data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. I. Butler
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C34 H62 Fe P4'
_chemical_formula_weight          650.57
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/n
_symmetry_space_group_name_hall   '-P 2yn'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    10.0484(7)
_cell_length_b                    12.2174(10)
_cell_length_c                    14.7534(19)
_cell_angle_alpha                 90.00
_cell_angle_beta                  100.896(9)
_cell_angle_gamma                 90.00
_cell_volume                      1778.6(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4280
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Shard
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.22
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.06
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.215
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              704
_exptl_absorpt_coefficient_mu     0.625
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8747
_exptl_absorpt_correction_T_max   0.9635
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
 
_exptl_special_details
;
 PLEASE NOTE cell_measurement_ fields are not relevant to area detector data,
 the entire data set is used to refine the cell, which is indexed from all
 observed reflections in a 10 degree phi range.
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             23588
_diffrn_reflns_av_R_equivalents   0.0463
_diffrn_reflns_av_sigmaI/netI     0.0293
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.18
_diffrn_reflns_theta_max          27.48
_reflns_number_total              4072
_reflns_number_gt                 3591
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection
' DENZO (Otwinowski and Minor, 1997)'
_computing_cell_refinement        
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction         
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_computing_publication_material   ? 
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0250P)²+0.9177P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          4072
_refine_ls_number_parameters      186
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0323
_refine_ls_R_factor_gt            0.0263
_refine_ls_wR_factor_ref          0.0651
_refine_ls_wR_factor_gt           0.0624
_refine_ls_goodness_of_fit_ref    1.027
_refine_ls_restrained_S_all       1.027
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.98954(12) 0.41259(10) 1.12038(8) 0.0122(2) Uani 1 1 d . . .
C2 C 1.12955(12) 0.43129(10) 1.11201(8) 0.0122(2) Uani 1 1 d . . .
C3 C 1.14741(13) 0.54754(10) 1.10767(8) 0.0137(3) Uani 1 1 d . . .
H3 H 1.2291 0.5835 1.1017 0.016 Uiso 1 1 calc R . .
C4 C 1.02379(13) 0.60030(10) 1.11375(9) 0.0146(3) Uani 1 1 d . . .
H4 H 1.0088 0.6771 1.1136 0.018 Uiso 1 1 calc R . .
C5 C 0.92693(13) 0.51833(10) 1.12002(9) 0.0139(3) Uani 1 1 d . . .
H5 H 0.8348 0.5311 1.1235 0.017 Uiso 1 1 calc R . .
C6 C 0.77659(13) 0.25539(11) 1.04943(9) 0.0161(3) Uani 1 1 d . . .
H6 H 0.8158 0.2688 0.9930 0.019 Uiso 1 1 calc R . .
C7 C 0.73808(15) 0.13371(12) 1.04670(10) 0.0236(3) Uani 1 1 d . . .
H7A H 0.6954 0.1165 1.0995 0.035 Uiso 1 1 calc R . .
H7B H 0.8198 0.0890 1.0497 0.035 Uiso 1 1 calc R . .
H7C H 0.6744 0.1179 0.9892 0.035 Uiso 1 1 calc R . .
C8 C 0.65132(14) 0.32835(12) 1.03967(10) 0.0215(3) Uani 1 1 d . . .
H8A H 0.5897 0.3115 0.9815 0.032 Uiso 1 1 calc R . .
H8B H 0.6788 0.4053 1.0398 0.032 Uiso 1 1 calc R . .
H8C H 0.6051 0.3150 1.0914 0.032 Uiso 1 1 calc R . .
C9 C 0.82655(14) 0.32904(12) 1.24222(9) 0.0180(3) Uani 1 1 d . . .
H9 H 0.7584 0.3862 1.2169 0.022 Uiso 1 1 calc R . .
C10 C 0.75394(16) 0.23112(13) 1.27547(10) 0.0255(3) Uani 1 1 d . . .
H10A H 0.8194 0.1724 1.2951 0.038 Uiso 1 1 calc R . .
H10B H 0.6834 0.2048 1.2250 0.038 Uiso 1 1 calc R . .
H10C H 0.7124 0.2535 1.3276 0.038 Uiso 1 1 calc R . .
C11 C 0.92749(16) 0.37670(14) 1.32264(10) 0.0269(3) Uani 1 1 d . . .
H11A H 0.8801 0.3964 1.3726 0.040 Uiso 1 1 calc R . .
H11B H 0.9697 0.4421 1.3020 0.040 Uiso 1 1 calc R . .
H11C H 0.9976 0.3222 1.3450 0.040 Uiso 1 1 calc R . .
C12 C 1.22987(13) 0.20189(11) 1.11032(9) 0.0151(3) Uani 1 1 d . . .
H12 H 1.1845 0.1907 1.1644 0.018 Uiso 1 1 calc R . .
C13 C 1.13400(14) 0.16667(11) 1.02200(10) 0.0188(3) Uani 1 1 d . . .
H13A H 1.1797 0.1748 0.9693 0.028 Uiso 1 1 calc R . .
H13B H 1.0527 0.2127 1.0126 0.028 Uiso 1 1 calc R . .
H13C H 1.1081 0.0900 1.0275 0.028 Uiso 1 1 calc R . .
C14 C 1.35857(14) 0.13201(12) 1.12242(11) 0.0232(3) Uani 1 1 d . . .
H14A H 1.3337 0.0546 1.1139 0.035 Uiso 1 1 calc R . .
H14B H 1.4119 0.1430 1.1846 0.035 Uiso 1 1 calc R . .
H14C H 1.4125 0.1537 1.0765 0.035 Uiso 1 1 calc R . .
C15 C 1.38047(14) 0.36778(12) 1.22314(10) 0.0209(3) Uani 1 1 d . . .
H15 H 1.4523 0.3100 1.2317 0.025 Uiso 1 1 calc R . .
C16 C 1.30238(16) 0.35248(14) 1.30086(10) 0.0286(4) Uani 1 1 d . . .
H16A H 1.3639 0.3620 1.3603 0.043 Uiso 1 1 calc R . .
H16B H 1.2634 0.2787 1.2975 0.043 Uiso 1 1 calc R . .
H16C H 1.2295 0.4068 1.2949 0.043 Uiso 1 1 calc R . .
C17 C 1.45442(17) 0.47767(13) 1.23186(12) 0.0332(4) Uani 1 1 d . . .
H17A H 1.3890 0.5369 1.2329 0.050 Uiso 1 1 calc R . .
H17B H 1.4996 0.4876 1.1791 0.050 Uiso 1 1 calc R . .
H17C H 1.5221 0.4789 1.2892 0.050 Uiso 1 1 calc R . .
P1 P 0.91676(3) 0.28269(3) 1.14983(2) 0.01352(8) Uani 1 1 d . . .
P2 P 1.27861(3) 0.34802(3) 1.10428(2) 0.01357(8) Uani 1 1 d . . .
Fe1 Fe 1.0000 0.5000 1.0000 0.01061(7) Uani 1 2 d S . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 C5 1.4365(17) . ?
C1 C2 1.4534(17) . ?
C1 P1 1.8336(13) . ?
C1 Fe1 2.0920(12) . ?
C2 C3 1.4345(18) . ?
C2 P2 1.8320(13) . ?
C2 Fe1 2.0777(12) . ?
C3 C4 1.4173(18) . ?
C3 Fe1 2.0408(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.4116(18) . ?
C4 Fe1 2.0551(13) . ?
C4 H4 0.9500 . ?
C5 Fe1 2.0533(13) . ?
C5 H5 0.9500 . ?
C6 C8 1.5269(19) . ?
C6 C7 1.5347(19) . ?
C6 P1 1.8710(13) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C11 1.5233(19) . ?
C9 C10 1.5295(19) . ?
C9 P1 1.8622(14) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.5286(18) . ?
C12 C14 1.5316(18) . ?
C12 P2 1.8579(14) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.518(2) . ?
C15 C17 1.528(2) . ?
C15 P2 1.8715(14) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
Fe1 C3 2.0408(12) 3_767 ?
Fe1 C5 2.0533(13) 3_767 ?
Fe1 C4 2.0551(13) 3_767 ?
Fe1 C2 2.0777(12) 3_767 ?
Fe1 C1 2.0920(12) 3_767 ?
 
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
C5 C1 C2 106.77(11) . . ?
C5 C1 P1 125.82(9) . . ?
C2 C1 P1 126.30(9) . . ?
C5 C1 Fe1 68.28(7) . . ?
C2 C1 Fe1 69.07(7) . . ?
P1 C1 Fe1 136.83(7) . . ?
C3 C2 C1 106.90(11) . . ?
C3 C2 P2 115.87(9) . . ?
C1 C2 P2 137.21(10) . . ?
C3 C2 Fe1 68.24(7) . . ?
C1 C2 Fe1 70.13(7) . . ?
P2 C2 Fe1 124.86(7) . . ?
C4 C3 C2 109.20(11) . . ?
C4 C3 Fe1 70.30(7) . . ?
C2 C3 Fe1 71.00(7) . . ?
C4 C3 H3 125.4 . . ?
C2 C3 H3 125.4 . . ?
Fe1 C3 H3 124.9 . . ?
C5 C4 C3 107.75(11) . . ?
C5 C4 Fe1 69.83(7) . . ?
C3 C4 Fe1 69.21(7) . . ?
C5 C4 H4 126.1 . . ?
C3 C4 H4 126.1 . . ?
Fe1 C4 H4 126.4 . . ?
C4 C5 C1 109.35(11) . . ?
C4 C5 Fe1 69.97(7) . . ?
C1 C5 Fe1 71.18(7) . . ?
C4 C5 H5 125.3 . . ?
C1 C5 H5 125.3 . . ?
Fe1 C5 H5 125.1 . . ?
C8 C6 C7 111.33(11) . . ?
C8 C6 P1 117.03(9) . . ?
C7 C6 P1 109.99(9) . . ?
C8 C6 H6 105.9 . . ?
C7 C6 H6 105.9 . . ?
P1 C6 H6 105.9 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11 C9 C10 109.69(12) . . ?
C11 C9 P1 109.98(10) . . ?
C10 C9 P1 108.94(10) . . ?
C11 C9 H9 109.4 . . ?
C10 C9 H9 109.4 . . ?
P1 C9 H9 109.4 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C14 108.94(11) . . ?
C13 C12 P2 111.04(9) . . ?
C14 C12 P2 108.47(9) . . ?
C13 C12 H12 109.5 . . ?
C14 C12 H12 109.5 . . ?
P2 C12 H12 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C17 110.92(13) . . ?
C16 C15 P2 115.00(10) . . ?
C17 C15 P2 111.31(11) . . ?
C16 C15 H15 106.3 . . ?
C17 C15 H15 106.3 . . ?
P2 C15 H15 106.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C1 P1 C9 100.45(6) . . ?
C1 P1 C6 103.95(6) . . ?
C9 P1 C6 103.65(6) . . ?
C2 P2 C12 107.74(6) . . ?
C2 P2 C15 100.30(6) . . ?
C12 P2 C15 100.45(6) . . ?
C3 Fe1 C3 180.0 3_767 . ?
C3 Fe1 C5 112.15(5) 3_767 . ?
C3 Fe1 C5 67.85(5) . . ?
C3 Fe1 C5 67.85(5) 3_767 3_767 ?
C3 Fe1 C5 112.15(5) . 3_767 ?
C5 Fe1 C5 180.0 . 3_767 ?
C3 Fe1 C4 139.51(5) 3_767 . ?
C3 Fe1 C4 40.49(5) . . ?
C5 Fe1 C4 40.19(5) . . ?
C5 Fe1 C4 139.81(5) 3_767 . ?
C3 Fe1 C4 40.49(5) 3_767 3_767 ?
C3 Fe1 C4 139.51(5) . 3_767 ?
C5 Fe1 C4 139.81(5) . 3_767 ?
C5 Fe1 C4 40.19(5) 3_767 3_767 ?
C4 Fe1 C4 180.0 . 3_767 ?
C3 Fe1 C2 40.75(5) 3_767 3_767 ?
C3 Fe1 C2 139.25(5) . 3_767 ?
C5 Fe1 C2 111.68(5) . 3_767 ?
C5 Fe1 C2 68.32(5) 3_767 3_767 ?
C4 Fe1 C2 111.55(5) . 3_767 ?
C4 Fe1 C2 68.45(5) 3_767 3_767 ?
C3 Fe1 C2 139.25(5) 3_767 . ?
C3 Fe1 C2 40.75(5) . . ?
C5 Fe1 C2 68.32(5) . . ?
C5 Fe1 C2 111.68(5) 3_767 . ?
C4 Fe1 C2 68.45(5) . . ?
C4 Fe1 C2 111.55(5) 3_767 . ?
C2 Fe1 C2 180.000(1) 3_767 . ?
C3 Fe1 C1 111.71(5) 3_767 . ?
C3 Fe1 C1 68.29(5) . . ?
C5 Fe1 C1 40.54(5) . . ?
C5 Fe1 C1 139.46(5) 3_767 . ?
C4 Fe1 C1 68.15(5) . . ?
C4 Fe1 C1 111.85(5) 3_767 . ?
C2 Fe1 C1 139.20(5) 3_767 . ?
C2 Fe1 C1 40.80(5) . . ?
C3 Fe1 C1 68.29(5) 3_767 3_767 ?
C3 Fe1 C1 111.71(5) . 3_767 ?
C5 Fe1 C1 139.46(5) . 3_767 ?
C5 Fe1 C1 40.54(5) 3_767 3_767 ?
C4 Fe1 C1 111.85(5) . 3_767 ?
C4 Fe1 C1 68.15(5) 3_767 3_767 ?
C2 Fe1 C1 40.80(5) 3_767 3_767 ?
C2 Fe1 C1 139.20(5) . 3_767 ?
C1 Fe1 C1 180.0 . 3_767 ?
 
_diffrn_measured_fraction_theta_max    0.999
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.999
_refine_diff_density_max    0.337
_refine_diff_density_min   -0.289
_refine_diff_density_rms    0.058
