# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ca9.83(SiO4)3(SO4)3Cl1.65
#============================================================================
_chemical_name_systematic        
;
ellestadite
;
_chemical_name_common            ellestadite
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca9.82 Cl1.64 O24 S3 Si3'
_chemical_formula_weight         1017.57

loop_
_atom_type_symbol
_atom_type_scat_length_neutron
_atom_type_scat_source
Ca 4.700 International_Tables_Vol_C
Cl 9.577 International_Tables_Vol_C
O 5.803 International_Tables_Vol_C
S 2.847 International_Tables_Vol_C
Si 4.149 International_Tables_Vol_C

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_Int_Tables_number      176

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -x,-y,z+1/2
5 y,-x+y,z+1/2
6 x-y,x,z+1/2
7 -x,-y,-z
8 y,-x+y,-z
9 x-y,x,-z
10 x,y,-z+1/2
11 -y,x-y,-z+1/2
12 -x+y,-x,-z+1/2
_cell_length_a                   9.66912(35)
_cell_length_b                   9.66912(35)
_cell_length_c                   6.85317(30)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     554.875(47)
_cell_formula_units_Z            1
_cell_measurement_temperature    298
_cell_measurement_reflns_used    618



_pd_char_particle_morphology     plate-like

_exptl_crystal_colour            blue
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.04
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             219.81


_pd_spec_mounting                
; packed powder in vanadium can
;
_pd_spec_mount_mode              reflection
_pd_spec_shape                   cylinder

_pd_prep_cool_rate               ?
_pd_prep_pressure                101.325
_pd_prep_temperature             1223

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     1.38994
_diffrn_radiation_type           neutron
_diffrn_radiation_monochromator  Ge
_diffrn_measurement_device_type  'ILL high resolution D1A diffractometer'
_diffrn_detector                 'He~3~ detector'
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       9
_pd_meas_scan_method             fixed


_pd_meas_number_of_points        3667
_pd_meas_2theta_range_min        0
_pd_meas_2theta_range_max        150
_pd_meas_2theta_range_inc        0.05

_pd_proc_ls_prof_R_factor        0.040
_pd_proc_ls_prof_wR_factor       0.052
_refine_ls_goodness_of_fit_all   0.77
_refine_ls_R_I_factor            0.032
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_number_parameters     33
_refine_ls_number_restraints     1
_refine_ls_number_constraints    3
_pd_proc_2theta_range_min        10
_pd_proc_2theta_range_max        150
_pd_proc_wavelength              1.38994
_pd_proc_info_excluded_regions   
'0.0 to 10 degrees unreliable due to background'

_computing_data_collection       ?
_computing_cell_refinement       'TOPAS (Bruker, 2005)'
_computing_data_reduction        ?
_computing_structure_solution    'TOPAS (Bruker, 2005)'
_computing_structure_refinement  'TOPAS (Bruker, 2005)'
_computing_molecular_graphics    'Diamond 3.2 (K. Brandenburg, 2011)'
_computing_publication_material  'TOPAS (Bruker, 2005)'

_refine_special_details          
;
The mole ratio of Si:S at the tetrahedral site was fixed at 1:1.
The cooupancies of Ca1 and Ca2 were jointly refined together with Cl.
Isotropic temperature displacement parameters for all atoms were refined in 
Ca1/Ca2/Cl and Si/S/O1/O2/O3 groups to the same value.
;



loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Ca1 Ca 4 f 0.3333333 0.6666667 -0.0022(10) 0.9837(81) 2.047(59)
Ca2 Ca 6 h 0.26004(70) -0.00046(82) 0.25 0.9830(53) 2.047(59)
Si1 Si 6 h 0.40307(42) 0.37287(41) 0.25 0.5 2.200(36)
S1 S 6 h 0.40307(42) 0.37287(41) 0.25 0.5 2.200(36)
O1 O 6 h 0.33619(36) 0.48802(35) 0.25 1 2.200(36)
O2 O 6 h 0.58863(39) 0.46724(52) 0.25 1 2.200(36)
O3 O 12 i 0.35383(37) 0.26655(33) 0.06546(36) 1 2.200(36)
Cl1 Cl 4 e 0 0 0.4249(10) 0.416(23) 2.047(59)


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.453(5) .
Ca1 O1 2.453(5) 2_665
Ca1 O1 2.453(5) 3_565
Ca1 O2 2.471(6) 4_664
Ca1 O2 2.471(6) 5_564
Ca1 O2 2.471(6) 6_554
Ca1 O3 2.793(4) 7_665
Ca1 O3 2.793(4) 8_565
Ca1 O3 2.793(4) 9_555
Ca2 O2 2.288(7) 2_655
Ca2 O3 2.597(7) .
Ca2 O3 2.331(4) 5_555
Ca2 O3 2.331(4) 8_555
Ca2 O3 2.597(7) 10_555
S1 O1 1.542(6) .
S1 O2 1.553(4) .
S1 O3 1.547(3) .
S1 O3 1.547(3) 10_555
Si1 O1 1.542(6) .
Si1 O2 1.553(4) .
Si1 O3 1.547(3) .
Si1 O3 1.547(3) 10_555
Cl1 Ca2 2.787(7) .
Cl1 Ca2 2.787(7) 2_555
Cl1 Ca2 2.787(7) 3_555

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
O1 S1 O2 110.7(2) . .
O1 S1 O3 112.3(2) . .
O2 S1 O3 105.7(2) . .
O3 S1 O3 109.6(2) . 10_555
O1 Si1 O2 110.7(2) . .
O1 Si1 O3 112.3(2) . .
O2 Si1 O3 105.7(2) . .
O3 Si1 O3 109.6(2) . 10_555
_database_code_depnum_ccdc_archive 'CCDC 996152'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ca9.84(SiO4)2.4(PO4)1.2(SO4)2.4Cl1.67
#============================================================================
_chemical_name_systematic        
;
ellestadite
;
_chemical_name_common            ellestadite
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca9.84 Cl1.67 O24 P1.2 S2.4 Si2.4'
_chemical_formula_weight         1018.95


loop_
_atom_type_symbol
_atom_type_scat_length_neutron
_atom_type_scat_source
Ca 4.700 International_Tables_Vol_C
Cl 9.577 International_Tables_Vol_C
P 5.130 International_Tables_Vol_C
O 5.803 International_Tables_Vol_C
S 2.847 International_Tables_Vol_C
Si 4.149 International_Tables_Vol_C

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_Int_Tables_number      176

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -x,-y,z+1/2
5 y,-x+y,z+1/2
6 x-y,x,z+1/2
7 -x,-y,-z
8 y,-x+y,-z
9 x-y,x,-z
10 x,y,-z+1/2
11 -y,x-y,-z+1/2
12 -x+y,-x,-z+1/2
_cell_length_a                   9.6622(3)
_cell_length_b                   9.6622(3)
_cell_length_c                   6.8438(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     553.32(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    298
_cell_measurement_reflns_used    590


_exptl_crystal_colour            blue
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             222.49


_pd_spec_mounting                
; packed powder in vanadium can
;
_pd_spec_mount_mode              reflection
_pd_spec_shape                   cylinder

_pd_prep_cool_rate               ?
_pd_prep_pressure                101.325
_pd_prep_temperature             1223

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     1.38994
_diffrn_radiation_type           neutron
_diffrn_radiation_monochromator  Ge
_diffrn_measurement_device_type  'ILL high resolution D1A diffractometer'
_diffrn_detector                 '3He detector'
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       9
_pd_meas_scan_method             fixed


_pd_meas_number_of_points        3667
_pd_meas_2theta_range_min        0
_pd_meas_2theta_range_max        150
_pd_meas_2theta_range_inc        0.05

_pd_proc_ls_prof_R_factor        0.036
_pd_proc_ls_prof_wR_factor       0.047
_refine_ls_goodness_of_fit_all   0.59
_refine_ls_R_I_factor            0.028
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_number_parameters     33
_refine_ls_number_restraints     1
_refine_ls_number_constraints    3
_pd_proc_2theta_range_min        10
_pd_proc_2theta_range_max        150
_pd_proc_wavelength              1.38994
_pd_proc_info_excluded_regions   
'0.0 to 10 degrees unreliable due to background'

_computing_data_collection       ?
_computing_cell_refinement       'TOPAS (Bruker, 2005)'
_computing_data_reduction        ?
_computing_structure_solution    'TOPAS (Bruker, 2005)'
_computing_structure_refinement  'TOPAS (Bruker, 2005)'
_computing_molecular_graphics    'Diamond 3.2 (K. Brandenburg, 2011)'
_computing_publication_material  'TOPAS (Bruker, 2005)'

_refine_special_details          
;
The mole ratio of Si:S at the tetrahedral site was fixed at 1:1.
The totel ocupancies of Si, P and S at the tetrahedral site was fixed to 1.
The cooupancies of Ca1 and Ca2 were jointly refined together with Cl.
Isotropic temperature displacement parameters for all atoms were refined in 
Ca1/Ca2/Cl and Si/S/P/O1/O2/O3 groups to the same value.
;



loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Ca1 Ca 4 f 0.3333333 0.6666667 -0.00275(89) 0.9958(69) 1.909(49)
Ca2 Ca 6 h 0.25959(61) -0.00089(71) 0.25 0.9754(44) 1.909(49)
S1 S 6 h 0.40440(34) 0.37397(33) 0.25 0.399(12) 2.147(31)
Si1 Si 6 h 0.40440(34) 0.37397(33) 0.25 0.399(12) 2.147(31)
P1 P 6 h 0.40440(34) 0.37397(33) 0.25 0.202(25) 2.147(31)
O1 O 6 h 0.33793(33) 0.48938(32) 0.25 1 2.147(31)
O2 O 6 h 0.58954(36) 0.46753(46) 0.25 1 2.147(31)
O3 O 12 i 0.35353(32) 0.26670(26) 0.06674(31) 1 2.147(31)
Cl1 Cl 4 e 0 0 0.42900(88) 0.418(19) 1.909(49)



loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.450(2) .
Ca1 O1 2.450(2) 2_665
Ca1 O1 2.450(2) 3_565
Ca1 O2 2.463(5) 4_664
Ca1 O2 2.463(5) 5_564
Ca1 O2 2.463(5) 6_554
Ca1 O3 2.795(3) 7_665
Ca1 O3 2.795(3) 8_565
Ca1 O3 2.795(3) 9_555
Ca2 O2 2.287(4) 2_655
Ca2 O3 2.595(6) .
Ca2 O3 2.335(4) 5_555
Ca2 O3 2.335(4) 8_555
Ca2 O3 2.595(6) 10_555
S1 O1 1.540(5) .
S1 O2 1.549(4) .
S1 O3 1.542(3) .
S1 O3 1.542(3) 10_555
Si1 O1 1.540(5) .
Si1 O2 1.549(4) .
Si1 O3 1.542(3) .
Si1 O3 1.542(3) 10_555
P1 O1 1.540(5) .
P1 O2 1.549(4) .
P1 O3 1.542(3) .
P1 O3 1.542(3) 10_555
Cl1 Ca2 2.795(7) .
Cl1 Ca2 2.795(7) 2_555
Cl1 Ca2 2.795(7) 3_555

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
O1 S1 O2 110.8(2) . .
O1 S1 O3 112.2(2) . .
O2 S1 O3 106.2(2) . .
O3 S1 O3 108.8(2) . 10_555
O1 Si1 O2 110.8(2) . .
O1 Si1 O3 112.2(2) . .
O2 Si1 O3 106.2(2) . .
O3 Si1 O3 108.8(2) . 10_555
O1 P1 O2 110.8(2) . .
O1 P1 O3 112.2(2) . .
O2 P1 O3 106.2(2) . .
O3 P1 O3 108.8(2) . 10_555
_database_code_depnum_ccdc_archive 'CCDC 996153'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ca9.84(SiO4)2.03(PO4)1.94(SO4)2.03Cl1.68
#============================================================================
_chemical_name_systematic        
;
ellestadite
;
_chemical_name_common            ellestadite
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca9.84 Cl1.68 O24 P1.94 S2.03 Si2.03'
_chemical_formula_weight         1019.9

loop_
_atom_type_symbol
_atom_type_scat_length_neutron
_atom_type_scat_source
Ca 4.700 International_Tables_Vol_C
Cl 9.577 International_Tables_Vol_C
P 5.130 International_Tables_Vol_C
O 5.803 International_Tables_Vol_C
S 2.847 International_Tables_Vol_C
Si 4.149 International_Tables_Vol_C

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_Int_Tables_number      176

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -x,-y,z+1/2
5 y,-x+y,z+1/2
6 x-y,x,z+1/2
7 -x,-y,-z
8 y,-x+y,-z
9 x-y,x,-z
10 x,y,-z+1/2
11 -y,x-y,-z+1/2
12 -x+y,-x,-z+1/2
_cell_length_a                   9.65368(50)
_cell_length_b                   9.65368(50)
_cell_length_c                   6.83542(42)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     551.673(67)
_cell_formula_units_Z            1
_cell_measurement_temperature    298
_cell_measurement_reflns_used    617


_exptl_crystal_colour            blue
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             225.12


_pd_spec_mounting                
; packed powder in vanadium can
;
_pd_spec_mount_mode              reflection
_pd_spec_shape                   cylinder

_pd_prep_cool_rate               ?
_pd_prep_pressure                101.325
_pd_prep_temperature             1223

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     1.38994
_diffrn_radiation_type           neutron
_diffrn_radiation_monochromator  Ge
_diffrn_measurement_device_type  'ILL high resolution D1A diffractometer'
_diffrn_detector                 'He~3~ detector'
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       9
_pd_meas_scan_method             fixed


_pd_meas_number_of_points        3667
_pd_meas_2theta_range_min        0
_pd_meas_2theta_range_max        150
_pd_meas_2theta_range_inc        0.05

_pd_proc_ls_prof_R_factor        0.037
_pd_proc_ls_prof_wR_factor       0.048
_refine_ls_goodness_of_fit_all   0.64
_refine_ls_R_I_factor            0.022
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_number_parameters     33
_refine_ls_number_restraints     1
_refine_ls_number_constraints    3
_pd_proc_2theta_range_min        10
_pd_proc_2theta_range_max        150
_pd_proc_wavelength              1.38994
_pd_proc_info_excluded_regions   
'0.0 to 10 degrees unreliable due to background'

_computing_data_collection       ?
_computing_cell_refinement       'TOPAS (Bruker, 2005)'
_computing_data_reduction        ?
_computing_structure_solution    'TOPAS (Bruker, 2005)'
_computing_structure_refinement  'TOPAS (Bruker, 2005)'
_computing_molecular_graphics    'Diamond 3.2 (K. Brandenburg, 2011)'
_computing_publication_material  'TOPAS (Bruker, 2005)'

_refine_special_details          
;
The mole ratio of Si:S at the tetrahedral site was fixed at 1:1.
The totel ocupancies of Si, P and S at the tetrahedral site was fixed to 1.
The cooupancies of Ca1 and Ca2 were jointly refined together with Cl.
Isotropic temperature displacement parameters for all atoms were refined in 
Ca1/Ca2/Cl and Si/S/P/O1/O2/O3 groups to the same value.
;



loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Ca1 Ca 4 f 0.3333333 0.6666667 -0.0028(10) 0.9952(74) 1.611(54)
Ca2 Ca 6 h 0.26023(68) 0.00046(81) 0.25 0.9753(48) 1.611(54)
S1 S 6 h 0.40537(35) 0.37460(35) 0.25 0.338(13) 1.877(34)
Si1 Si 6 h 0.40537(35) 0.37460(35) 0.25 0.338(13) 1.877(34)
P1 P 6 h 0.40537(35) 0.37460(35) 0.25 0.323(27) 1.877(34)
O1 O 6 h 0.33902(36) 0.48982(35) 0.25 1 1.877(34)
O2 O 6 h 0.59033(40) 0.46873(52) 0.25 1 1.877(34)
O3 O 12 i 0.35348(36) 0.26684(30) 0.06771(34) 1 1.877(34)
Cl1 Cl 4 e 0 0 0.4308(10) 0.42(2) 1.611(54)


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.449(5) .
Ca1 O1 2.449(5) 2_665
Ca1 O1 2.449(5) 3_565
Ca1 O2 2.464(6) 4_664
Ca1 O2 2.464(6) 5_564
Ca1 O2 2.464(6) 6_554
Ca1 O3 2.794(4) 7_665
Ca1 O3 2.794(4) 8_565
Ca1 O3 2.794(4) 9_555
Ca2 O2 2.270(7) 2_655
Ca2 O3 2.581(3) .
Ca2 O3 2.341(3) 5_555
Ca2 O3 2.341(3) 8_555
Ca2 O3 2.581(3) 10_555
S1 O1 1.536(5) .
S1 O2 1.546(4) .
S1 O3 1.538(2) .
S1 O3 1.538(2) 10_555
Si1 O1 1.536(5) .
Si1 O2 1.546(4) .
Si1 O3 1.538(2) .
Si1 O3 1.538(2) 10_555
P1 O1 1.536(5) .
P1 O2 1.546(4) .
P1 O3 1.538(2) .
P1 O3 1.538(2) 10_555
Cl1 Ca2 2.798(6) .
Cl1 Ca2 2.798(6) 2_555
Cl1 Ca2 2.798(6) 3_555

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
O1 S1 O2 110.6(9) . .
O1 S1 O3 112.1(2) . .
O2 S1 O3 106.7(2) . .
O3 S1 O3 108.2(2) . 10_555
O1 Si1 O2 110.6(9) . .
O1 Si1 O3 112.1(2) . .
O2 Si1 O3 106.7(2) . .
O3 Si1 O3 108.2(2) . 10_555
O1 P1 O2 110.6(9) . .
O1 P1 O3 112.1(2) . .
O2 P1 O3 106.7(2) . .
O3 P1 O3 108.2(2) . 10_555
_database_code_depnum_ccdc_archive 'CCDC 996154'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ca10(SiO4)0.66(PO4)4.67(SO4)0.66Cl2
#============================================================================
_chemical_name_systematic        
;
ellestadite
;
_chemical_name_common            ellestadite
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca10 Cl2 O24 P4.67 S0.66 Si0.66'
_chemical_formula_weight         1040.31

loop_
_atom_type_symbol
_atom_type_scat_length_neutron
_atom_type_scat_source
Ca 4.700 International_Tables_Vol_C
Cl 9.577 International_Tables_Vol_C
P 5.130 International_Tables_Vol_C
O 5.803 International_Tables_Vol_C
S 2.847 International_Tables_Vol_C
Si 4.149 International_Tables_Vol_C

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_Int_Tables_number      176

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -x,-y,z+1/2
5 y,-x+y,z+1/2
6 x-y,x,z+1/2
7 -x,-y,-z
8 y,-x+y,-z
9 x-y,x,-z
10 x,y,-z+1/2
11 -y,x-y,-z+1/2
12 -x+y,-x,-z+1/2
_cell_length_a                   9.62574(39)
_cell_length_b                   9.62574(39)
_cell_length_c                   6.78918(36)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     544.773(53)
_cell_formula_units_Z            1
_cell_measurement_temperature    298
_cell_measurement_reflns_used    585


_exptl_crystal_colour            blue
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.17
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             229.128


_pd_spec_mounting                
; packed powder in vanadium can
;
_pd_spec_mount_mode              reflection
_pd_spec_shape                   cylinder

_pd_prep_cool_rate               ?
_pd_prep_pressure                101.325
_pd_prep_temperature             1223

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     1.38994
_diffrn_radiation_type           neutron
_diffrn_radiation_monochromator  Ge
_diffrn_measurement_device_type  'ILL high resolution D1A diffractometer'
_diffrn_detector                 '3He detector'
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       9
_pd_meas_scan_method             fixed


_pd_meas_number_of_points        3667
_pd_meas_2theta_range_min        0
_pd_meas_2theta_range_max        150
_pd_meas_2theta_range_inc        0.05

_pd_proc_ls_prof_R_factor        0.046
_pd_proc_ls_prof_wR_factor       0.059
_refine_ls_goodness_of_fit_all   0.77
_refine_ls_R_I_factor            0.021
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_number_parameters     33
_refine_ls_number_restraints     1
_refine_ls_number_constraints    4
_pd_proc_2theta_range_min        10
_pd_proc_2theta_range_max        150
_pd_proc_wavelength              1.38994
_pd_proc_info_excluded_regions   
'0.0 to 10 degrees unreliable due to background'

_computing_data_collection       ?
_computing_cell_refinement       'TOPAS (Bruker, 2005)'
_computing_data_reduction        ?
_computing_structure_solution    'TOPAS (Bruker, 2005)'
_computing_structure_refinement  'TOPAS (Bruker, 2005)'
_computing_molecular_graphics    'Diamond 3.2 (K. Brandenburg, 2011)'
_computing_publication_material  'TOPAS (Bruker, 2005)'

_refine_special_details          
;
The mole ratio of Si:S at the tetrahedral site was fixed at 1:1.
The total occupancies of Si, P and S at the tetrahedral site was fixed to 1.
The total occupancies of Cl1 and Cl2 was fixed to 0.5.
Isotropic temperature displacement parameters for all atoms were refined in 
Ca1/Ca2/Cl and Si/S/O1/O2/O3 groups to the same value.
;



loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Ca1 Ca 4 f 0.3333333 0.6666667 0.0018(11) 1 1.023(50)
Ca2 Ca 6 h 0.25839(68) 0.00241(77) 0.25 1 1.023(50)
S1 S 6 h 0.40712(33) 0.37503(31) 0.25 0.111(16) 1.023(50)
Si1 Si 6 h 0.40712(33) 0.37503(31) 0.25 0.111(16) 1.023(50)
P1 P 6 h 0.40712(33) 0.37503(31) 0.25 0.778(32) 1.023(50)
O1 O 6 h 0.34159(37) 0.49183(36) 0.25 1 1.126(30)
O2 O 6 h 0.59194(38) 0.46695(52) 0.25 1 1.126(30)
O3 O 12 i 0.35141(36) 0.26638(31) 0.06714(36) 1 1.126(30)
Cl1 Cl 4 e 0 0 0.4388(13) 0.4039(84) 1.023(50)
Cl2 Cl 4 e 0 0 0.1545(60) 0.0961(84) 1.023(50)


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.411(5) .
Ca1 O1 2.411(5) 2_665
Ca1 O1 2.411(5) 3_565
Ca1 O2 2.459(6) 4_664
Ca1 O2 2.459(6) 5_564
Ca1 O2 2.459(6) 6_554
Ca1 O3 2.808(4) 7_665
Ca1 O3 2.808(4) 8_565
Ca1 O3 2.808(4) 9_555
Ca2 O2 2.294(7) 2_655
Ca2 O3 2.554(3) .
Ca2 O3 2.327(3) 5_555
Ca2 O3 2.327(3) 8_555
Ca2 O3 2.554(3) 10_555
S1 O1 1.540(5) .
S1 O2 1.541(4) .
S1 O3 1.537(3) .
S1 O3 1.537(3) 10_555
Si1 O1 1.540(5) .
Si1 O2 1.541(4) .
Si1 O3 1.537(3) .
Si1 O3 1.537(3) 10_555
P1 O1 1.540(5) .
P1 O2 1.541(4) .
P1 O3 1.537(3) .
P1 O3 1.537(3) 10_555
Cl1 Ca2 2.788(7) .
Cl1 Ca2 2.788(7) 2_555
Cl1 Ca2 2.788(7) 3_555
Cl2 Ca2 2.56(1) .
Cl2 Ca2 2.56(1) 2_555
Cl2 Ca2 2.56(1) 3_555

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
O1 S1 O2 110.9(3) . .
O1 S1 O3 111.5(2) . .
O2 S1 O3 107.5(2) . .
O3 S1 O3 107.7(2) . 10_555
O1 Si1 O2 110.9(3) . .
O1 Si1 O3 111.5(2) . .
O2 Si1 O3 107.5(2) . .
O3 Si1 O3 107.7(2) . 10_555
O1 P1 O2 110.9(3) . .
O1 P1 O3 111.5(2) . .
O2 P1 O3 107.5(2) . .
O3 P1 O3 107.7(2) . 10_555
_database_code_depnum_ccdc_archive 'CCDC 996155'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ca10(SiO4)0.27(PO4)5.46(SO4)0.27Cl2
#============================================================================
_chemical_name_systematic        
;
ellestadite
;
_chemical_name_common            ellestadite
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca10 Cl2 O24 P5.46 S0.27 Si0.27'
_chemical_formula_weight         1041.02

loop_
_atom_type_symbol
_atom_type_scat_length_neutron
_atom_type_scat_source
Ca 4.700 International_Tables_Vol_C
Cl 9.577 International_Tables_Vol_C
P 5.130 International_Tables_Vol_C
O 5.803 International_Tables_Vol_C
S 2.847 International_Tables_Vol_C
Si 4.149 International_Tables_Vol_C

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_Int_Tables_number      176

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -x,-y,z+1/2
5 y,-x+y,z+1/2
6 x-y,x,z+1/2
7 -x,-y,-z
8 y,-x+y,-z
9 x-y,x,-z
10 x,y,-z+1/2
11 -y,x-y,-z+1/2
12 -x+y,-x,-z+1/2
_cell_length_a                   9.62986(22)
_cell_length_b                   9.62986(22)
_cell_length_c                   6.78332(21)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     544.770(30)
_cell_formula_units_Z            1
_cell_measurement_temperature    298
_cell_measurement_reflns_used    584


_exptl_crystal_colour            blue
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.17
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             229.02

_pd_spec_mounting                
; packed powder in vanadium can
;
_pd_spec_mount_mode              reflection
_pd_spec_shape                   cylinder

_pd_prep_cool_rate               ?
_pd_prep_pressure                101.325
_pd_prep_temperature             1223

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     1.38994
_diffrn_radiation_type           neutron
_diffrn_radiation_monochromator  Ge
_diffrn_measurement_device_type  'ILL high resolution D1A diffractometer'
_diffrn_detector                 '3He detector'
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       9
_pd_meas_scan_method             fixed


_pd_meas_number_of_points        3667
_pd_meas_2theta_range_min        0
_pd_meas_2theta_range_max        150
_pd_meas_2theta_range_inc        0.05

_pd_proc_ls_prof_R_factor        0.040
_pd_proc_ls_prof_wR_factor       0.052
_refine_ls_goodness_of_fit_all   0.67
_refine_ls_R_I_factor            0.022
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_number_parameters     33
_refine_ls_number_restraints     1
_refine_ls_number_constraints    3
_pd_proc_2theta_range_min        10
_pd_proc_2theta_range_max        150
_pd_proc_wavelength              1.38994
_pd_proc_info_excluded_regions   
'0.0 to 10 degrees unreliable due to background'

_computing_data_collection       ?
_computing_cell_refinement       'TOPAS (Bruker, 2005)'
_computing_data_reduction        ?
_computing_structure_solution    'TOPAS (Bruker, 2005)'
_computing_structure_refinement  'TOPAS (Bruker, 2005)'
_computing_molecular_graphics    'Diamond 3.2 (K. Brandenburg, 2011)'
_computing_publication_material  'TOPAS (Bruker, 2005)'

_refine_special_details          
;
The mole ratio of Si:S at the tetrahedral site was fixed at 1:1.
The totel ocupancies of Si, P and S at the tetrahedral site was fixed to 1.
The total occupancies of Cl1 and Cl2 was fixed to 0.5.
Isotropic temperature displacement parameters for all atoms were refined in 
Ca1/Ca2/Cl and Si/S/P/O1/O2/O3 groups to the same value.
;



loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Ca1 Ca 4 f 0.3333333 0.6666667 0.00124(78) 1 0.895(35)
Ca2 Ca 6 h 0.25861(48) 0.00312(54) 0.25 1 0.895(35)
S1 S 6 h 0.40766(23) 0.37522(24) 0.25 0.045(13) 0.954(21)
Si1 Si 6 h 0.40766(23) 0.37522(24) 0.25 0.045(13) 0.954(21)
P1 P 6 h 0.40766(23) 0.37522(24) 0.25 0.909(25) 0.954(21)
O1 O 6 h 0.34225(26) 0.49167(25) 0.25 1 0.954(21)
O2 O 6 h 0.59247(27) 0.46717(37) 0.25 1 0.954(21)
O3 O 12 i 0.35252(25) 0.26654(22) 0.06717(26) 1 0.954(21)
Cl1 Cl 4 e 0 0 0.44185(89) 0.4107(67) 0.895(35)
Cl2 Cl 4 e 0 0 0.1404(45) 0.0893(67) 0.895(35)


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.416(4) .
Ca1 O1 2.416(4) 2_665
Ca1 O1 2.416(4) 3_565
Ca1 O2 2.449(5) 4_664
Ca1 O2 2.449(5) 5_564
Ca1 O2 2.449(5) 6_554
Ca1 O3 2.800(3) 7_665
Ca1 O3 2.800(3) 8_565
Ca1 O3 2.800(3) 9_555
Ca2 O2 2.291(7) 2_655
Ca2 O3 2.549(5) .
Ca2 O3 2.332(3) 5_555
Ca2 O3 2.332(3) 8_555
Ca2 O3 2.549(5) 10_555
S1 O1 1.536(4) .
S1 O2 1.541(2) .
S1 O3 1.536(2) .
S1 O3 1.536(2) 10_555
Si1 O1 1.536(4) .
Si1 O2 1.541(2) .
Si1 O3 1.536(2) .
Si1 O3 1.536(2) 10_555
P1 O1 1.536(4) .
P1 O2 1.541(2) .
P1 O3 1.536(2) .
P1 O3 1.536(2) 10_555
Cl1 Ca2 2.797(3) .
Cl1 Ca2 2.797(3) 2_555
Cl1 Ca2 2.797(3) 3_555
Cl2 Ca2 2.585(8) .
Cl2 Ca2 2.585(8) 2_555
Cl2 Ca2 2.585(8) 3_555

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
O1 S1 O2 110.9(2) . .
O1 S1 O3 111.6(1) . .
O2 S1 O3 107.3(1) . .
O3 S1 O3 107.7(2) . 10_555
O1 Si1 O2 110.9(2) . .
O1 Si1 O3 111.6(1) . .
O2 Si1 O3 107.3(1) . .
O3 Si1 O3 107.7(2) . 10_555
O1 P1 O2 110.9(2) . .
O1 P1 O3 111.6(1) . .
O2 P1 O3 107.3(1) . .
O3 P1 O3 107.7(2) . 10_555
_database_code_depnum_ccdc_archive 'CCDC 996156'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ca10(PO4)6Cl2
#============================================================================
_chemical_name_systematic        
;
ellestadite
;
_chemical_name_common            apatite
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca10 Cl2 O24 P6'
_chemical_formula_weight         1041.51

loop_
_atom_type_symbol
_atom_type_scat_length_neutron
_atom_type_scat_source
Ca 4.700 International_Tables_Vol_C
Cl 9.577 International_Tables_Vol_C
P 5.130 International_Tables_Vol_C
O 5.803 International_Tables_Vol_C


_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_Int_Tables_number      176

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -x,-y,z+1/2
5 y,-x+y,z+1/2
6 x-y,x,z+1/2
7 -x,-y,-z
8 y,-x+y,-z
9 x-y,x,-z
10 x,y,-z+1/2
11 -y,x-y,-z+1/2
12 -x+y,-x,-z+1/2
_cell_length_a                   9.61822(16)
_cell_length_b                   9.61822(16)
_cell_length_c                   6.79199(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     544.147(21)
_cell_formula_units_Z            1
_cell_measurement_temperature    298
_cell_measurement_reflns_used    582


_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.17
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             229.19


_pd_spec_mounting                
; packed powder in vanadium can
;
_pd_spec_mount_mode              reflection
_pd_spec_shape                   cylinder

_pd_prep_cool_rate               ?
_pd_prep_pressure                101.325
_pd_prep_temperature             1223

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     1.38994
_diffrn_radiation_type           neutron
_diffrn_radiation_monochromator  Ge
_diffrn_measurement_device_type  'ILL high resolution D1A diffractometer'
_diffrn_detector                 '3He detector'
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       9
_pd_meas_scan_method             fixed


_pd_meas_number_of_points        3667
_pd_meas_2theta_range_min        0
_pd_meas_2theta_range_max        150
_pd_meas_2theta_range_inc        0.05

_pd_proc_ls_prof_R_factor        0.044
_pd_proc_ls_prof_wR_factor       0.056
_refine_ls_goodness_of_fit_all   0.69
_refine_ls_R_I_factor            0.029
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_number_parameters     27
_refine_ls_number_restraints     1
_refine_ls_number_constraints    3
_pd_proc_2theta_range_min        10
_pd_proc_2theta_range_max        150
_pd_proc_wavelength              1.38994
_pd_proc_info_excluded_regions   
'0.0 to 10 degrees unreliable due to background'

_computing_data_collection       ?
_computing_cell_refinement       'TOPAS (Bruker, 2005)'
_computing_data_reduction        ?
_computing_structure_solution    'TOPAS (Bruker, 2005)'
_computing_structure_refinement  'TOPAS (Bruker, 2005)'
_computing_molecular_graphics    'Diamond 3.2 (K. Brandenburg, 2011)'
_computing_publication_material  'TOPAS (Bruker, 2005)'

_refine_special_details          
;
The total occupancies of Cl1 and Cl2 was fixed to 0.5.
Isotropic temperature displacement parameters for all atoms were refined in 
Ca1/Ca2/Cl and P/O1/O2/O3 groups to the same value.
;



loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Ca1 Ca 4 f 0.3333333 0.6666667 -0.00093(67) 1 0.876(30)
Ca2 Ca 6 h 0.25819(44) 0.00065(48) 0.25 1 0.876(30)
P1 P 6 h 0.40644(21) 0.37397(20) 0.25 1 1.055(18)
O1 O 6 h 0.34080(24) 0.49066(24) 0.25 1 1.055(18)
O2 O 6 h 0.59133(25) 0.46702(33) 0.25 1 1.055(18)
O3 O 12 i 0.3517(2) 0.2653(2) 0.0674(2) 1.0 1.055(18)
Cl1 Cl 4 e 0 0 0.4342(8) 0.3741(56) 0.876(30)
Cl2 Cl 4 e 0 0 0.153(2) 0.1259(56) 0.876(30)


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.428(4) .
Ca1 O1 2.428(4) 2_665
Ca1 O1 2.428(4) 3_565
Ca1 O2 2.444(4) 4_664
Ca1 O2 2.444(4) 5_564
Ca1 O2 2.444(4) 6_554
Ca1 O3 2.797(2) 7_665
Ca1 O3 2.797(2) 8_565
Ca1 O3 2.797(2) 9_555
Ca2 O2 2.293(4) 2_655
Ca2 O3 2.557(4) .
Ca2 O3 2.326(3) 5_555
Ca2 O3 2.326(3) 8_555
Ca2 O3 2.557(4) 10_555
P1 O1 1.538(4) .
P1 O2 1.540(2) .
P1 O3 1.535(2) .
P1 O3 1.535(2) 10_555
Cl1 Ca2 2.778(5) .
Cl1 Ca2 2.778(5) 2_555
Cl1 Ca2 2.778(5) 3_555
Cl2 Ca2 2.566(5) .
Cl2 Ca2 2.566(5) 2_555
Cl2 Ca2 2.566(5) 3_555

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
O1 P1 O2 110.6(2) . .
O1 P1 O3 111.7(1) . .
O2 P1 O3 107.4(1) . .
O3 P1 O3 107.8(2) . 10_555

#===END
_database_code_depnum_ccdc_archive 'CCDC 996157'
