# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_kk45
_database_code_depnum_ccdc_archive 'CCDC 1908875'
loop_
_audit_author_name
_audit_author_address
'Brian Skelton'
;University of Western Australia
Australia
;
_audit_update_record             
;
2019-04-09 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;

_audit_creation_date             2015-08-13T11:25:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C16 H16 Cl Fe O7'
_chemical_formula_moiety         'C16 H16 Cl Fe O7'
_chemical_formula_weight         411.59

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
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                   9.3705(2)
_cell_length_b                   13.1255(3)
_cell_length_c                   13.9195(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.818(2)
_cell_angle_gamma                90
_cell_volume                     1655.06(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5127
_cell_measurement_theta_min      4.693
_cell_measurement_theta_max      66.963

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.025
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_F_000             844

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    9.14
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
      CrysAlisPro, Oxford Diffraction Ltd.
;
_exptl_absorpt_correction_T_min  0.424
_exptl_absorpt_correction_T_max  0.82

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'sealed X-ray tube'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_number            13206
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.706
_diffrn_reflns_theta_max         67.226
_diffrn_reflns_theta_full        67.226
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_reflns_number_total             2957
_reflns_number_gt                2596
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;


_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
The water molecule  hydrogen atoms were located and refined with O-H distances 
restrained to ideal values. 

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0503P)²+0.4129P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2957
_refine_ls_number_parameters     236
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0869
_refine_ls_wR_factor_gt          0.0823
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.061

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.31516(4) 0.62352(3) 0.50155(3) 0.02473(12) Uani 1 d . .
Cl1 Cl 0.24561(7) 0.78626(5) 0.44763(5) 0.03980(17) Uani 1 d . .
C11 C 0.5882(2) 0.69514(17) 0.64210(17) 0.0259(5) Uani 1 d . .
O11 O 0.52266(17) 0.65345(13) 0.55639(12) 0.0287(4) Uani 1 d . .
C12 C 0.7389(3) 0.72300(17) 0.65890(18) 0.0269(5) Uani 1 d . .
O12 O 0.79981(17) 0.70394(13) 0.58170(12) 0.0316(4) Uani 1 d . .
C121 C 0.9480(3) 0.7390(2) 0.5925(2) 0.0415(6) Uani 1 d . .
H12A H 0.9532 0.8123 0.6064 0.062 Uiso 1 calc . .
H12B H 0.9774 0.7259 0.5309 0.062 Uiso 1 calc . .
H12C H 1.0148 0.7027 0.6476 0.062 Uiso 1 calc . .
C13 C 0.8137(3) 0.76419(19) 0.74912(19) 0.0336(6) Uani 1 d . .
H13 H 0.9149 0.7816 0.7599 0.04 Uiso 1 calc . .
C14 C 0.7427(3) 0.7806(2) 0.8248(2) 0.0373(6) Uani 1 d . .
H14 H 0.7958 0.8093 0.8862 0.045 Uiso 1 calc . .
C15 C 0.5980(3) 0.75577(19) 0.81084(19) 0.0325(5) Uani 1 d . .
H15 H 0.5504 0.7664 0.8626 0.039 Uiso 1 calc . .
C16 C 0.5179(3) 0.71384(18) 0.71872(17) 0.0278(5) Uani 1 d . .
C161 C 0.3670(3) 0.69045(19) 0.71057(18) 0.0318(5) Uani 1 d . .
H161 H 0.3307 0.7062 0.7666 0.038 Uiso 1 calc . .
O161 O 0.27650(18) 0.65136(14) 0.63752(13) 0.0347(4) Uani 1 d . .
C21 C 0.2482(2) 0.53666(17) 0.29958(17) 0.0259(5) Uani 1 d . .
O21 O 0.34310(17) 0.57234(13) 0.37832(12) 0.0283(4) Uani 1 d . .
C22 C 0.2996(3) 0.51467(18) 0.21448(18) 0.0286(5) Uani 1 d . .
O22 O 0.44682(18) 0.53248(13) 0.22709(12) 0.0304(4) Uani 1 d . .
C221 C 0.5048(3) 0.5254(2) 0.1414(2) 0.0368(6) Uani 1 d . .
H22A H 0.4961 0.4551 0.117 0.055 Uiso 1 calc . .
H22B H 0.6089 0.5456 0.1594 0.055 Uiso 1 calc . .
H22C H 0.449 0.5707 0.0892 0.055 Uiso 1 calc . .
C23 C 0.2042(3) 0.4779(2) 0.12904(19) 0.0330(5) Uani 1 d . .
H23 H 0.2393 0.4658 0.0718 0.04 Uiso 1 calc . .
C24 C 0.0564(3) 0.4582(2) 0.12595(19) 0.0350(6) Uani 1 d . .
H24 H -0.008 0.4323 0.0669 0.042 Uiso 1 calc . .
C25 C 0.0044(3) 0.47607(19) 0.20732(19) 0.0310(5) Uani 1 d . .
H25 H -0.0956 0.4609 0.2051 0.037 Uiso 1 calc . .
C26 C 0.0978(3) 0.51692(18) 0.29490(18) 0.0275(5) Uani 1 d . .
C261 C 0.0370(2) 0.53477(19) 0.37778(18) 0.0288(5) Uani 1 d . .
H261 H -0.063 0.5151 0.3697 0.035 Uiso 1 calc . .
O261 O 0.10011(17) 0.57304(14) 0.45898(12) 0.0307(4) Uani 1 d . .
O1 O 0.34922(18) 0.47333(13) 0.56132(13) 0.0286(4) Uani 1 d . .
H1BO H 0.419(3) 0.473(2) 0.6039(18) 0.037(8) Uiso 1 d . .
H1AO H 0.356(4) 0.433(2) 0.520(2) 0.057(11) Uiso 1 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O21 1.9214(16) . ?
Fe1 O11 1.9387(16) . ?
Fe1 O161 2.0488(17) . ?
Fe1 O261 2.0592(16) . ?
Fe1 O1 2.1317(18) . ?
Fe1 Cl1 2.3023(7) . ?
C11 O11 1.313(3) . ?
C11 C16 1.411(3) . ?
C11 C12 1.420(3) . ?
C12 O12 1.362(3) . ?
C12 C13 1.382(3) . ?
O12 C121 1.434(3) . ?
C121 H12A 0.98 . ?
C121 H12B 0.98 . ?
C121 H12C 0.98 . ?
C13 C14 1.399(4) . ?
C13 H13 0.95 . ?
C14 C15 1.359(4) . ?
C14 H14 0.95 . ?
C15 C16 1.420(3) . ?
C15 H15 0.95 . ?
C16 C161 1.423(4) . ?
C161 O161 1.255(3) . ?
C161 H161 0.95 . ?
C21 O21 1.309(3) . ?
C21 C26 1.417(3) . ?
C21 C22 1.418(3) . ?
C22 O22 1.366(3) . ?
C22 C23 1.379(3) . ?
O22 C221 1.435(3) . ?
C221 H22A 0.98 . ?
C221 H22B 0.98 . ?
C221 H22C 0.98 . ?
C23 C24 1.399(4) . ?
C23 H23 0.95 . ?
C24 C25 1.363(4) . ?
C24 H24 0.95 . ?
C25 C26 1.412(3) . ?
C25 H25 0.95 . ?
C26 C261 1.431(3) . ?
C261 O261 1.240(3) . ?
C261 H261 0.95 . ?
O1 H1BO 0.765(18) . ?
O1 H1AO 0.792(18) . ?

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
O21 Fe1 O11 94.04(7) . . ?
O21 Fe1 O161 169.65(7) . . ?
O11 Fe1 O161 89.81(7) . . ?
O21 Fe1 O261 88.70(7) . . ?
O11 Fe1 O261 170.99(7) . . ?
O161 Fe1 O261 86.10(7) . . ?
O21 Fe1 O1 89.09(7) . . ?
O11 Fe1 O1 89.93(7) . . ?
O161 Fe1 O1 81.29(7) . . ?
O261 Fe1 O1 81.52(7) . . ?
O21 Fe1 Cl1 97.19(5) . . ?
O11 Fe1 Cl1 96.44(6) . . ?
O161 Fe1 Cl1 91.91(6) . . ?
O261 Fe1 Cl1 91.72(5) . . ?
O1 Fe1 Cl1 170.69(5) . . ?
O11 C11 C16 124.0(2) . . ?
O11 C11 C12 118.1(2) . . ?
C16 C11 C12 117.9(2) . . ?
C11 O11 Fe1 129.11(15) . . ?
O12 C12 C13 124.9(2) . . ?
O12 C12 C11 115.0(2) . . ?
C13 C12 C11 120.1(2) . . ?
C12 O12 C121 116.61(19) . . ?
O12 C121 H12A 109.5 . . ?
O12 C121 H12B 109.5 . . ?
H12A C121 H12B 109.5 . . ?
O12 C121 H12C 109.5 . . ?
H12A C121 H12C 109.5 . . ?
H12B C121 H12C 109.5 . . ?
C12 C13 C14 121.1(2) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C13 120.3(2) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 120.0(2) . . ?
C14 C15 H15 120 . . ?
C16 C15 H15 120 . . ?
C11 C16 C15 120.6(2) . . ?
C11 C16 C161 123.3(2) . . ?
C15 C16 C161 116.1(2) . . ?
O161 C161 C16 127.2(2) . . ?
O161 C161 H161 116.4 . . ?
C16 C161 H161 116.4 . . ?
C161 O161 Fe1 125.38(16) . . ?
O21 C21 C26 123.9(2) . . ?
O21 C21 C22 118.0(2) . . ?
C26 C21 C22 118.1(2) . . ?
C21 O21 Fe1 130.85(15) . . ?
O22 C22 C23 125.5(2) . . ?
O22 C22 C21 113.9(2) . . ?
C23 C22 C21 120.6(2) . . ?
C22 O22 C221 117.84(19) . . ?
O22 C221 H22A 109.5 . . ?
O22 C221 H22B 109.5 . . ?
H22A C221 H22B 109.5 . . ?
O22 C221 H22C 109.5 . . ?
H22A C221 H22C 109.5 . . ?
H22B C221 H22C 109.5 . . ?
C22 C23 C24 120.6(2) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C25 C24 C23 120.3(2) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.5(2) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C21 119.9(2) . . ?
C25 C26 C261 118.1(2) . . ?
C21 C26 C261 122.0(2) . . ?
O261 C261 C26 127.2(2) . . ?
O261 C261 H261 116.4 . . ?
C26 C261 H261 116.4 . . ?
C261 O261 Fe1 126.61(16) . . ?
Fe1 O1 H1BO 109(2) . . ?
Fe1 O1 H1AO 111(3) . . ?
H1BO O1 H1AO 110(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
C121 H12C O161 0.98 2.58 3.194(3) 120.6 1_655
C161 H161 Cl1 0.95 2.83 3.768(3) 168.4 4_576
O1 H1BO O21 0.765(18) 2.26(3) 2.853(2) 136(3) 3_666
O1 H1BO O22 0.765(18) 2.37(2) 3.075(2) 155(3) 3_666
O1 H1AO O11 0.792(18) 2.08(2) 2.811(2) 153(4) 3_666
O1 H1AO O12 0.792(18) 2.52(3) 3.147(2) 138(3) 3_666


#===END
