# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_a10929bz
_database_code_depnum_ccdc_archive 'CCDC 906321'
_audit_update_record             
;
2012-10-17 deposited with the CCDC.
2016-05-27 downloaded from the CCDC.
;
#TrackingRef 'Co2.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H8 Co N3 O4 P'
_chemical_formula_sum            'C8 H8 Co N3 O4 P'
_chemical_formula_weight         300.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   10.960(9)
_cell_length_b                   7.193(6)
_cell_length_c                   12.908(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.925(9)
_cell_angle_gamma                90.00
_cell_volume                     968.2(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    950
_cell_measurement_theta_min      3.549
_cell_measurement_theta_max      27.346

_exptl_crystal_description       sheet
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             604
_exptl_absorpt_coefficient_mu    1.944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7210
_exptl_absorpt_correction_T_max  0.8002
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4545
_diffrn_reflns_av_R_equivalents  0.1428
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         25.19
_reflns_number_total             1735
_reflns_number_gt                1642
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1062P)²+0.0571P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1735
_refine_ls_number_parameters     162
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1481
_refine_ls_wR_factor_gt          0.1459
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co -0.01075(4) 0.04856(5) 0.20590(3) 0.0137(3) Uani 1 1 d . . .
O1 O 0.1618(2) 0.4039(3) 0.3719(2) 0.0223(5) Uani 1 1 d . . .
O2 O 0.1215(2) 0.0576(3) 0.35392(19) 0.0177(5) Uani 1 1 d . . .
O4 O 0.0096(3) 0.2594(4) 0.1125(2) 0.0248(6) Uani 1 1 d D . .
N1 N 0.8626(3) 0.1917(4) 0.2781(2) 0.0166(6) Uani 1 1 d . . .
N2 N 0.8875(3) 0.3549(4) 0.3385(2) 0.0159(6) Uani 1 1 d . . .
O3 O 0.2049(2) 0.2050(3) 0.54099(18) 0.0219(5) Uani 1 1 d . . .
N3 N 0.7202(2) 0.2231(4) 0.3629(2) 0.0164(6) Uani 1 1 d . . .
P1 P 0.20031(7) 0.21387(10) 0.42363(6) 0.0122(3) Uani 1 1 d . . .
C1 C 0.3617(3) 0.1904(4) 0.4159(2) 0.0147(6) Uani 1 1 d . . .
C2 C 0.3793(3) 0.1318(6) 0.3190(3) 0.0338(10) Uani 1 1 d . . .
H2 H 0.3094 0.0882 0.2632 0.041 Uiso 1 1 calc R . .
C3 C 0.4977(4) 0.1368(7) 0.3039(3) 0.0324(9) Uani 1 1 d . . .
H3 H 0.5079 0.0956 0.2388 0.039 Uiso 1 1 calc R . .
C4 C 0.6014(3) 0.2033(4) 0.3857(3) 0.0158(7) Uani 1 1 d . . .
C5 C 0.5881(3) 0.2587(6) 0.4832(3) 0.0295(9) Uani 1 1 d . . .
H5 H 0.6588 0.2995 0.5392 0.035 Uiso 1 1 calc R . .
C6 C 0.4680(3) 0.2529(6) 0.4971(3) 0.0276(9) Uani 1 1 d . . .
H6 H 0.4586 0.2922 0.5629 0.033 Uiso 1 1 calc R . .
C7 C 0.8020(3) 0.3683(4) 0.3880(3) 0.0162(7) Uani 1 1 d . . .
H7 H 0.7974 0.4647 0.4346 0.019 Uiso 1 1 calc R . .
C8 C 0.7625(3) 0.1164(4) 0.2948(3) 0.0169(7) Uani 1 1 d . . .
H8 H 0.7253 0.0050 0.2643 0.020 Uiso 1 1 calc R . .
H4A H -0.034(4) 0.353(4) 0.110(3) 0.020(10) Uiso 1 1 d D . .
H4B H 0.071(5) 0.279(11) 0.086(5) 0.08(2) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0092(4) 0.0129(4) 0.0161(4) -0.00190(13) -0.0005(2) -0.00053(14)
O1 0.0143(12) 0.0163(11) 0.0325(14) 0.0085(10) 0.0018(10) 0.0038(10)
O2 0.0113(11) 0.0167(12) 0.0212(12) -0.0012(8) -0.0009(9) -0.0033(8)
O4 0.0280(13) 0.0168(12) 0.0331(14) 0.0059(9) 0.0146(11) 0.0050(11)
N1 0.0114(12) 0.0145(14) 0.0216(14) -0.0032(10) 0.0016(10) -0.0008(10)
N2 0.0121(13) 0.0137(13) 0.0192(13) -0.0003(10) 0.0007(10) -0.0003(10)
O3 0.0175(11) 0.0293(13) 0.0165(13) 0.0002(9) 0.0019(9) 0.0012(10)
N3 0.0120(13) 0.0164(14) 0.0197(14) 0.0003(10) 0.0032(10) 0.0011(10)
P1 0.0074(4) 0.0113(5) 0.0150(5) 0.0000(3) -0.0010(3) 0.0002(3)
C1 0.0115(15) 0.0122(15) 0.0172(16) 0.0018(11) -0.0004(12) 0.0026(11)
C2 0.0145(18) 0.055(3) 0.028(2) -0.0200(18) 0.0016(15) -0.0084(17)
C3 0.0224(19) 0.051(3) 0.0249(19) -0.0175(16) 0.0095(15) -0.0090(17)
C4 0.0101(14) 0.0164(16) 0.0199(17) 0.0028(11) 0.0030(12) 0.0002(11)
C5 0.0108(16) 0.050(2) 0.023(2) -0.0135(16) -0.0026(14) -0.0069(16)
C6 0.0130(17) 0.052(2) 0.0168(19) -0.0132(15) 0.0033(14) -0.0030(16)
C7 0.0124(15) 0.0153(16) 0.0180(16) 0.0003(11) 0.0005(12) -0.0008(12)
C8 0.0117(14) 0.0116(15) 0.0260(17) -0.0040(12) 0.0038(12) -0.0022(11)

_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 O1 1.951(2) 2_545 ?
Co1 O4 1.992(3) . ?
Co1 O2 2.012(3) . ?
Co1 N2 2.137(3) 2_645 ?
Co1 N1 2.156(3) 1_455 ?
O1 P1 1.523(3) . ?
O1 Co1 1.951(2) 2 ?
O2 P1 1.530(2) . ?
O4 H4A 0.820(19) . ?
O4 H4B 0.85(2) . ?
N1 C8 1.300(4) . ?
N1 N2 1.389(4) . ?
N1 Co1 2.156(3) 1_655 ?
N2 C7 1.290(4) . ?
N2 Co1 2.137(3) 2_655 ?
O3 P1 1.501(3) . ?
N3 C7 1.350(4) . ?
N3 C8 1.351(4) . ?
N3 C4 1.427(4) . ?
P1 C1 1.810(3) . ?
C1 C6 1.381(5) . ?
C1 C2 1.389(5) . ?
C2 C3 1.370(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.377(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(5) . ?
C5 C6 1.383(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8 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 Co1 O4 109.24(12) 2_545 . ?
O1 Co1 O2 139.01(10) 2_545 . ?
O4 Co1 O2 111.58(11) . . ?
O1 Co1 N2 91.16(12) 2_545 2_645 ?
O4 Co1 N2 97.83(12) . 2_645 ?
O2 Co1 N2 86.90(11) . 2_645 ?
O1 Co1 N1 85.44(12) 2_545 1_455 ?
O4 Co1 N1 96.01(11) . 1_455 ?
O2 Co1 N1 86.86(11) . 1_455 ?
N2 Co1 N1 166.10(11) 2_645 1_455 ?
P1 O1 Co1 141.37(15) . 2 ?
P1 O2 Co1 133.90(13) . . ?
Co1 O4 H4A 118(3) . . ?
Co1 O4 H4B 128(5) . . ?
H4A O4 H4B 112(6) . . ?
C8 N1 N2 106.8(3) . . ?
C8 N1 Co1 124.1(2) . 1_655 ?
N2 N1 Co1 127.2(2) . 1_655 ?
C7 N2 N1 107.1(3) . . ?
C7 N2 Co1 134.4(2) . 2_655 ?
N1 N2 Co1 115.6(2) . 2_655 ?
C7 N3 C8 105.1(3) . . ?
C7 N3 C4 127.5(3) . . ?
C8 N3 C4 126.5(3) . . ?
O3 P1 O1 113.50(15) . . ?
O3 P1 O2 113.56(14) . . ?
O1 P1 O2 111.80(14) . . ?
O3 P1 C1 108.76(14) . . ?
O1 P1 C1 101.74(14) . . ?
O2 P1 C1 106.50(14) . . ?
C6 C1 C2 117.6(3) . . ?
C6 C1 P1 122.6(2) . . ?
C2 C1 P1 119.2(2) . . ?
C3 C2 C1 121.4(3) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 119.7(3) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 120.6(3) . . ?
C5 C4 N3 121.5(3) . . ?
C3 C4 N3 117.8(3) . . ?
C4 C5 C6 119.1(3) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C1 C6 C5 121.7(3) . . ?
C1 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
N2 C7 N3 110.7(3) . . ?
N2 C7 H7 124.6 . . ?
N3 C7 H7 124.6 . . ?
N1 C8 N3 110.3(3) . . ?
N1 C8 H8 124.8 . . ?
N3 C8 H8 124.8 . . ?

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
O1 Co1 O2 P1 -149.47(16) 2_545 . . . ?
O4 Co1 O2 P1 25.1(2) . . . . ?
N2 Co1 O2 P1 122.3(2) 2_645 . . . ?
N1 Co1 O2 P1 -70.1(2) 1_455 . . . ?
C8 N1 N2 C7 0.2(3) . . . . ?
Co1 N1 N2 C7 -164.6(2) 1_655 . . . ?
C8 N1 N2 Co1 -163.2(2) . . . 2_655 ?
Co1 N1 N2 Co1 32.0(3) 1_655 . . 2_655 ?
Co1 O1 P1 O3 -89.0(3) 2 . . . ?
Co1 O1 P1 O2 41.0(3) 2 . . . ?
Co1 O1 P1 C1 154.3(2) 2 . . . ?
Co1 O2 P1 O3 135.39(19) . . . . ?
Co1 O2 P1 O1 5.4(2) . . . . ?
Co1 O2 P1 C1 -104.9(2) . . . . ?
O3 P1 C1 C6 -31.0(3) . . . . ?
O1 P1 C1 C6 89.0(3) . . . . ?
O2 P1 C1 C6 -153.7(3) . . . . ?
O3 P1 C1 C2 158.3(3) . . . . ?
O1 P1 C1 C2 -81.6(3) . . . . ?
O2 P1 C1 C2 35.6(3) . . . . ?
C6 C1 C2 C3 -0.5(7) . . . . ?
P1 C1 C2 C3 170.7(4) . . . . ?
C1 C2 C3 C4 -0.8(7) . . . . ?
C2 C3 C4 C5 2.1(7) . . . . ?
C2 C3 C4 N3 -174.0(4) . . . . ?
C7 N3 C4 C5 -40.7(5) . . . . ?
C8 N3 C4 C5 152.2(4) . . . . ?
C7 N3 C4 C3 135.4(4) . . . . ?
C8 N3 C4 C3 -31.7(5) . . . . ?
C3 C4 C5 C6 -2.2(6) . . . . ?
N3 C4 C5 C6 173.8(4) . . . . ?
C2 C1 C6 C5 0.4(6) . . . . ?
P1 C1 C6 C5 -170.4(3) . . . . ?
C4 C5 C6 C1 0.9(7) . . . . ?
N1 N2 C7 N3 -0.7(3) . . . . ?
Co1 N2 C7 N3 158.2(2) 2_655 . . . ?
C8 N3 C7 N2 0.9(4) . . . . ?
C4 N3 C7 N2 -168.4(3) . . . . ?
N2 N1 C8 N3 0.3(3) . . . . ?
Co1 N1 C8 N3 165.7(2) 1_655 . . . ?
C7 N3 C8 N1 -0.7(4) . . . . ?
C4 N3 C8 N1 168.7(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4B O3 0.85(2) 1.74(2) 2.591(4) 173(7) 4_565
O4 H4A O2 0.820(19) 1.89(2) 2.690(4) 164(4) 2

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.19
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.664
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.210
####################################################################### 
# 
# 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_a11221bz
_database_code_depnum_ccdc_archive 'CCDC 906322'
_audit_update_record             
;
2012-10-17 deposited with the CCDC.
2016-05-27 downloaded from the CCDC.
;
#TrackingRef 'Cu.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H8 Cu N3 O4 P'
_chemical_formula_sum            'C8 H8 Cu N3 O4 P'
_chemical_formula_weight         304.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   10.945(5)
_cell_length_b                   7.148(3)
_cell_length_c                   12.967(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.675(5)
_cell_angle_gamma                90.00
_cell_volume                     961.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            'light blue'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             612
_exptl_absorpt_coefficient_mu    2.445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6673
_exptl_absorpt_correction_T_max  0.8672
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4486
_diffrn_reflns_av_R_equivalents  0.1074
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.18
_reflns_number_total             1725
_reflns_number_gt                1521
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0512P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1725
_refine_ls_number_parameters     162
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.1126
_refine_ls_wR_factor_gt          0.1087
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.01328(4) 0.02903(7) 0.21412(4) 0.0134(2) Uani 1 1 d . . .
O1 O 0.1668(3) 0.4169(4) 0.3823(2) 0.0191(6) Uani 1 1 d . . .
O2 O 0.1280(3) 0.0674(4) 0.3510(2) 0.0193(6) Uani 1 1 d . . .
O4 O 0.0097(4) 0.2613(5) 0.1099(3) 0.0305(8) Uani 1 1 d D . .
N1 N 0.8696(3) 0.1781(5) 0.2771(3) 0.0158(7) Uani 1 1 d . . .
N2 N 0.8970(3) 0.3478(5) 0.3311(3) 0.0151(7) Uani 1 1 d . . .
O3 O 0.2160(3) 0.1969(4) 0.5427(2) 0.0219(7) Uani 1 1 d . . .
N3 N 0.7285(3) 0.2273(5) 0.3599(3) 0.0163(7) Uani 1 1 d . . .
P1 P 0.20777(9) 0.22002(14) 0.42536(7) 0.0121(3) Uani 1 1 d . . .
C1 C 0.3695(4) 0.2025(6) 0.4148(3) 0.0143(8) Uani 1 1 d . . .
C2 C 0.3842(4) 0.1481(8) 0.3181(4) 0.0336(12) Uani 1 1 d . . .
H2 H 0.3122 0.1078 0.2622 0.040 Uiso 1 1 calc R . .
C3 C 0.5025(4) 0.1513(9) 0.3010(4) 0.0353(13) Uani 1 1 d . . .
H3 H 0.5104 0.1122 0.2350 0.042 Uiso 1 1 calc R . .
C4 C 0.6084(4) 0.2134(6) 0.3835(3) 0.0161(8) Uani 1 1 d . . .
C5 C 0.5998(5) 0.2646(8) 0.4822(4) 0.0314(12) Uani 1 1 d . . .
H5 H 0.6726 0.3022 0.5383 0.038 Uiso 1 1 calc R . .
C6 C 0.4786(4) 0.2591(7) 0.4970(4) 0.0319(12) Uani 1 1 d . . .
H6 H 0.4713 0.2944 0.5638 0.038 Uiso 1 1 calc R . .
C7 C 0.8121(4) 0.3729(6) 0.3811(3) 0.0152(8) Uani 1 1 d . . .
H7 H 0.8094 0.4751 0.4246 0.018 Uiso 1 1 calc R . .
C8 C 0.7684(4) 0.1097(6) 0.2967(3) 0.0188(9) Uani 1 1 d . . .
H8 H 0.7297 -0.0042 0.2706 0.023 Uiso 1 1 calc R . .
H4A H -0.045(4) 0.348(5) 0.091(4) 0.042(17) Uiso 1 1 d D . .
H4B H 0.077(3) 0.289(8) 0.095(5) 0.056(19) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0123(3) 0.0143(3) 0.0161(3) -0.00323(18) 0.0081(2) 0.00017(18)
O1 0.0161(14) 0.0174(15) 0.0210(14) 0.0052(12) 0.0019(12) 0.0005(12)
O2 0.0171(15) 0.0188(15) 0.0224(15) -0.0033(12) 0.0068(12) 0.0009(12)
O4 0.041(2) 0.0207(17) 0.0398(19) 0.0083(15) 0.0267(18) 0.0050(15)
N1 0.0154(17) 0.0163(17) 0.0179(16) -0.0025(14) 0.0086(14) 0.0004(13)
N2 0.0156(16) 0.0149(17) 0.0169(15) -0.0020(13) 0.0083(14) -0.0010(13)
O3 0.0231(16) 0.0324(17) 0.0140(13) 0.0036(13) 0.0113(12) 0.0031(13)
N3 0.0172(18) 0.0185(17) 0.0177(16) -0.0004(14) 0.0121(14) -0.0002(14)
P1 0.0117(5) 0.0148(5) 0.0118(5) -0.0001(4) 0.0066(4) 0.0006(4)
C1 0.0117(19) 0.018(2) 0.0154(18) 0.0024(16) 0.0076(16) 0.0026(15)
C2 0.015(2) 0.062(3) 0.024(2) -0.022(2) 0.0072(19) -0.010(2)
C3 0.023(2) 0.067(4) 0.022(2) -0.019(2) 0.015(2) -0.009(2)
C4 0.015(2) 0.018(2) 0.0195(19) 0.0011(17) 0.0113(16) -0.0007(16)
C5 0.020(2) 0.057(3) 0.020(2) -0.015(2) 0.0108(18) -0.009(2)
C6 0.017(2) 0.062(4) 0.019(2) -0.018(2) 0.0100(19) -0.006(2)
C7 0.017(2) 0.015(2) 0.0163(19) -0.0031(16) 0.0099(16) -0.0014(16)
C8 0.018(2) 0.015(2) 0.028(2) -0.0023(18) 0.0125(18) -0.0027(16)

_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
Cu1 O1 1.919(3) 2_545 ?
Cu1 O2 1.964(3) . ?
Cu1 N1 2.029(3) 1_455 ?
Cu1 N2 2.029(3) 2_645 ?
Cu1 O4 2.206(3) . ?
O1 P1 1.528(3) . ?
O1 Cu1 1.919(3) 2 ?
O2 P1 1.531(3) . ?
O4 H4A 0.848(10) . ?
O4 H4B 0.849(10) . ?
N1 C8 1.308(5) . ?
N1 N2 1.385(5) . ?
N1 Cu1 2.029(3) 1_655 ?
N2 C7 1.304(5) . ?
N2 Cu1 2.029(3) 2_655 ?
O3 P1 1.504(3) . ?
N3 C8 1.341(5) . ?
N3 C7 1.354(5) . ?
N3 C4 1.445(5) . ?
P1 C1 1.822(4) . ?
C1 C2 1.370(6) . ?
C1 C6 1.382(6) . ?
C2 C3 1.383(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.375(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.363(6) . ?
C5 C6 1.401(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8 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 Cu1 O2 156.72(13) 2_545 . ?
O1 Cu1 N1 86.98(13) 2_545 1_455 ?
O2 Cu1 N1 88.80(13) . 1_455 ?
O1 Cu1 N2 92.53(13) 2_545 2_645 ?
O2 Cu1 N2 88.01(12) . 2_645 ?
N1 Cu1 N2 170.74(13) 1_455 2_645 ?
O1 Cu1 O4 99.38(13) 2_545 . ?
O2 Cu1 O4 103.73(13) . . ?
N1 Cu1 O4 93.57(13) 1_455 . ?
N2 Cu1 O4 95.63(13) 2_645 . ?
P1 O1 Cu1 135.76(17) . 2 ?
P1 O2 Cu1 142.56(18) . . ?
Cu1 O4 H4A 122(4) . . ?
Cu1 O4 H4B 127(4) . . ?
H4A O4 H4B 111(5) . . ?
C8 N1 N2 106.8(3) . . ?
C8 N1 Cu1 124.4(3) . 1_655 ?
N2 N1 Cu1 126.9(2) . 1_655 ?
C7 N2 N1 107.3(3) . . ?
C7 N2 Cu1 131.9(3) . 2_655 ?
N1 N2 Cu1 117.9(2) . 2_655 ?
C8 N3 C7 105.9(3) . . ?
C8 N3 C4 125.6(3) . . ?
C7 N3 C4 127.7(3) . . ?
O3 P1 O1 112.72(18) . . ?
O3 P1 O2 113.36(17) . . ?
O1 P1 O2 112.62(16) . . ?
O3 P1 C1 108.85(17) . . ?
O1 P1 C1 102.40(17) . . ?
O2 P1 C1 106.00(18) . . ?
C2 C1 C6 117.6(4) . . ?
C2 C1 P1 119.3(3) . . ?
C6 C1 P1 122.8(3) . . ?
C1 C2 C3 122.2(4) . . ?
C1 C2 H2 118.9 . . ?
C3 C2 H2 118.9 . . ?
C4 C3 C2 118.7(4) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 121.5(4) . . ?
C5 C4 N3 121.4(4) . . ?
C3 C4 N3 117.1(4) . . ?
C4 C5 C6 118.3(4) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C1 C6 C5 121.6(4) . . ?
C1 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
N2 C7 N3 109.7(3) . . ?
N2 C7 H7 125.2 . . ?
N3 C7 H7 125.2 . . ?
N1 C8 N3 110.3(4) . . ?
N1 C8 H8 124.9 . . ?
N3 C8 H8 124.9 . . ?

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
O1 Cu1 O2 P1 -139.5(3) 2_545 . . . ?
N1 Cu1 O2 P1 -59.9(3) 1_455 . . . ?
N2 Cu1 O2 P1 128.8(3) 2_645 . . . ?
O4 Cu1 O2 P1 33.4(3) . . . . ?
C8 N1 N2 C7 0.4(4) . . . . ?
Cu1 N1 N2 C7 -164.6(3) 1_655 . . . ?
C8 N1 N2 Cu1 -162.7(3) . . . 2_655 ?
Cu1 N1 N2 Cu1 32.3(4) 1_655 . . 2_655 ?
Cu1 O1 P1 O3 -106.7(3) 2 . . . ?
Cu1 O1 P1 O2 23.1(3) 2 . . . ?
Cu1 O1 P1 C1 136.5(3) 2 . . . ?
Cu1 O2 P1 O3 130.0(3) . . . . ?
Cu1 O2 P1 O1 0.6(4) . . . . ?
Cu1 O2 P1 C1 -110.6(3) . . . . ?
O3 P1 C1 C2 155.3(4) . . . . ?
O1 P1 C1 C2 -85.2(4) . . . . ?
O2 P1 C1 C2 33.0(4) . . . . ?
O3 P1 C1 C6 -31.2(4) . . . . ?
O1 P1 C1 C6 88.3(4) . . . . ?
O2 P1 C1 C6 -153.5(4) . . . . ?
C6 C1 C2 C3 -1.0(8) . . . . ?
P1 C1 C2 C3 172.9(5) . . . . ?
C1 C2 C3 C4 -0.8(9) . . . . ?
C2 C3 C4 C5 2.5(8) . . . . ?
C2 C3 C4 N3 -175.7(5) . . . . ?
C8 N3 C4 C5 145.6(5) . . . . ?
C7 N3 C4 C5 -46.0(6) . . . . ?
C8 N3 C4 C3 -36.2(6) . . . . ?
C7 N3 C4 C3 132.3(5) . . . . ?
C3 C4 C5 C6 -2.3(8) . . . . ?
N3 C4 C5 C6 175.9(4) . . . . ?
C2 C1 C6 C5 1.2(7) . . . . ?
P1 C1 C6 C5 -172.4(4) . . . . ?
C4 C5 C6 C1 0.4(8) . . . . ?
N1 N2 C7 N3 -1.2(4) . . . . ?
Cu1 N2 C7 N3 158.6(3) 2_655 . . . ?
C8 N3 C7 N2 1.5(5) . . . . ?
C4 N3 C7 N2 -168.7(4) . . . . ?
N2 N1 C8 N3 0.5(4) . . . . ?
Cu1 N1 C8 N3 166.0(2) 1_655 . . . ?
C7 N3 C8 N1 -1.2(5) . . . . ?
C4 N3 C8 N1 169.3(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4B O3 0.849(10) 1.849(18) 2.684(5) 167(6) 4_565
O4 H4A O2 0.848(10) 2.07(4) 2.794(5) 143(5) 2

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.18
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.139
####################################################################### 
# 
# 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_mo_20603a_0m
_database_code_depnum_ccdc_archive 'CCDC 906323'
_audit_update_record             
;
2012-10-17 deposited with the CCDC.
2016-05-27 downloaded from the CCDC.
;
#TrackingRef 'Fe.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H8 Fe N3 O4 P'
_chemical_formula_sum            'C8 H8 Fe N3 O4 P'
_chemical_formula_weight         296.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.0479(14)
_cell_length_b                   7.2597(9)
_cell_length_c                   12.9092(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.188(2)
_cell_angle_gamma                90.00
_cell_volume                     977.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3854
_cell_measurement_theta_min      3.34
_cell_measurement_theta_max      27.47

_exptl_crystal_description       sheet
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             600
_exptl_absorpt_coefficient_mu    1.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7258
_exptl_absorpt_correction_T_max  0.8752
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_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            5702
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         25.19
_reflns_number_total             1736
_reflns_number_gt                1578
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0587P)²+0.5261P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1736
_refine_ls_number_parameters     162
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0983
_refine_ls_wR_factor_gt          0.0806
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_restrained_S_all      1.216
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe -0.01183(4) 0.04257(5) 0.20817(3) 0.01231(18) Uani 1 1 d . . .
O1 O 0.16223(19) 0.4069(3) 0.38509(17) 0.0167(4) Uani 1 1 d . . .
O2 O 0.12181(19) 0.0649(3) 0.35774(17) 0.0155(4) Uani 1 1 d . . .
O4 O 0.0162(2) 0.2652(3) 0.11869(19) 0.0212(5) Uani 1 1 d D . .
N1 N 0.8557(2) 0.1881(3) 0.2753(2) 0.0152(5) Uani 1 1 d . . .
N2 N 0.8834(2) 0.3507(3) 0.33536(19) 0.0149(5) Uani 1 1 d . . .
O3 O 0.21311(19) 0.1976(3) 0.54951(16) 0.0176(5) Uani 1 1 d . . .
N3 N 0.7147(2) 0.2241(3) 0.3589(2) 0.0152(5) Uani 1 1 d . . .
P1 P 0.20391(6) 0.21505(9) 0.43120(6) 0.0105(2) Uani 1 1 d . . .
C1 C 0.3621(3) 0.1956(4) 0.4194(2) 0.0130(6) Uani 1 1 d . . .
C2 C 0.3756(4) 0.1369(7) 0.3213(3) 0.0453(11) Uani 1 1 d . . .
H2 H 0.3040 0.0931 0.2661 0.054 Uiso 1 1 calc R . .
C3 C 0.4912(4) 0.1415(7) 0.3034(3) 0.0461(12) Uani 1 1 d . . .
H3 H 0.4975 0.1008 0.2370 0.055 Uiso 1 1 calc R . .
C4 C 0.5976(3) 0.2066(4) 0.3839(2) 0.0158(6) Uani 1 1 d . . .
C5 C 0.5894(3) 0.2614(7) 0.4818(3) 0.0428(10) Uani 1 1 d . . .
H5 H 0.6620 0.3024 0.5370 0.051 Uiso 1 1 calc R . .
C6 C 0.4720(4) 0.2560(7) 0.4990(3) 0.0446(11) Uani 1 1 d . . .
H6 H 0.4672 0.2943 0.5663 0.053 Uiso 1 1 calc R . .
C7 C 0.7985(3) 0.3694(4) 0.3846(2) 0.0160(6) Uani 1 1 d . . .
H7 H 0.7952 0.4669 0.4303 0.019 Uiso 1 1 calc R . .
C8 C 0.7551(3) 0.1168(4) 0.2917(2) 0.0166(6) Uani 1 1 d . . .
H8 H 0.7165 0.0068 0.2612 0.020 Uiso 1 1 calc R . .
H4A H -0.031(3) 0.354(4) 0.099(3) 0.017(9) Uiso 1 1 d D . .
H4B H 0.079(3) 0.274(6) 0.094(4) 0.048(13) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0089(3) 0.0124(3) 0.0169(3) -0.00320(14) 0.00597(18) -0.00042(14)
O1 0.0123(10) 0.0129(9) 0.0243(11) 0.0033(8) 0.0052(8) 0.0013(8)
O2 0.0136(10) 0.0136(9) 0.0200(10) -0.0011(8) 0.0067(8) -0.0023(8)
O4 0.0229(12) 0.0167(11) 0.0316(12) 0.0051(9) 0.0193(10) 0.0035(9)
N1 0.0132(12) 0.0116(11) 0.0229(12) -0.0022(10) 0.0087(10) -0.0001(9)
N2 0.0133(12) 0.0147(12) 0.0185(12) -0.0012(9) 0.0076(10) -0.0002(10)
O3 0.0159(10) 0.0240(11) 0.0164(10) 0.0004(8) 0.0100(8) 0.0005(9)
N3 0.0114(12) 0.0175(12) 0.0199(12) -0.0001(10) 0.0095(10) -0.0012(10)
P1 0.0083(4) 0.0109(4) 0.0138(4) 0.0000(3) 0.0057(3) 0.0004(3)
C1 0.0138(14) 0.0106(13) 0.0158(14) 0.0025(10) 0.0065(11) 0.0014(11)
C2 0.0214(18) 0.077(3) 0.042(2) -0.034(2) 0.0160(17) -0.020(2)
C3 0.029(2) 0.076(3) 0.042(2) -0.036(2) 0.0246(18) -0.021(2)
C4 0.0122(13) 0.0172(14) 0.0217(15) 0.0030(12) 0.0106(12) 0.0004(11)
C5 0.0165(17) 0.086(3) 0.0269(18) -0.022(2) 0.0089(14) -0.0143(19)
C6 0.0227(18) 0.089(3) 0.0258(19) -0.023(2) 0.0131(16) -0.009(2)
C7 0.0155(14) 0.0166(14) 0.0183(14) -0.0023(11) 0.0089(12) -0.0025(11)
C8 0.0159(14) 0.0135(13) 0.0233(15) -0.0030(12) 0.0104(12) -0.0012(12)

_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 O1 1.966(2) 2_545 ?
Fe1 O2 2.015(2) . ?
Fe1 O4 2.068(2) . ?
Fe1 N2 2.189(2) 2_645 ?
Fe1 N1 2.201(2) 1_455 ?
O1 P1 1.525(2) . ?
O1 Fe1 1.966(2) 2 ?
O2 P1 1.531(2) . ?
O4 H4A 0.816(18) . ?
O4 H4B 0.85(2) . ?
N1 C8 1.305(4) . ?
N1 N2 1.390(3) . ?
N1 Fe1 2.201(2) 1_655 ?
N2 C7 1.301(4) . ?
N2 Fe1 2.189(2) 2_655 ?
O3 P1 1.502(2) . ?
N3 C8 1.346(4) . ?
N3 C7 1.371(4) . ?
N3 C4 1.439(4) . ?
P1 C1 1.809(3) . ?
C1 C6 1.379(5) . ?
C1 C2 1.390(5) . ?
C2 C3 1.372(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.372(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.356(5) . ?
C5 C6 1.387(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8 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 Fe1 O2 146.36(8) 2_545 . ?
O1 Fe1 O4 107.52(9) 2_545 . ?
O2 Fe1 O4 105.99(9) . . ?
O1 Fe1 N2 90.73(9) 2_545 2_645 ?
O2 Fe1 N2 87.96(8) . 2_645 ?
O4 Fe1 N2 97.20(9) . 2_645 ?
O1 Fe1 N1 86.79(9) 2_545 1_455 ?
O2 Fe1 N1 87.53(9) . 1_455 ?
O4 Fe1 N1 94.90(9) . 1_455 ?
N2 Fe1 N1 167.83(9) 2_645 1_455 ?
P1 O1 Fe1 141.50(13) . 2 ?
P1 O2 Fe1 138.49(12) . . ?
Fe1 O4 H4A 126(2) . . ?
Fe1 O4 H4B 124(3) . . ?
H4A O4 H4B 110(4) . . ?
C8 N1 N2 106.8(2) . . ?
C8 N1 Fe1 125.86(19) . 1_655 ?
N2 N1 Fe1 125.04(17) . 1_655 ?
C7 N2 N1 107.4(2) . . ?
C7 N2 Fe1 133.7(2) . 2_655 ?
N1 N2 Fe1 116.08(17) . 2_655 ?
C8 N3 C7 105.1(2) . . ?
C8 N3 C4 127.3(2) . . ?
C7 N3 C4 126.9(2) . . ?
O3 P1 O1 112.62(12) . . ?
O3 P1 O2 113.45(12) . . ?
O1 P1 O2 111.53(11) . . ?
O3 P1 C1 109.54(12) . . ?
O1 P1 C1 102.39(12) . . ?
O2 P1 C1 106.52(12) . . ?
C6 C1 C2 116.4(3) . . ?
C6 C1 P1 123.4(2) . . ?
C2 C1 P1 119.8(2) . . ?
C3 C2 C1 122.1(3) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C2 C3 C4 119.6(3) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 120.3(3) . . ?
C5 C4 N3 121.6(3) . . ?
C3 C4 N3 118.0(3) . . ?
C4 C5 C6 119.6(3) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 122.0(3) . . ?
C1 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
N2 C7 N3 109.9(3) . . ?
N2 C7 H7 125.1 . . ?
N3 C7 H7 125.1 . . ?
N1 C8 N3 110.8(3) . . ?
N1 C8 H8 124.6 . . ?
N3 C8 H8 124.6 . . ?

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
O1 Fe1 O2 P1 -151.21(16) 2_545 . . . ?
O4 Fe1 O2 P1 23.6(2) . . . . ?
N2 Fe1 O2 P1 120.5(2) 2_645 . . . ?
N1 Fe1 O2 P1 -70.77(19) 1_455 . . . ?
C8 N1 N2 C7 -0.1(3) . . . . ?
Fe1 N1 N2 C7 -163.7(2) 1_655 . . . ?
C8 N1 N2 Fe1 -163.72(19) . . . 2_655 ?
Fe1 N1 N2 Fe1 32.7(3) 1_655 . . 2_655 ?
Fe1 O1 P1 O3 -102.5(2) 2 . . . ?
Fe1 O1 P1 O2 26.3(2) 2 . . . ?
Fe1 O1 P1 C1 139.9(2) 2 . . . ?
Fe1 O2 P1 O3 138.14(17) . . . . ?
Fe1 O2 P1 O1 9.7(2) . . . . ?
Fe1 O2 P1 C1 -101.26(19) . . . . ?
O3 P1 C1 C6 -32.4(3) . . . . ?
O1 P1 C1 C6 87.3(3) . . . . ?
O2 P1 C1 C6 -155.5(3) . . . . ?
O3 P1 C1 C2 155.2(3) . . . . ?
O1 P1 C1 C2 -85.1(3) . . . . ?
O2 P1 C1 C2 32.1(3) . . . . ?
C6 C1 C2 C3 -1.1(7) . . . . ?
P1 C1 C2 C3 171.7(4) . . . . ?
C1 C2 C3 C4 -0.3(8) . . . . ?
C2 C3 C4 C5 1.8(7) . . . . ?
C2 C3 C4 N3 -174.8(4) . . . . ?
C8 N3 C4 C5 150.6(4) . . . . ?
C7 N3 C4 C5 -40.5(5) . . . . ?
C8 N3 C4 C3 -32.8(5) . . . . ?
C7 N3 C4 C3 136.1(4) . . . . ?
C3 C4 C5 C6 -1.7(7) . . . . ?
N3 C4 C5 C6 174.7(4) . . . . ?
C2 C1 C6 C5 1.2(7) . . . . ?
P1 C1 C6 C5 -171.4(4) . . . . ?
C4 C5 C6 C1 0.2(8) . . . . ?
N1 N2 C7 N3 -0.1(3) . . . . ?
Fe1 N2 C7 N3 159.3(2) 2_655 . . . ?
C8 N3 C7 N2 0.3(3) . . . . ?
C4 N3 C7 N2 -170.6(3) . . . . ?
N2 N1 C8 N3 0.3(3) . . . . ?
Fe1 N1 C8 N3 163.75(19) 1_655 . . . ?
C7 N3 C8 N1 -0.4(3) . . . . ?
C4 N3 C8 N1 170.4(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4A O2 0.816(18) 2.00(2) 2.730(3) 148(3) 2
O4 H4B O3 0.85(2) 1.77(2) 2.623(3) 177(5) 4_565

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.19
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.176
####################################################################### 
# 
# 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_a21115a
_database_code_depnum_ccdc_archive 'CCDC 921253'
_audit_update_record             
;
2013-01-22 deposited with the CCDC.
2016-05-27 downloaded from the CCDC.
;
#TrackingRef 'a21115a.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H7 Cl Co N3 O3 P, 2(H2 O)'
_chemical_formula_sum            'C8 H11 Cl Co N3 O5 P'
_chemical_formula_weight         354.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/m
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   20.71(2)
_cell_length_b                   7.527(8)
_cell_length_c                   8.437(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.746(10)
_cell_angle_gamma                90.00
_cell_volume                     1296(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2197
_cell_measurement_theta_min      2.88
_cell_measurement_theta_max      27.65

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             716
_exptl_absorpt_coefficient_mu    1.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7876
_exptl_absorpt_correction_T_max  0.8779
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_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_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3227
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.50
_reflns_number_total             1288
_reflns_number_gt                1197
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0504P)²+4.0802P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1288
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0961
_refine_ls_wR_factor_gt          0.0949
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.7500 0.2500 0.5000 0.0209(2) Uani 1 2 d S . .
N1 N 1.18000(10) -0.0907(3) 0.5915(3) 0.0250(5) Uani 1 1 d . . .
O2 O 0.78573(9) 0.1694(3) 0.7334(2) 0.0253(4) Uani 1 1 d . . .
Cl1 Cl 0.67204(4) 0.0000 0.46507(12) 0.0255(3) Uani 1 2 d S . .
O1 O 0.81999(14) 0.0000 0.9911(3) 0.0318(7) Uani 1 2 d S . .
H1A H 0.7827 0.0000 1.0121 0.048 Uiso 1 2 calc SR . .
P1 P 0.81655(4) 0.0000 0.80441(12) 0.0204(3) Uani 1 2 d S . .
N2 N 1.09192(15) 0.0000 0.6747(4) 0.0217(7) Uani 1 2 d S . .
C1 C 0.90171(18) 0.0000 0.7838(5) 0.0240(8) Uani 1 2 d S . .
C2 C 0.93397(17) 0.1560(5) 0.7684(6) 0.0542(11) Uani 1 1 d . . .
H2 H 0.9128 0.2634 0.7781 0.065 Uiso 1 1 calc R . .
C3 C 0.99761(18) 0.1566(5) 0.7386(6) 0.0572(12) Uani 1 1 d . . .
H3 H 1.0193 0.2635 0.7306 0.069 Uiso 1 1 calc R . .
C4 C 1.02818(18) 0.0000 0.7213(5) 0.0247(8) Uani 1 2 d S . .
C5 C 1.12692(14) -0.1411(4) 0.6425(4) 0.0337(7) Uani 1 1 d . . .
H5 H 1.1150 -0.2588 0.6548 0.040 Uiso 1 1 calc R . .
O3 O 0.70828(15) 0.0000 0.0956(4) 0.0357(7) Uani 1 2 d S . .
H3A H 0.7046 0.0778 0.1665 0.043 Uiso 1 1 d R . .
O4 O 0.8905(4) 0.5000 0.1678(9) 0.160(4) Uani 1 2 d S . .
H4 H 0.8922 0.4104 0.0892 0.191 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0165(3) 0.0171(3) 0.0315(3) -0.00108(19) 0.0107(2) 0.00035(18)
N1 0.0194(11) 0.0190(12) 0.0394(13) -0.0022(10) 0.0129(10) -0.0003(9)
O2 0.0229(9) 0.0219(11) 0.0324(10) -0.0009(8) 0.0081(8) 0.0016(8)
Cl1 0.0190(5) 0.0182(5) 0.0410(6) 0.000 0.0102(4) 0.000
O1 0.0219(14) 0.050(2) 0.0255(15) 0.000 0.0090(11) 0.000
P1 0.0149(5) 0.0231(5) 0.0248(5) 0.000 0.0079(4) 0.000
N2 0.0156(15) 0.0230(17) 0.0291(17) 0.000 0.0109(13) 0.000
C1 0.0156(17) 0.030(2) 0.028(2) 0.000 0.0106(15) 0.000
C2 0.0304(17) 0.0279(19) 0.113(3) -0.020(2) 0.038(2) -0.0051(14)
C3 0.0323(18) 0.0260(19) 0.124(4) -0.019(2) 0.043(2) -0.0106(15)
C4 0.0158(17) 0.030(2) 0.030(2) 0.000 0.0082(15) 0.000
C5 0.0274(15) 0.0195(14) 0.060(2) -0.0050(14) 0.0237(14) -0.0042(12)
O3 0.0357(17) 0.0419(19) 0.0322(16) 0.000 0.0136(13) 0.000
O4 0.208(8) 0.057(4) 0.161(7) 0.000 -0.121(6) 0.000

_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 2.074(3) 7_656 ?
Co1 O2 2.074(3) . ?
Co1 N1 2.125(3) 5_756 ?
Co1 N1 2.125(3) 3_455 ?
Co1 Cl1 2.4645(18) . ?
Co1 Cl1 2.4645(18) 7_656 ?
N1 C5 1.303(4) . ?
N1 N1 1.365(5) 6 ?
N1 Co1 2.125(3) 3_545 ?
O2 P1 1.505(2) . ?
Cl1 Co1 2.4645(18) 4_646 ?
O1 P1 1.565(3) . ?
O1 H1A 0.8200 . ?
P1 O2 1.505(2) 6 ?
P1 C1 1.801(4) . ?
N2 C5 1.340(4) 6 ?
N2 C5 1.340(4) . ?
N2 C4 1.439(5) . ?
C1 C2 1.368(4) 6 ?
C1 C2 1.368(4) . ?
C2 C3 1.383(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.358(4) . ?
C3 H3 0.9300 . ?
C4 C3 1.358(4) 6 ?
C5 H5 0.9300 . ?
O3 H3A 0.8500 . ?
O4 H4 0.9508 . ?

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 180.0 7_656 . ?
O2 Co1 N1 88.62(10) 7_656 5_756 ?
O2 Co1 N1 91.38(10) . 5_756 ?
O2 Co1 N1 91.38(10) 7_656 3_455 ?
O2 Co1 N1 88.62(10) . 3_455 ?
N1 Co1 N1 180.000(1) 5_756 3_455 ?
O2 Co1 Cl1 89.34(7) 7_656 . ?
O2 Co1 Cl1 90.66(7) . . ?
N1 Co1 Cl1 89.95(10) 5_756 . ?
N1 Co1 Cl1 90.05(10) 3_455 . ?
O2 Co1 Cl1 90.66(7) 7_656 7_656 ?
O2 Co1 Cl1 89.34(7) . 7_656 ?
N1 Co1 Cl1 90.05(10) 5_756 7_656 ?
N1 Co1 Cl1 89.95(10) 3_455 7_656 ?
Cl1 Co1 Cl1 180.00(3) . 7_656 ?
C5 N1 N1 106.95(18) . 6 ?
C5 N1 Co1 128.4(2) . 3_545 ?
N1 N1 Co1 124.36(7) 6 3_545 ?
P1 O2 Co1 133.25(12) . . ?
Co1 Cl1 Co1 99.56(9) . 4_646 ?
P1 O1 H1A 109.5 . . ?
O2 P1 O2 115.93(17) 6 . ?
O2 P1 O1 110.17(10) 6 . ?
O2 P1 O1 110.17(10) . . ?
O2 P1 C1 108.53(10) 6 . ?
O2 P1 C1 108.53(10) . . ?
O1 P1 C1 102.64(17) . . ?
C5 N2 C5 104.9(3) 6 . ?
C5 N2 C4 127.45(16) 6 . ?
C5 N2 C4 127.45(16) . . ?
C2 C1 C2 118.3(4) 6 . ?
C2 C1 P1 120.7(2) 6 . ?
C2 C1 P1 120.7(2) . . ?
C1 C2 C3 121.0(3) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C4 C3 C2 119.6(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C3 120.5(4) 6 . ?
C3 C4 N2 119.7(2) 6 . ?
C3 C4 N2 119.7(2) . . ?
N1 C5 N2 110.6(3) . . ?
N1 C5 H5 124.7 . . ?
N2 C5 H5 124.7 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.133



