# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_3a
_database_code_depnum_ccdc_archive 'CCDC 1061921'
_audit_update_record             
;
2015-04-27 deposited with the CCDC.
2015-09-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H31 B Cl Fe O3 P Si'
_chemical_formula_sum            'C19 H31 B Cl Fe O3 P Si'
_chemical_formula_weight         468.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_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                   8.606(2)
_cell_length_b                   18.251(10)
_cell_length_c                   14.997(7)
_cell_angle_alpha                90
_cell_angle_beta                 91.994(15)
_cell_angle_gamma                90
_cell_volume                     2354.3(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    99(2)
_cell_measurement_reflns_used    8068
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      27.06

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.889
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6265
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SadAbs 2008/1 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      99(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            41848
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.758
_diffrn_reflns_theta_max         25.983
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4598
_reflns_number_gt                4037
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V7.68A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V7.68A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_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     
'w=1/[σ²(Fo²)+(0.0316P)²+1.2242P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   iterative
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4598
_refine_ls_number_parameters     254
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0691
_refine_ls_wR_factor_gt          0.0623
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.001
_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_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
Fe1 Fe 0.62820(2) 0.01305(2) 0.30411(2) 0.01689(7) Uani 1 1 d . . . . .
C1 C 0.48214(19) 0.03801(9) 0.37987(11) 0.0230(3) Uani 1 1 d . . . . .
O1 O 0.39055(15) 0.05295(7) 0.43026(9) 0.0334(3) Uani 1 1 d . . . . .
C2 C 0.7818(2) 0.00091(9) 0.38412(12) 0.0247(4) Uani 1 1 d . . . . .
O2 O 0.87970(16) -0.00962(7) 0.43619(9) 0.0376(3) Uani 1 1 d . . . . .
C3 C 0.52719(19) 0.02417(9) 0.19915(11) 0.0231(3) Uani 1 1 d . . . . .
O3 O 0.45922(16) 0.03104(7) 0.13294(8) 0.0349(3) Uani 1 1 d . . . . .
B1 B 0.6720(2) 0.12247(10) 0.29751(12) 0.0192(4) Uani 1 1 d . . . . .
Cl1 Cl 0.71853(5) 0.16668(2) 0.19328(3) 0.02620(10) Uani 1 1 d . . . . .
P1_1 P 0.54643(5) -0.10501(2) 0.31129(3) 0.02183(10) Uani 1 1 d . . . . .
C1_1 C 0.3486(2) -0.11423(10) 0.34954(15) 0.0366(4) Uani 1 1 d . . . . .
H1A_1 H 0.3158 -0.1655 0.3445 0.055 Uiso 1 1 calc R U . . .
H1B_1 H 0.2785 -0.0835 0.3127 0.055 Uiso 1 1 calc R U . . .
H1C_1 H 0.3451 -0.0986 0.4119 0.055 Uiso 1 1 calc R U . . .
C2_1 C 0.6514(2) -0.16506(9) 0.38825(12) 0.0291(4) Uani 1 1 d . . . . .
H2A_1 H 0.6019 -0.2134 0.3878 0.044 Uiso 1 1 calc R U . . .
H2B_1 H 0.6499 -0.1444 0.4485 0.044 Uiso 1 1 calc R U . . .
H2C_1 H 0.7593 -0.1698 0.3701 0.044 Uiso 1 1 calc R U . . .
C3_1 C 0.5325(2) -0.15738(10) 0.20787(12) 0.0326(4) Uani 1 1 d . . . . .
H3A_1 H 0.6358 -0.1617 0.1829 0.049 Uiso 1 1 calc R U . . .
H3B_1 H 0.4624 -0.1322 0.1650 0.049 Uiso 1 1 calc R U . . .
H3C_1 H 0.4917 -0.2064 0.2200 0.049 Uiso 1 1 calc R U . . .
Si1_2 Si 0.85164(5) -0.01723(3) 0.21388(3) 0.02472(11) Uani 1 1 d . . . . .
C1_2 C 0.9408(2) -0.10906(10) 0.24367(13) 0.0325(4) Uani 1 1 d . . . . .
H1A_2 H 0.8646 -0.1479 0.2311 0.049 Uiso 1 1 calc R U . . .
H1B_2 H 0.9714 -0.1097 0.3072 0.049 Uiso 1 1 calc R U . . .
H1C_2 H 1.0326 -0.1172 0.2081 0.049 Uiso 1 1 calc R U . . .
C2_2 C 0.8042(3) -0.01991(11) 0.09081(13) 0.0363(4) Uani 1 1 d . . . . .
H2A_2 H 0.8975 -0.0332 0.0589 0.054 Uiso 1 1 calc R U . . .
H2B_2 H 0.7676 0.0284 0.0709 0.054 Uiso 1 1 calc R U . . .
H2C_2 H 0.7227 -0.0564 0.0785 0.054 Uiso 1 1 calc R U . . .
C3_2 C 1.0261(2) 0.04493(11) 0.22841(15) 0.0370(4) Uani 1 1 d . . . . .
H3A_2 H 1.1069 0.0294 0.1880 0.055 Uiso 1 1 calc R U . . .
H3B_2 H 1.0665 0.0422 0.2902 0.055 Uiso 1 1 calc R U . . .
H3C_2 H 0.9953 0.0955 0.2145 0.055 Uiso 1 1 calc R U . . .
C1_3 C 0.65276(18) 0.18261(8) 0.37254(10) 0.0189(3) Uani 1 1 d . . . . .
C2_3 C 0.77826(18) 0.20293(8) 0.42994(10) 0.0204(3) Uani 1 1 d . . . . .
C3_3 C 0.7592(2) 0.25825(9) 0.49356(11) 0.0231(3) Uani 1 1 d . . . . .
C4_3 C 0.6156(2) 0.29190(9) 0.49895(11) 0.0234(3) Uani 1 1 d . . . . .
H4_3 H 0.6027 0.3290 0.5425 0.028 Uiso 1 1 calc R U . . .
C5_3 C 0.48999(19) 0.27334(9) 0.44298(11) 0.0220(3) Uani 1 1 d . . . . .
C6_3 C 0.50871(18) 0.21863(8) 0.37865(10) 0.0197(3) Uani 1 1 d . . . . .
C7_3 C 0.93529(19) 0.16721(9) 0.42242(12) 0.0264(4) Uani 1 1 d . . . . .
H7A_3 H 0.9581 0.1375 0.4757 0.040 Uiso 1 1 calc R U . . .
H7B_3 H 1.0151 0.2051 0.4173 0.040 Uiso 1 1 calc R U . . .
H7C_3 H 0.9346 0.1358 0.3694 0.040 Uiso 1 1 calc R U . . .
C8_3 C 0.8926(2) 0.28181(11) 0.55470(12) 0.0316(4) Uani 1 1 d . . . . .
H8A_3 H 0.8566 0.3192 0.5961 0.047 Uiso 1 1 calc R U . . .
H8B_3 H 0.9758 0.3022 0.5192 0.047 Uiso 1 1 calc R U . . .
H8C_3 H 0.9322 0.2394 0.5885 0.047 Uiso 1 1 calc R U . . .
C9_3 C 0.3366(2) 0.31233(10) 0.45202(12) 0.0283(4) Uani 1 1 d . . . . .
H9A_3 H 0.3065 0.3358 0.3952 0.043 Uiso 1 1 calc R U . . .
H9B_3 H 0.3470 0.3497 0.4988 0.043 Uiso 1 1 calc R U . . .
H9C_3 H 0.2567 0.2768 0.4679 0.043 Uiso 1 1 calc R U . . .
C10_3 C 0.37379(19) 0.20137(9) 0.31475(11) 0.0246(4) Uani 1 1 d . . . . .
H10A_3 H 0.2824 0.1884 0.3487 0.037 Uiso 1 1 calc R U . . .
H10B_3 H 0.4014 0.1601 0.2766 0.037 Uiso 1 1 calc R U . . .
H10C_3 H 0.3501 0.2444 0.2776 0.037 Uiso 1 1 calc R U . . .


_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
Fe1 C2 1.7682(18) . ?
Fe1 C1 1.7828(18) . ?
Fe1 C3 1.7830(18) . ?
Fe1 B1 2.035(2) . ?
Fe1 P1_1 2.2705(12) . ?
Fe1 Si1_2 2.4526(8) . ?
C1 O1 1.144(2) . ?
C2 O2 1.145(2) . ?
C3 O3 1.142(2) . ?
B1 C1_3 1.585(2) . ?
B1 Cl1 1.8163(19) . ?
P1_1 C2_1 1.8104(18) . ?
P1_1 C3_1 1.8222(19) . ?
P1_1 C1_1 1.8232(19) . ?
C1_1 H1A_1 0.9800 . ?
C1_1 H1B_1 0.9800 . ?
C1_1 H1C_1 0.9800 . ?
C2_1 H2A_1 0.9800 . ?
C2_1 H2B_1 0.9800 . ?
C2_1 H2C_1 0.9800 . ?
C3_1 H3A_1 0.9800 . ?
C3_1 H3B_1 0.9800 . ?
C3_1 H3C_1 0.9800 . ?
Si1_2 C2_2 1.877(2) . ?
Si1_2 C3_2 1.8884(19) . ?
Si1_2 C1_2 1.890(2) . ?
C1_2 H1A_2 0.9800 . ?
C1_2 H1B_2 0.9800 . ?
C1_2 H1C_2 0.9800 . ?
C2_2 H2A_2 0.9800 . ?
C2_2 H2B_2 0.9800 . ?
C2_2 H2C_2 0.9800 . ?
C3_2 H3A_2 0.9800 . ?
C3_2 H3B_2 0.9800 . ?
C3_2 H3C_2 0.9800 . ?
C1_3 C2_3 1.407(2) . ?
C1_3 C6_3 1.409(2) . ?
C2_3 C3_3 1.403(2) . ?
C2_3 C7_3 1.508(2) . ?
C3_3 C4_3 1.385(2) . ?
C3_3 C8_3 1.507(2) . ?
C4_3 C5_3 1.387(2) . ?
C4_3 H4_3 0.9500 . ?
C5_3 C6_3 1.402(2) . ?
C5_3 C9_3 1.510(2) . ?
C6_3 C10_3 1.513(2) . ?
C7_3 H7A_3 0.9800 . ?
C7_3 H7B_3 0.9800 . ?
C7_3 H7C_3 0.9800 . ?
C8_3 H8A_3 0.9800 . ?
C8_3 H8B_3 0.9800 . ?
C8_3 H8C_3 0.9800 . ?
C9_3 H9A_3 0.9800 . ?
C9_3 H9B_3 0.9800 . ?
C9_3 H9C_3 0.9800 . ?
C10_3 H10A_3 0.9800 . ?
C10_3 H10B_3 0.9800 . ?
C10_3 H10C_3 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
C2 Fe1 C1 97.27(8) . . ?
C2 Fe1 C3 160.64(8) . . ?
C1 Fe1 C3 101.57(8) . . ?
C2 Fe1 B1 91.18(7) . . ?
C1 Fe1 B1 85.18(7) . . ?
C3 Fe1 B1 86.03(7) . . ?
C2 Fe1 P1_1 94.28(6) . . ?
C1 Fe1 P1_1 89.18(5) . . ?
C3 Fe1 P1_1 90.43(5) . . ?
B1 Fe1 P1_1 172.61(5) . . ?
C2 Fe1 Si1_2 76.36(7) . . ?
C1 Fe1 Si1_2 173.22(6) . . ?
C3 Fe1 Si1_2 84.62(6) . . ?
B1 Fe1 Si1_2 92.54(5) . . ?
P1_1 Fe1 Si1_2 93.59(2) . . ?
O1 C1 Fe1 178.13(16) . . ?
O2 C2 Fe1 177.45(15) . . ?
O3 C3 Fe1 178.36(16) . . ?
C1_3 B1 Cl1 109.58(12) . . ?
C1_3 B1 Fe1 128.39(12) . . ?
Cl1 B1 Fe1 121.63(10) . . ?
C2_1 P1_1 C3_1 103.99(9) . . ?
C2_1 P1_1 C1_1 101.21(9) . . ?
C3_1 P1_1 C1_1 100.64(9) . . ?
C2_1 P1_1 Fe1 117.14(7) . . ?
C3_1 P1_1 Fe1 117.95(7) . . ?
C1_1 P1_1 Fe1 113.38(6) . . ?
P1_1 C1_1 H1A_1 109.5 . . ?
P1_1 C1_1 H1B_1 109.5 . . ?
H1A_1 C1_1 H1B_1 109.5 . . ?
P1_1 C1_1 H1C_1 109.5 . . ?
H1A_1 C1_1 H1C_1 109.5 . . ?
H1B_1 C1_1 H1C_1 109.5 . . ?
P1_1 C2_1 H2A_1 109.5 . . ?
P1_1 C2_1 H2B_1 109.5 . . ?
H2A_1 C2_1 H2B_1 109.5 . . ?
P1_1 C2_1 H2C_1 109.5 . . ?
H2A_1 C2_1 H2C_1 109.5 . . ?
H2B_1 C2_1 H2C_1 109.5 . . ?
P1_1 C3_1 H3A_1 109.5 . . ?
P1_1 C3_1 H3B_1 109.5 . . ?
H3A_1 C3_1 H3B_1 109.5 . . ?
P1_1 C3_1 H3C_1 109.5 . . ?
H3A_1 C3_1 H3C_1 109.5 . . ?
H3B_1 C3_1 H3C_1 109.5 . . ?
C2_2 Si1_2 C3_2 105.91(10) . . ?
C2_2 Si1_2 C1_2 106.38(9) . . ?
C3_2 Si1_2 C1_2 101.01(9) . . ?
C2_2 Si1_2 Fe1 113.60(7) . . ?
C3_2 Si1_2 Fe1 115.87(7) . . ?
C1_2 Si1_2 Fe1 112.89(6) . . ?
Si1_2 C1_2 H1A_2 109.5 . . ?
Si1_2 C1_2 H1B_2 109.5 . . ?
H1A_2 C1_2 H1B_2 109.5 . . ?
Si1_2 C1_2 H1C_2 109.5 . . ?
H1A_2 C1_2 H1C_2 109.5 . . ?
H1B_2 C1_2 H1C_2 109.5 . . ?
Si1_2 C2_2 H2A_2 109.5 . . ?
Si1_2 C2_2 H2B_2 109.5 . . ?
H2A_2 C2_2 H2B_2 109.5 . . ?
Si1_2 C2_2 H2C_2 109.5 . . ?
H2A_2 C2_2 H2C_2 109.5 . . ?
H2B_2 C2_2 H2C_2 109.5 . . ?
Si1_2 C3_2 H3A_2 109.5 . . ?
Si1_2 C3_2 H3B_2 109.5 . . ?
H3A_2 C3_2 H3B_2 109.5 . . ?
Si1_2 C3_2 H3C_2 109.5 . . ?
H3A_2 C3_2 H3C_2 109.5 . . ?
H3B_2 C3_2 H3C_2 109.5 . . ?
C2_3 C1_3 C6_3 119.71(14) . . ?
C2_3 C1_3 B1 121.34(14) . . ?
C6_3 C1_3 B1 118.89(14) . . ?
C3_3 C2_3 C1_3 120.03(15) . . ?
C3_3 C2_3 C7_3 119.22(14) . . ?
C1_3 C2_3 C7_3 120.73(14) . . ?
C4_3 C3_3 C2_3 118.98(15) . . ?
C4_3 C3_3 C8_3 120.03(15) . . ?
C2_3 C3_3 C8_3 120.99(16) . . ?
C3_3 C4_3 C5_3 122.31(15) . . ?
C3_3 C4_3 H4_3 118.8 . . ?
C5_3 C4_3 H4_3 118.8 . . ?
C4_3 C5_3 C6_3 118.98(15) . . ?
C4_3 C5_3 C9_3 119.73(15) . . ?
C6_3 C5_3 C9_3 121.28(15) . . ?
C5_3 C6_3 C1_3 119.97(15) . . ?
C5_3 C6_3 C10_3 118.70(14) . . ?
C1_3 C6_3 C10_3 121.29(14) . . ?
C2_3 C7_3 H7A_3 109.5 . . ?
C2_3 C7_3 H7B_3 109.5 . . ?
H7A_3 C7_3 H7B_3 109.5 . . ?
C2_3 C7_3 H7C_3 109.5 . . ?
H7A_3 C7_3 H7C_3 109.5 . . ?
H7B_3 C7_3 H7C_3 109.5 . . ?
C3_3 C8_3 H8A_3 109.5 . . ?
C3_3 C8_3 H8B_3 109.5 . . ?
H8A_3 C8_3 H8B_3 109.5 . . ?
C3_3 C8_3 H8C_3 109.5 . . ?
H8A_3 C8_3 H8C_3 109.5 . . ?
H8B_3 C8_3 H8C_3 109.5 . . ?
C5_3 C9_3 H9A_3 109.5 . . ?
C5_3 C9_3 H9B_3 109.5 . . ?
H9A_3 C9_3 H9B_3 109.5 . . ?
C5_3 C9_3 H9C_3 109.5 . . ?
H9A_3 C9_3 H9C_3 109.5 . . ?
H9B_3 C9_3 H9C_3 109.5 . . ?
C6_3 C10_3 H10A_3 109.5 . . ?
C6_3 C10_3 H10B_3 109.5 . . ?
H10A_3 C10_3 H10B_3 109.5 . . ?
C6_3 C10_3 H10C_3 109.5 . . ?
H10A_3 C10_3 H10C_3 109.5 . . ?
H10B_3 C10_3 H10C_3 109.5 . . ?

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
Cl1 B1 C1_3 C2_3 -93.38(15) . . . . ?
Fe1 B1 C1_3 C2_3 93.87(18) . . . . ?
Cl1 B1 C1_3 C6_3 83.58(16) . . . . ?
Fe1 B1 C1_3 C6_3 -89.16(18) . . . . ?
C6_3 C1_3 C2_3 C3_3 0.7(2) . . . . ?
B1 C1_3 C2_3 C3_3 177.65(14) . . . . ?
C6_3 C1_3 C2_3 C7_3 -177.67(14) . . . . ?
B1 C1_3 C2_3 C7_3 -0.7(2) . . . . ?
C1_3 C2_3 C3_3 C4_3 0.3(2) . . . . ?
C7_3 C2_3 C3_3 C4_3 178.69(15) . . . . ?
C1_3 C2_3 C3_3 C8_3 -178.97(15) . . . . ?
C7_3 C2_3 C3_3 C8_3 -0.6(2) . . . . ?
C2_3 C3_3 C4_3 C5_3 -0.7(2) . . . . ?
C8_3 C3_3 C4_3 C5_3 178.61(16) . . . . ?
C3_3 C4_3 C5_3 C6_3 0.0(2) . . . . ?
C3_3 C4_3 C5_3 C9_3 -179.76(15) . . . . ?
C4_3 C5_3 C6_3 C1_3 1.0(2) . . . . ?
C9_3 C5_3 C6_3 C1_3 -179.23(15) . . . . ?
C4_3 C5_3 C6_3 C10_3 -176.90(14) . . . . ?
C9_3 C5_3 C6_3 C10_3 2.9(2) . . . . ?
C2_3 C1_3 C6_3 C5_3 -1.4(2) . . . . ?
B1 C1_3 C6_3 C5_3 -178.38(14) . . . . ?
C2_3 C1_3 C6_3 C10_3 176.50(14) . . . . ?
B1 C1_3 C6_3 C10_3 -0.5(2) . . . . ?

_refine_diff_density_max         0.424
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.053

_shelxl_version_number           2014/6


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6c
_database_code_depnum_ccdc_archive 'CCDC 1061922'
_audit_update_record             
;
2015-04-27 deposited with the CCDC.
2015-09-01 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H38 Fe2 O6 P2 Si2'
_chemical_formula_sum            'C20 H38 Fe2 O6 P2 Si2'
_chemical_formula_weight         604.32

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_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                   10.1597(16)
_cell_length_b                   12.900(2)
_cell_length_c                   10.7901(18)
_cell_angle_alpha                90
_cell_angle_beta                 105.385(5)
_cell_angle_gamma                90
_cell_volume                     1363.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5482
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      26.78

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_F_000             632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.301
_shelx_estimated_absorpt_T_min   0.839
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5920
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/4 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker SMART-APEX'
_diffrn_detector                 'CCD area detector (Apex1)'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            11947
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.449
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2785
_reflns_number_gt                2487
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Smart NT ver. 5.63 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.27B (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.27B (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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     
'w=1/[σ²(Fo²)+(0.0335P)²+0.3510P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   iterative
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2785
_refine_ls_number_parameters     150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0660
_refine_ls_wR_factor_gt          0.0634
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_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_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
Fe1 Fe 0.36704(2) 0.51786(2) 0.59805(2) 0.01000(9) Uani 1 1 d . . . . .
O1 O 0.27309(12) 0.68904(10) 0.41903(11) 0.0221(3) Uani 1 1 d . . . . .
C1 C 0.40905(16) 0.27671(12) 0.47101(15) 0.0138(3) Uani 1 1 d . . . . .
H1A H 0.4715 0.2676 0.5579 0.017 Uiso 1 1 calc R U . . .
H1B H 0.3158 0.2609 0.4775 0.017 Uiso 1 1 calc R U . . .
P1 P 0.32327(4) 0.60454(3) 0.76239(4) 0.01288(11) Uani 1 1 d . . . . .
Si1 Si 0.41325(4) 0.41993(3) 0.42621(4) 0.01019(11) Uani 1 1 d . . . . .
C4 C 0.13257(18) 0.39669(15) 0.26342(17) 0.0234(4) Uani 1 1 d . . . . .
H4A H 0.0748 0.4002 0.1750 0.035 Uiso 1 1 calc R U . . .
H4B H 0.0948 0.4418 0.3185 0.035 Uiso 1 1 calc R U . . .
H4C H 0.1355 0.3251 0.2945 0.035 Uiso 1 1 calc R U . . .
C3 C 0.27686(16) 0.43240(13) 0.26696(15) 0.0150(3) Uani 1 1 d . . . . .
H3A H 0.2720 0.5061 0.2407 0.018 Uiso 1 1 calc R U . . .
H3B H 0.3076 0.3925 0.2014 0.018 Uiso 1 1 calc R U . . .
O3 O 0.11123(12) 0.40335(10) 0.56179(12) 0.0238(3) Uani 1 1 d . . . . .
C2 C 0.44644(18) 0.19527(13) 0.38349(16) 0.0195(4) Uani 1 1 d . . . . .
H2A H 0.4380 0.1260 0.4178 0.029 Uiso 1 1 calc R U . . .
H2B H 0.5407 0.2063 0.3795 0.029 Uiso 1 1 calc R U . . .
H2C H 0.3847 0.2013 0.2970 0.029 Uiso 1 1 calc R U . . .
O2 O 0.54108(12) 0.38017(9) 0.78763(11) 0.0187(3) Uani 1 1 d . . . . .
C11 C 0.20378(18) 0.71150(14) 0.71676(17) 0.0185(4) Uani 1 1 d . . . . .
H11A H 0.1820 0.7393 0.7935 0.028 Uiso 1 1 calc R U . . .
H11B H 0.1200 0.6868 0.6560 0.028 Uiso 1 1 calc R U . . .
H11C H 0.2449 0.7661 0.6761 0.028 Uiso 1 1 calc R U . . .
C12 C 0.46119(18) 0.66028(14) 0.88779(16) 0.0193(4) Uani 1 1 d . . . . .
H12A H 0.4240 0.6902 0.9549 0.029 Uiso 1 1 calc R U . . .
H12B H 0.5066 0.7147 0.8509 0.029 Uiso 1 1 calc R U . . .
H12C H 0.5274 0.6060 0.9252 0.029 Uiso 1 1 calc R U . . .
C13 C 0.24118(19) 0.52424(14) 0.85994(17) 0.0205(4) Uani 1 1 d . . . . .
H13A H 0.2257 0.5656 0.9309 0.031 Uiso 1 1 calc R U . . .
H13B H 0.3003 0.4652 0.8946 0.031 Uiso 1 1 calc R U . . .
H13C H 0.1535 0.4988 0.8065 0.031 Uiso 1 1 calc R U . . .
C21 C 0.31174(16) 0.62115(13) 0.48837(15) 0.0144(3) Uani 1 1 d . . . . .
C22 C 0.47455(16) 0.43348(13) 0.71018(15) 0.0131(3) Uani 1 1 d . . . . .
C23 C 0.21136(17) 0.44804(14) 0.57335(15) 0.0155(3) 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
Fe1 C21 1.7717(17) . ?
Fe1 C22 1.7721(17) . ?
Fe1 C23 1.7777(17) . ?
Fe1 P1 2.2385(5) . ?
Fe1 Si1 2.3908(5) . ?
Fe1 Si1 2.4506(6) 3_666 ?
O1 C21 1.151(2) . ?
C1 C2 1.527(2) . ?
C1 Si1 1.9131(17) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
P1 C11 1.8174(17) . ?
P1 C12 1.8181(17) . ?
P1 C13 1.8283(18) . ?
Si1 C3 1.9066(16) . ?
Si1 Fe1 2.4506(6) 3_666 ?
C4 C3 1.527(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O3 C23 1.147(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O2 C22 1.153(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 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
C21 Fe1 C22 161.22(7) . . ?
C21 Fe1 C23 99.73(8) . . ?
C22 Fe1 C23 98.85(7) . . ?
C21 Fe1 P1 93.38(5) . . ?
C22 Fe1 P1 88.97(5) . . ?
C23 Fe1 P1 90.92(5) . . ?
C21 Fe1 Si1 88.40(5) . . ?
C22 Fe1 Si1 89.58(5) . . ?
C23 Fe1 Si1 88.05(5) . . ?
P1 Fe1 Si1 178.072(18) . . ?
C21 Fe1 Si1 79.56(5) . 3_666 ?
C22 Fe1 Si1 81.96(5) . 3_666 ?
C23 Fe1 Si1 161.68(5) . 3_666 ?
P1 Fe1 Si1 107.401(18) . 3_666 ?
Si1 Fe1 Si1 73.641(19) . 3_666 ?
C2 C1 Si1 118.85(11) . . ?
C2 C1 H1A 107.6 . . ?
Si1 C1 H1A 107.6 . . ?
C2 C1 H1B 107.6 . . ?
Si1 C1 H1B 107.6 . . ?
H1A C1 H1B 107.0 . . ?
C11 P1 C12 103.23(8) . . ?
C11 P1 C13 102.25(8) . . ?
C12 P1 C13 100.07(8) . . ?
C11 P1 Fe1 115.06(6) . . ?
C12 P1 Fe1 120.75(6) . . ?
C13 P1 Fe1 112.94(6) . . ?
C3 Si1 C1 104.45(7) . . ?
C3 Si1 Fe1 114.15(6) . . ?
C1 Si1 Fe1 106.99(5) . . ?
C3 Si1 Fe1 109.93(5) . 3_666 ?
C1 Si1 Fe1 115.17(5) . 3_666 ?
Fe1 Si1 Fe1 106.360(19) . 3_666 ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C4 C3 Si1 117.41(12) . . ?
C4 C3 H3A 108.0 . . ?
Si1 C3 H3A 107.9 . . ?
C4 C3 H3B 107.9 . . ?
Si1 C3 H3B 108.0 . . ?
H3A C3 H3B 107.2 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
P1 C11 H11A 109.5 . . ?
P1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P1 C12 H12A 109.5 . . ?
P1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
P1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
P1 C13 H13A 109.5 . . ?
P1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
P1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C21 Fe1 178.01(15) . . ?
O2 C22 Fe1 176.53(14) . . ?
O3 C23 Fe1 177.66(15) . . ?

_refine_diff_density_max         0.503
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.064


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7c
_database_code_depnum_ccdc_archive 'CCDC 1061923'
_audit_update_record             
;
2015-04-27 deposited with the CCDC.
2015-09-01 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H38 Fe2 O5 P2 Si2'
_chemical_formula_sum            'C19 H38 Fe2 O5 P2 Si2'
_chemical_formula_weight         576.31

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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.
;

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

_cell_length_a                   9.1382(6)
_cell_length_b                   12.4474(8)
_cell_length_c                   11.8729(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.852(2)
_cell_angle_gamma                90
_cell_volume                     1340.86(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9903
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      26.73

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_F_000             604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.316
_shelx_estimated_absorpt_T_min   0.779
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6238
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/4 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker SMART-APEX'
_diffrn_detector                 'CCD area detector (Apex1)'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            25930
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.728
_diffrn_reflns_theta_max         26.874
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5701
_reflns_number_gt                5521
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_max     0.983
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       'Smart NT ver. 5.63 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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     
'w=1/[σ²(Fo²)+(0.0190P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   iterative
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2506 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5701
_refine_ls_number_parameters     281
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0191
_refine_ls_wR_factor_ref         0.0429
_refine_ls_wR_factor_gt          0.0426
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.001
_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_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
Fe1 Fe 0.83667(3) 0.56578(2) 0.73751(3) 0.00931(8) Uani 1 1 d . . . . .
P1 P 0.86342(6) 0.72555(5) 0.65818(6) 0.01365(14) Uani 1 1 d . . . . .
Si1 Si 0.61353(6) 0.52723(5) 0.62905(6) 0.01104(14) Uani 1 1 d . . . . .
O1 O 0.67817(18) 0.69898(13) 0.89042(16) 0.0195(4) Uani 1 1 d . . . . .
C1 C 0.7016(2) 0.62048(18) 0.8399(2) 0.0130(5) Uani 1 1 d . . . . .
Fe2 Fe 0.61176(3) 0.47445(2) 0.81626(3) 0.01034(8) Uani 1 1 d . . . . .
P2 P 0.62334(6) 0.45595(5) 1.00463(6) 0.01316(13) Uani 1 1 d . . . . .
Si2 Si 0.83863(6) 0.39030(5) 0.80835(6) 0.01184(14) Uani 1 1 d . . . . .
O2 O 1.07074(17) 0.61293(14) 0.92252(15) 0.0181(4) Uani 1 1 d . . . . .
C2 C 0.9816(2) 0.59200(17) 0.8491(2) 0.0119(5) Uani 1 1 d . . . . .
O3 O 0.97936(18) 0.46635(15) 0.55546(16) 0.0232(4) Uani 1 1 d . . . . .
C3 C 0.9226(2) 0.50299(18) 0.6292(2) 0.0153(5) Uani 1 1 d . . . . .
O4 O 0.32705(16) 0.58283(15) 0.80109(16) 0.0243(4) Uani 1 1 d . . . . .
C4 C 0.4389(2) 0.54094(18) 0.8060(2) 0.0154(5) Uani 1 1 d . . . . .
O5 O 0.4895(2) 0.26509(15) 0.74478(19) 0.0298(5) Uani 1 1 d . . . . .
C5 C 0.5419(3) 0.3461(2) 0.7734(2) 0.0176(5) Uani 1 1 d . . . . .
C6 C 0.7545(3) 0.83963(19) 0.6952(3) 0.0238(6) Uani 1 1 d . . . . .
H6A H 0.7849 0.9041 0.6567 0.036 Uiso 1 1 calc R U . . .
H6B H 0.7699 0.8508 0.7775 0.036 Uiso 1 1 calc R U . . .
H6C H 0.6499 0.8255 0.6713 0.036 Uiso 1 1 calc R U . . .
C7 C 0.8440(3) 0.7314(2) 0.5036(2) 0.0233(6) Uani 1 1 d . . . . .
H7A H 0.8699 0.8035 0.4794 0.035 Uiso 1 1 calc R U . . .
H7B H 0.7418 0.7153 0.4735 0.035 Uiso 1 1 calc R U . . .
H7C H 0.9098 0.6785 0.4749 0.035 Uiso 1 1 calc R U . . .
C8 C 1.0494(3) 0.7802(2) 0.6917(3) 0.0255(7) Uani 1 1 d . . . . .
H8A H 1.0587 0.8462 0.6481 0.038 Uiso 1 1 calc R U . . .
H8B H 1.1217 0.7274 0.6719 0.038 Uiso 1 1 calc R U . . .
H8C H 1.0676 0.7963 0.7729 0.038 Uiso 1 1 calc R U . . .
C9 C 0.4604(3) 0.5060(2) 1.0628(2) 0.0232(6) Uani 1 1 d . . . . .
H9A H 0.4708 0.4932 1.1448 0.035 Uiso 1 1 calc R U . . .
H9B H 0.3727 0.4685 1.0268 0.035 Uiso 1 1 calc R U . . .
H9C H 0.4500 0.5833 1.0480 0.035 Uiso 1 1 calc R U . . .
C10 C 0.7668(3) 0.5258(2) 1.0982(2) 0.0232(6) Uani 1 1 d . . . . .
H10A H 0.7534 0.5114 1.1775 0.035 Uiso 1 1 calc R U . . .
H10B H 0.7597 0.6032 1.0838 0.035 Uiso 1 1 calc R U . . .
H10C H 0.8640 0.5000 1.0833 0.035 Uiso 1 1 calc R U . . .
C11 C 0.6329(3) 0.31896(19) 1.0586(2) 0.0194(6) Uani 1 1 d . . . . .
H11A H 0.6319 0.3200 1.1410 0.029 Uiso 1 1 calc R U . . .
H11B H 0.7240 0.2850 1.0405 0.029 Uiso 1 1 calc R U . . .
H11C H 0.5478 0.2781 1.0232 0.029 Uiso 1 1 calc R U . . .
C12 C 0.9887(3) 0.3575(2) 0.9287(2) 0.0195(6) Uani 1 1 d . . . . .
H12A H 0.9984 0.4175 0.9838 0.023 Uiso 1 1 calc R U . . .
H12B H 0.9608 0.2922 0.9687 0.023 Uiso 1 1 calc R U . . .
C13 C 1.1373(3) 0.3388(2) 0.8829(3) 0.0259(7) Uani 1 1 d . . . . .
H13A H 1.2121 0.3194 0.9457 0.039 Uiso 1 1 calc R U . . .
H13B H 1.1673 0.4047 0.8467 0.039 Uiso 1 1 calc R U . . .
H13C H 1.1271 0.2804 0.8271 0.039 Uiso 1 1 calc R U . . .
C14 C 0.8471(3) 0.26805(19) 0.7132(2) 0.0190(6) Uani 1 1 d . . . . .
H14A H 0.7628 0.2708 0.6526 0.023 Uiso 1 1 calc R U . . .
H14B H 0.9386 0.2718 0.6764 0.023 Uiso 1 1 calc R U . . .
C15 C 0.8435(3) 0.1597(2) 0.7756(3) 0.0262(7) Uani 1 1 d . . . . .
H15A H 0.8438 0.1009 0.7208 0.039 Uiso 1 1 calc R U . . .
H15B H 0.7541 0.1556 0.8135 0.039 Uiso 1 1 calc R U . . .
H15C H 0.9305 0.1538 0.8322 0.039 Uiso 1 1 calc R U . . .
C16 C 0.6001(3) 0.42810(19) 0.5074(2) 0.0168(5) Uani 1 1 d . . . . .
H16A H 0.6736 0.3705 0.5265 0.020 Uiso 1 1 calc R U . . .
H16B H 0.5013 0.3945 0.5002 0.020 Uiso 1 1 calc R U . . .
C17 C 0.6248(3) 0.4757(2) 0.3922(2) 0.0213(6) Uani 1 1 d . . . . .
H17A H 0.6113 0.4195 0.3341 0.032 Uiso 1 1 calc R U . . .
H17B H 0.7252 0.5044 0.3963 0.032 Uiso 1 1 calc R U . . .
H17C H 0.5537 0.5336 0.3726 0.032 Uiso 1 1 calc R U . . .
C18 C 0.4777(2) 0.63723(19) 0.5760(2) 0.0159(5) Uani 1 1 d . . . . .
H18A H 0.4655 0.6869 0.6393 0.019 Uiso 1 1 calc R U . . .
H18B H 0.5187 0.6788 0.5160 0.019 Uiso 1 1 calc R U . . .
C19 C 0.3258(3) 0.5927(2) 0.5283(2) 0.0225(6) Uani 1 1 d . . . . .
H19A H 0.2566 0.6524 0.5117 0.034 Uiso 1 1 calc R U . . .
H19B H 0.2894 0.5449 0.5844 0.034 Uiso 1 1 calc R U . . .
H19C H 0.3346 0.5525 0.4585 0.034 Uiso 1 1 calc R U . . .


_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
Fe1 C3 1.766(3) . ?
Fe1 C2 1.788(2) . ?
Fe1 C1 1.955(2) . ?
Fe1 P1 2.2264(7) . ?
Fe1 Si1 2.3281(7) . ?
Fe1 Si2 2.3399(7) . ?
Fe1 Fe2 2.6171(4) . ?
P1 C6 1.818(3) . ?
P1 C7 1.824(3) . ?
P1 C8 1.830(2) . ?
Si1 C16 1.893(3) . ?
Si1 C18 1.904(2) . ?
Si1 Fe2 2.3197(8) . ?
O1 C1 1.180(3) . ?
C1 Fe2 2.001(2) . ?
Fe2 C5 1.773(3) . ?
Fe2 C4 1.774(2) . ?
Fe2 P2 2.2382(8) . ?
Fe2 Si2 2.3346(7) . ?
P2 C11 1.820(2) . ?
P2 C9 1.824(3) . ?
P2 C10 1.833(3) . ?
Si2 C14 1.902(3) . ?
Si2 C12 1.903(3) . ?
O2 C2 1.150(3) . ?
O3 C3 1.163(3) . ?
O4 C4 1.143(3) . ?
O5 C5 1.150(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
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 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
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 1.540(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.540(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.531(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.539(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 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
C3 Fe1 C2 105.42(11) . . ?
C3 Fe1 C1 167.12(10) . . ?
C2 Fe1 C1 86.69(10) . . ?
C3 Fe1 P1 90.38(8) . . ?
C2 Fe1 P1 92.37(7) . . ?
C1 Fe1 P1 93.51(7) . . ?
C3 Fe1 Si1 86.68(8) . . ?
C2 Fe1 Si1 165.91(8) . . ?
C1 Fe1 Si1 80.76(7) . . ?
P1 Fe1 Si1 94.77(3) . . ?
C3 Fe1 Si2 82.16(8) . . ?
C2 Fe1 Si2 86.04(7) . . ?
C1 Fe1 Si2 94.59(7) . . ?
P1 Fe1 Si2 171.64(3) . . ?
Si1 Fe1 Si2 88.57(2) . . ?
C3 Fe1 Fe2 120.25(7) . . ?
C2 Fe1 Fe2 111.00(7) . . ?
C1 Fe1 Fe2 49.33(7) . . ?
P1 Fe1 Fe2 132.04(2) . . ?
Si1 Fe1 Fe2 55.58(2) . . ?
Si2 Fe1 Fe2 55.857(17) . . ?
C6 P1 C7 102.81(13) . . ?
C6 P1 C8 100.28(13) . . ?
C7 P1 C8 100.38(14) . . ?
C6 P1 Fe1 120.29(10) . . ?
C7 P1 Fe1 117.30(9) . . ?
C8 P1 Fe1 112.72(9) . . ?
C16 Si1 C18 103.67(11) . . ?
C16 Si1 Fe2 122.65(8) . . ?
C18 Si1 Fe2 116.21(9) . . ?
C16 Si1 Fe1 121.95(8) . . ?
C18 Si1 Fe1 121.88(8) . . ?
Fe2 Si1 Fe1 68.54(2) . . ?
O1 C1 Fe1 140.48(18) . . ?
O1 C1 Fe2 136.67(18) . . ?
Fe1 C1 Fe2 82.85(9) . . ?
C5 Fe2 C4 96.52(11) . . ?
C5 Fe2 C1 170.77(12) . . ?
C4 Fe2 C1 86.16(10) . . ?
C5 Fe2 P2 99.58(9) . . ?
C4 Fe2 P2 93.00(9) . . ?
C1 Fe2 P2 89.07(8) . . ?
C5 Fe2 Si1 91.36(9) . . ?
C4 Fe2 Si1 84.83(8) . . ?
C1 Fe2 Si1 80.06(8) . . ?
P2 Fe2 Si1 169.02(3) . . ?
C5 Fe2 Si2 82.83(8) . . ?
C4 Fe2 Si2 173.68(9) . . ?
C1 Fe2 Si2 93.53(6) . . ?
P2 Fe2 Si2 93.31(3) . . ?
Si1 Fe2 Si2 88.90(3) . . ?
C5 Fe2 Fe1 124.08(9) . . ?
C4 Fe2 Fe1 120.22(8) . . ?
C1 Fe2 Fe1 47.82(7) . . ?
P2 Fe2 Fe1 117.14(2) . . ?
Si1 Fe2 Fe1 55.883(18) . . ?
Si2 Fe2 Fe1 56.049(18) . . ?
C11 P2 C9 101.18(13) . . ?
C11 P2 C10 103.31(12) . . ?
C9 P2 C10 99.55(13) . . ?
C11 P2 Fe2 116.27(9) . . ?
C9 P2 Fe2 113.54(9) . . ?
C10 P2 Fe2 120.12(9) . . ?
C14 Si2 C12 101.37(11) . . ?
C14 Si2 Fe2 118.82(8) . . ?
C12 Si2 Fe2 129.05(9) . . ?
C14 Si2 Fe1 122.18(9) . . ?
C12 Si2 Fe1 116.38(8) . . ?
Fe2 Si2 Fe1 68.094(19) . . ?
O2 C2 Fe1 176.7(2) . . ?
O3 C3 Fe1 176.8(2) . . ?
O4 C4 Fe2 178.8(2) . . ?
O5 C5 Fe2 176.5(2) . . ?
P1 C6 H6A 109.5 . . ?
P1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
P1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P1 C7 H7A 109.5 . . ?
P1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P1 C8 H8A 109.5 . . ?
P1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P2 C11 H11A 109.5 . . ?
P2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 Si2 110.8(2) . . ?
C13 C12 H12A 109.5 . . ?
Si2 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
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 . . ?
C15 C14 Si2 114.2(2) . . ?
C15 C14 H14A 108.7 . . ?
Si2 C14 H14A 108.7 . . ?
C15 C14 H14B 108.7 . . ?
Si2 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 Si1 115.24(17) . . ?
C17 C16 H16A 108.5 . . ?
Si1 C16 H16A 108.5 . . ?
C17 C16 H16B 108.5 . . ?
Si1 C16 H16B 108.5 . . ?
H16A C16 H16B 107.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 Si1 112.74(16) . . ?
C19 C18 H18A 109.0 . . ?
Si1 C18 H18A 109.0 . . ?
C19 C18 H18B 109.0 . . ?
Si1 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

_refine_diff_density_max         0.351
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.047


# start Validation Reply Form
_vrf_PLAT987_7c                  
;
PROBLEM: The Flack x is >> 0 - Do a BASF/TWIN Refinement Please Check
RESPONSE: _refine_ls_abs_structure_Flack value is 0.014(4)
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# end Validation Reply Form





_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
