# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1504603'
_audit_update_record             
;
2016-09-15 deposited with the CCDC.
2016-10-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        MnSb2O3(OH)Cl
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cl H Mn O4 Sb2'
_chemical_formula_weight         398.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.943(6)
_cell_length_b                   8.209(7)
_cell_length_c                   10.524(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.542(13)
_cell_angle_gamma                90
_cell_volume                     595.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1799
_cell_measurement_theta_min      2.4812
_cell_measurement_theta_max      27.5205

_exptl_crystal_description       plate-shaped
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.446
_exptl_crystal_F_000             708
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    11.457
_shelx_estimated_absorpt_T_min   0.092
_shelx_estimated_absorpt_T_max   0.278
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6464
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Mercury70 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5354
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.953
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             1347
_reflns_number_gt                1227
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0226P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1347
_refine_ls_number_parameters     77
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0211
_refine_ls_wR_factor_ref         0.0508
_refine_ls_wR_factor_gt          0.0500
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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
Sb1 Sb 0.22169(4) 0.00720(4) 0.27767(2) 0.01073(10) Uani 1 1 d . . . . .
Sb2 Sb 0.23269(4) 0.41842(4) 0.26060(2) 0.01127(10) Uani 1 1 d . . . . .
Mn1 Mn 0.00324(9) 0.21110(8) 0.00716(5) 0.01167(16) Uani 1 1 d . . . . .
Cl1 Cl 0.35152(17) 0.74937(16) 0.05076(11) 0.0289(3) Uani 1 1 d . . . . .
O1 O 0.0002(4) 0.0110(3) 0.1374(2) 0.0127(6) Uani 1 1 d . . . . .
O2 O -0.0001(4) 0.4122(3) 0.1328(2) 0.0129(6) Uani 1 1 d . . . . .
O3 O 0.1579(4) 0.2200(3) 0.3531(3) 0.0129(6) Uani 1 1 d . . . . .
O4 O 0.3039(5) 0.2176(4) 0.1373(3) 0.0158(7) Uani 1 1 d D . . . .
H1 H 0.427(5) 0.201(8) 0.115(7) 0.09(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 O3 1.990(3) . ?
Sb1 O1 2.007(3) . ?
Sb1 O2 2.048(3) 2_545 ?
Sb1 O4 2.384(3) . ?
Sb1 Sb2 3.218(3) 2_545 ?
Sb2 O2 1.982(3) . ?
Sb2 O3 1.996(3) . ?
Sb2 O1 2.177(3) 2 ?
Sb2 O4 2.189(3) . ?
Sb2 Sb1 3.218(3) 2 ?
Mn1 O2 2.117(3) . ?
Mn1 O3 2.121(3) 4_565 ?
Mn1 O1 2.141(3) . ?
Mn1 O4 2.364(4) . ?
Mn1 O1 2.373(3) 3 ?
Mn1 Cl1 2.490(2) 3_565 ?
Cl1 Mn1 2.490(2) 3_565 ?
O1 Sb2 2.177(3) 2_545 ?
O1 Mn1 2.373(3) 3 ?
O2 Sb1 2.048(3) 2 ?
O3 Mn1 2.121(3) 4_566 ?

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
O3 Sb1 O1 95.32(12) . . ?
O3 Sb1 O2 86.42(12) . 2_545 ?
O1 Sb1 O2 77.98(13) . 2_545 ?
O3 Sb1 O4 71.99(13) . . ?
O1 Sb1 O4 75.55(12) . . ?
O2 Sb1 O4 143.77(11) 2_545 . ?
O3 Sb1 Sb2 89.37(9) . 2_545 ?
O1 Sb1 Sb2 41.70(9) . 2_545 ?
O2 Sb1 Sb2 36.32(8) 2_545 2_545 ?
O4 Sb1 Sb2 112.78(8) . 2_545 ?
O2 Sb2 O3 94.16(12) . . ?
O2 Sb2 O1 75.50(12) . 2 ?
O3 Sb2 O1 78.19(12) . 2 ?
O2 Sb2 O4 78.48(12) . . ?
O3 Sb2 O4 76.31(13) . . ?
O1 Sb2 O4 141.80(11) 2 . ?
O2 Sb2 Sb1 37.72(9) . 2 ?
O3 Sb2 Sb1 86.55(9) . 2 ?
O1 Sb2 Sb1 37.83(8) 2 2 ?
O4 Sb2 Sb1 112.39(8) . 2 ?
O2 Mn1 O3 108.18(12) . 4_565 ?
O2 Mn1 O1 101.36(13) . . ?
O3 Mn1 O1 137.46(12) 4_565 . ?
O2 Mn1 O4 72.08(11) . . ?
O3 Mn1 O4 86.94(13) 4_565 . ?
O1 Mn1 O4 73.66(11) . . ?
O2 Mn1 O1 178.40(9) . 3 ?
O3 Mn1 O1 71.56(11) 4_565 3 ?
O1 Mn1 O1 79.68(13) . 3 ?
O4 Mn1 O1 109.43(11) . 3 ?
O2 Mn1 Cl1 88.29(8) . 3_565 ?
O3 Mn1 Cl1 110.53(10) 4_565 3_565 ?
O1 Mn1 Cl1 100.08(9) . 3_565 ?
O4 Mn1 Cl1 157.31(9) . 3_565 ?
O1 Mn1 Cl1 90.33(8) 3 3_565 ?
Sb1 O1 Mn1 114.86(13) . . ?
Sb1 O1 Sb2 100.47(13) . 2_545 ?
Mn1 O1 Sb2 130.21(14) . 2_545 ?
Sb1 O1 Mn1 114.23(13) . 3 ?
Mn1 O1 Mn1 100.32(13) . 3 ?
Sb2 O1 Mn1 95.40(11) 2_545 3 ?
Sb2 O2 Sb1 105.96(14) . 2 ?
Sb2 O2 Mn1 112.18(13) . . ?
Sb1 O2 Mn1 130.30(14) 2 . ?
Sb1 O3 Sb2 116.10(15) . . ?
Sb1 O3 Mn1 133.96(15) . 4_566 ?
Sb2 O3 Mn1 109.74(13) . 4_566 ?
Sb2 O4 Mn1 96.67(12) . . ?
Sb2 O4 Sb1 95.29(13) . . ?
Mn1 O4 Sb1 94.86(12) . . ?

_refine_diff_density_max         1.766
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.203

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1504604'
_audit_update_record             
;
2016-09-15 deposited with the CCDC.
2016-10-17 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            'Cl Fe H O4 Sb2'
_chemical_formula_weight         399.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.901(3)
_cell_length_b                   8.158(4)
_cell_length_c                   10.320(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.516(7)
_cell_angle_gamma                90
_cell_volume                     578.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1684
_cell_measurement_theta_min      2.4966
_cell_measurement_theta_max      27.5050

_exptl_crystal_description       plate-shaped
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.592
_exptl_crystal_F_000             712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    12.132
_shelx_estimated_absorpt_T_min   0.065
_shelx_estimated_absorpt_T_max   0.195
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7145
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Mercury70 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4232
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.966
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1304
_reflns_number_gt                1225
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0256P)²+0.0387P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1304
_refine_ls_number_parameters     77
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0158
_refine_ls_wR_factor_ref         0.0421
_refine_ls_wR_factor_gt          0.0413
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.21687(3) 0.00331(3) 0.28081(2) 0.01071(8) Uani 1 1 d . . . . .
Sb2 Sb 0.24097(3) 0.41665(3) 0.26122(2) 0.01137(8) Uani 1 1 d . . . . .
Fe1 Fe 0.01029(7) 0.20588(5) 0.01053(4) 0.01140(12) Uani 1 1 d . . . . .
Cl1 Cl 0.33980(13) 0.75572(13) 0.05222(9) 0.0262(2) Uani 1 1 d . . . . .
O1 O -0.0044(3) 0.0163(3) 0.1387(2) 0.0128(5) Uani 1 1 d . . . . .
O2 O 0.0116(3) 0.4079(3) 0.1310(2) 0.0127(5) Uani 1 1 d . . . . .
O3 O 0.1563(3) 0.2199(3) 0.3581(2) 0.0122(5) Uani 1 1 d . . . . .
O4 O 0.3111(4) 0.2100(3) 0.1404(2) 0.0141(5) Uani 1 1 d D . . . .
H1 H 0.403(5) 0.175(5) 0.104(4) 0.043(15) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 O3 1.999(2) . ?
Sb1 O1 2.015(2) . ?
Sb1 O2 2.048(2) 2_545 ?
Sb1 O4 2.355(2) . ?
Sb1 Sb2 3.2258(15) 2_545 ?
Sb2 O2 1.977(2) . ?
Sb2 O3 2.008(2) . ?
Sb2 O1 2.172(2) 2 ?
Sb2 O4 2.179(2) . ?
Sb2 Sb1 3.2258(15) 2 ?
Fe1 O3 2.039(2) 4_565 ?
Fe1 O1 2.044(2) . ?
Fe1 O2 2.064(2) . ?
Fe1 O4 2.360(3) . ?
Fe1 O1 2.376(2) 3 ?
Fe1 Cl1 2.4602(15) 3_565 ?
Cl1 Fe1 2.4603(15) 3_565 ?
O1 Sb2 2.172(2) 2_545 ?
O1 Fe1 2.376(2) 3 ?
O2 Sb1 2.048(2) 2 ?
O3 Fe1 2.039(2) 4_566 ?

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
O3 Sb1 O1 94.08(9) . . ?
O3 Sb1 O2 87.64(9) . 2_545 ?
O1 Sb1 O2 77.38(10) . 2_545 ?
O3 Sb1 O4 72.16(9) . . ?
O1 Sb1 O4 75.49(9) . . ?
O2 Sb1 O4 144.61(9) 2_545 . ?
O3 Sb1 Sb2 90.44(7) . 2_545 ?
O1 Sb1 Sb2 41.41(7) . 2_545 ?
O2 Sb1 Sb2 35.98(6) 2_545 2_545 ?
O4 Sb1 Sb2 113.51(6) . 2_545 ?
O2 Sb2 O3 93.30(9) . . ?
O2 Sb2 O1 75.37(9) . 2 ?
O3 Sb2 O1 78.13(9) . 2 ?
O2 Sb2 O4 77.91(9) . . ?
O3 Sb2 O4 75.97(10) . . ?
O1 Sb2 O4 141.27(9) 2 . ?
O2 Sb2 Sb1 37.50(7) . 2 ?
O3 Sb2 Sb1 85.07(7) . 2 ?
O1 Sb2 Sb1 37.87(6) 2 2 ?
O4 Sb2 Sb1 111.17(7) . 2 ?
O3 Fe1 O1 141.50(10) 4_565 . ?
O3 Fe1 O2 104.67(9) 4_565 . ?
O1 Fe1 O2 102.25(10) . . ?
O3 Fe1 O4 87.77(9) 4_565 . ?
O1 Fe1 O4 74.85(9) . . ?
O2 Fe1 O4 72.19(8) . . ?
O3 Fe1 O1 72.88(9) 4_565 3 ?
O1 Fe1 O1 81.00(10) . 3 ?
O2 Fe1 O1 176.64(8) . 3 ?
O4 Fe1 O1 109.76(8) . 3 ?
O3 Fe1 Cl1 107.73(7) 4_565 3_565 ?
O1 Fe1 Cl1 99.10(7) . 3_565 ?
O2 Fe1 Cl1 90.24(7) . 3_565 ?
O4 Fe1 Cl1 159.28(7) . 3_565 ?
O1 Fe1 Cl1 88.36(6) 3 3_565 ?
Sb1 O1 Fe1 115.42(11) . . ?
Sb1 O1 Sb2 100.72(10) . 2_545 ?
Fe1 O1 Sb2 132.63(11) . 2_545 ?
Sb1 O1 Fe1 113.33(10) . 3 ?
Fe1 O1 Fe1 99.00(10) . 3 ?
Sb2 O1 Fe1 93.20(9) 2_545 3 ?
Sb2 O2 Sb1 106.53(10) . 2 ?
Sb2 O2 Fe1 113.27(11) . . ?
Sb1 O2 Fe1 127.73(11) 2 . ?
Sb1 O3 Sb2 115.19(11) . . ?
Sb1 O3 Fe1 135.07(12) . 4_566 ?
Sb2 O3 Fe1 109.61(10) . 4_566 ?
Sb2 O4 Sb1 96.45(10) . . ?
Sb2 O4 Fe1 95.98(9) . . ?
Sb1 O4 Fe1 93.42(9) . . ?

_refine_diff_density_max         0.879
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.165

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1504605'
_audit_update_record             
;
2016-09-15 deposited with the CCDC.
2016-10-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_a                   
;
PROBLEM: Short Inter D...A Contact  O2     ..  O2      ..       2.52 Ang.
RESPONSE: The O-O distance falling around 2.5 Ang. is normal in antimony oxide compounds, such as in Sb2O3 and SbO2.
;
_vrf_PLAT430_a_2                 
;
PROBLEM: Short Inter D...A Contact  O3     ..  O3      ..       2.57 Ang.
RESPONSE: The O-O distance falling around 2.5 Ang. is normal in antimony oxide compounds, such as in Sb2O3 and SbO2.
;
# Added during the CSD deposition process: Friday 16 September 2016 12:13 AM
# end Validation Reply Form


_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            'Cl Co H O4 Sb2'
_chemical_formula_weight         402.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.910(2)
_cell_length_b                   8.115(3)
_cell_length_c                   20.458(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.024(5)
_cell_angle_gamma                90
_cell_volume                     1140.9(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3064
_cell_measurement_theta_min      2.5100
_cell_measurement_theta_max      27.5360

_exptl_crystal_description       plate-shaped
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.691
_exptl_crystal_F_000             1432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    12.663
_shelx_estimated_absorpt_T_min   0.115
_shelx_estimated_absorpt_T_max   0.364
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6664
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Mercury70 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8502
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.702
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2599
_reflns_number_gt                2263
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0320P)²+0.0050P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2599
_refine_ls_number_parameters     153
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0204
_refine_ls_wR_factor_ref         0.0544
_refine_ls_wR_factor_gt          0.0520
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.22111(4) 0.53257(3) 0.26606(2) 0.01064(8) Uani 1 1 d . . . . .
Sb2 Sb 0.22408(4) 0.04281(3) 0.01478(2) 0.01152(8) Uani 1 1 d . . . . .
Sb3 Sb 0.23504(4) 0.45853(3) 0.00820(2) 0.01058(8) Uani 1 1 d . . . . .
Sb4 Sb 0.23722(3) 0.11751(3) 0.25620(2) 0.01105(8) Uani 1 1 d . . . . .
Co1 Co 0.00862(8) 0.32859(6) 0.13173(2) 0.01065(12) Uani 1 1 d . . . . .
Co2 Co 0.00936(8) 0.24708(6) 0.38138(2) 0.01132(13) Uani 1 1 d . . . . .
Cl1 Cl 0.66516(15) 0.28428(14) 0.34943(5) 0.0232(2) Uani 1 1 d . . . . .
Cl2 Cl 0.66138(15) 0.28672(15) 0.10015(5) 0.0246(2) Uani 1 1 d . . . . .
O1 O 0.0024(4) 0.0216(3) 0.30571(12) 0.0129(6) Uani 1 1 d . . . . .
O2 O 0.0042(4) 0.4374(3) 0.44384(13) 0.0136(6) Uani 1 1 d . . . . .
O3 O 0.0045(4) 0.0444(3) 0.43994(12) 0.0113(5) Uani 1 1 d . . . . .
O4 O 0.0079(4) 0.1281(3) 0.18942(12) 0.0121(6) Uani 1 1 d . . . . .
O5 O 0.1590(4) 0.2553(3) 0.05518(12) 0.0123(6) Uani 1 1 d . . . . .
O6 O 0.1602(4) 0.3163(3) 0.30558(12) 0.0125(6) Uani 1 1 d . . . . .
O7 O 0.3063(4) 0.3262(4) 0.19443(13) 0.0157(6) Uani 1 1 d D . . . .
O8 O 0.3082(4) 0.2398(4) 0.44448(13) 0.0157(6) Uani 1 1 d D . . . .
H1 H 0.408(5) 0.218(7) 0.430(2) 0.039(17) Uiso 1 1 d D . . . .
H2 H 0.400(7) 0.351(8) 0.176(3) 0.08(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 O6 1.996(3) . ?
Sb1 O1 2.018(3) 2 ?
Sb1 O4 2.059(3) 2 ?
Sb1 O7 2.341(3) . ?
Sb1 Sb4 3.2266(10) 2 ?
Sb2 O5 1.984(3) . ?
Sb2 O2 1.995(3) 4_565 ?
Sb2 O2 2.054(3) 2_545 ?
Sb2 O8 2.386(3) 4_565 ?
Sb2 Sb2 3.1696(11) 3 ?
Sb3 O3 2.005(3) 4_565 ?
Sb3 O5 2.006(3) . ?
Sb3 O8 2.164(3) 4_565 ?
Sb3 O3 2.173(3) 2 ?
Sb3 Sb3 3.2997(11) 3_565 ?
Sb4 O4 1.982(3) . ?
Sb4 O6 2.005(3) . ?
Sb4 O1 2.147(3) . ?
Sb4 O7 2.196(3) . ?
Sb4 Sb1 3.2265(10) 2_545 ?
Co1 O4 2.010(3) . ?
Co1 O1 2.029(3) 2 ?
Co1 O5 2.056(3) . ?
Co1 O3 2.279(3) 2 ?
Co1 O7 2.307(3) . ?
Co1 Cl2 2.4423(14) 1_455 ?
Co2 O2 2.007(3) . ?
Co2 O6 2.036(3) . ?
Co2 O3 2.037(3) . ?
Co2 O8 2.318(3) . ?
Co2 O1 2.394(3) . ?
Co2 Cl1 2.4185(14) 1_455 ?
Cl1 Co2 2.4185(14) 1_655 ?
Cl2 Co1 2.4423(14) 1_655 ?
O1 Sb1 2.018(3) 2_545 ?
O1 Co1 2.029(3) 2_545 ?
O2 Sb2 1.995(3) 4_566 ?
O2 Sb2 2.054(3) 2 ?
O3 Sb3 2.005(3) 4_566 ?
O3 Sb3 2.173(3) 2_545 ?
O3 Co1 2.279(3) 2_545 ?
O4 Sb1 2.059(3) 2_545 ?
O8 Sb3 2.164(3) 4_566 ?
O8 Sb2 2.386(3) 4_566 ?

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
O6 Sb1 O1 94.48(11) . 2 ?
O6 Sb1 O4 86.97(11) . 2 ?
O1 Sb1 O4 76.89(10) 2 2 ?
O6 Sb1 O7 72.67(11) . . ?
O1 Sb1 O7 74.73(10) 2 . ?
O4 Sb1 O7 143.31(10) 2 . ?
O6 Sb1 Sb4 89.96(8) . 2 ?
O1 Sb1 Sb4 40.69(7) 2 2 ?
O4 Sb1 Sb4 36.21(7) 2 2 ?
O7 Sb1 Sb4 111.84(7) . 2 ?
O5 Sb2 O2 92.54(11) . 4_565 ?
O5 Sb2 O2 88.44(11) . 2_545 ?
O2 Sb2 O2 76.94(12) 4_565 2_545 ?
O5 Sb2 O8 71.87(10) . 4_565 ?
O2 Sb2 O8 73.56(10) 4_565 4_565 ?
O2 Sb2 O8 143.39(11) 2_545 4_565 ?
O5 Sb2 Sb2 90.59(8) . 3 ?
O2 Sb2 Sb2 39.14(7) 4_565 3 ?
O2 Sb2 Sb2 37.81(7) 2_545 3 ?
O8 Sb2 Sb2 110.00(7) 4_565 3 ?
O3 Sb3 O5 95.46(11) 4_565 . ?
O3 Sb3 O8 77.91(11) 4_565 4_565 ?
O5 Sb3 O8 76.52(10) . 4_565 ?
O3 Sb3 O3 75.73(11) 4_565 2 ?
O5 Sb3 O3 77.18(10) . 2 ?
O8 Sb3 O3 140.42(10) 4_565 2 ?
O3 Sb3 Sb3 39.65(7) 4_565 3_565 ?
O5 Sb3 Sb3 84.94(8) . 3_565 ?
O8 Sb3 Sb3 112.35(8) 4_565 3_565 ?
O3 Sb3 Sb3 36.08(7) 2 3_565 ?
O4 Sb4 O6 94.43(11) . . ?
O4 Sb4 O1 75.63(10) . . ?
O6 Sb4 O1 78.47(10) . . ?
O4 Sb4 O7 77.07(11) . . ?
O6 Sb4 O7 75.79(11) . . ?
O1 Sb4 O7 140.52(11) . . ?
O4 Sb4 Sb1 37.84(7) . 2_545 ?
O6 Sb4 Sb1 86.24(8) . 2_545 ?
O1 Sb4 Sb1 37.80(7) . 2_545 ?
O7 Sb4 Sb1 110.67(8) . 2_545 ?
O4 Co1 O1 104.59(11) . 2 ?
O4 Co1 O5 104.22(11) . . ?
O1 Co1 O5 139.38(11) 2 . ?
O4 Co1 O3 175.51(10) . 2 ?
O1 Co1 O3 79.11(11) 2 2 ?
O5 Co1 O3 73.83(10) . 2 ?
O4 Co1 O7 73.96(10) . . ?
O1 Co1 O7 75.29(10) 2 . ?
O5 Co1 O7 85.92(11) . . ?
O3 Co1 O7 109.70(10) 2 . ?
O4 Co1 Cl2 88.85(8) . 1_455 ?
O1 Co1 Cl2 99.98(8) 2 1_455 ?
O5 Co1 Cl2 108.62(9) . 1_455 ?
O3 Co1 Cl2 87.99(7) 2 1_455 ?
O7 Co1 Cl2 160.01(8) . 1_455 ?
O2 Co2 O6 108.50(11) . . ?
O2 Co2 O3 104.15(11) . . ?
O6 Co2 O3 135.38(11) . . ?
O2 Co2 O8 74.89(10) . . ?
O6 Co2 O8 86.21(11) . . ?
O3 Co2 O8 73.77(10) . . ?
O2 Co2 O1 177.80(10) . . ?
O6 Co2 O1 72.27(10) . . ?
O3 Co2 O1 76.27(10) . . ?
O8 Co2 O1 107.27(10) . . ?
O2 Co2 Cl1 89.62(8) . 1_455 ?
O6 Co2 Cl1 109.10(9) . 1_455 ?
O3 Co2 Cl1 100.57(8) . 1_455 ?
O8 Co2 Cl1 161.26(7) . 1_455 ?
O1 Co2 Cl1 88.17(7) . 1_455 ?
Sb1 O1 Co1 114.60(13) 2_545 2_545 ?
Sb1 O1 Sb4 101.50(11) 2_545 . ?
Co1 O1 Sb4 131.11(13) 2_545 . ?
Sb1 O1 Co2 113.50(12) 2_545 . ?
Co1 O1 Co2 100.46(11) 2_545 . ?
Sb4 O1 Co2 93.63(10) . . ?
Sb2 O2 Co2 117.53(13) 4_566 . ?
Sb2 O2 Sb2 103.06(12) 4_566 2 ?
Co2 O2 Sb2 130.44(14) . 2 ?
Sb3 O3 Co2 110.99(12) 4_566 . ?
Sb3 O3 Sb3 104.26(11) 4_566 2_545 ?
Co2 O3 Sb3 127.32(13) . 2_545 ?
Sb3 O3 Co1 114.47(12) 4_566 2_545 ?
Co2 O3 Co1 104.12(11) . 2_545 ?
Sb3 O3 Co1 94.98(10) 2_545 2_545 ?
Sb4 O4 Co1 112.87(13) . . ?
Sb4 O4 Sb1 105.95(11) . 2_545 ?
Co1 O4 Sb1 127.86(14) . 2_545 ?
Sb2 O5 Sb3 115.63(12) . . ?
Sb2 O5 Co1 136.34(13) . . ?
Sb3 O5 Co1 107.81(12) . . ?
Sb1 O6 Sb4 115.15(12) . . ?
Sb1 O6 Co2 134.25(13) . . ?
Sb4 O6 Co2 110.24(12) . . ?
Sb4 O7 Co1 95.24(11) . . ?
Sb4 O7 Sb1 96.16(11) . . ?
Co1 O7 Sb1 94.25(11) . . ?
Sb3 O8 Co2 95.95(11) 4_566 . ?
Sb3 O8 Sb2 95.71(10) 4_566 4_566 ?
Co2 O8 Sb2 93.31(10) . 4_566 ?

_refine_diff_density_max         0.852
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.230

