# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_B
_database_code_depnum_ccdc_archive 'CCDC 1862751'

_audit_update_record             
;
2018-11-28 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;
_publcif_datablock.id            {9086793c-12e5-456d-9879-5d89bdfd0adc}
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H42 Fe2 O4 P4'
_chemical_formula_sum            'C20 H42 Fe2 O4 P4'
_chemical_formula_weight         582.12

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'
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           5
_space_group_name_H-M_alt        'a 1 2 1'
_space_group_name_Hall           'A 2y'

_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, -z'
'x, y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'

_cell_length_a                   33.553(3)
_cell_length_b                   6.68483(14)
_cell_length_c                   22.247(2)
_cell_angle_alpha                90
_cell_angle_beta                 144.35(2)
_cell_angle_gamma                90
_cell_volume                     2908.3(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    4405
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      31.9

_exptl_crystal_description       'Rectangular prism'
_exptl_crystal_colour            Orange

_exptl_crystal_density_method    ?
_exptl_absorpt_coefficient_mu    1.239
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_F_000             1224


_exptl_transmission_factor_min   0.878
_exptl_transmission_factor_max   1
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.900
_oxdiff_exptl_absorpt_empirical_full_max 1.101
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.812

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_measurement_specimen_support Fiber
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
SCXMini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            37437
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.918
_diffrn_reflns_theta_max         31.867
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9616
_reflns_number_gt                8402
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_max     0.981
_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       'CrysAlisPro 1.171.39.28e (Rigaku, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku, 2015)'
_computing_structure_solution    'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    OLEX2
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²+1.1691P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.432(13)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         9616
_refine_ls_number_parameters     314
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0769
_refine_ls_wR_factor_gt          0.0726
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_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 0.45694(2) 0.23371(5) 0.49342(3) 0.02062(8) Uani 1 1 d . . . . .
Fe2 Fe 0.02763(2) 0.37964(6) 0.08935(3) 0.02412(9) Uani 1 1 d D . . . .
P1 P 0.44566(3) 0.06261(11) 0.39419(5) 0.02149(13) Uani 1 1 d . . . . .
P2 P 0.39453(4) 0.03467(12) 0.47221(6) 0.02923(16) Uani 1 1 d . . . . .
P3 P 0.06431(3) 0.54651(11) 0.05405(5) 0.02403(14) Uani 1 1 d . . . . .
P4 P 0.05515(5) 0.59121(14) 0.19389(7) 0.0411(2) Uani 1 1 d D . . . .
O12 O 0.50391(14) 0.5325(4) 0.63709(19) 0.0521(7) Uani 1 1 d . . . . .
O21 O 0.13861(15) 0.0880(5) 0.2302(2) 0.0629(8) Uani 1 1 d . . . . .
C101 C 0.36858(14) 0.0589(5) 0.24913(19) 0.0286(6) Uani 1 1 d . . . . .
O11 O 0.35517(13) 0.5331(4) 0.3363(2) 0.0529(7) Uani 1 1 d . . . . .
C301 C 0.15134(14) 0.5478(5) 0.1251(2) 0.0328(6) Uani 1 1 d . . . . .
C12 C 0.48811(15) 0.4100(5) 0.5843(2) 0.0308(6) Uani 1 1 d . . . . .
C203 C 0.44068(19) 0.0730(8) 0.6456(3) 0.0511(10) Uani 1 1 d . . . . .
H20A H 0.460421 -0.058017 0.666479 0.077 Uiso 1 1 calc R U . . .
H20B H 0.430957 0.101274 0.675132 0.077 Uiso 1 1 calc R U . . .
H20C H 0.472266 0.170497 0.669064 0.077 Uiso 1 1 calc R U . . .
C401 C 0.11885(18) 0.5472(7) 0.3315(2) 0.0431(8) Uani 1 1 d D . . . .
C201 C 0.37437(16) 0.0814(6) 0.5279(2) 0.0343(7) Uani 1 1 d . . . . .
O22 O -0.04867(16) 0.0900(5) 0.0671(3) 0.0644(9) Uani 1 1 d . . . . .
C11 C 0.39446(15) 0.4113(5) 0.3959(2) 0.0302(6) Uani 1 1 d . . . . .
C403 C 0.1235(2) 0.7279(9) 0.3787(3) 0.0656(12) Uani 1 1 d . . . . .
H40A H 0.140390 0.840821 0.377313 0.098 Uiso 1 1 calc R U . . .
H40B H 0.153997 0.698495 0.448703 0.098 Uiso 1 1 calc R U . . .
H40C H 0.078900 0.758084 0.339715 0.098 Uiso 1 1 calc R U . . .
C21 C 0.09609(17) 0.2077(5) 0.1738(3) 0.0380(7) Uani 1 1 d . . . . .
C22 C -0.02049(17) 0.2073(5) 0.0731(3) 0.0367(7) Uani 1 1 d . . . . .
C303 C 0.1835(2) 0.3413(7) 0.1626(4) 0.0651(14) Uani 1 1 d . . . . .
H30A H 0.194730 0.299388 0.216393 0.098 Uiso 1 1 calc R U . . .
H30B H 0.224395 0.345737 0.188783 0.098 Uiso 1 1 calc R U . . .
H30C H 0.151855 0.248243 0.106323 0.098 Uiso 1 1 calc R U . . .
C304 C 0.1446(2) 0.6228(8) 0.0526(4) 0.0616(12) Uani 1 1 d . . . . .
H30D H 0.116710 0.531625 -0.004189 0.092 Uiso 1 1 calc R U . . .
H30E H 0.189078 0.631327 0.089119 0.092 Uiso 1 1 calc R U . . .
H30F H 0.123649 0.752663 0.027053 0.092 Uiso 1 1 calc R U . . .
C102 C 0.3803(2) -0.1026(10) 0.2165(3) 0.0722(16) Uani 1 1 d . . . . .
H10A H 0.419528 -0.068735 0.240697 0.108 Uiso 1 1 calc R U . . .
H10B H 0.340800 -0.112627 0.142652 0.108 Uiso 1 1 calc R U . . .
H10C H 0.388008 -0.228498 0.245579 0.108 Uiso 1 1 calc R U . . .
C204 C 0.3247(2) -0.0800(9) 0.4893(4) 0.0642(13) Uani 1 1 d . . . . .
H20D H 0.282631 -0.071153 0.415639 0.096 Uiso 1 1 calc R U . . .
H20E H 0.315641 -0.060141 0.520224 0.096 Uiso 1 1 calc R U . . .
H20F H 0.344613 -0.209747 0.507812 0.096 Uiso 1 1 calc R U . . .
C302 C 0.19617(19) 0.6883(9) 0.2165(3) 0.0716(16) Uani 1 1 d . . . . .
H30G H 0.178526 0.821982 0.192006 0.107 Uiso 1 1 calc R U . . .
H30H H 0.241986 0.685011 0.257135 0.107 Uiso 1 1 calc R U . . .
H30I H 0.196338 0.646729 0.257963 0.107 Uiso 1 1 calc R U . . .
C104 C 0.30688(16) -0.0009(6) 0.2112(2) 0.0449(9) Uani 1 1 d . . . . .
H10D H 0.314929 -0.129457 0.238948 0.067 Uiso 1 1 calc R U . . .
H10E H 0.267071 -0.007485 0.137253 0.067 Uiso 1 1 calc R U . . .
H10F H 0.299753 0.096591 0.233541 0.067 Uiso 1 1 calc R U . . .
C202 C 0.3418(2) 0.2888(7) 0.4929(4) 0.0586(12) Uani 1 1 d . . . . .
H20G H 0.373339 0.387697 0.516987 0.088 Uiso 1 1 calc R U . . .
H20H H 0.330929 0.316257 0.520823 0.088 Uiso 1 1 calc R U . . .
H20I H 0.300785 0.292665 0.418971 0.088 Uiso 1 1 calc R U . . .
C103 C 0.3554(2) 0.2570(7) 0.2033(3) 0.0638(13) Uani 1 1 d . . . . .
H10G H 0.350947 0.358839 0.228069 0.096 Uiso 1 1 calc R U . . .
H10H H 0.313875 0.249580 0.129476 0.096 Uiso 1 1 calc R U . . .
H10I H 0.392794 0.289361 0.222993 0.096 Uiso 1 1 calc R U . . .
C404 C 0.0997(4) 0.3625(11) 0.3422(5) 0.112(3) Uani 1 1 d . . . . .
H40D H 0.055072 0.379265 0.304695 0.169 Uiso 1 1 calc R U . . .
H40E H 0.132420 0.340060 0.413776 0.169 Uiso 1 1 calc R U . . .
H40F H 0.099453 0.249830 0.315143 0.169 Uiso 1 1 calc R U . . .
C402 C 0.1884(2) 0.5233(13) 0.3862(3) 0.101(2) Uani 1 1 d . . . . .
H40G H 0.189633 0.398763 0.366199 0.152 Uiso 1 1 calc R U . . .
H40H H 0.223849 0.524410 0.459470 0.152 Uiso 1 1 calc R U . . .
H40I H 0.195488 0.631754 0.367234 0.152 Uiso 1 1 calc R U . . .
H1 H 0.4525(16) -0.136(6) 0.409(2) 0.031(9) Uiso 1 1 d . . . . .
H3 H 0.0544(18) 0.743(6) 0.041(3) 0.041(10) Uiso 1 1 d . . . . .
H2A H 0.4125(19) -0.147(6) 0.497(3) 0.043(10) Uiso 1 1 d . . . . .
H4A H 0.071(3) 0.776(9) 0.198(4) 0.10(2) Uiso 1 1 d D . . . .
H2B H 0.333(2) 0.014(7) 0.378(3) 0.059(13) Uiso 1 1 d . . . . .
H4B H 0.000(3) 0.649(9) 0.167(4) 0.10(2) Uiso 1 1 d 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 C11 1.766(3) . ?
Fe1 C12 1.770(3) . ?
Fe1 P2 2.1845(9) . ?
Fe1 P1 2.2273(11) 2_656 ?
Fe1 P1 2.2285(8) . ?
Fe1 Fe1 2.6571(8) 2_656 ?
Fe2 C21 1.765(3) . ?
Fe2 C22 1.765(3) . ?
Fe2 P4 2.1844(10) . ?
Fe2 P3 2.2235(13) 2 ?
Fe2 P3 2.2242(8) . ?
Fe2 Fe2 2.6953(10) 2 ?
P1 C101 1.881(3) . ?
P2 C201 1.859(3) . ?
P3 C301 1.877(3) . ?
P4 C401 1.841(3) . ?
O12 C12 1.149(4) . ?
O21 C21 1.158(4) . ?
C101 C103 1.502(5) . ?
C101 C102 1.521(5) . ?
C101 C104 1.523(4) . ?
O11 C11 1.148(4) . ?
C301 C303 1.518(5) . ?
C301 C302 1.519(5) . ?
C301 C304 1.520(5) . ?
C203 C201 1.530(5) . ?
C401 C404 1.498(8) . ?
C401 C403 1.523(6) . ?
C401 C402 1.530(6) . ?
C201 C202 1.530(6) . ?
C201 C204 1.534(6) . ?
O22 C22 1.149(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
C11 Fe1 C12 87.99(15) . . ?
C11 Fe1 P2 99.86(11) . . ?
C12 Fe1 P2 103.02(11) . . ?
C11 Fe1 P1 156.71(10) . 2_656 ?
C12 Fe1 P1 95.37(11) . 2_656 ?
P2 Fe1 P1 101.79(4) . 2_656 ?
C11 Fe1 P1 92.98(10) . . ?
C12 Fe1 P1 160.06(11) . . ?
P2 Fe1 P1 96.43(3) . . ?
P1 Fe1 P1 76.21(4) 2_656 . ?
C11 Fe1 Fe1 103.58(10) . 2_656 ?
C12 Fe1 Fe1 107.07(10) . 2_656 ?
P2 Fe1 Fe1 142.14(2) . 2_656 ?
P1 Fe1 Fe1 53.41(2) 2_656 2_656 ?
P1 Fe1 Fe1 53.37(3) . 2_656 ?
C21 Fe2 C22 88.59(16) . . ?
C21 Fe2 P4 103.28(12) . . ?
C22 Fe2 P4 99.55(12) . . ?
C21 Fe2 P3 160.47(12) . 2 ?
C22 Fe2 P3 93.55(11) . 2 ?
P4 Fe2 P3 95.52(4) . 2 ?
C21 Fe2 P3 95.04(12) . . ?
C22 Fe2 P3 158.65(11) . . ?
P4 Fe2 P3 100.06(4) . . ?
P3 Fe2 P3 76.25(4) 2 . ?
C21 Fe2 Fe2 108.11(12) . 2 ?
C22 Fe2 Fe2 106.22(11) . 2 ?
P4 Fe2 Fe2 139.42(3) . 2 ?
P3 Fe2 Fe2 52.71(3) 2 2 ?
P3 Fe2 Fe2 52.69(3) . 2 ?
C101 P1 Fe1 130.55(11) . 2_656 ?
C101 P1 Fe1 126.59(10) . . ?
Fe1 P1 Fe1 73.22(3) 2_656 . ?
C201 P2 Fe1 123.93(12) . . ?
C301 P3 Fe2 127.27(11) . 2 ?
C301 P3 Fe2 129.30(11) . . ?
Fe2 P3 Fe2 74.60(3) 2 . ?
C401 P4 Fe2 125.57(14) . . ?
C103 C101 C102 110.5(4) . . ?
C103 C101 C104 109.7(3) . . ?
C102 C101 C104 108.2(3) . . ?
C103 C101 P1 112.9(2) . . ?
C102 C101 P1 107.4(2) . . ?
C104 C101 P1 108.0(2) . . ?
C303 C301 C302 109.8(4) . . ?
C303 C301 C304 108.0(4) . . ?
C302 C301 C304 110.3(4) . . ?
C303 C301 P3 112.6(2) . . ?
C302 C301 P3 107.5(2) . . ?
C304 C301 P3 108.6(2) . . ?
O12 C12 Fe1 174.8(3) . . ?
C404 C401 C403 111.1(4) . . ?
C404 C401 C402 111.2(5) . . ?
C403 C401 C402 107.4(4) . . ?
C404 C401 P4 109.2(3) . . ?
C403 C401 P4 110.5(3) . . ?
C402 C401 P4 107.4(3) . . ?
C202 C201 C203 110.4(4) . . ?
C202 C201 C204 110.5(3) . . ?
C203 C201 C204 109.9(3) . . ?
C202 C201 P2 108.0(2) . . ?
C203 C201 P2 108.9(2) . . ?
C204 C201 P2 109.1(3) . . ?
O11 C11 Fe1 176.6(3) . . ?
O21 C21 Fe2 174.6(3) . . ?
O22 C22 Fe2 176.4(3) . . ?

_refine_diff_density_max         0.903
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.067


# start Validation Reply Form
_vrf_PLAT129_B                   
;
PROBLEM: Unusual Space Group Specified ..................       A121 Check 
RESPONSE: This was checked several times. A121 is consistent with the structure.
;

loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?
