# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_mil14
_audit_block_doi                 10.5517/ccdc.csd.cc20h4k7
_database_code_depnum_ccdc_archive 'CCDC 1861598'
_audit_update_record             
;
2019-01-09 deposited with the CCDC.
2019-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C10 H10 Fe O4 P2 Zn'
_chemical_formula_sum            'C10 H10 Fe O4 P2 Zn'
_chemical_melting_point          ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_diffrn_ambient_temperature      296(2)
_chemical_formula_weight         377.34

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           95
_space_group_name_H-M_alt        'P 43 2 2'
_space_group_name_Hall           'P 4cw 2c'
_chemical_absolute_configuration ad

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+3/4'
'y, -x, z+1/4'
'-x, y, -z'
'x, -y, -z+1/2'
'y, x, -z+1/4'
'-y, -x, -z+3/4'

_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.
;

_cell_length_a                   8.250(2)
_cell_length_b                   8.250(2)
_cell_length_c                   18.655(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1269.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5936
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      25.52
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_F_000             752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.078
_exptl_absorpt_coefficient_mu    3.283
_shelx_estimated_absorpt_T_min   0.380
_shelx_estimated_absorpt_T_max   0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3804
_exptl_absorpt_correction_T_max  0.7838
_exptl_absorpt_process_details   'SADABS, Bruker 2007'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23622
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_av_R_equivalents  0.1185
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.469
_diffrn_reflns_theta_max         28.672
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1602
_reflns_number_gt                1313
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.588
_reflns_Friedel_fraction_max     0.952
_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       'APEX3 v2016.5-0'
_computing_cell_refinement       'APEX3 v2016.5-0'
_computing_data_reduction        'SAINT NT v6.0 (Bruker AXS, 2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY 3.10.1 (Macrae, 2018)'
_computing_publication_material  'enCIFer (Allen et al. 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0418P)²] 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 
;
 Flack x determined using 434 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(10)
_refine_ls_number_reflns         1602
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0752
_refine_ls_wR_factor_gt          0.0723
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_restrained_S_all      0.979
_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
Zn1 Zn 0.92697(6) 1.07303(6) 0.8750 0.0346(2) Uani 1 2 d S T P . .
Fe1 Fe 0.50165(12) 1.0000 0.7500 0.0427(3) Uani 1 2 d S T P . .
C5 C 0.5370(7) 0.8426(7) 0.8329(3) 0.0521(14) Uani 1 1 d . . . . .
H5 H 0.5754 0.8690 0.8784 0.062 Uiso 1 1 calc R U . . .
C4 C 0.3729(7) 0.8416(9) 0.8113(3) 0.0666(17) Uani 1 1 d . . . . .
H4 H 0.2847 0.8664 0.8404 0.080 Uiso 1 1 calc R U . . .
P1 P 0.84466(16) 0.76008(15) 0.77353(5) 0.0339(3) Uani 1 1 d . . . . .
O2 O 0.9098(4) 0.7622(4) 0.69834(13) 0.0426(8) Uani 1 1 d . . . . .
C1 C 0.6335(6) 0.7962(6) 0.7729(2) 0.0424(12) Uani 1 1 d . . . . .
C2 C 0.5261(7) 0.7654(7) 0.7142(3) 0.0536(14) Uani 1 1 d . . . . .
H2 H 0.5557 0.7312 0.6685 0.064 Uiso 1 1 calc R U . . .
C3 C 0.3649(7) 0.7970(8) 0.7387(4) 0.0690(18) Uani 1 1 d . . . . .
H3 H 0.2710 0.7893 0.7113 0.083 Uiso 1 1 calc R U . . .
O1 O 0.9264(4) 0.8647(4) 0.82817(15) 0.0429(8) Uani 1 1 d . . . . .
H1 H 0.850(5) 0.610(5) 0.7982(19) 0.019(10) Uiso 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
Zn1 O1 1.928(3) . ?
Zn1 O1 1.928(3) 8_776 ?
Zn1 O2 1.934(3) 4_575 ?
Zn1 O2 1.934(3) 6_576 ?
Fe1 C3 2.030(6) 6_576 ?
Fe1 C3 2.030(6) . ?
Fe1 C4 2.036(6) . ?
Fe1 C4 2.036(6) 6_576 ?
Fe1 C5 2.041(5) 6_576 ?
Fe1 C5 2.041(5) . ?
Fe1 C1 2.048(5) . ?
Fe1 C1 2.048(5) 6_576 ?
Fe1 C2 2.057(6) . ?
Fe1 C2 2.057(6) 6_576 ?
C5 C4 1.412(8) . ?
C5 C1 1.427(7) . ?
C5 H5 0.9300 . ?
C4 C3 1.407(9) . ?
C4 H4 0.9300 . ?
P1 O1 1.496(3) . ?
P1 O2 1.502(3) . ?
P1 C1 1.767(5) . ?
P1 H1 1.33(4) . ?
O2 Zn1 1.934(3) 3_754 ?
C1 C2 1.432(7) . ?
C2 C3 1.430(8) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?

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 Zn1 O1 102.13(19) . 8_776 ?
O1 Zn1 O2 112.58(16) . 4_575 ?
O1 Zn1 O2 107.81(13) 8_776 4_575 ?
O1 Zn1 O2 107.81(13) . 6_576 ?
O1 Zn1 O2 112.58(16) 8_776 6_576 ?
O2 Zn1 O2 113.4(2) 4_575 6_576 ?
C3 Fe1 C3 112.5(4) 6_576 . ?
C3 Fe1 C4 100.4(3) 6_576 . ?
C3 Fe1 C4 40.5(3) . . ?
C3 Fe1 C4 40.5(3) 6_576 6_576 ?
C3 Fe1 C4 100.4(3) . 6_576 ?
C4 Fe1 C4 117.1(4) . 6_576 ?
C3 Fe1 C5 68.5(3) 6_576 6_576 ?
C3 Fe1 C5 121.7(2) . 6_576 ?
C4 Fe1 C5 155.4(2) . 6_576 ?
C4 Fe1 C5 40.5(2) 6_576 6_576 ?
C3 Fe1 C5 121.7(2) 6_576 . ?
C3 Fe1 C5 68.5(3) . . ?
C4 Fe1 C5 40.5(2) . . ?
C4 Fe1 C5 155.4(2) 6_576 . ?
C5 Fe1 C5 163.6(3) 6_576 . ?
C3 Fe1 C1 161.9(2) 6_576 . ?
C3 Fe1 C1 68.9(2) . . ?
C4 Fe1 C1 68.5(2) . . ?
C4 Fe1 C1 157.1(2) 6_576 . ?
C5 Fe1 C1 127.2(2) 6_576 . ?
C5 Fe1 C1 40.85(19) . . ?
C3 Fe1 C1 68.9(2) 6_576 6_576 ?
C3 Fe1 C1 161.9(2) . 6_576 ?
C4 Fe1 C1 157.1(2) . 6_576 ?
C4 Fe1 C1 68.5(2) 6_576 6_576 ?
C5 Fe1 C1 40.85(19) 6_576 6_576 ?
C5 Fe1 C1 127.2(2) . 6_576 ?
C1 Fe1 C1 115.8(3) . 6_576 ?
C3 Fe1 C2 149.8(3) 6_576 . ?
C3 Fe1 C2 40.9(2) . . ?
C4 Fe1 C2 68.3(2) . . ?
C4 Fe1 C2 118.2(3) 6_576 . ?
C5 Fe1 C2 109.8(2) 6_576 . ?
C5 Fe1 C2 68.5(2) . . ?
C1 Fe1 C2 40.82(19) . . ?
C1 Fe1 C2 130.7(2) 6_576 . ?
C3 Fe1 C2 40.9(2) 6_576 6_576 ?
C3 Fe1 C2 149.8(3) . 6_576 ?
C4 Fe1 C2 118.2(3) . 6_576 ?
C4 Fe1 C2 68.3(2) 6_576 6_576 ?
C5 Fe1 C2 68.5(2) 6_576 6_576 ?
C5 Fe1 C2 109.8(2) . 6_576 ?
C1 Fe1 C2 130.7(2) . 6_576 ?
C1 Fe1 C2 40.82(19) 6_576 6_576 ?
C2 Fe1 C2 168.7(3) . 6_576 ?
C4 C5 C1 108.0(5) . . ?
C4 C5 Fe1 69.5(3) . . ?
C1 C5 Fe1 69.8(3) . . ?
C4 C5 H5 126.0 . . ?
C1 C5 H5 126.0 . . ?
Fe1 C5 H5 126.2 . . ?
C3 C4 C5 108.8(5) . . ?
C3 C4 Fe1 69.6(3) . . ?
C5 C4 Fe1 69.9(3) . . ?
C3 C4 H4 125.6 . . ?
C5 C4 H4 125.6 . . ?
Fe1 C4 H4 126.5 . . ?
O1 P1 O2 117.9(2) . . ?
O1 P1 C1 110.6(2) . . ?
O2 P1 C1 110.1(2) . . ?
O1 P1 H1 106.7(16) . . ?
O2 P1 H1 108.8(16) . . ?
C1 P1 H1 101.3(18) . . ?
P1 O2 Zn1 134.0(2) . 3_754 ?
C5 C1 C2 107.6(5) . . ?
C5 C1 P1 126.2(4) . . ?
C2 C1 P1 125.8(4) . . ?
C5 C1 Fe1 69.3(3) . . ?
C2 C1 Fe1 69.9(3) . . ?
P1 C1 Fe1 131.6(3) . . ?
C3 C2 C1 107.4(5) . . ?
C3 C2 Fe1 68.5(3) . . ?
C1 C2 Fe1 69.2(3) . . ?
C3 C2 H2 126.3 . . ?
C1 C2 H2 126.3 . . ?
Fe1 C2 H2 127.5 . . ?
C4 C3 C2 108.2(5) . . ?
C4 C3 Fe1 70.0(3) . . ?
C2 C3 Fe1 70.5(3) . . ?
C4 C3 H3 125.9 . . ?
C2 C3 H3 125.9 . . ?
Fe1 C3 H3 125.2 . . ?
P1 O1 Zn1 145.5(2) . . ?

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
C1 C5 C4 C3 -0.6(7) . . . . ?
Fe1 C5 C4 C3 58.9(5) . . . . ?
C1 C5 C4 Fe1 -59.5(4) . . . . ?
O1 P1 O2 Zn1 -63.6(4) . . . 3_754 ?
C1 P1 O2 Zn1 64.5(4) . . . 3_754 ?
C4 C5 C1 C2 -0.4(7) . . . . ?
Fe1 C5 C1 C2 -59.7(4) . . . . ?
C4 C5 C1 P1 -173.7(4) . . . . ?
Fe1 C5 C1 P1 127.0(4) . . . . ?
C4 C5 C1 Fe1 59.3(4) . . . . ?
O1 P1 C1 C5 -31.3(5) . . . . ?
O2 P1 C1 C5 -163.4(4) . . . . ?
O1 P1 C1 C2 156.6(4) . . . . ?
O2 P1 C1 C2 24.5(5) . . . . ?
O1 P1 C1 Fe1 62.3(3) . . . . ?
O2 P1 C1 Fe1 -69.8(3) . . . . ?
C5 C1 C2 C3 1.2(6) . . . . ?
P1 C1 C2 C3 174.6(4) . . . . ?
Fe1 C1 C2 C3 -58.0(4) . . . . ?
C5 C1 C2 Fe1 59.3(4) . . . . ?
P1 C1 C2 Fe1 -127.4(4) . . . . ?
C5 C4 C3 C2 1.4(7) . . . . ?
Fe1 C4 C3 C2 60.5(4) . . . . ?
C5 C4 C3 Fe1 -59.1(5) . . . . ?
C1 C2 C3 C4 -1.6(7) . . . . ?
Fe1 C2 C3 C4 -60.1(4) . . . . ?
C1 C2 C3 Fe1 58.5(4) . . . . ?
O2 P1 O1 Zn1 93.0(4) . . . . ?
C1 P1 O1 Zn1 -35.0(5) . . . . ?

_refine_diff_density_max         0.489
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.088

####################################################################### 
# 
# 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_mil9
_audit_block_doi                 10.5517/ccdc.csd.cc20h4l8
_database_code_depnum_ccdc_archive 'CCDC 1861599'
_audit_update_record             
;
2019-01-09 deposited with the CCDC.
2019-01-21 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C10 H10 Fe O4 P2 Zn'
_chemical_formula_sum            'C10 H10 Fe O4 P2 Zn'
_chemical_melting_point          ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         377.34

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'
Fe Fe 0.3463 0.8444 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           91
_space_group_name_H-M_alt        'P 41 2 2'
_space_group_name_Hall           'P 4w 2c'
_chemical_absolute_configuration ad

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z+1/4'
'-x, -y, z+1/2'
'y, -x, z+3/4'
'x, -y, -z+1/2'
'y, x, -z+3/4'
'-x, y, -z'
'-y, -x, -z+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.
;

_cell_length_a                   8.2537(12)
_cell_length_b                   8.2537(12)
_cell_length_c                   18.659(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1271.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2601
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      28.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_F_000             752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    3.279
_shelx_estimated_absorpt_T_min   0.590
_shelx_estimated_absorpt_T_max   0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_process_details   'SADABS, Bruker 2007'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3369
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.698
_diffrn_reflns_theta_max         25.618
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1194
_reflns_number_gt                1051
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.571
_reflns_Friedel_fraction_max     0.991
_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       'APEX3 v2016.5-0'
_computing_cell_refinement       'APEX3 v2016.5-0'
_computing_data_reduction        'SAINT NT v6.0 (Bruker AXS, 2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY 3.10.1 (Macrae, 2018)'
_computing_publication_material  'enCIFer (Allen et al. 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 346 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_number_reflns         1194
_refine_ls_number_parameters     86
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0510
_refine_ls_wR_factor_gt          0.0500
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_restrained_S_all      1.174
_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
Zn1 Zn 0.42716(8) 0.42716(8) 0.3750 0.0364(2) Uani 1 2 d S T P . .
Fe1 Fe 0.00158(15) 0.5000 0.2500 0.0429(3) Uani 1 2 d S T P . .
P1 P 0.34443(18) 0.26042(18) 0.22642(6) 0.0340(3) Uani 1 1 d . . . . .
H1P H 0.370(6) 0.106(7) 0.206(2) 0.041 Uiso 1 1 d . U . . .
O1 O 0.4104(5) 0.2624(5) 0.30155(15) 0.0423(10) Uani 1 1 d . . . . .
O2 O 0.4272(5) 0.3653(4) 0.17215(15) 0.0411(9) Uani 1 1 d . . . . .
C1 C 0.1330(7) 0.2963(7) 0.2273(2) 0.0400(14) Uani 1 1 d . . . . .
C2 C 0.0352(8) 0.3418(8) 0.1673(3) 0.0528(17) Uani 1 1 d . . . . .
H2 H 0.0729 0.3683 0.1218 0.063 Uiso 1 1 d R U . . .
C3 C -0.1270(9) 0.3403(9) 0.1888(3) 0.066(2) Uani 1 1 d . . . . .
H3 H -0.2155 0.3658 0.1601 0.079 Uiso 1 1 d R U . . .
C4 C -0.1342(9) 0.2971(9) 0.2610(3) 0.067(2) Uani 1 1 d . . . . .
H4 H -0.2280 0.2872 0.2882 0.080 Uiso 1 1 d R U . . .
C5 C 0.0255(8) 0.2690(8) 0.2848(3) 0.0545(17) Uani 1 1 d . . . . .
H5 H 0.0545 0.2362 0.3307 0.065 Uiso 1 1 d 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
Zn1 O2 1.926(3) 2_655 ?
Zn1 O2 1.926(3) 5_565 ?
Zn1 O1 1.936(4) 6 ?
Zn1 O1 1.936(4) . ?
Fe1 C5 2.023(7) 5_565 ?
Fe1 C5 2.023(7) . ?
Fe1 C4 2.025(7) . ?
Fe1 C4 2.025(7) 5_565 ?
Fe1 C2 2.041(6) . ?
Fe1 C2 2.041(6) 5_565 ?
Fe1 C3 2.041(6) 5_565 ?
Fe1 C3 2.041(7) . ?
Fe1 C1 2.045(6) 5_565 ?
Fe1 C1 2.045(6) . ?
P1 O2 1.497(3) . ?
P1 O1 1.504(3) . ?
P1 C1 1.770(6) . ?
P1 H1P 1.34(5) . ?
O2 Zn1 1.926(3) 4_564 ?
C1 C5 1.410(7) . ?
C1 C2 1.430(7) . ?
C2 C3 1.399(9) . ?
C2 H2 0.9301 . ?
C3 C4 1.393(9) . ?
C3 H3 0.9299 . ?
C4 C5 1.410(9) . ?
C4 H4 0.9298 . ?
C5 H5 0.9301 . ?

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
O2 Zn1 O2 102.0(2) 2_655 5_565 ?
O2 Zn1 O1 107.56(15) 2_655 6 ?
O2 Zn1 O1 112.78(18) 5_565 6 ?
O2 Zn1 O1 112.78(18) 2_655 . ?
O2 Zn1 O1 107.55(15) 5_565 . ?
O1 Zn1 O1 113.6(2) 6 . ?
C5 Fe1 C5 168.8(4) 5_565 . ?
C5 Fe1 C4 149.9(3) 5_565 . ?
C5 Fe1 C4 40.8(2) . . ?
C5 Fe1 C4 40.8(2) 5_565 5_565 ?
C5 Fe1 C4 149.9(3) . 5_565 ?
C4 Fe1 C4 112.8(4) . 5_565 ?
C5 Fe1 C2 110.3(2) 5_565 . ?
C5 Fe1 C2 68.1(2) . . ?
C4 Fe1 C2 67.8(3) . . ?
C4 Fe1 C2 121.9(2) 5_565 . ?
C5 Fe1 C2 68.1(2) 5_565 5_565 ?
C5 Fe1 C2 110.3(2) . 5_565 ?
C4 Fe1 C2 121.9(2) . 5_565 ?
C4 Fe1 C2 67.8(3) 5_565 5_565 ?
C2 Fe1 C2 164.3(4) . 5_565 ?
C5 Fe1 C3 67.8(3) 5_565 5_565 ?
C5 Fe1 C3 118.7(3) . 5_565 ?
C4 Fe1 C3 100.9(3) . 5_565 ?
C4 Fe1 C3 40.1(3) 5_565 5_565 ?
C2 Fe1 C3 155.1(3) . 5_565 ?
C2 Fe1 C3 40.1(3) 5_565 5_565 ?
C5 Fe1 C3 118.7(3) 5_565 . ?
C5 Fe1 C3 67.8(3) . . ?
C4 Fe1 C3 40.1(3) . . ?
C4 Fe1 C3 100.9(3) 5_565 . ?
C2 Fe1 C3 40.1(3) . . ?
C2 Fe1 C3 155.1(3) 5_565 . ?
C3 Fe1 C3 117.3(4) 5_565 . ?
C5 Fe1 C1 40.6(2) 5_565 5_565 ?
C5 Fe1 C1 131.0(2) . 5_565 ?
C4 Fe1 C1 162.2(2) . 5_565 ?
C4 Fe1 C1 68.6(3) 5_565 5_565 ?
C2 Fe1 C1 127.6(2) . 5_565 ?
C2 Fe1 C1 41.0(2) 5_565 5_565 ?
C3 Fe1 C1 68.2(3) 5_565 5_565 ?
C3 Fe1 C1 157.3(2) . 5_565 ?
C5 Fe1 C1 131.0(2) 5_565 . ?
C5 Fe1 C1 40.6(2) . . ?
C4 Fe1 C1 68.6(3) . . ?
C4 Fe1 C1 162.2(2) 5_565 . ?
C2 Fe1 C1 41.0(2) . . ?
C2 Fe1 C1 127.6(2) 5_565 . ?
C3 Fe1 C1 157.3(2) 5_565 . ?
C3 Fe1 C1 68.2(3) . . ?
C1 Fe1 C1 116.0(3) 5_565 . ?
O2 P1 O1 117.3(2) . . ?
O2 P1 C1 111.1(2) . . ?
O1 P1 C1 110.3(2) . . ?
O2 P1 H1P 107(2) . . ?
O1 P1 H1P 102.6(17) . . ?
C1 P1 H1P 108(2) . . ?
P1 O1 Zn1 133.9(3) . . ?
P1 O2 Zn1 145.4(2) . 4_564 ?
C5 C1 C2 106.4(5) . . ?
C5 C1 P1 126.9(4) . . ?
C2 C1 P1 126.4(4) . . ?
C5 C1 Fe1 68.9(4) . . ?
C2 C1 Fe1 69.4(3) . . ?
P1 C1 Fe1 131.4(3) . . ?
C3 C2 C1 108.2(5) . . ?
C3 C2 Fe1 70.0(4) . . ?
C1 C2 Fe1 69.7(3) . . ?
C3 C2 H2 125.8 . . ?
C1 C2 H2 126.0 . . ?
Fe1 C2 H2 125.8 . . ?
C4 C3 C2 108.7(6) . . ?
C4 C3 Fe1 69.3(4) . . ?
C2 C3 Fe1 69.9(4) . . ?
C4 C3 H3 125.6 . . ?
C2 C3 H3 125.7 . . ?
Fe1 C3 H3 125.8 . . ?
C3 C4 C5 107.9(6) . . ?
C3 C4 Fe1 70.6(4) . . ?
C5 C4 Fe1 69.6(4) . . ?
C3 C4 H4 125.9 . . ?
C5 C4 H4 126.3 . . ?
Fe1 C4 H4 126.1 . . ?
C4 C5 C1 108.8(5) . . ?
C4 C5 Fe1 69.7(4) . . ?
C1 C5 Fe1 70.6(3) . . ?
C4 C5 H5 125.4 . . ?
C1 C5 H5 125.8 . . ?
Fe1 C5 H5 126.5 . . ?

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
O2 P1 O1 Zn1 64.2(4) . . . . ?
C1 P1 O1 Zn1 -64.3(4) . . . . ?
O1 P1 O2 Zn1 -94.3(4) . . . 4_564 ?
C1 P1 O2 Zn1 33.8(5) . . . 4_564 ?
O2 P1 C1 C5 -155.3(5) . . . . ?
O1 P1 C1 C5 -23.5(6) . . . . ?
O2 P1 C1 C2 32.0(6) . . . . ?
O1 P1 C1 C2 163.8(5) . . . . ?
O2 P1 C1 Fe1 -61.8(3) . . . . ?
O1 P1 C1 Fe1 70.1(4) . . . . ?
C5 C1 C2 C3 -0.4(7) . . . . ?
P1 C1 C2 C3 173.5(5) . . . . ?
Fe1 C1 C2 C3 -59.6(5) . . . . ?
C5 C1 C2 Fe1 59.2(4) . . . . ?
P1 C1 C2 Fe1 -126.9(5) . . . . ?
C1 C2 C3 C4 0.7(8) . . . . ?
Fe1 C2 C3 C4 -58.7(5) . . . . ?
C1 C2 C3 Fe1 59.4(4) . . . . ?
C2 C3 C4 C5 -0.8(9) . . . . ?
Fe1 C3 C4 C5 -59.8(5) . . . . ?
C2 C3 C4 Fe1 59.0(5) . . . . ?
C3 C4 C5 C1 0.5(8) . . . . ?
Fe1 C4 C5 C1 -59.9(5) . . . . ?
C3 C4 C5 Fe1 60.5(5) . . . . ?
C2 C1 C5 C4 -0.1(7) . . . . ?
P1 C1 C5 C4 -173.9(5) . . . . ?
Fe1 C1 C5 C4 59.4(5) . . . . ?
C2 C1 C5 Fe1 -59.5(4) . . . . ?
P1 C1 C5 Fe1 126.7(5) . . . . ?

_refine_diff_density_max         0.271
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_p4
_database_code_depnum_ccdc_archive 'CCDC 1866808'
_audit_update_record             
;
2018-09-10 deposited with the CCDC.
2019-01-21 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         ?
_chemical_formula_sum            'C10 H10 Co Fe O4 P2'
_chemical_formula_weight         370.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1460 0.1480 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3410 1.2590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3090 1.4430 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           91
_space_group_name_H-M_alt        'P 41 2 2'
_space_group_name_Hall           'P 4w 2c'

_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+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'
'-x, y, -z'
'x, -y, -z+1/2'
'y, x, -z+3/4'
'-y, -x, -z+1/4'

_cell_length_a                   8.2200(12)
_cell_length_b                   8.2200(12)
_cell_length_c                   18.840(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1273.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    487
_cell_measurement_theta_min      3.54
_cell_measurement_theta_max      26.32

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_F_000             740
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    4.909
_shelx_estimated_absorpt_T_min   0.526
_shelx_estimated_absorpt_T_max   0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Scala (Diederichs, 1997)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_reflns_number            1374
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.369
_diffrn_reflns_theta_max         34.118
_diffrn_reflns_theta_full        32.098
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             1341
_reflns_number_gt                1172
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.595
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    0.995

_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       'marCCD 1994-2002'
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_reduction        scala
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1627P)²+0.1425P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.22(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 392 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.23(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         1341
_refine_ls_number_parameters     88
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0749
_refine_ls_wR_factor_ref         0.2287
_refine_ls_wR_factor_gt          0.2034
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.149
_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
Co1 Co 0.42543(17) 0.42543(17) 0.3750 0.0536(9) Uani 1 2 d S T P . .
Fe1 Fe 0.5000 0.0008(3) 0.5000 0.0602(9) Uani 1 2 d S T P . .
P1 P 0.7414(4) 0.3454(4) 0.47666(15) 0.0541(9) Uani 1 1 d . . . . .
O1 O 0.6375(10) 0.4263(10) 0.4239(4) 0.0619(19) Uani 1 1 d . . . . .
O2 O 0.7405(11) 0.4102(10) 0.5511(4) 0.0629(19) Uani 1 1 d . . . . .
C1 C 0.7063(15) 0.1343(16) 0.4770(7) 0.063(3) Uani 1 1 d . . . . .
C4 C 0.710(2) -0.1331(18) 0.5118(11) 0.087(5) Uani 1 1 d . . . . .
H4 H 0.7231 -0.2267 0.5389 0.105 Uiso 1 1 calc R U . . .
C3 C 0.659(2) -0.1297(18) 0.4384(10) 0.085(4) Uani 1 1 d . . . . .
H3 H 0.6328 -0.2190 0.4104 0.102 Uiso 1 1 calc R U . . .
C2 C 0.6578(16) 0.0367(15) 0.4171(7) 0.066(3) Uani 1 1 d . . . . .
H2 H 0.6304 0.0754 0.3723 0.080 Uiso 1 1 calc R U . . .
C5 C 0.7346(18) 0.0254(16) 0.5359(8) 0.074(3) Uani 1 1 d . . . . .
H5 H 0.7642 0.0555 0.5816 0.088 Uiso 1 1 calc R U . . .
H1 H 0.891(11) 0.362(11) 0.452(5) 0.03(2) Uiso 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
Co1 O2 1.953(8) 4_564 ?
Co1 O2 1.953(8) 5_656 ?
Co1 O1 1.971(8) . ?
Co1 O1 1.971(8) 7 ?
Fe1 C3 2.052(13) 5_656 ?
Fe1 C3 2.052(13) . ?
Fe1 C2 2.052(13) 5_656 ?
Fe1 C2 2.052(13) . ?
Fe1 C5 2.053(14) 5_656 ?
Fe1 C5 2.053(14) . ?
Fe1 C4 2.056(15) . ?
Fe1 C4 2.056(15) 5_656 ?
Fe1 C1 2.066(13) 5_656 ?
Fe1 C1 2.066(13) . ?
P1 O1 1.470(8) . ?
P1 O2 1.501(8) . ?
P1 C1 1.759(13) . ?
P1 H1 1.32(9) . ?
O2 Co1 1.953(8) 3_655 ?
C1 C2 1.441(17) . ?
C1 C5 1.444(18) . ?
C4 C5 1.39(2) . ?
C4 C3 1.44(3) . ?
C4 H4 0.9300 . ?
C3 C2 1.43(2) . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C5 H5 0.9300 . ?

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
O2 Co1 O2 114.7(5) 4_564 5_656 ?
O2 Co1 O1 113.1(4) 4_564 . ?
O2 Co1 O1 106.6(3) 5_656 . ?
O2 Co1 O1 106.6(3) 4_564 7 ?
O2 Co1 O1 113.1(4) 5_656 7 ?
O1 Co1 O1 102.2(5) . 7 ?
C3 Fe1 C3 117.0(9) 5_656 . ?
C3 Fe1 C2 40.7(6) 5_656 5_656 ?
C3 Fe1 C2 155.4(6) . 5_656 ?
C3 Fe1 C2 155.4(6) 5_656 . ?
C3 Fe1 C2 40.6(6) . . ?
C2 Fe1 C2 163.5(7) 5_656 . ?
C3 Fe1 C5 68.8(7) 5_656 5_656 ?
C3 Fe1 C5 117.7(7) . 5_656 ?
C2 Fe1 C5 69.1(6) 5_656 5_656 ?
C2 Fe1 C5 109.2(6) . 5_656 ?
C3 Fe1 C5 117.7(7) 5_656 . ?
C3 Fe1 C5 68.8(7) . . ?
C2 Fe1 C5 109.2(6) 5_656 . ?
C2 Fe1 C5 69.1(6) . . ?
C5 Fe1 C5 168.7(7) 5_656 . ?
C3 Fe1 C4 101.2(7) 5_656 . ?
C3 Fe1 C4 41.1(7) . . ?
C2 Fe1 C4 121.6(7) 5_656 . ?
C2 Fe1 C4 68.3(6) . . ?
C5 Fe1 C4 151.1(7) 5_656 . ?
C5 Fe1 C4 39.7(6) . . ?
C3 Fe1 C4 41.1(8) 5_656 5_656 ?
C3 Fe1 C4 101.2(7) . 5_656 ?
C2 Fe1 C4 68.3(6) 5_656 5_656 ?
C2 Fe1 C4 121.6(7) . 5_656 ?
C5 Fe1 C4 39.7(6) 5_656 5_656 ?
C5 Fe1 C4 151.1(7) . 5_656 ?
C4 Fe1 C4 115.3(10) . 5_656 ?
C3 Fe1 C1 68.6(6) 5_656 5_656 ?
C3 Fe1 C1 156.9(6) . 5_656 ?
C2 Fe1 C1 41.0(5) 5_656 5_656 ?
C2 Fe1 C1 127.0(5) . 5_656 ?
C5 Fe1 C1 41.1(5) 5_656 5_656 ?
C5 Fe1 C1 130.5(5) . 5_656 ?
C4 Fe1 C1 161.7(7) . 5_656 ?
C4 Fe1 C1 67.6(6) 5_656 5_656 ?
C3 Fe1 C1 156.9(6) 5_656 . ?
C3 Fe1 C1 68.6(6) . . ?
C2 Fe1 C1 127.0(5) 5_656 . ?
C2 Fe1 C1 41.0(5) . . ?
C5 Fe1 C1 130.5(5) 5_656 . ?
C5 Fe1 C1 41.1(5) . . ?
C4 Fe1 C1 67.6(6) . . ?
C4 Fe1 C1 161.7(7) 5_656 . ?
C1 Fe1 C1 115.8(7) 5_656 . ?
O1 P1 O2 118.0(5) . . ?
O1 P1 C1 110.7(6) . . ?
O2 P1 C1 110.2(5) . . ?
O1 P1 H1 105(4) . . ?
O2 P1 H1 107(4) . . ?
C1 P1 H1 105(4) . . ?
P1 O1 Co1 145.9(5) . . ?
P1 O2 Co1 133.8(5) . 3_655 ?
C2 C1 C5 107.5(11) . . ?
C2 C1 P1 126.3(10) . . ?
C5 C1 P1 126.0(10) . . ?
C2 C1 Fe1 69.0(7) . . ?
C5 C1 Fe1 69.0(8) . . ?
P1 C1 Fe1 131.3(7) . . ?
C5 C4 C3 109.6(13) . . ?
C5 C4 Fe1 70.1(8) . . ?
C3 C4 Fe1 69.3(8) . . ?
C5 C4 H4 125.2 . . ?
C3 C4 H4 125.2 . . ?
Fe1 C4 H4 127.1 . . ?
C2 C3 C4 106.9(13) . . ?
C2 C3 Fe1 69.7(7) . . ?
C4 C3 Fe1 69.6(8) . . ?
C2 C3 H3 126.5 . . ?
C4 C3 H3 126.5 . . ?
Fe1 C3 H3 125.8 . . ?
C3 C2 C1 108.1(13) . . ?
C3 C2 Fe1 69.7(8) . . ?
C1 C2 Fe1 70.0(7) . . ?
C3 C2 H2 125.9 . . ?
C1 C2 H2 125.9 . . ?
Fe1 C2 H2 125.9 . . ?
C4 C5 C1 107.8(13) . . ?
C4 C5 Fe1 70.3(9) . . ?
C1 C5 Fe1 70.0(7) . . ?
C4 C5 H5 126.1 . . ?
C1 C5 H5 126.1 . . ?
Fe1 C5 H5 125.3 . . ?

_refine_diff_density_max         1.232
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.140

