# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_mf933
_audit_creation_date             2014-07-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C23 H37 Fe N2 P'
_chemical_formula_sum            'C23 H37 Fe N2 P'
_chemical_formula_weight         428.36
_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 0.0030 0.0020 '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'
Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1020 0.0940 '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                   8.526(3)
_cell_length_b                   11.951(3)
_cell_length_c                   12.272(4)
_cell_angle_alpha                69.55(2)
_cell_angle_beta                 87.64(3)
_cell_angle_gamma                80.07(3)
_cell_volume                     1153.8(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    90
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   0.873
_shelx_estimated_absorpt_T_min   0.784
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  .7460
_exptl_absorpt_correction_T_min  .6655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.19
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26609
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.084
_diffrn_reflns_theta_min         1.771
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  ?
_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                5811
_reflns_number_total             6724
_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 > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         6724
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0313
_refine_ls_restrained_S_all      1.050
_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/[σ²(Fo²)+(0.0393P)²+0.6912P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0852
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H13(0.022) H12(0.025) H11(0.024) H15(0.023) H17A(0.044)
 H17B(0.044) H17C(0.044) H16A(0.035) H16B(0.035) H16C(0.035) H8(0.026)
 H10A(0.06) H10B(0.06) H10C(0.06) H9A(0.049) H9B(0.049) H9C(0.049) H5A(0.023)
 H5B(0.023) H4A(0.027) H4B(0.027) H3A(0.025) H3B(0.025) H18(0.025) H19A(0.056)
 H19B(0.056) H19C(0.056) H20A(0.056) H20B(0.056) H20C(0.056) H21(0.031)
 H22A(0.05) H22B(0.05) H22C(0.05) H23A(0.062) H23B(0.062) H23C(0.062)
 Fixed X: H13(0.252) H12(0.1358) H11(-0.0941) H15(0.093801) H17A(0.3535)
 H17B(0.3857) H17C(0.254) H16A(0.298901) H16B(0.1664) H16C(0.3315) H8(-
 0.295601) H10A(-0.318199) H10B(-0.1401) H10C(-0.181499) H9A(-0.4891) H9B(-
 0.361799) H9C(-0.4221) H5A(-0.354199) H5B(-0.1929) H4A(-0.4477) H4B(-0.2731)
 H3A(-0.3652) H3B(-0.484099) H18(-0.0432) H19A(0.135301) H19B(0.153101)
 H19C(0.0598) H20A(-0.257401) H20B(-0.184) H20C(-0.0901) H21(-0.436399) H22A(-
 0.4951) H22B(-0.569) H22C(-0.408199) H23A(-0.2702) H23B(-0.2703) H23C(-
 0.431299)
 Fixed Y: H13(0.3397) H12(0.2535) H11(0.1707) H15(0.3822) H17A(0.2962)
 H17B(0.2291) H17C(0.192901) H16A(0.497399) H16B(0.5297) H16C(0.4438)
 H8(0.156301) H10A(-0.0284) H10B(-0.029601) H10C(-0.0086) H9A(0.163701)
 H9B(0.1925) H9C(0.2888) H5A(0.406599) H5B(0.463301) H4A(0.561901) H4B(0.5677)
 H3A(0.4674) H3B(0.406899) H18(0.2089) H19A(0.221601) H19B(0.3184)
 H19C(0.361201) H20A(0.367701) H20B(0.4519) H20C(0.4088) H21(0.2627)
 H22A(0.1724) H22B(0.108001) H22C(0.0429) H23A(0.1444) H23B(0.0255) H23C(0.0906)
 Fixed Z: H13(-0.0121) H12(-0.1251) H11(-0.062901) H15(0.246099)
 H17A(0.325801) H17B(0.232699) H17C(0.3296) H16A(0.1773) H16B(0.077399)
 H16C(0.0743) H8(0.2039) H10A(0.1805) H10B(0.218101) H10C(0.0856) H9A(0.067201)
 H9B(-0.0341) H9C(0.028501) H5A(0.164901) H5B(0.1491) H4A(0.2299) H4B(0.2709)
 H3A(0.4502) H3B(0.3976) H18(0.7038) H19A(0.5496) H19B(0.609301) H19C(0.4872)
 H20A(0.6897) H20B(0.5742) H20C(0.6961) H21(0.627301) H22A(0.4931) H22B(0.6167)
 H22C(0.5772) H23A(0.7931) H23B(0.761301) H23C(0.8006)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_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
C6 C -0.03632(15) 0.24624(11) 0.16230(10) 0.0145(2) Uani 1 1 d . . . . .
C14 C 0.09848(15) 0.30205(11) 0.12245(10) 0.0155(2) Uani 1 1 d . . . . .
C13 C 0.16030(16) 0.30361(12) 0.01499(11) 0.0180(2) Uani 1 1 d . . . . .
H13 H 0.2520 0.3397 -0.0121 0.022 Uiso 1 1 d . . . . .
C12 C 0.09062(17) 0.25344(13) -0.05304(11) 0.0204(3) Uani 1 1 d . . . . .
H12 H 0.1358 0.2535 -0.1251 0.025 Uiso 1 1 d . . . . .
C11 C -0.04512(17) 0.20320(12) -0.01526(11) 0.0196(2) Uani 1 1 d . . . . .
H11 H -0.0941 0.1707 -0.0629 0.024 Uiso 1 1 d . . . . .
C7 C -0.11139(15) 0.19953(12) 0.09176(11) 0.0168(2) Uani 1 1 d . . . . .
C15 C 0.17768(16) 0.35569(12) 0.19678(11) 0.0190(2) Uani 1 1 d . . . . .
H15 H 0.0938 0.3822 0.2461 0.023 Uiso 1 1 d . . . . .
C17 C 0.3041(2) 0.25991(15) 0.27853(13) 0.0291(3) Uani 1 1 d . . . . .
H17A H 0.3535 0.2962 0.3258 0.044 Uiso 1 1 d . . . . .
H17B H 0.3857 0.2291 0.2327 0.044 Uiso 1 1 d . . . . .
H17C H 0.2540 0.1929 0.3296 0.044 Uiso 1 1 d . . . . .
C16 C 0.25009(18) 0.46657(13) 0.12501(12) 0.0232(3) Uani 1 1 d . . . . .
H16A H 0.2989 0.4974 0.1773 0.035 Uiso 1 1 d . . . . .
H16B H 0.1664 0.5297 0.0774 0.035 Uiso 1 1 d . . . . .
H16C H 0.3315 0.4438 0.0743 0.035 Uiso 1 1 d . . . . .
C8 C -0.25962(16) 0.14287(13) 0.13015(12) 0.0214(3) Uani 1 1 d . . . . .
H8 H -0.2956 0.1563 0.2039 0.026 Uiso 1 1 d . . . . .
C10 C -0.2214(2) 0.00705(16) 0.15590(19) 0.0399(4) Uani 1 1 d . . . . .
H10A H -0.3182 -0.0284 0.1805 0.060 Uiso 1 1 d . . . . .
H10B H -0.1401 -0.0296 0.2181 0.060 Uiso 1 1 d . . . . .
H10C H -0.1815 -0.0086 0.0856 0.060 Uiso 1 1 d . . . . .
C9 C -0.39537(19) 0.20234(18) 0.03981(15) 0.0327(3) Uani 1 1 d . . . . .
H9A H -0.4891 0.1637 0.0672 0.049 Uiso 1 1 d . . . . .
H9B H -0.3618 0.1925 -0.0341 0.049 Uiso 1 1 d . . . . .
H9C H -0.4221 0.2888 0.0285 0.049 Uiso 1 1 d . . . . .
C1 C -0.19206(15) 0.31538(11) 0.30299(10) 0.0154(2) Uani 1 1 d . . . . .
C5 C -0.27183(16) 0.42685(12) 0.20601(11) 0.0192(2) Uani 1 1 d . . . . .
H5A H -0.3542 0.4066 0.1649 0.023 Uiso 1 1 d . . . . .
H5B H -0.1929 0.4633 0.1491 0.023 Uiso 1 1 d . . . . .
C4 C -0.34661(18) 0.51272(13) 0.26886(12) 0.0227(3) Uani 1 1 d . . . . .
H4A H -0.4477 0.5619 0.2299 0.027 Uiso 1 1 d . . . . .
H4B H -0.2731 0.5677 0.2709 0.027 Uiso 1 1 d . . . . .
C3 C -0.37654(17) 0.42892(13) 0.39213(12) 0.0207(3) Uani 1 1 d . . . . .
H3A H -0.3652 0.4674 0.4502 0.025 Uiso 1 1 d . . . . .
H3B H -0.4841 0.4069 0.3976 0.025 Uiso 1 1 d . . . . .
C2 C -0.24731(16) 0.31850(12) 0.40943(11) 0.0168(2) Uani 1 1 d . . . . .
C18 C -0.07234(17) 0.27285(13) 0.62608(12) 0.0209(3) Uani 1 1 d . . . . .
H18 H -0.0432 0.2089 0.7038 0.025 Uiso 1 1 d . . . . .
C19 C 0.0828(2) 0.29553(19) 0.56237(16) 0.0371(4) Uani 1 1 d . . . . .
H19A H 0.1353 0.2216 0.5496 0.056 Uiso 1 1 d . . . . .
H19B H 0.1531 0.3184 0.6093 0.056 Uiso 1 1 d . . . . .
H19C H 0.0598 0.3612 0.4872 0.056 Uiso 1 1 d . . . . .
C20 C -0.1587(2) 0.38537(16) 0.64855(17) 0.0374(4) Uani 1 1 d . . . . .
H20A H -0.2574 0.3677 0.6897 0.056 Uiso 1 1 d . . . . .
H20B H -0.1840 0.4519 0.5742 0.056 Uiso 1 1 d . . . . .
H20C H -0.0901 0.4088 0.6961 0.056 Uiso 1 1 d . . . . .
C21 C -0.37276(18) 0.18317(15) 0.63030(12) 0.0257(3) Uani 1 1 d . . . . .
H21 H -0.4364 0.2627 0.6273 0.031 Uiso 1 1 d . . . . .
C22 C -0.4699(2) 0.12109(17) 0.57427(14) 0.0336(4) Uani 1 1 d . . . . .
H22A H -0.4951 0.1724 0.4931 0.050 Uiso 1 1 d . . . . .
H22B H -0.5690 0.1080 0.6167 0.050 Uiso 1 1 d . . . . .
H22C H -0.4082 0.0429 0.5772 0.050 Uiso 1 1 d . . . . .
C23 C -0.3325(2) 0.1038(2) 0.75792(13) 0.0410(5) Uani 1 1 d . . . . .
H23A H -0.2702 0.1444 0.7931 0.062 Uiso 1 1 d . . . . .
H23B H -0.2703 0.0255 0.7613 0.062 Uiso 1 1 d . . . . .
H23C H -0.4313 0.0906 0.8006 0.062 Uiso 1 1 d . . . . .
N1 N -0.08758(13) 0.22815(10) 0.27872(9) 0.0161(2) Uani 1 1 d . . . . .
N2 N -0.09205(16) 0.08606(10) 0.54375(10) 0.0225(2) Uani 1 1 d . . . . .
P1 P -0.19077(4) 0.20963(3) 0.54782(3) 0.01575(7) Uani 1 1 d . . . . .
Fe1 Fe -0.01473(2) 0.07380(2) 0.39808(2) 0.01759(6) Uani 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
C6 C14 1.4125(19) . ?
C6 C7 1.4062(18) . ?
C6 N1 1.4298(15) . ?
C14 C13 1.3951(17) . ?
C14 C15 1.5191(18) . ?
C13 C12 1.3866(19) . ?
C12 C11 1.384(2) . ?
C11 C7 1.3975(18) . ?
C7 C8 1.5168(19) . ?
C15 C17 1.529(2) . ?
C15 C16 1.528(2) . ?
C8 C10 1.519(2) . ?
C8 C9 1.531(2) . ?
C1 C5 1.5166(18) . ?
C1 C2 1.3809(17) . ?
C1 N1 1.3578(17) . ?
C5 C4 1.5302(19) . ?
C4 C3 1.534(2) . ?
C3 C2 1.5240(19) . ?
C2 P1 1.7654(14) . ?
C18 C19 1.525(2) . ?
C18 C20 1.526(2) . ?
C18 P1 1.8338(15) . ?
C21 C22 1.525(2) . ?
C21 C23 1.538(2) . ?
C21 P1 1.8298(16) . ?
N1 Fe1 1.9303(13) . ?
N2 P1 1.5847(13) . ?
N2 Fe1 1.8678(14) 2_556 ?
N2 Fe1 1.9247(13) . ?
Fe1 N2 1.8678(14) 2_556 ?
Fe1 Fe1 2.4996(9) 2_556 ?

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
C14 C6 N1 119.42(11) . . ?
C7 C6 C14 120.35(11) . . ?
C7 C6 N1 120.02(11) . . ?
C6 C14 C15 120.69(11) . . ?
C13 C14 C6 118.62(12) . . ?
C13 C14 C15 120.67(12) . . ?
C12 C13 C14 121.31(12) . . ?
C11 C12 C13 119.61(12) . . ?
C12 C11 C7 121.14(12) . . ?
C6 C7 C8 121.71(11) . . ?
C11 C7 C6 118.87(12) . . ?
C11 C7 C8 119.41(12) . . ?
C14 C15 C17 110.75(12) . . ?
C14 C15 C16 113.07(11) . . ?
C16 C15 C17 110.22(12) . . ?
C7 C8 C10 110.32(12) . . ?
C7 C8 C9 111.57(12) . . ?
C10 C8 C9 111.15(14) . . ?
C2 C1 C5 110.05(11) . . ?
N1 C1 C5 120.77(11) . . ?
N1 C1 C2 129.13(12) . . ?
C1 C5 C4 103.91(11) . . ?
C5 C4 C3 104.59(11) . . ?
C2 C3 C4 102.95(11) . . ?
C1 C2 C3 110.04(11) . . ?
C1 C2 P1 127.17(10) . . ?
C3 C2 P1 122.70(9) . . ?
C19 C18 C20 111.57(14) . . ?
C19 C18 P1 109.07(10) . . ?
C20 C18 P1 115.00(11) . . ?
C22 C21 C23 110.11(14) . . ?
C22 C21 P1 108.62(10) . . ?
C23 C21 P1 110.69(12) . . ?
C6 N1 Fe1 118.44(8) . . ?
C1 N1 C6 120.47(11) . . ?
C1 N1 Fe1 120.99(9) . . ?
P1 N2 Fe1 157.30(7) . 2_556 ?
P1 N2 Fe1 120.17(7) . . ?
Fe1 N2 Fe1 82.44(5) 2_556 . ?
C2 P1 C18 109.34(7) . . ?
C2 P1 C21 107.44(7) . . ?
C21 P1 C18 106.43(7) . . ?
N2 P1 C2 113.94(6) . . ?
N2 P1 C18 108.85(7) . . ?
N2 P1 C21 110.57(8) . . ?
N1 Fe1 Fe1 154.91(4) . 2_556 ?
N2 Fe1 N1 107.11(5) . . ?
N2 Fe1 N1 155.34(5) 2_556 . ?
N2 Fe1 N2 97.55(5) 2_556 . ?
N2 Fe1 Fe1 49.76(4) 2_556 2_556 ?
N2 Fe1 Fe1 47.80(4) . 2_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C14 C13 C12 1.00(19) . . . . ?
C6 C14 C15 C17 88.21(15) . . . . ?
C6 C14 C15 C16 -147.52(12) . . . . ?
C6 C7 C8 C10 -110.31(16) . . . . ?
C6 C7 C8 C9 125.63(14) . . . . ?
C14 C6 C7 C11 3.57(18) . . . . ?
C14 C6 C7 C8 -177.89(12) . . . . ?
C14 C6 N1 C1 88.76(15) . . . . ?
C14 C6 N1 Fe1 -94.83(12) . . . . ?
C14 C13 C12 C11 1.5(2) . . . . ?
C13 C14 C15 C17 -89.81(15) . . . . ?
C13 C14 C15 C16 34.46(17) . . . . ?
C13 C12 C11 C7 -1.5(2) . . . . ?
C12 C11 C7 C6 -1.0(2) . . . . ?
C12 C11 C7 C8 -179.60(13) . . . . ?
C11 C7 C8 C10 68.23(18) . . . . ?
C11 C7 C8 C9 -55.83(17) . . . . ?
C7 C6 C14 C13 -3.55(18) . . . . ?
C7 C6 C14 C15 178.38(11) . . . . ?
C7 C6 N1 C1 -96.61(15) . . . . ?
C7 C6 N1 Fe1 79.79(13) . . . . ?
C15 C14 C13 C12 179.06(12) . . . . ?
C1 C5 C4 C3 -26.72(14) . . . . ?
C1 C2 P1 C18 109.59(13) . . . . ?
C1 C2 P1 C21 -135.29(13) . . . . ?
C1 C2 P1 N2 -12.45(15) . . . . ?
C5 C1 C2 C3 3.42(15) . . . . ?
C5 C1 C2 P1 179.95(10) . . . . ?
C5 C1 N1 C6 7.44(18) . . . . ?
C5 C1 N1 Fe1 -168.87(9) . . . . ?
C5 C4 C3 C2 28.40(14) . . . . ?
C4 C3 C2 C1 -20.18(15) . . . . ?
C4 C3 C2 P1 163.10(10) . . . . ?
C3 C2 P1 C18 -74.28(13) . . . . ?
C3 C2 P1 C21 40.84(13) . . . . ?
C3 C2 P1 N2 163.69(11) . . . . ?
C2 C1 C5 C4 14.89(15) . . . . ?
C2 C1 N1 C6 -175.35(13) . . . . ?
C2 C1 N1 Fe1 8.33(19) . . . . ?
C19 C18 P1 C2 -64.98(13) . . . . ?
C19 C18 P1 C21 179.25(11) . . . . ?
C19 C18 P1 N2 60.06(13) . . . . ?
C20 C18 P1 C2 61.19(14) . . . . ?
C20 C18 P1 C21 -54.57(14) . . . . ?
C20 C18 P1 N2 -173.76(12) . . . . ?
C22 C21 P1 C2 67.42(13) . . . . ?
C22 C21 P1 C18 -175.54(11) . . . . ?
C22 C21 P1 N2 -57.48(13) . . . . ?
C23 C21 P1 C2 -171.57(12) . . . . ?
C23 C21 P1 C18 -54.54(14) . . . . ?
C23 C21 P1 N2 63.53(14) . . . . ?
N1 C6 C14 C13 171.05(11) . . . . ?
N1 C6 C14 C15 -7.01(17) . . . . ?
N1 C6 C7 C11 -171.01(12) . . . . ?
N1 C6 C7 C8 7.53(18) . . . . ?
N1 C1 C5 C4 -167.42(12) . . . . ?
N1 C1 C2 C3 -174.02(13) . . . . ?
N1 C1 C2 P1 2.5(2) . . . . ?
Fe1 N2 P1 C2 -175.4(2) 2_556 . . . ?
Fe1 N2 P1 C2 9.97(11) . . . . ?
Fe1 N2 P1 C18 62.3(2) 2_556 . . . ?
Fe1 N2 P1 C18 -112.34(9) . . . . ?
Fe1 N2 P1 C21 -54.3(2) 2_556 . . . ?
Fe1 N2 P1 C21 131.09(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_database_code_depnum_ccdc_archive 'CCDC 1028480'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_mo_mf936_0m
_audit_creation_date             2014-07-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C31 H47 N4 P'
_chemical_formula_sum            'C31 H47 N4 P'
_chemical_formula_weight         506.70
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   8.4137(10)
_cell_length_b                   12.3149(14)
_cell_length_c                   16.0458(19)
_cell_angle_alpha                68.433(2)
_cell_angle_beta                 80.379(2)
_cell_angle_gamma                83.219(3)
_cell_volume                     1521.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    90
_cell_measurement_theta_max      29.687
_cell_measurement_theta_min      2.460
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0604 before and 0.0336 after correction. The Ratio of minimum to maximum transmission is 0.9536. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32276
_diffrn_reflns_theta_full        29.71
_diffrn_reflns_theta_max         29.71
_diffrn_reflns_theta_min         1.38
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                7553
_reflns_number_total             8629
_reflns_threshold_expression     >2σ(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         8629
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0372
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0503P)²+0.5686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1026
_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 > 2σ(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.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21), C18(H18), C8(H8), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C3(H3a,H3b), C4(H4a,H4b)
2.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C13(H13), C27(H27), C11(H11), C29(H29), C12(H12)
2.d Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C19(H19a,H19b,H19c), C9(H9a,H9b,H9c), C16(H16a,H16b,
 H16c), C20(H20a,H20b,H20c), C31(H31a,H31b,H31c), C17(H17a,H17b,H17c), C23(H23a,
 H23b,H23c), C10(H10a,H10b,H10c), C22(H22a,H22b,H22c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
P1 P 0.16519(3) 0.47824(2) 0.220001(16) 0.01257(6) Uani 1 1 d . . .
N3 N -0.10360(10) 0.58281(7) 0.21578(5) 0.01354(15) Uani 1 1 d . . .
N4 N -0.25612(10) 0.58384(7) 0.23328(6) 0.01560(16) Uani 1 1 d . . .
N1 N -0.01112(10) 0.23899(7) 0.25505(6) 0.01391(15) Uani 1 1 d . . .
N2 N -0.03182(10) 0.47295(7) 0.23997(6) 0.01525(16) Uani 1 1 d . . .
C2 C 0.24042(11) 0.33434(8) 0.23448(7) 0.01491(17) Uani 1 1 d . . .
C24 C -0.32720(11) 0.70078(8) 0.20458(6) 0.01327(17) Uani 1 1 d . . .
C6 C -0.09744(11) 0.13578(8) 0.30474(7) 0.01509(18) Uani 1 1 d . . .
C21 C 0.24841(13) 0.52419(10) 0.29932(7) 0.0209(2) Uani 1 1 d . . .
H21 H 0.3687 0.5219 0.2842 0.025 Uiso 1 1 calc R . .
C28 C -0.49448(13) 0.91834(9) 0.15438(8) 0.0227(2) Uani 1 1 d . . .
H28 H -0.5526 0.9924 0.1370 0.027 Uiso 1 1 calc R . .
C14 C -0.10976(12) 0.05480(9) 0.26352(7) 0.01728(18) Uani 1 1 d . . .
C18 C 0.23027(12) 0.57799(8) 0.10561(7) 0.01579(18) Uani 1 1 d . . .
H18 H 0.1688 0.6550 0.0977 0.019 Uiso 1 1 calc R . .
C30 C -0.31587(11) 0.77194(9) 0.11285(7) 0.01530(18) Uani 1 1 d . . .
C1 C 0.15164(11) 0.24021(8) 0.25285(6) 0.01397(17) Uani 1 1 d . . .
C7 C -0.17242(12) 0.12050(9) 0.39330(7) 0.01841(19) Uani 1 1 d . . .
C13 C -0.19522(13) -0.04466(9) 0.31406(8) 0.0227(2) Uani 1 1 d . . .
H13 H -0.2020 -0.1020 0.2884 0.027 Uiso 1 1 calc R . .
C27 C -0.50340(13) 0.84776(10) 0.24475(7) 0.0215(2) Uani 1 1 d . . .
H27 H -0.5667 0.8743 0.2892 0.026 Uiso 1 1 calc R . .
C25 C -0.42057(12) 0.73831(9) 0.27124(7) 0.01668(18) Uani 1 1 d . . .
C5 C 0.26002(13) 0.12970(9) 0.26866(8) 0.0233(2) Uani 1 1 d . . .
H5A H 0.2745 0.1046 0.2158 0.028 Uiso 1 1 calc R . .
H5B H 0.2152 0.0655 0.3229 0.028 Uiso 1 1 calc R . .
C11 C -0.26003(14) 0.02146(10) 0.44009(8) 0.0255(2) Uani 1 1 d . . .
H11 H -0.3135 0.0102 0.4994 0.031 Uiso 1 1 calc R . .
C26 C -0.42649(15) 0.66164(11) 0.36931(7) 0.0257(2) Uani 1 1 d . . .
H26A H -0.4572 0.5837 0.3775 0.039 Uiso 1 1 calc R . .
H26B H -0.5062 0.6961 0.4060 0.039 Uiso 1 1 calc R . .
H26C H -0.3199 0.6552 0.3883 0.039 Uiso 1 1 calc R . .
C19 C 0.18099(15) 0.53035(11) 0.03887(7) 0.0250(2) Uani 1 1 d . . .
H19A H 0.2446 0.4572 0.0422 0.037 Uiso 1 1 calc R . .
H19B H 0.2008 0.5878 -0.0226 0.037 Uiso 1 1 calc R . .
H19C H 0.0659 0.5155 0.0541 0.037 Uiso 1 1 calc R . .
C9 C -0.30358(14) 0.30399(10) 0.41440(8) 0.0253(2) Uani 1 1 d . . .
H9A H -0.3002 0.3426 0.3488 0.038 Uiso 1 1 calc R . .
H9B H -0.2953 0.3622 0.4415 0.038 Uiso 1 1 calc R . .
H9C H -0.4057 0.2660 0.4398 0.038 Uiso 1 1 calc R . .
C3 C 0.41976(12) 0.29653(10) 0.23187(8) 0.0235(2) Uani 1 1 d . . .
H3A H 0.4746 0.3345 0.2630 0.028 Uiso 1 1 calc R . .
H3B H 0.4736 0.3152 0.1689 0.028 Uiso 1 1 calc R . .
C8 C -0.16206(13) 0.21174(10) 0.43494(7) 0.0209(2) Uani 1 1 d . . .
H8 H -0.0601 0.2523 0.4057 0.025 Uiso 1 1 calc R . .
C15 C -0.04391(13) 0.07786(9) 0.16478(7) 0.0200(2) Uani 1 1 d . . .
H15 H 0.0400 0.1364 0.1467 0.024 Uiso 1 1 calc R . .
C29 C -0.40061(13) 0.88087(9) 0.08911(7) 0.0201(2) Uani 1 1 d . . .
H29 H -0.3940 0.9302 0.0273 0.024 Uiso 1 1 calc R . .
C16 C -0.17991(16) 0.13247(12) 0.10663(8) 0.0311(3) Uani 1 1 d . . .
H16A H -0.2650 0.0774 0.1238 0.047 Uiso 1 1 calc R . .
H16B H -0.1369 0.1502 0.0427 0.047 Uiso 1 1 calc R . .
H16C H -0.2248 0.2048 0.1161 0.047 Uiso 1 1 calc R . .
C20 C 0.40980(14) 0.59990(11) 0.08615(8) 0.0275(2) Uani 1 1 d . . .
H20A H 0.4366 0.6329 0.1287 0.041 Uiso 1 1 calc R . .
H20B H 0.4346 0.6550 0.0242 0.041 Uiso 1 1 calc R . .
H20C H 0.4734 0.5259 0.0930 0.041 Uiso 1 1 calc R . .
C12 C -0.27017(14) -0.06064(10) 0.40124(8) 0.0271(2) Uani 1 1 d . . .
H12 H -0.3287 -0.1282 0.4345 0.033 Uiso 1 1 calc R . .
C31 C -0.21963(13) 0.73149(10) 0.04051(7) 0.0216(2) Uani 1 1 d . . .
H31A H -0.1052 0.7439 0.0363 0.032 Uiso 1 1 calc R . .
H31B H -0.2581 0.7762 -0.0177 0.032 Uiso 1 1 calc R . .
H31C H -0.2330 0.6481 0.0559 0.032 Uiso 1 1 calc R . .
C17 C 0.03531(17) -0.03096(11) 0.14665(10) 0.0334(3) Uani 1 1 d . . .
H17A H 0.1166 -0.0680 0.1874 0.050 Uiso 1 1 calc R . .
H17B H 0.0872 -0.0084 0.0838 0.050 Uiso 1 1 calc R . .
H17C H -0.0471 -0.0862 0.1571 0.050 Uiso 1 1 calc R . .
C23 C 0.18779(16) 0.64983(11) 0.29035(9) 0.0302(3) Uani 1 1 d . . .
H23A H 0.2200 0.7027 0.2284 0.045 Uiso 1 1 calc R . .
H23B H 0.2348 0.6730 0.3328 0.045 Uiso 1 1 calc R . .
H23C H 0.0698 0.6542 0.3041 0.045 Uiso 1 1 calc R . .
C4 C 0.41872(14) 0.16431(11) 0.28230(10) 0.0329(3) Uani 1 1 d . . .
H4A H 0.5115 0.1234 0.2570 0.039 Uiso 1 1 calc R . .
H4B H 0.4243 0.1448 0.3474 0.039 Uiso 1 1 calc R . .
C10 C -0.15555(17) 0.15909(12) 0.53692(8) 0.0321(3) Uani 1 1 d . . .
H10A H -0.2598 0.1278 0.5682 0.048 Uiso 1 1 calc R . .
H10B H -0.1322 0.2199 0.5582 0.048 Uiso 1 1 calc R . .
H10C H -0.0705 0.0959 0.5497 0.048 Uiso 1 1 calc R . .
C22 C 0.20584(19) 0.43879(13) 0.39588(8) 0.0354(3) Uani 1 1 d . . .
H22A H 0.0882 0.4400 0.4121 0.053 Uiso 1 1 calc R . .
H22B H 0.2543 0.4620 0.4378 0.053 Uiso 1 1 calc R . .
H22C H 0.2477 0.3596 0.3997 0.053 Uiso 1 1 calc R . .
H1 H -0.0649(19) 0.3051(14) 0.2533(10) 0.031(4) Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N2 1.6393(9) . ?
P1 C2 1.7540(10) . ?
P1 C21 1.8307(10) . ?
P1 C18 1.8284(10) . ?
N3 N4 1.2665(11) . ?
N3 N2 1.3583(11) . ?
N4 C24 1.4300(12) . ?
N1 C6 1.4346(12) . ?
N1 C1 1.3657(12) . ?
N1 H1 0.877(16) . ?
C2 C1 1.3668(13) . ?
C2 C3 1.5241(14) . ?
C24 C30 1.4028(13) . ?
C24 C25 1.4042(13) . ?
C6 C14 1.4053(14) . ?
C6 C7 1.4087(14) . ?
C21 H21 1.0000 . ?
C21 C23 1.5327(16) . ?
C21 C22 1.5299(17) . ?
C28 H28 0.9500 . ?
C28 C27 1.3843(16) . ?
C28 C29 1.3878(15) . ?
C14 C13 1.3991(14) . ?
C14 C15 1.5201(15) . ?
C18 H18 1.0000 . ?
C18 C19 1.5268(14) . ?
C18 C20 1.5260(14) . ?
C30 C29 1.3937(14) . ?
C30 C31 1.5056(14) . ?
C1 C5 1.5094(13) . ?
C7 C11 1.3960(15) . ?
C7 C8 1.5203(15) . ?
C13 H13 0.9500 . ?
C13 C12 1.3875(17) . ?
C27 H27 0.9500 . ?
C27 C25 1.3925(14) . ?
C25 C26 1.5042(14) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C4 1.5209(17) . ?
C11 H11 0.9500 . ?
C11 C12 1.3856(18) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 C8 1.5341(15) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.5292(16) . ?
C8 H8 1.0000 . ?
C8 C10 1.5305(15) . ?
C15 H15 1.0000 . ?
C15 C16 1.5318(16) . ?
C15 C17 1.5283(15) . ?
C29 H29 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C12 H12 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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
N2 P1 C2 105.37(4) . . ?
N2 P1 C21 113.25(5) . . ?
N2 P1 C18 111.41(4) . . ?
C2 P1 C21 107.91(5) . . ?
C2 P1 C18 111.05(5) . . ?
C18 P1 C21 107.83(5) . . ?
N4 N3 N2 112.92(8) . . ?
N3 N4 C24 111.18(8) . . ?
C6 N1 H1 115.2(10) . . ?
C1 N1 C6 122.10(8) . . ?
C1 N1 H1 114.1(10) . . ?
N3 N2 P1 110.29(6) . . ?
C1 C2 P1 126.64(7) . . ?
C1 C2 C3 110.17(8) . . ?
C3 C2 P1 123.14(7) . . ?
C30 C24 N4 121.54(8) . . ?
C30 C24 C25 121.03(9) . . ?
C25 C24 N4 117.21(8) . . ?
C14 C6 N1 119.73(9) . . ?
C14 C6 C7 121.70(9) . . ?
C7 C6 N1 118.54(9) . . ?
P1 C21 H21 108.2 . . ?
C23 C21 P1 110.83(8) . . ?
C23 C21 H21 108.2 . . ?
C22 C21 P1 109.84(8) . . ?
C22 C21 H21 108.2 . . ?
C22 C21 C23 111.42(10) . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 120.00(10) . . ?
C29 C28 H28 120.0 . . ?
C6 C14 C15 121.51(9) . . ?
C13 C14 C6 118.07(10) . . ?
C13 C14 C15 120.26(9) . . ?
P1 C18 H18 107.5 . . ?
C19 C18 P1 107.97(7) . . ?
C19 C18 H18 107.5 . . ?
C20 C18 P1 114.41(7) . . ?
C20 C18 H18 107.5 . . ?
C20 C18 C19 111.55(9) . . ?
C24 C30 C31 121.55(9) . . ?
C29 C30 C24 118.42(9) . . ?
C29 C30 C31 120.00(9) . . ?
N1 C1 C2 128.07(9) . . ?
N1 C1 C5 121.36(9) . . ?
C2 C1 C5 110.55(8) . . ?
C6 C7 C8 120.55(9) . . ?
C11 C7 C6 118.07(10) . . ?
C11 C7 C8 121.35(10) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 C14 120.82(10) . . ?
C12 C13 H13 119.6 . . ?
C28 C27 H27 119.6 . . ?
C28 C27 C25 120.74(9) . . ?
C25 C27 H27 119.6 . . ?
C24 C25 C26 119.85(9) . . ?
C27 C25 C24 118.79(9) . . ?
C27 C25 C26 121.35(9) . . ?
C1 C5 H5A 111.0 . . ?
C1 C5 H5B 111.0 . . ?
C1 C5 C4 103.72(9) . . ?
H5A C5 H5B 109.0 . . ?
C4 C5 H5A 111.0 . . ?
C4 C5 H5B 111.0 . . ?
C7 C11 H11 119.5 . . ?
C12 C11 C7 120.95(10) . . ?
C12 C11 H11 119.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
C2 C3 H3A 111.2 . . ?
C2 C3 H3B 111.2 . . ?
C2 C3 C4 102.69(9) . . ?
H3A C3 H3B 109.1 . . ?
C4 C3 H3A 111.2 . . ?
C4 C3 H3B 111.2 . . ?
C7 C8 C9 110.36(9) . . ?
C7 C8 H8 107.6 . . ?
C7 C8 C10 113.20(10) . . ?
C9 C8 H8 107.6 . . ?
C10 C8 C9 110.17(9) . . ?
C10 C8 H8 107.6 . . ?
C14 C15 H15 107.8 . . ?
C14 C15 C16 109.27(9) . . ?
C14 C15 C17 113.62(9) . . ?
C16 C15 H15 107.8 . . ?
C17 C15 H15 107.8 . . ?
C17 C15 C16 110.48(10) . . ?
C28 C29 C30 121.01(10) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C13 C12 H12 119.8 . . ?
C11 C12 C13 120.34(10) . . ?
C11 C12 H12 119.8 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C5 C4 C3 105.20(9) . . ?
C5 C4 H4A 110.7 . . ?
C5 C4 H4B 110.7 . . ?
C3 C4 H4A 110.7 . . ?
C3 C4 H4B 110.7 . . ?
H4A C4 H4B 108.8 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C2 C1 N1 7.11(16) . . . . ?
P1 C2 C1 C5 -174.93(8) . . . . ?
P1 C2 C3 C4 158.96(9) . . . . ?
N3 N4 C24 C30 65.33(11) . . . . ?
N3 N4 C24 C25 -119.92(9) . . . . ?
N4 N3 N2 P1 -177.26(7) . . . . ?
N4 C24 C30 C29 174.09(9) . . . . ?
N4 C24 C30 C31 -3.86(14) . . . . ?
N4 C24 C25 C27 -174.33(9) . . . . ?
N4 C24 C25 C26 7.05(14) . . . . ?
N1 C6 C14 C13 -179.85(9) . . . . ?
N1 C6 C14 C15 -4.45(14) . . . . ?
N1 C6 C7 C11 178.18(9) . . . . ?
N1 C6 C7 C8 0.13(14) . . . . ?
N1 C1 C5 C4 -167.16(10) . . . . ?
N2 P1 C2 C1 3.72(10) . . . . ?
N2 P1 C2 C3 -173.53(8) . . . . ?
N2 P1 C21 C23 -63.86(9) . . . . ?
N2 P1 C21 C22 59.69(10) . . . . ?
N2 P1 C18 C19 -62.80(8) . . . . ?
N2 P1 C18 C20 172.36(8) . . . . ?
N2 N3 N4 C24 -178.40(7) . . . . ?
C2 P1 N2 N3 -169.63(6) . . . . ?
C2 P1 C21 C23 179.91(8) . . . . ?
C2 P1 C21 C22 -56.54(10) . . . . ?
C2 P1 C18 C19 54.33(8) . . . . ?
C2 P1 C18 C20 -70.51(9) . . . . ?
C2 C1 C5 C4 14.72(12) . . . . ?
C2 C3 C4 C5 26.96(13) . . . . ?
C24 C30 C29 C28 -0.17(15) . . . . ?
C6 N1 C1 C2 -157.39(10) . . . . ?
C6 N1 C1 C5 24.85(14) . . . . ?
C6 C14 C13 C12 2.16(16) . . . . ?
C6 C14 C15 C16 -94.69(12) . . . . ?
C6 C14 C15 C17 141.43(10) . . . . ?
C6 C7 C11 C12 1.30(16) . . . . ?
C6 C7 C8 C9 89.90(11) . . . . ?
C6 C7 C8 C10 -146.10(10) . . . . ?
C21 P1 N2 N3 72.65(8) . . . . ?
C21 P1 C2 C1 124.99(9) . . . . ?
C21 P1 C2 C3 -52.26(10) . . . . ?
C21 P1 C18 C19 172.35(7) . . . . ?
C21 P1 C18 C20 47.51(9) . . . . ?
C28 C27 C25 C24 0.19(16) . . . . ?
C28 C27 C25 C26 178.79(10) . . . . ?
C14 C6 C7 C11 0.25(15) . . . . ?
C14 C6 C7 C8 -177.79(9) . . . . ?
C14 C13 C12 C11 -0.68(18) . . . . ?
C18 P1 N2 N3 -49.11(8) . . . . ?
C18 P1 C2 C1 -117.03(9) . . . . ?
C18 P1 C2 C3 65.72(10) . . . . ?
C18 P1 C21 C23 59.88(9) . . . . ?
C18 P1 C21 C22 -176.57(8) . . . . ?
C30 C24 C25 C27 0.45(14) . . . . ?
C30 C24 C25 C26 -178.18(9) . . . . ?
C1 N1 C6 C14 -87.20(12) . . . . ?
C1 N1 C6 C7 94.84(11) . . . . ?
C1 C2 C3 C4 -18.69(12) . . . . ?
C1 C5 C4 C3 -25.75(13) . . . . ?
C7 C6 C14 C13 -1.95(15) . . . . ?
C7 C6 C14 C15 173.45(9) . . . . ?
C7 C11 C12 C13 -1.11(18) . . . . ?
C13 C14 C15 C16 80.62(12) . . . . ?
C13 C14 C15 C17 -43.26(14) . . . . ?
C27 C28 C29 C30 0.79(17) . . . . ?
C25 C24 C30 C29 -0.46(14) . . . . ?
C25 C24 C30 C31 -178.41(9) . . . . ?
C11 C7 C8 C9 -88.08(12) . . . . ?
C11 C7 C8 C10 35.91(14) . . . . ?
C3 C2 C1 N1 -175.34(10) . . . . ?
C3 C2 C1 C5 2.62(12) . . . . ?
C8 C7 C11 C12 179.33(10) . . . . ?
C15 C14 C13 C12 -173.30(10) . . . . ?
C29 C28 C27 C25 -0.80(17) . . . . ?
C31 C30 C29 C28 177.82(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_database_code_depnum_ccdc_archive 'CCDC 1028481'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_mo_mf941_0m
_audit_creation_date             2014-07-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.5(C39 H62 K N4 O2 P)'
_chemical_formula_sum            'C19.50 H31 K0.50 N2 O P0.50'
_chemical_formula_weight         344.50
_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'
K K 0.2009 0.2494 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.742(2)
_cell_length_b                   10.616(2)
_cell_length_c                   19.454(5)
_cell_angle_alpha                74.814(5)
_cell_angle_beta                 79.099(5)
_cell_angle_gamma                84.049(5)
_cell_volume                     1903.6(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.31
_cell_measurement_theta_min      2.58
_shelx_estimated_absorpt_T_max   0.959
_shelx_estimated_absorpt_T_min   0.935
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39455
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.544
_diffrn_reflns_theta_min         1.991
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9244
_reflns_number_total             11257
_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 > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         11257
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0625
_refine_ls_restrained_S_all      1.207
_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/[σ²(Fo²)+5.7861P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.1637
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C15(H15), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C5(H5a,H5b), C33(H33a,H33b), C32(H32a,H32b), C4(H4a,H4b),
 C35(H35a,H35b), C37(H37a,H37b), C36(H36a,H36b), C39(H39a,H39b), C34(H34a,H34b),
  C38(H38a,H38b)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C29(H29), C11(H11), C28(H28), C27(H27)
2.d Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C31(H31a,H31b,H31c), C9(H9a,H9b,H9c), C20(H20a,H20b,
 H20c), C17(H17a,H17b,H17c), C16(H16a,H16b,H16c), C22(H22a,H22b,H22c), C26(H26a,
 H26b,H26c), C19(H19a,H19b,H19c), C10(H10a,H10b,H10c)
;
_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
K1 K 0.05974(6) 0.35697(6) 0.73134(3) 0.01689(12) Uani 1 1 d . . . . .
P1 P 0.23877(6) 0.98374(6) 0.78274(3) 0.01144(12) Uani 1 1 d . . . . .
O1 O -0.1656(2) 0.3142(2) 0.83515(11) 0.0238(4) Uani 1 1 d . . . . .
N3 N 0.2304(2) 1.1558(2) 0.85032(11) 0.0135(4) Uani 1 1 d . . . . .
O2 O -0.0979(2) 0.2637(2) 0.64647(11) 0.0246(4) Uani 1 1 d . . . . .
N2 N 0.2152(2) 1.1392(2) 0.78617(11) 0.0137(4) Uani 1 1 d . . . . .
N4 N 0.1981(2) 1.2736(2) 0.85425(11) 0.0144(4) Uani 1 1 d . . . . .
N1 N 0.1719(2) 0.7837(2) 0.68998(11) 0.0138(4) Uani 1 1 d . . . . .
C2 C 0.2689(3) 0.9868(2) 0.69183(13) 0.0128(4) Uani 1 1 d . . . . .
C24 C 0.2157(2) 1.3025(2) 0.91935(13) 0.0126(4) Uani 1 1 d . . . . .
C30 C 0.2797(3) 1.2209(2) 0.97620(13) 0.0143(4) Uani 1 1 d . . . . .
C6 C 0.1493(3) 0.7010(2) 0.64854(13) 0.0131(4) Uani 1 1 d . . . . .
C14 C 0.0100(3) 0.6879(2) 0.63959(13) 0.0142(4) Uani 1 1 d . . . . .
C1 C 0.2351(2) 0.8935(2) 0.65905(13) 0.0128(4) Uani 1 1 d . . . . .
C25 C 0.1653(3) 1.4300(3) 0.92384(14) 0.0155(5) Uani 1 1 d . . . . .
C13 C -0.0153(3) 0.6000(3) 0.60204(13) 0.0158(5) Uani 1 1 d . . . . .
H13 H -0.1085 0.5919 0.5964 0.019 Uiso 1 1 calc R . . . .
C3 C 0.3365(3) 1.1027(3) 0.63628(13) 0.0155(5) Uani 1 1 d . . . . .
H3A H 0.4177 1.1289 0.6521 0.019 Uiso 1 1 calc R . . . .
H3B H 0.2685 1.1787 0.6270 0.019 Uiso 1 1 calc R . . . .
C18 C 0.0851(3) 0.8940(2) 0.83104(13) 0.0142(4) Uani 1 1 d . . . . .
H18 H 0.0943 0.8077 0.8185 0.017 Uiso 1 1 calc R . . . .
C12 C 0.0930(3) 0.5239(3) 0.57262(14) 0.0164(5) Uani 1 1 d . . . . .
H12 H 0.0745 0.4658 0.5461 0.020 Uiso 1 1 calc R . . . .
C21 C 0.3864(3) 0.9044(2) 0.82786(14) 0.0146(4) Uani 1 1 d . . . . .
H21 H 0.3639 0.9072 0.8798 0.017 Uiso 1 1 calc R . . . .
C15 C -0.1093(3) 0.7700(3) 0.67177(14) 0.0162(5) Uani 1 1 d . . . . .
H15 H -0.0730 0.8564 0.6687 0.019 Uiso 1 1 calc R . . . .
C23 C 0.4093(3) 0.7617(3) 0.82398(16) 0.0204(5) Uani 1 1 d . . . . .
H23A H 0.3260 0.7145 0.8497 0.031 Uiso 1 1 calc GR . . . .
H23B H 0.4905 0.7215 0.8464 0.031 Uiso 1 1 calc GR . . . .
H23C H 0.4262 0.7576 0.7733 0.031 Uiso 1 1 calc GR . . . .
C29 C 0.2941(3) 1.2714(3) 1.03359(14) 0.0179(5) Uani 1 1 d . . . . .
H29 H 0.3387 1.2177 1.0713 0.021 Uiso 1 1 calc R . . . .
C7 C 0.2590(3) 0.6205(2) 0.62029(13) 0.0143(4) Uani 1 1 d . . . . .
C5 C 0.2783(3) 0.9452(3) 0.57687(13) 0.0152(5) Uani 1 1 d . . . . .
H5A H 0.3227 0.8740 0.5545 0.018 Uiso 1 1 calc R . . . .
H5B H 0.1962 0.9847 0.5540 0.018 Uiso 1 1 calc R . . . .
C11 C 0.2285(3) 0.5340(3) 0.58249(14) 0.0163(5) Uani 1 1 d . . . . .
H11 H 0.3025 0.4809 0.5631 0.020 Uiso 1 1 calc R . . . .
C33 C -0.3380(3) 0.2853(3) 0.94240(16) 0.0228(6) Uani 1 1 d . . . . .
H33A H -0.3454 0.3393 0.9776 0.027 Uiso 1 1 calc R . . . .
H33B H -0.3857 0.2033 0.9664 0.027 Uiso 1 1 calc R . . . .
C31 C 0.3336(3) 1.0826(3) 0.97895(16) 0.0215(5) Uani 1 1 d . . . . .
H31A H 0.2567 1.0305 0.9784 0.032 Uiso 1 1 calc GR . . . .
H31B H 0.3728 1.0461 1.0233 0.032 Uiso 1 1 calc GR . . . .
H31C H 0.4067 1.0808 0.9369 0.032 Uiso 1 1 calc GR . . . .
C9 C 0.4334(3) 0.5228(3) 0.70152(16) 0.0269(6) Uani 1 1 d . . . . .
H9A H 0.3632 0.5380 0.7422 0.040 Uiso 1 1 calc GR . . . .
H9B H 0.5272 0.5306 0.7108 0.040 Uiso 1 1 calc GR . . . .
H9C H 0.4260 0.4348 0.6958 0.040 Uiso 1 1 calc GR . . . .
C20 C -0.0460(3) 0.9692(3) 0.80515(15) 0.0196(5) Uani 1 1 d . . . . .
H20A H -0.0550 1.0558 0.8151 0.029 Uiso 1 1 calc GR . . . .
H20B H -0.1288 0.9210 0.8307 0.029 Uiso 1 1 calc GR . . . .
H20C H -0.0382 0.9789 0.7531 0.029 Uiso 1 1 calc GR . . . .
C28 C 0.2461(3) 1.3960(3) 1.03765(15) 0.0233(6) Uani 1 1 d . . . . .
H28 H 0.2572 1.4279 1.0775 0.028 Uiso 1 1 calc R . . . .
C32 C -0.1844(3) 0.2563(3) 0.91168(14) 0.0212(5) Uani 1 1 d . . . . .
H32A H -0.1216 0.2945 0.9344 0.025 Uiso 1 1 calc R . . . .
H32B H -0.1625 0.1608 0.9212 0.025 Uiso 1 1 calc R . . . .
C17 C -0.1560(3) 0.7039(3) 0.75206(15) 0.0222(5) Uani 1 1 d . . . . .
H17A H -0.1937 0.6196 0.7565 0.033 Uiso 1 1 calc GR . . . .
H17B H -0.2285 0.7601 0.7735 0.033 Uiso 1 1 calc GR . . . .
H17C H -0.0756 0.6901 0.7773 0.033 Uiso 1 1 calc GR . . . .
C16 C -0.2347(3) 0.7957(3) 0.63272(17) 0.0229(6) Uani 1 1 d . . . . .
H16A H -0.2027 0.8275 0.5806 0.034 Uiso 1 1 calc GR . . . .
H16B H -0.2997 0.8617 0.6502 0.034 Uiso 1 1 calc GR . . . .
H16C H -0.2823 0.7145 0.6421 0.034 Uiso 1 1 calc GR . . . .
C22 C 0.5171(3) 0.9802(3) 0.79210(15) 0.0199(5) Uani 1 1 d . . . . .
H22A H 0.5409 0.9769 0.7413 0.030 Uiso 1 1 calc GR . . . .
H22B H 0.5952 0.9410 0.8172 0.030 Uiso 1 1 calc GR . . . .
H22C H 0.4987 1.0715 0.7949 0.030 Uiso 1 1 calc GR . . . .
C4 C 0.3826(3) 1.0479(3) 0.56918(14) 0.0194(5) Uani 1 1 d . . . . .
H4A H 0.3791 1.1180 0.5244 0.023 Uiso 1 1 calc R . . . .
H4B H 0.4792 1.0079 0.5680 0.023 Uiso 1 1 calc R . . . .
C26 C 0.0914(3) 1.5182(3) 0.86612(14) 0.0181(5) Uani 1 1 d . . . . .
H26A H 0.1572 1.5391 0.8204 0.027 Uiso 1 1 calc GR . . . .
H26B H 0.0561 1.5990 0.8804 0.027 Uiso 1 1 calc GR . . . .
H26C H 0.0130 1.4737 0.8600 0.027 Uiso 1 1 calc GR . . . .
C35 C -0.2998(3) 0.3218(3) 0.81433(17) 0.0284(6) Uani 1 1 d . . . . .
H35A H -0.3214 0.2363 0.8087 0.034 Uiso 1 1 calc R . . . .
H35B H -0.3037 0.3883 0.7682 0.034 Uiso 1 1 calc R . . . .
C19 C 0.0723(3) 0.8681(3) 0.91337(14) 0.0193(5) Uani 1 1 d . . . . .
H19A H 0.1552 0.8159 0.9288 0.029 Uiso 1 1 calc GR . . . .
H19B H -0.0117 0.8202 0.9369 0.029 Uiso 1 1 calc GR . . . .
H19C H 0.0654 0.9515 0.9269 0.029 Uiso 1 1 calc GR . . . .
C37 C -0.1151(3) 0.1400(3) 0.56189(16) 0.0238(6) Uani 1 1 d . . . . .
H37A H -0.1000 0.1862 0.5100 0.029 Uiso 1 1 calc R . . . .
H37B H -0.1028 0.0446 0.5665 0.029 Uiso 1 1 calc R . . . .
C36 C -0.0158(3) 0.1842(3) 0.60202(16) 0.0217(5) Uani 1 1 d . . . . .
H36A H 0.0292 0.1073 0.6324 0.026 Uiso 1 1 calc R . . . .
H36B H 0.0582 0.2354 0.5671 0.026 Uiso 1 1 calc R . . . .
C39 C -0.2310(3) 0.2944(4) 0.62333(18) 0.0308(7) Uani 1 1 d . . . . .
H39A H -0.2278 0.3737 0.5828 0.037 Uiso 1 1 calc R . . . .
H39B H -0.3047 0.3093 0.6635 0.037 Uiso 1 1 calc R . . . .
C8 C 0.4080(3) 0.6239(3) 0.63246(14) 0.0168(5) Uani 1 1 d . . . . .
H8 H 0.4197 0.7124 0.6388 0.020 Uiso 1 1 calc R . . . .
C34 C -0.4008(3) 0.3604(4) 0.87551(18) 0.0309(7) Uani 1 1 d . . . . .
H34A H -0.4962 0.3334 0.8780 0.037 Uiso 1 1 calc R . . . .
H34B H -0.4045 0.4560 0.8703 0.037 Uiso 1 1 calc R . . . .
C10 C 0.5171(3) 0.6013(3) 0.56855(16) 0.0239(6) Uani 1 1 d . . . . .
H10A H 0.5158 0.5110 0.5651 0.036 Uiso 1 1 calc GR . . . .
H10B H 0.6102 0.6169 0.5757 0.036 Uiso 1 1 calc GR . . . .
H10C H 0.4953 0.6616 0.5239 0.036 Uiso 1 1 calc GR . . . .
C27 C 0.1812(3) 1.4743(3) 0.98263(15) 0.0216(5) Uani 1 1 d . . . . .
H27 H 0.1468 1.5603 0.9853 0.026 Uiso 1 1 calc R . . . .
C38 C -0.2585(3) 0.1771(4) 0.5996(2) 0.0369(8) Uani 1 1 d . . . . .
H38A H -0.3272 0.1994 0.5661 0.044 Uiso 1 1 calc R . . . .
H38B H -0.2933 0.1056 0.6415 0.044 Uiso 1 1 calc R . . . .


_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
K1 O1 2.675(2) . ?
K1 N3 3.288(2) 1_545 ?
K1 O2 2.863(2) . ?
K1 N2 2.715(2) 1_545 ?
K1 N4 2.860(2) 1_545 ?
K1 C14 3.529(3) . ?
K1 C13 3.228(3) . ?
K1 C12 3.107(3) . ?
K1 C11 3.257(3) . ?
P1 N2 1.660(2) . ?
P1 C2 1.729(2) . ?
P1 C18 1.824(3) . ?
P1 C21 1.840(3) . ?
O1 C32 1.438(3) . ?
O1 C35 1.429(4) . ?
N3 K1 3.288(2) 1_565 ?
N3 N2 1.342(3) . ?
N3 N4 1.276(3) . ?
O2 C36 1.442(4) . ?
O2 C39 1.430(4) . ?
N2 K1 2.715(2) 1_565 ?
N4 K1 2.860(2) 1_565 ?
N4 C24 1.423(3) . ?
N1 C6 1.396(3) . ?
N1 C1 1.320(3) . ?
C2 C1 1.405(3) . ?
C2 C3 1.522(3) . ?
C24 C30 1.417(3) . ?
C24 C25 1.411(4) . ?
C30 C29 1.394(4) . ?
C30 C31 1.498(4) . ?
C6 C14 1.426(3) . ?
C6 C7 1.417(3) . ?
C14 C13 1.392(4) . ?
C14 C15 1.517(4) . ?
C1 C5 1.539(3) . ?
C25 C26 1.507(4) . ?
C25 C27 1.385(4) . ?
C13 C12 1.389(4) . ?
C3 C4 1.538(4) . ?
C18 C20 1.531(4) . ?
C18 C19 1.535(4) . ?
C12 C11 1.389(4) . ?
C21 C23 1.527(4) . ?
C21 C22 1.529(4) . ?
C15 C17 1.537(4) . ?
C15 C16 1.522(4) . ?
C29 C28 1.374(4) . ?
C7 C11 1.402(3) . ?
C7 C8 1.520(4) . ?
C5 C4 1.527(4) . ?
C33 C32 1.534(4) . ?
C33 C34 1.536(4) . ?
C9 C8 1.528(4) . ?
C28 C27 1.385(4) . ?
C35 C34 1.511(5) . ?
C37 C36 1.528(4) . ?
C37 C38 1.515(5) . ?
C39 C38 1.501(5) . ?
C8 C10 1.529(4) . ?

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
O1 K1 N3 85.63(6) . 1_545 ?
O1 K1 O2 85.83(7) . . ?
O1 K1 N2 96.97(7) . 1_545 ?
O1 K1 N4 81.13(7) . 1_545 ?
O1 K1 C14 104.02(7) . . ?
O1 K1 C13 108.72(7) . . ?
O1 K1 C12 131.07(7) . . ?
O1 K1 C11 151.39(7) . . ?
N3 K1 C14 143.86(6) 1_545 . ?
O2 K1 N3 121.80(6) . 1_545 ?
O2 K1 C14 93.89(6) . . ?
O2 K1 C13 71.85(7) . . ?
O2 K1 C12 67.81(7) . . ?
O2 K1 C11 88.82(7) . . ?
N2 K1 N3 23.43(6) 1_545 1_545 ?
N2 K1 O2 102.22(7) 1_545 . ?
N2 K1 N4 45.55(6) 1_545 1_545 ?
N2 K1 C14 154.39(7) 1_545 . ?
N2 K1 C13 152.85(7) 1_545 . ?
N2 K1 C12 127.67(7) 1_545 . ?
N2 K1 C11 111.63(7) 1_545 . ?
N4 K1 N3 22.60(6) 1_545 1_545 ?
N4 K1 O2 142.45(7) 1_545 . ?
N4 K1 C14 123.39(6) 1_545 . ?
N4 K1 C13 145.69(7) 1_545 . ?
N4 K1 C12 143.16(7) 1_545 . ?
N4 K1 C11 118.22(7) 1_545 . ?
C13 K1 N3 161.71(6) . 1_545 ?
C13 K1 C14 23.23(6) . . ?
C13 K1 C11 43.31(7) . . ?
C12 K1 N3 143.26(7) . 1_545 ?
C12 K1 C14 42.27(6) . . ?
C12 K1 C13 25.23(7) . . ?
C12 K1 C11 25.06(7) . . ?
C11 K1 N3 120.60(6) . 1_545 ?
C11 K1 C14 48.31(6) . . ?
N2 P1 C2 105.48(11) . . ?
N2 P1 C18 110.69(12) . . ?
N2 P1 C21 110.11(11) . . ?
C2 P1 C18 111.66(12) . . ?
C2 P1 C21 112.41(12) . . ?
C18 P1 C21 106.55(12) . . ?
C32 O1 K1 133.44(16) . . ?
C35 O1 K1 118.43(17) . . ?
C35 O1 C32 106.7(2) . . ?
N2 N3 K1 53.55(12) . 1_565 ?
N4 N3 K1 59.49(13) . 1_565 ?
N4 N3 N2 111.3(2) . . ?
C36 O2 K1 113.99(16) . . ?
C39 O2 K1 137.17(18) . . ?
C39 O2 C36 107.3(2) . . ?
P1 N2 K1 138.67(11) . 1_565 ?
N3 N2 K1 103.02(14) . 1_565 ?
N3 N2 P1 112.50(17) . . ?
N3 N4 K1 97.91(15) . 1_565 ?
N3 N4 C24 115.7(2) . . ?
C24 N4 K1 144.57(16) . 1_565 ?
C1 N1 C6 120.5(2) . . ?
C1 C2 P1 128.02(19) . . ?
C1 C2 C3 111.8(2) . . ?
C3 C2 P1 120.21(18) . . ?
C30 C24 N4 127.7(2) . . ?
C25 C24 N4 113.2(2) . . ?
C25 C24 C30 119.0(2) . . ?
C24 C30 C31 124.2(2) . . ?
C29 C30 C24 118.5(2) . . ?
C29 C30 C31 117.2(2) . . ?
N1 C6 C14 119.2(2) . . ?
N1 C6 C7 122.0(2) . . ?
C7 C6 C14 118.6(2) . . ?
C6 C14 K1 85.75(14) . . ?
C6 C14 C15 119.2(2) . . ?
C13 C14 K1 66.18(14) . . ?
C13 C14 C6 119.9(2) . . ?
C13 C14 C15 120.9(2) . . ?
C15 C14 K1 118.37(15) . . ?
N1 C1 C2 128.4(2) . . ?
N1 C1 C5 124.1(2) . . ?
C2 C1 C5 107.5(2) . . ?
C24 C25 C26 120.8(2) . . ?
C27 C25 C24 119.8(2) . . ?
C27 C25 C26 119.3(2) . . ?
C14 C13 K1 90.60(15) . . ?
C12 C13 K1 72.50(15) . . ?
C12 C13 C14 121.4(2) . . ?
C2 C3 C4 102.3(2) . . ?
C20 C18 P1 109.22(18) . . ?
C20 C18 C19 111.1(2) . . ?
C19 C18 P1 112.39(18) . . ?
C13 C12 K1 82.27(15) . . ?
C11 C12 K1 83.52(15) . . ?
C11 C12 C13 119.0(2) . . ?
C23 C21 P1 110.20(18) . . ?
C23 C21 C22 111.4(2) . . ?
C22 C21 P1 108.89(18) . . ?
C14 C15 C17 109.6(2) . . ?
C14 C15 C16 113.8(2) . . ?
C16 C15 C17 109.7(2) . . ?
C28 C29 C30 122.4(3) . . ?
C6 C7 C8 120.9(2) . . ?
C11 C7 C6 119.4(2) . . ?
C11 C7 C8 119.7(2) . . ?
C4 C5 C1 104.1(2) . . ?
C12 C11 K1 71.41(15) . . ?
C12 C11 C7 121.6(2) . . ?
C7 C11 K1 90.38(15) . . ?
C32 C33 C34 103.7(2) . . ?
C29 C28 C27 118.8(3) . . ?
O1 C32 C33 107.0(2) . . ?
C5 C4 C3 105.0(2) . . ?
O1 C35 C34 104.4(2) . . ?
C38 C37 C36 103.1(2) . . ?
O2 C36 C37 107.5(2) . . ?
O2 C39 C38 104.8(3) . . ?
C7 C8 C9 110.3(2) . . ?
C7 C8 C10 112.5(2) . . ?
C9 C8 C10 110.0(2) . . ?
C35 C34 C33 102.8(3) . . ?
C25 C27 C28 121.4(3) . . ?
C39 C38 C37 102.4(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
K1 O1 C32 C33 169.29(19) . . . . ?
K1 O1 C35 C34 -152.7(2) . . . . ?
K1 N3 N2 P1 -158.44(19) 1_565 . . . ?
K1 N3 N4 C24 168.3(2) 1_565 . . . ?
K1 O2 C36 C37 178.72(17) . . . . ?
K1 O2 C39 C38 -163.0(2) . . . . ?
K1 N4 C24 C30 167.8(2) 1_565 . . . ?
K1 N4 C24 C25 -14.2(4) 1_565 . . . ?
K1 C14 C13 C12 -69.8(2) . . . . ?
K1 C14 C15 C17 18.9(3) . . . . ?
K1 C14 C15 C16 -104.4(2) . . . . ?
K1 C13 C12 C11 -78.1(2) . . . . ?
K1 C12 C11 C7 -78.5(2) . . . . ?
P1 C2 C1 N1 0.8(4) . . . . ?
P1 C2 C1 C5 177.62(19) . . . . ?
P1 C2 C3 C4 163.74(19) . . . . ?
O1 C35 C34 C33 -37.0(3) . . . . ?
N3 N4 C24 C30 8.0(4) . . . . ?
N3 N4 C24 C25 -174.0(2) . . . . ?
O2 C39 C38 C37 -39.3(3) . . . . ?
N2 P1 C2 C1 -149.2(2) . . . . ?
N2 P1 C2 C3 29.0(2) . . . . ?
N2 P1 C18 C20 50.2(2) . . . . ?
N2 P1 C18 C19 -73.5(2) . . . . ?
N2 P1 C21 C23 -179.33(18) . . . . ?
N2 P1 C21 C22 -56.9(2) . . . . ?
N2 N3 N4 K1 13.9(2) . . . 1_565 ?
N2 N3 N4 C24 -177.7(2) . . . . ?
N4 N3 N2 K1 -14.9(2) . . . 1_565 ?
N4 N3 N2 P1 -173.38(17) . . . . ?
N4 C24 C30 C29 176.0(2) . . . . ?
N4 C24 C30 C31 -3.9(4) . . . . ?
N4 C24 C25 C26 4.3(3) . . . . ?
N4 C24 C25 C27 -177.0(2) . . . . ?
N1 C6 C14 K1 -116.9(2) . . . . ?
N1 C6 C14 C13 -176.2(2) . . . . ?
N1 C6 C14 C15 3.4(3) . . . . ?
N1 C6 C7 C11 176.4(2) . . . . ?
N1 C6 C7 C8 -1.6(4) . . . . ?
N1 C1 C5 C4 -163.7(2) . . . . ?
C2 P1 N2 K1 50.74(19) . . . 1_565 ?
C2 P1 N2 N3 -162.10(17) . . . . ?
C2 P1 C18 C20 -67.0(2) . . . . ?
C2 P1 C18 C19 169.29(18) . . . . ?
C2 P1 C21 C23 -62.0(2) . . . . ?
C2 P1 C21 C22 60.4(2) . . . . ?
C2 C1 C5 C4 19.2(3) . . . . ?
C2 C3 C4 C5 28.9(3) . . . . ?
C24 C30 C29 C28 1.4(4) . . . . ?
C24 C25 C27 C28 0.1(4) . . . . ?
C30 C24 C25 C26 -177.5(2) . . . . ?
C30 C24 C25 C27 1.2(4) . . . . ?
C30 C29 C28 C27 -0.1(4) . . . . ?
C6 N1 C1 C2 -178.7(2) . . . . ?
C6 N1 C1 C5 4.9(4) . . . . ?
C6 C14 C13 K1 69.7(2) . . . . ?
C6 C14 C13 C12 -0.1(4) . . . . ?
C6 C14 C15 C17 -82.9(3) . . . . ?
C6 C14 C15 C16 153.8(2) . . . . ?
C6 C7 C11 K1 -69.0(2) . . . . ?
C6 C7 C11 C12 -0.7(4) . . . . ?
C6 C7 C8 C9 90.5(3) . . . . ?
C6 C7 C8 C10 -146.3(2) . . . . ?
C14 C6 C7 C11 2.1(4) . . . . ?
C14 C6 C7 C8 -176.0(2) . . . . ?
C14 C13 C12 K1 79.7(2) . . . . ?
C14 C13 C12 C11 1.5(4) . . . . ?
C1 N1 C6 C14 -110.6(3) . . . . ?
C1 N1 C6 C7 75.1(3) . . . . ?
C1 C2 C3 C4 -17.7(3) . . . . ?
C1 C5 C4 C3 -29.9(3) . . . . ?
C25 C24 C30 C29 -1.9(4) . . . . ?
C25 C24 C30 C31 178.1(2) . . . . ?
C13 C14 C15 C17 96.7(3) . . . . ?
C13 C14 C15 C16 -26.6(3) . . . . ?
C13 C12 C11 K1 77.4(2) . . . . ?
C13 C12 C11 C7 -1.1(4) . . . . ?
C3 C2 C1 N1 -177.6(2) . . . . ?
C3 C2 C1 C5 -0.8(3) . . . . ?
C18 P1 N2 K1 -70.20(19) . . . 1_565 ?
C18 P1 N2 N3 76.97(19) . . . . ?
C18 P1 C2 C1 -28.9(3) . . . . ?
C18 P1 C2 C3 149.34(19) . . . . ?
C18 P1 C21 C23 60.6(2) . . . . ?
C18 P1 C21 C22 -176.97(18) . . . . ?
C21 P1 N2 K1 172.25(15) . . . 1_565 ?
C21 P1 N2 N3 -40.6(2) . . . . ?
C21 P1 C2 C1 90.8(2) . . . . ?
C21 P1 C2 C3 -91.0(2) . . . . ?
C21 P1 C18 C20 169.94(18) . . . . ?
C21 P1 C18 C19 46.2(2) . . . . ?
C15 C14 C13 K1 -109.9(2) . . . . ?
C15 C14 C13 C12 -179.7(2) . . . . ?
C29 C28 C27 C25 -0.6(5) . . . . ?
C7 C6 C14 K1 57.6(2) . . . . ?
C7 C6 C14 C13 -1.7(4) . . . . ?
C7 C6 C14 C15 177.9(2) . . . . ?
C11 C7 C8 C9 -87.5(3) . . . . ?
C11 C7 C8 C10 35.6(3) . . . . ?
C31 C30 C29 C28 -178.7(3) . . . . ?
C32 O1 C35 C34 39.3(3) . . . . ?
C32 C33 C34 C35 21.1(3) . . . . ?
C26 C25 C27 C28 178.8(3) . . . . ?
C35 O1 C32 C33 -25.2(3) . . . . ?
C36 O2 C39 C38 32.9(3) . . . . ?
C36 C37 C38 C39 30.2(3) . . . . ?
C39 O2 C36 C37 -13.0(3) . . . . ?
C8 C7 C11 K1 109.1(2) . . . . ?
C8 C7 C11 C12 177.4(2) . . . . ?
C34 C33 C32 O1 1.4(3) . . . . ?
C38 C37 C36 O2 -11.5(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Moisture-sensitive
_database_code_depnum_ccdc_archive 'CCDC 1028482'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_mf966test
_audit_creation_date             2014-07-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        '[NpN3]FeBr(THF)'
_chemical_formula_moiety         'C35 H54 Br Fe N4 O P'
_chemical_formula_sum            'C35 H54 Br Fe N4 O P'
_chemical_formula_weight         713.55
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   17.547(5)
_cell_length_b                   10.262(5)
_cell_length_c                   20.588(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_volume                     3707(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4591
_cell_measurement_temperature    90
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.799
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11758
_diffrn_reflns_point_group_measured_fraction_full 0.755
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         23.333
_diffrn_reflns_theta_min         1.978
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.799
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.708
_reflns_Friedel_fraction_max     0.883
_reflns_number_gt                3951
_reflns_number_total             5063
_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 > 2σ(I)'
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 
;
 Flack x determined using 1506 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5063
_refine_ls_number_restraints     109
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0472
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0425P)²+1.8763P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1105
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C29) = Uanis(C28) = Uanis(C27) = Uanis(C26) = Uanis(C25) =
Uanis(C30) = Uanis(C31)
Uanis(C24A) = Uanis(C29A) = Uanis(C28A) = Uanis(C27A) = Uanis(C26A) =
Uanis(C25A) = Uanis(C31A) = Uanis(C30A)
Uanis(C35) = Uanis(C34) = Uanis(C33) = Uanis(C32)
3. Rigid body (RIGU) restrains
 C24A, C29A, C28A, C27A, C26A, C25A, C31A, C30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C29, C28, C27, C26, C25, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C24A)=Sof(C29A)=Sof(C28A)=Sof(H28A)=Sof(C27A)=Sof(H27A)=Sof(C26A)=
 Sof(H26A)=Sof(C25A)=1-FVAR(1)
 Sof(C24)=Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=
 Sof(C29)=FVAR(1)
 Sof(C30A)=Sof(H30a)=Sof(H30b)=Sof(H30c)=1-FVAR(2)
 Sof(C30)=Sof(H30d)=Sof(H30e)=Sof(H30f)=FVAR(2)
 Sof(C31A)=Sof(H31a)=Sof(H31b)=Sof(H31c)=1-FVAR(3)
 Sof(C31)=Sof(H31d)=Sof(H31e)=Sof(H31f)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C18(H18), C21(H21), C15(H15)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C4(H4a,H4b), C35(H35a,H35b), C3(H3a,H3b), C34(H34a,H34b),
 C33(H33a,H33b), C32(H32a,H32b)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C28A(H28A), C27A(H27A), C26A(H26A), C26(H26),
 C27(H27), C28(H28)
5.d Fitted hexagon refined as free rotating group:
 C24A(C29A,C28A,C27A,C26A,C25A), C24(C25,C26,C27,C28,C29)
5.e Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C16(H16a,H16b,H16c), C9(H9a,H9b,
 H9c), C19(H19a,H19b,H19c), C17(H17a,H17b,H17c), C20(H20a,H20b,H20c), C10(H10a,
 H10b,H10c), C31A(H31a,H31b,H31c), C30A(H30a,H30b,H30c), C30(H30d,H30e,H30f),
 C31(H31d,H31e,H31f)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Br1 Br -0.02338(5) 0.25399(10) 0.12643(6) 0.0501(3) Uani 1 1 d . . . . .
Fe1 Fe 0.10879(6) 0.23282(10) 0.15771(6) 0.0230(3) Uani 1 1 d . . . . .
P1 P 0.22705(13) 0.4351(2) 0.07831(12) 0.0232(5) Uani 1 1 d . . . . .
O1 O 0.0958(3) 0.0478(5) 0.2024(3) 0.0278(14) Uani 1 1 d . . . . .
N1 N 0.1573(4) 0.3558(6) 0.2231(3) 0.0213(16) Uani 1 1 d . . . . .
N2 N 0.1858(4) 0.2913(6) 0.0895(4) 0.0283(18) Uani 1 1 d . . . . .
N3 N 0.2001(4) 0.2034(7) 0.0420(4) 0.0327(19) Uani 1 1 d . . . . .
N4 N 0.1618(5) 0.0993(7) 0.0535(4) 0.038(2) Uani 1 1 d . . . . .
C11 C 0.1962(5) 0.1644(9) 0.3727(5) 0.031(2) Uani 1 1 d . . . . .
H11 H 0.2324 0.1029 0.3880 0.038 Uiso 1 1 calc R . . . .
C8 C 0.2750(5) 0.1856(8) 0.2706(5) 0.031(2) Uani 1 1 d . . . . .
H8 H 0.2683 0.2272 0.2270 0.037 Uiso 1 1 calc R . . . .
C18 C 0.3237(5) 0.4082(8) 0.0487(4) 0.028(2) Uani 1 1 d . . . . .
H18 H 0.3213 0.3393 0.0144 0.034 Uiso 1 1 calc R . . . .
C1 C 0.1976(5) 0.4653(8) 0.2118(4) 0.024(2) Uani 1 1 d . . . . .
C2 C 0.2232(4) 0.5142(7) 0.1523(4) 0.025(2) Uani 1 1 d . . . . .
C5 C 0.2220(6) 0.5562(9) 0.2656(5) 0.041(3) Uani 1 1 d . . . . .
H5A H 0.1779 0.5810 0.2929 0.049 Uiso 1 1 calc R . . . .
H5B H 0.2609 0.5142 0.2935 0.049 Uiso 1 1 calc R . . . .
C4 C 0.2545(6) 0.6730(8) 0.2325(5) 0.042(3) Uani 1 1 d . . . . .
H4A H 0.3053 0.6935 0.2508 0.050 Uiso 1 1 calc R . . . .
H4B H 0.2208 0.7492 0.2396 0.050 Uiso 1 1 calc R . . . .
C12 C 0.1346(6) 0.1962(8) 0.4111(5) 0.034(2) Uani 1 1 d . . . . .
H12 H 0.1270 0.1543 0.4517 0.040 Uiso 1 1 calc R . . . .
C35 C 0.0480(7) 0.0344(10) 0.2598(6) 0.0560(16) Uani 1 1 d . . . . .
H35A H -0.0055 0.0567 0.2496 0.067 Uiso 1 1 calc R . . . .
H35B H 0.0662 0.0925 0.2950 0.067 Uiso 1 1 calc R . . . .
C21 C 0.1771(5) 0.5277(9) 0.0158(5) 0.032(2) Uani 1 1 d . . . . .
H21 H 0.2050 0.6119 0.0104 0.038 Uiso 1 1 calc R . . . .
C13 C 0.0840(5) 0.2901(8) 0.3897(5) 0.034(2) Uani 1 1 d . . . . .
H13 H 0.0433 0.3153 0.4174 0.041 Uiso 1 1 calc R . . . .
C22 C 0.1774(6) 0.4599(10) -0.0505(5) 0.047(3) Uani 1 1 d . . . . .
H22A H 0.2300 0.4419 -0.0636 0.070 Uiso 1 1 calc GR . . . .
H22B H 0.1532 0.5166 -0.0828 0.070 Uiso 1 1 calc GR . . . .
H22C H 0.1490 0.3778 -0.0475 0.070 Uiso 1 1 calc GR . . . .
C15 C 0.0328(5) 0.4517(8) 0.3081(5) 0.030(2) Uani 1 1 d . . . . .
H15 H 0.0494 0.4863 0.2649 0.036 Uiso 1 1 calc R . . . .
C23 C 0.0965(6) 0.5613(9) 0.0386(6) 0.051(3) Uani 1 1 d . . . . .
H23A H 0.0667 0.4810 0.0432 0.077 Uiso 1 1 calc GR . . . .
H23B H 0.0720 0.6183 0.0066 0.077 Uiso 1 1 calc GR . . . .
H23C H 0.0991 0.6060 0.0806 0.077 Uiso 1 1 calc GR . . . .
C16 C -0.0461(5) 0.3899(9) 0.2998(6) 0.046(3) Uani 1 1 d . . . . .
H16A H -0.0806 0.4528 0.2794 0.069 Uiso 1 1 calc GR . . . .
H16B H -0.0663 0.3653 0.3425 0.069 Uiso 1 1 calc GR . . . .
H16C H -0.0420 0.3122 0.2724 0.069 Uiso 1 1 calc GR . . . .
C9 C 0.2835(6) 0.0387(9) 0.2603(6) 0.046(3) Uani 1 1 d . . . . .
H9A H 0.2384 0.0051 0.2378 0.069 Uiso 1 1 calc GR . . . .
H9B H 0.2886 -0.0047 0.3025 0.069 Uiso 1 1 calc GR . . . .
H9C H 0.3289 0.0215 0.2340 0.069 Uiso 1 1 calc GR . . . .
C3 C 0.2615(6) 0.6458(8) 0.1609(5) 0.044(3) Uani 1 1 d . . . . .
H3A H 0.3157 0.6421 0.1476 0.052 Uiso 1 1 calc R . . . .
H3B H 0.2353 0.7138 0.1351 0.052 Uiso 1 1 calc R . . . .
C19 C 0.3734(5) 0.3548(9) 0.1051(5) 0.044(3) Uani 1 1 d . . . . .
H19A H 0.3763 0.4200 0.1398 0.067 Uiso 1 1 calc GR . . . .
H19B H 0.4247 0.3358 0.0890 0.067 Uiso 1 1 calc GR . . . .
H19C H 0.3504 0.2748 0.1222 0.067 Uiso 1 1 calc GR . . . .
C17 C 0.0284(5) 0.5666(8) 0.3560(5) 0.038(2) Uani 1 1 d . . . . .
H17A H 0.0780 0.6102 0.3581 0.057 Uiso 1 1 calc GR . . . .
H17B H 0.0146 0.5342 0.3992 0.057 Uiso 1 1 calc GR . . . .
H17C H -0.0103 0.6287 0.3411 0.057 Uiso 1 1 calc GR . . . .
C20 C 0.3616(5) 0.5296(8) 0.0185(5) 0.036(2) Uani 1 1 d . . . . .
H20A H 0.3331 0.5562 -0.0202 0.054 Uiso 1 1 calc GR . . . .
H20B H 0.4142 0.5088 0.0063 0.054 Uiso 1 1 calc GR . . . .
H20C H 0.3616 0.6008 0.0502 0.054 Uiso 1 1 calc GR . . . .
C34 C 0.0545(7) -0.1026(9) 0.2793(6) 0.0560(16) Uani 1 1 d . . . . .
H34A H 0.0130 -0.1296 0.3091 0.067 Uiso 1 1 calc R . . . .
H34B H 0.1046 -0.1228 0.2989 0.067 Uiso 1 1 calc R . . . .
C33 C 0.0450(7) -0.1651(10) 0.2069(6) 0.0560(16) Uani 1 1 d . . . . .
H33A H 0.0664 -0.2542 0.2051 0.067 Uiso 1 1 calc R . . . .
H33B H -0.0093 -0.1682 0.1938 0.067 Uiso 1 1 calc R . . . .
C32 C 0.0900(6) -0.0721(9) 0.1635(6) 0.0560(16) Uani 1 1 d . . . . .
H32A H 0.1411 -0.1077 0.1536 0.067 Uiso 1 1 calc R . . . .
H32B H 0.0627 -0.0557 0.1222 0.067 Uiso 1 1 calc R . . . .
C10 C 0.3477(6) 0.2397(12) 0.3007(8) 0.087(5) Uani 1 1 d . . . . .
H10A H 0.3885 0.2395 0.2683 0.130 Uiso 1 1 calc GR . . . .
H10B H 0.3626 0.1854 0.3378 0.130 Uiso 1 1 calc GR . . . .
H10C H 0.3387 0.3291 0.3156 0.130 Uiso 1 1 calc GR . . . .
C7 C 0.2062(5) 0.2206(8) 0.3120(4) 0.025(2) Uani 1 1 d . . . . .
C6 C 0.1521(5) 0.3130(7) 0.2897(4) 0.023(2) Uani 1 1 d . . . . .
C14 C 0.0901(5) 0.3488(8) 0.3296(4) 0.026(2) Uani 1 1 d . . . . .
C24A C 0.1947(13) -0.0103(17) 0.0104(9) 0.044(5) Uani 0.38(2) 1 d . . P A 2
C29A C 0.2686(12) -0.0589(18) 0.0130(9) 0.044(5) Uani 0.38(2) 1 d G . P A 2
C28A C 0.2925(12) -0.1512(17) -0.0321(10) 0.044(5) Uani 0.38(2) 1 d G . P A 2
H28A H 0.3430 -0.1844 -0.0304 0.053 Uiso 0.38(2) 1 calc R . P A 2
C27A C 0.2424(15) -0.1948(14) -0.0797(8) 0.044(5) Uani 0.38(2) 1 d G . P A 2
H27A H 0.2587 -0.2578 -0.1105 0.053 Uiso 0.38(2) 1 calc R . P A 2
C26A C 0.1686(14) -0.1462(18) -0.0823(8) 0.044(5) Uani 0.38(2) 1 d G . P A 2
H26A H 0.1344 -0.1760 -0.1148 0.053 Uiso 0.38(2) 1 calc R . P A 2
C25A C 0.1447(11) -0.0539(19) -0.0372(10) 0.044(5) Uani 0.38(2) 1 d G . P A 2
C31A C 0.320(2) -0.015(3) 0.068(2) 0.044(5) Uani 0.41(6) 1 d . . P A 2
H31A H 0.3308 0.0789 0.0639 0.066 Uiso 0.41(6) 1 calc GR . P A 2
H31B H 0.3685 -0.0631 0.0665 0.066 Uiso 0.41(6) 1 calc GR . P A 2
H31C H 0.2953 -0.0310 0.1100 0.066 Uiso 0.41(6) 1 calc GR . P A 2
C30A C 0.068(2) 0.003(3) -0.0394(14) 0.044(5) Uani 0.37(3) 1 d . . P A 2
H30A H 0.0478 0.0100 0.0048 0.066 Uiso 0.37(3) 1 calc GR . P A 2
H30B H 0.0345 -0.0538 -0.0652 0.066 Uiso 0.37(3) 1 calc GR . P A 2
H30C H 0.0703 0.0891 -0.0594 0.066 Uiso 0.37(3) 1 calc GR . P A 2
C30 C 0.0349(12) 0.0617(18) -0.0353(8) 0.043(3) Uani 0.63(3) 1 d . . P A 1
H30D H 0.0131 0.0561 0.0085 0.065 Uiso 0.63(3) 1 calc GR . P A 1
H30E H -0.0016 0.0266 -0.0668 0.065 Uiso 0.63(3) 1 calc GR . P A 1
H30F H 0.0458 0.1529 -0.0457 0.065 Uiso 0.63(3) 1 calc GR . P A 1
C31 C 0.2996(17) -0.042(2) 0.0506(13) 0.043(3) Uani 0.59(6) 1 d . . P A 1
H31D H 0.3264 0.0396 0.0407 0.065 Uiso 0.59(6) 1 calc GR . P A 1
H31E H 0.3355 -0.1148 0.0483 0.065 Uiso 0.59(6) 1 calc GR . P A 1
H31F H 0.2778 -0.0369 0.0943 0.065 Uiso 0.59(6) 1 calc GR . P A 1
C24 C 0.1691(8) 0.0071(11) 0.0054(6) 0.043(3) Uani 0.62(2) 1 d . . P A 1
C25 C 0.1106(7) -0.0195(11) -0.0382(6) 0.043(3) Uani 0.62(2) 1 d G . P A 1
C26 C 0.1201(8) -0.1155(11) -0.0851(5) 0.043(3) Uani 0.62(2) 1 d G . P A 1
H26 H 0.0801 -0.1337 -0.1149 0.052 Uiso 0.62(2) 1 calc R . P A 1
C27 C 0.1880(9) -0.1849(9) -0.0885(5) 0.043(3) Uani 0.62(2) 1 d G . P A 1
H27 H 0.1945 -0.2505 -0.1205 0.052 Uiso 0.62(2) 1 calc R . P A 1
C28 C 0.2465(8) -0.1582(10) -0.0449(6) 0.043(3) Uani 0.62(2) 1 d G . P A 1
H28 H 0.2929 -0.2056 -0.0472 0.052 Uiso 0.62(2) 1 calc R . P A 1
C29 C 0.2370(7) -0.0622(11) 0.0020(6) 0.043(3) Uani 0.62(2) 1 d G . P A 1


_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
Br1 Fe1 2.4168(16) . ?
Fe1 O1 2.122(5) . ?
Fe1 N1 2.032(7) . ?
Fe1 N2 2.039(7) . ?
P1 N2 1.660(7) . ?
P1 C18 1.824(9) . ?
P1 C2 1.726(9) . ?
P1 C21 1.824(9) . ?
O1 C35 1.456(12) . ?
O1 C32 1.471(11) . ?
N1 C1 1.348(10) . ?
N1 C6 1.443(11) . ?
N2 N3 1.354(9) . ?
N3 N4 1.285(9) . ?
N4 C24A 1.544(16) . ?
N4 C24 1.375(10) . ?
C11 C12 1.378(13) . ?
C11 C7 1.387(13) . ?
C8 C9 1.529(12) . ?
C8 C10 1.523(14) . ?
C8 C7 1.522(12) . ?
C18 C19 1.550(13) . ?
C18 C20 1.544(11) . ?
C1 C2 1.398(12) . ?
C1 C5 1.512(12) . ?
C2 C3 1.520(11) . ?
C5 C4 1.492(12) . ?
C4 C3 1.505(14) . ?
C12 C13 1.383(13) . ?
C35 C34 1.467(13) . ?
C21 C22 1.531(13) . ?
C21 C23 1.530(13) . ?
C13 C14 1.380(12) . ?
C15 C16 1.533(12) . ?
C15 C17 1.540(12) . ?
C15 C14 1.524(12) . ?
C34 C33 1.632(16) . ?
C33 C32 1.528(14) . ?
C7 C6 1.418(11) . ?
C6 C14 1.411(12) . ?
C24A C29A 1.3900 . ?
C24A C25A 1.3900 . ?
C29A C28A 1.3900 . ?
C29A C31A 1.53(5) . ?
C28A C27A 1.3900 . ?
C27A C26A 1.3900 . ?
C26A C25A 1.3900 . ?
C25A C30A 1.47(4) . ?
C30 C25 1.57(2) . ?
C31 C29 1.50(4) . ?
C24 C25 1.3900 . ?
C24 C29 1.3900 . ?
C25 C26 1.3900 . ?
C26 C27 1.3900 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?

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
O1 Fe1 Br1 95.32(16) . . ?
N1 Fe1 Br1 121.51(19) . . ?
N1 Fe1 O1 108.3(2) . . ?
N1 Fe1 N2 89.7(3) . . ?
N2 Fe1 Br1 115.2(2) . . ?
N2 Fe1 O1 129.3(3) . . ?
N2 P1 C18 108.4(4) . . ?
N2 P1 C2 106.1(4) . . ?
N2 P1 C21 110.6(4) . . ?
C18 P1 C21 106.9(4) . . ?
C2 P1 C18 113.7(4) . . ?
C2 P1 C21 111.1(4) . . ?
C35 O1 Fe1 119.9(5) . . ?
C35 O1 C32 108.9(7) . . ?
C32 O1 Fe1 121.3(5) . . ?
C1 N1 Fe1 128.5(6) . . ?
C1 N1 C6 116.8(7) . . ?
C6 N1 Fe1 114.5(5) . . ?
P1 N2 Fe1 130.2(4) . . ?
N3 N2 Fe1 115.1(5) . . ?
N3 N2 P1 114.3(6) . . ?
N4 N3 N2 108.9(7) . . ?
N3 N4 C24A 107.7(11) . . ?
N3 N4 C24 113.0(9) . . ?
C12 C11 C7 121.1(8) . . ?
C10 C8 C9 109.6(8) . . ?
C7 C8 C9 112.8(8) . . ?
C7 C8 C10 110.5(8) . . ?
C19 C18 P1 109.0(6) . . ?
C20 C18 P1 114.4(6) . . ?
C20 C18 C19 110.2(8) . . ?
N1 C1 C2 128.3(8) . . ?
N1 C1 C5 122.4(8) . . ?
C2 C1 C5 109.3(7) . . ?
C1 C2 P1 128.1(6) . . ?
C1 C2 C3 111.0(7) . . ?
C3 C2 P1 120.3(6) . . ?
C4 C5 C1 105.6(8) . . ?
C5 C4 C3 109.3(7) . . ?
C11 C12 C13 119.1(9) . . ?
O1 C35 C34 105.6(9) . . ?
C22 C21 P1 113.0(6) . . ?
C23 C21 P1 110.1(7) . . ?
C23 C21 C22 112.3(9) . . ?
C14 C13 C12 122.7(9) . . ?
C16 C15 C17 110.0(8) . . ?
C14 C15 C16 110.0(7) . . ?
C14 C15 C17 112.2(8) . . ?
C4 C3 C2 104.1(8) . . ?
C35 C34 C33 96.8(9) . . ?
C32 C33 C34 103.7(8) . . ?
O1 C32 C33 103.9(9) . . ?
C11 C7 C8 120.4(8) . . ?
C11 C7 C6 119.1(8) . . ?
C6 C7 C8 120.5(8) . . ?
C7 C6 N1 118.0(7) . . ?
C14 C6 N1 121.5(7) . . ?
C14 C6 C7 120.0(8) . . ?
C13 C14 C15 120.7(8) . . ?
C13 C14 C6 117.9(8) . . ?
C6 C14 C15 121.3(7) . . ?
C29A C24A N4 126.1(13) . . ?
C29A C24A C25A 120.0 . . ?
C25A C24A N4 113.7(13) . . ?
C24A C29A C28A 120.0 . . ?
C24A C29A C31A 118.5(16) . . ?
C28A C29A C31A 121.4(16) . . ?
C27A C28A C29A 120.0 . . ?
C28A C27A C26A 120.0 . . ?
C25A C26A C27A 120.0 . . ?
C24A C25A C30A 118.3(17) . . ?
C26A C25A C24A 120.0 . . ?
C26A C25A C30A 121.6(17) . . ?
N4 C24 C25 122.1(9) . . ?
N4 C24 C29 117.9(9) . . ?
C25 C24 C29 120.0 . . ?
C24 C25 C30 119.7(9) . . ?
C24 C25 C26 120.0 . . ?
C26 C25 C30 120.2(9) . . ?
C27 C26 C25 120.0 . . ?
C26 C27 C28 120.0 . . ?
C27 C28 C29 120.0 . . ?
C24 C29 C31 121.6(11) . . ?
C28 C29 C31 118.3(11) . . ?
C28 C29 C24 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 O1 C35 C34 -177.6(7) . . . . ?
Fe1 O1 C32 C33 -153.7(7) . . . . ?
Fe1 N1 C1 C2 -7.7(12) . . . . ?
Fe1 N1 C1 C5 172.2(7) . . . . ?
Fe1 N1 C6 C7 81.8(8) . . . . ?
Fe1 N1 C6 C14 -90.6(8) . . . . ?
Fe1 N2 N3 N4 -2.2(8) . . . . ?
P1 N2 N3 N4 -175.9(6) . . . . ?
P1 C2 C3 C4 -172.9(6) . . . . ?
O1 C35 C34 C33 -44.8(11) . . . . ?
N1 C1 C2 P1 -13.6(13) . . . . ?
N1 C1 C2 C3 175.8(8) . . . . ?
N1 C1 C5 C4 -171.9(8) . . . . ?
N1 C6 C14 C13 171.5(8) . . . . ?
N1 C6 C14 C15 -10.2(12) . . . . ?
N2 P1 C18 C19 -72.0(7) . . . . ?
N2 P1 C18 C20 164.1(6) . . . . ?
N2 P1 C2 C1 5.4(9) . . . . ?
N2 P1 C2 C3 175.4(7) . . . . ?
N2 P1 C21 C22 -61.1(8) . . . . ?
N2 P1 C21 C23 65.4(7) . . . . ?
N2 N3 N4 C24A -165.0(10) . . . . ?
N2 N3 N4 C24 176.3(8) . . . . ?
N3 N4 C24A C29A 61.9(14) . . . . ?
N3 N4 C24A C25A -113.4(11) . . . . ?
N3 N4 C24 C25 -106.7(10) . . . . ?
N3 N4 C24 C29 74.6(10) . . . . ?
N4 C24A C29A C28A -175.1(18) . . . . ?
N4 C24A C29A C31A 8.4(18) . . . . ?
N4 C24A C25A C26A 175.7(16) . . . . ?
N4 C24A C25A C30A -2.6(18) . . . . ?
N4 C24 C25 C30 3.0(13) . . . . ?
N4 C24 C25 C26 -178.6(13) . . . . ?
N4 C24 C29 C31 2.3(13) . . . . ?
N4 C24 C29 C28 178.7(12) . . . . ?
C11 C12 C13 C14 3.6(14) . . . . ?
C11 C7 C6 N1 -171.1(7) . . . . ?
C11 C7 C6 C14 1.5(12) . . . . ?
C8 C7 C6 N1 10.0(11) . . . . ?
C8 C7 C6 C14 -177.4(7) . . . . ?
C18 P1 N2 Fe1 145.6(5) . . . . ?
C18 P1 N2 N3 -41.8(7) . . . . ?
C18 P1 C2 C1 -113.7(8) . . . . ?
C18 P1 C2 C3 56.2(8) . . . . ?
C18 P1 C21 C22 56.8(8) . . . . ?
C18 P1 C21 C23 -176.7(7) . . . . ?
C1 N1 C6 C7 -93.7(9) . . . . ?
C1 N1 C6 C14 93.9(9) . . . . ?
C1 C2 C3 C4 -1.4(10) . . . . ?
C1 C5 C4 C3 -8.9(11) . . . . ?
C2 P1 N2 Fe1 23.1(6) . . . . ?
C2 P1 N2 N3 -164.4(6) . . . . ?
C2 P1 C18 C19 45.8(7) . . . . ?
C2 P1 C18 C20 -78.1(7) . . . . ?
C2 P1 C21 C22 -178.7(6) . . . . ?
C2 P1 C21 C23 -52.2(7) . . . . ?
C2 C1 C5 C4 8.0(10) . . . . ?
C5 C1 C2 P1 166.5(7) . . . . ?
C5 C1 C2 C3 -4.2(10) . . . . ?
C5 C4 C3 C2 6.4(11) . . . . ?
C12 C11 C7 C8 179.3(8) . . . . ?
C12 C11 C7 C6 0.4(13) . . . . ?
C12 C13 C14 C15 179.9(8) . . . . ?
C12 C13 C14 C6 -1.7(13) . . . . ?
C35 O1 C32 C33 -8.2(11) . . . . ?
C35 C34 C33 C32 39.2(11) . . . . ?
C21 P1 N2 Fe1 -97.5(6) . . . . ?
C21 P1 N2 N3 75.1(6) . . . . ?
C21 P1 C18 C19 168.7(6) . . . . ?
C21 P1 C18 C20 44.9(8) . . . . ?
C21 P1 C2 C1 125.7(8) . . . . ?
C21 P1 C2 C3 -64.4(8) . . . . ?
C16 C15 C14 C13 -66.1(11) . . . . ?
C16 C15 C14 C6 115.6(9) . . . . ?
C9 C8 C7 C11 53.8(11) . . . . ?
C9 C8 C7 C6 -127.4(9) . . . . ?
C17 C15 C14 C13 56.6(11) . . . . ?
C17 C15 C14 C6 -121.7(9) . . . . ?
C34 C33 C32 O1 -19.4(11) . . . . ?
C32 O1 C35 C34 36.3(12) . . . . ?
C10 C8 C7 C11 -69.2(11) . . . . ?
C10 C8 C7 C6 109.6(10) . . . . ?
C7 C11 C12 C13 -2.9(14) . . . . ?
C7 C6 C14 C13 -0.8(12) . . . . ?
C7 C6 C14 C15 177.5(7) . . . . ?
C6 N1 C1 C2 167.1(8) . . . . ?
C6 N1 C1 C5 -13.0(11) . . . . ?
C24A N4 C24 C25 177(5) . . . . ?
C24A N4 C24 C29 -2(4) . . . . ?
C24A C29A C28A C27A 0.0 . . . . ?
C29A C24A C25A C26A 0.0 . . . . ?
C29A C24A C25A C30A -178.2(19) . . . . ?
C29A C28A C27A C26A 0.0 . . . . ?
C28A C27A C26A C25A 0.0 . . . . ?
C27A C26A C25A C24A 0.0 . . . . ?
C27A C26A C25A C30A 178.2(19) . . . . ?
C25A C24A C29A C28A 0.0 . . . . ?
C25A C24A C29A C31A -177(2) . . . . ?
C31A C29A C28A C27A 176(2) . . . . ?
C30 C25 C26 C27 178.4(12) . . . . ?
C24 N4 C24A C29A 172(5) . . . . ?
C24 N4 C24A C25A -3(4) . . . . ?
C24 C25 C26 C27 0.0 . . . . ?
C25 C24 C29 C31 -176.4(13) . . . . ?
C25 C24 C29 C28 0.0 . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C31 176.5(13) . . . . ?
C27 C28 C29 C24 0.0 . . . . ?
C29 C24 C25 C30 -178.4(12) . . . . ?
C29 C24 C25 C26 0.0 . . . . ?

_olex2_submission_original_sample_id mf966
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT019_mf966test           
;
PROBLEM: _diffrn_measured_fraction_theta_full/_max < 1.0      0.805 Why ? 
RESPONSE: No useful reflections were found beyond the current integration limit
;
_vrf_THETM01_mf966test           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: No useful reflections were found beyond the current integration limit
;
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_database_code_depnum_ccdc_archive 'CCDC 1028483'
