.067(3) 0.056(3) 0.042(3) 0.004(2) 0.002(2) 0.006(2)
C6 0.067(3) 0.062(3) 0.040(3) -0.007(2) 0.003(2) -0.002(2)
C7 0.068(3) 0.063(3) 0.044(3) 0.000(2) -0.003(2) -0.014(3)
C8 0.088(4) 0.069(4) 0.084(4) -0.016(3) -0.020(3) -0.007(3)
C9 0.055(3) 0.069(3) 0.055(3) -0.001(3) -0.001(2) 0.000(3)
C10 0.058(3) 0.063(3) 0.043(3) 0.012(2) 0.006(2) 0.002(2)
C11 0.077(4) 0.076(4) 0.062(3) 0.004(3) 0.001(3) 0.015(3)
C12 0.072(3) 0.066(3) 0.045(3) -0.010(3) -0.006(2) -0.001(3)
C13 0.090(4) 0.079(4) 0.042(3) -0.023(3) 0.019(3) -0.016(3)
C14 0.190(8) 0.093(5) 0.042(3) -0.012(3) 0.011(4) -0.007(5)
C15 0.089(4) 0.068(4) 0.063(4) -0.025(3) 0.026(3) -0.022(3)
C16 0.071(3) 0.052(3) 0.062(3) -0.007(3) 0.015(3) -0.005(3)
C17 0.109(5) 0.061(4) 0.081(4) -0.005(3) -0.001(4) 0.015(3)
C18 0.075(3) 0.054(3) 0.041(3) -0.008(2) 0.006(2) -0.017(2)
C19 0.095(4) 0.048(3) 0.069(4) 0.002(3) 0.021(3) 0.007(3)
C20 0.109(5) 0.062(4) 0.125(7) 0.005(4) 0.030(5) 0.012(4)
C21 0.122(6) 0.080(5) 0.131(7) -0.037(5) 0.069(6) -0.013(5)
C22 0.101(5) 0.090(5) 0.071(4) -0.020(4) 0.032(4) -0.031(4)
C23 0.081(4) 0.082(4) 0.039(3) -0.009(3) 0.009(3) -0.020(3)
C24 0.064(3) 0.065(3) 0.033(2) 0.008(2) -0.003(2) -0.011(2)
C25 0.085(4) 0.068(4) 0.040(3) -0.003(3) -0.010(3) -0.009(3)
C26 0.089(4) 0.109(6) 0.049(3) -0.009(4) -0.009(3) -0.013(4)
C27 0.108(5) 0.128(7) 0.051(4) 0.014(4) -0.030(3) 0.001(5)
C28 0.141(6) 0.073(4) 0.071(4) 0.026(4) -0.024(4) -0.010(4)
C29 0.100(4) 0.067(4) 0.056(3) 0.007(3) -0.015(3) -0.015(3)
C30 0.072(3) 0.046(3) 0.037(2) -0.006(2) -0.006(2) -0.014(2)

_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
Cu N5 2.052(4) . ?
Cu N3 2.091(4) . ?
Cu N1 2.111(4) . ?
Cu P 2.2163(14) . ?
Cl O4 1.338(8) . ?
Cl O2 1.349(13) . ?
Cl O1 1.363(8) . ?
Cl O3 1.406(12) . ?
P C18 1.814(6) . ?
P C24 1.837(5) . ?
P C30 1.841(4) . ?
N1 C1 1.340(6) . ?
N1 C5 1.360(6) . ?
N2 C7 1.353(6) . ?
N2 N3 1.367(5) . ?
N2 C6 1.448(6) . ?
N3 C10 1.341(6) . ?
N4 C13 1.357(6) . ?
N4 N5 1.366(6) . ?
N4 C12 1.444(7) . ?
N5 C16 1.337(7) . ?
C1 C2 1.383(7) . ?
C1 C6 1.506(6) . ?
C2 C3 1.393(8) . ?
C3 C4 1.349(9) . ?
C4 C5 1.369(7) . ?
C5 C12 1.495(7) . ?
C7 C9 1.351(7) . ?
C7 C8 1.505(8) . ?
C9 C10 1.384(7) . ?
C10 C11 1.500(8) . ?
C13 C15 1.354(8) . ?
C13 C14 1.496(8) . ?
C15 C16 1.407(8) . ?
C16 C17 1.496(8) . ?
C18 C19 1.368(7) . ?
C18 C23 1.404(7) . ?
C19 C20 1.379(9) . ?
C20 C21 1.406(11) . ?
C21 C22 1.362(10) . ?
C22 C23 1.383(9) . ?
C24 C25 1.363(7) . ?
C24 C29 1.393(8) . ?
C25 C26 1.388(8) . ?
C26 C27 1.360(10) . ?
C27 C28 1.351(9) . ?
C28 C29 1.349(8) . ?
C30 C30 1.552(9) 7 ?

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
N5 Cu N3 120.6(2) . . ?
N5 Cu N1 93.9(2) . . ?
N3 Cu N1 88.97(15) . . ?
N5 Cu P 115.77(13) . . ?
N3 Cu P 109.58(11) . . ?
N1 Cu P 125.67(11) . . ?
O4 Cl O2 113.2(8) . . ?
O4 Cl O1 114.9(6) . . ?
O2 Cl O1 106.1(8) . . ?
O4 Cl O3 110.0(7) . . ?
O2 Cl O3 101.0(9) . . ?
O1 Cl O3 110.7(7) . . ?
C18 P C24 103.1(2) . . ?
C18 P C30 101.6(2) . . ?
C24 P C30 103.8(2) . . ?
C18 P Cu 115.9(2) . . ?
C24 P Cu 114.4(2) . . ?
C30 P Cu 116.3(2) . . ?
C1 N1 C5 118.2(4) . . ?
C1 N1 Cu 118.9(3) . . ?
C5 N1 Cu 119.3(3) . . ?
C7 N2 N3 111.2(4) . . ?
C7 N2 C6 129.3(4) . . ?
N3 N2 C6 119.4(4) . . ?
C10 N3 N2 104.8(4) . . ?
C10 N3 Cu 138.2(4) . . ?
N2 N3 Cu 116.5(3) . . ?
C13 N4 N5 111.3(5) . . ?
C13 N4 C12 127.1(5) . . ?
N5 N4 C12 119.5(4) . . ?
C16 N5 N4 105.7(4) . . ?
C16 N5 Cu 133.9(4) . . ?
N4 N5 Cu 120.3(3) . . ?
N1 C1 C2 123.2(5) . . ?
N1 C1 C6 114.6(4) . . ?
C2 C1 C6 122.1(5) . . ?
C1 C2 C3 117.5(5) . . ?
C4 C3 C2 119.1(5) . . ?
C3 C4 C5 121.4(5) . . ?
N1 C5 C4 120.5(5) . . ?
N1 C5 C12 116.3(4) . . ?
C4 C5 C12 122.9(5) . . ?
N2 C6 C1 112.0(4) . . ?
C9 C7 N2 106.7(5) . . ?
C9 C7 C8 131.7(5) . . ?
N2 C7 C8 121.6(5) . . ?
C7 C9 C10 107.1(5) . . ?
N3 C10 C9 110.2(5) . . ?
N3 C10 C11 120.6(5) . . ?
C9 C10 C11 129.2(5) . . ?
N4 C12 C5 114.0(4) . . ?
C15 C13 N4 106.5(5) . . ?
C15 C13 C14 130.5(6) . . ?
N4 C13 C14 123.0(6) . . ?
C13 C15 C16 107.1(5) . . ?
N5 C16 C15 109.3(5) . . ?
N5 C16 C17 121.2(5) . . ?
C15 C16 C17 129.5(5) . . ?
C19 C18 C23 118.7(5) . . ?
C19 C18 P 119.0(4) . . ?
C23 C18 P 122.3(4) . . ?
C18 C19 C20 122.4(6) . . ?
C19 C20 C21 118.1(7) . . ?
C22 C21 C20 120.2(7) . . ?
C21 C22 C23 121.0(6) . . ?
C22 C23 C18 119.5(6) . . ?
C25 C24 C29 118.4(5) . . ?
C25 C24 P 118.3(4) . . ?
C29 C24 P 123.2(4) . . ?
C24 C25 C26 120.0(6) . . ?
C27 C26 C25 119.9(6) . . ?
C28 C27 C26 120.2(6) . . ?
C29 C28 C27 120.6(6) . . ?
C28 C29 C24 120.8(6) . . ?
C30 C30 P 110.0(4) 7 . ?

_refine_diff_density_max    0.495
_refine_diff_density_min   -0.331
_refine_diff_density_rms    0.062