
data_Apatite_P1

_publ_requested_journal          'American Mineralogist'
_publ_contact_author_name        
'Melinda J. Rucks or Thomas S. Duffy (princeton University)'
_publ_contact_author_address     
;218 Guyot Hall
Princeton University
Princeton, NJ, 08544
;
_publ_contact_author_email       mrucks@princeton.edu
_publ_contact_author_phone       609-258-6769
loop_
_publ_author_name
_publ_author_address
'Melinda J. Rucks or Thomas S. Duffy (princeton University)'
;218 Guyot Hall
Princeton University
Princeton, NJ, 08544
;
'Finkelstein, Gregory J.' ''
'Zhang, Dongzhou' ''
'Dera, Przemyslaw K.' ''
'Duffy, Thomas S.' ''

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_mineral           fluorapatite
_chemical_formula_moiety         '3(O4 P), F, 5(Ca)'
_chemical_formula_sum            'Ca5 F O12 P3'
_chemical_compound_source        'Durango, Mexico'
_chemical_formula_weight         504.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.1055 0.1172
'ShelXle using methods of L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
F F 0.0045 0.0035
'ShelXle using methods of L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O 0.0024 0.0021
'ShelXle using methods of L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
P P 0.0396 0.0346
'ShelXle using methods of L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'

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

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

_cell_length_a                   9.3768(3)
_cell_length_b                   9.3768(3)
_cell_length_c                   6.8755(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     523.53(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    889
_cell_measurement_theta_min      2.3701
_cell_measurement_theta_max      19.3196
_exptl_crystal_recrystallization_method none

_exptl_crystal_description       platlet
_exptl_crystal_colour            colorless
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         540000
_exptl_crystal_density_diffrn    3.199
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.018
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.008
_exptl_absorpt_coefficient_mu    0.759
_shelx_estimated_absorpt_T_min   0.986
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5963
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_process_details   'SADABS-2016/2 (Krause et al., 2015)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.434
_diffrn_source                   
'APS, GSECARS, 13BMC'
_diffrn_measurement_device_type  'Dectris Pilatus3 1M Pixel Array Detector'
_diffrn_reflns_number            1585
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.531
_diffrn_reflns_theta_max         19.453
_diffrn_reflns_theta_full        15.094
_diffrn_measured_fraction_theta_max 0.677
_diffrn_measured_fraction_theta_full 0.820
_diffrn_reflns_Laue_measured_fraction_max 0.677
_diffrn_reflns_Laue_measured_fraction_full 0.820
_diffrn_reflns_point_group_measured_fraction_max 0.677
_diffrn_reflns_point_group_measured_fraction_full 0.820
_reflns_number_total             481
_reflns_number_gt                430
_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_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          
;This data collection was done while the crystal 
was subjected to 0.54 GPa pressure, within a 
Boehler-Almax-type diamond anvil cell with a 70 
degree conical opening. Data were collected along
a single rotation axis ober a 65 defree angular
range.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0622P)²+0.4882P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   ?
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         481
_refine_ls_number_parameters     40
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.1117
_refine_ls_wR_factor_gt          0.1060
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.151
_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
Ca1 Ca 0.666667 0.333333 0.00110(14) 0.0080(3) Uani 1 3 d S T P . .
Ca2 Ca -0.00781(10) 0.24184(10) 0.250000 0.0063(2) Uani 1 2 d S T P . .
P1 P 0.36903(12) 0.39847(12) 0.250000 0.0040(3) Uani 1 2 d S T P . .
O1 O 0.4843(4) 0.3260(4) 0.250000 0.0090(6) Uani 1 2 d S T P . .
O2 O 0.4672(4) 0.5882(4) 0.250000 0.0105(6) Uani 1 2 d S T P . .
O3 O 0.2569(2) 0.3417(3) 0.0705(3) 0.0127(5) Uani 1 1 d . . . . .
F1 F 0.000000 0.000000 0.269(10) 0.019(7) Uani 0.5 3 d S TU P . .


_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
Ca1 O1 2.396(2) 2_655 ?
Ca1 O1 2.396(2) 3_665 ?
Ca1 O1 2.396(2) . ?
Ca1 O2 2.453(2) 8 ?
Ca1 O2 2.453(2) 9_655 ?
Ca1 O2 2.453(2) 7_665 ?
Ca1 O3 2.803(2) 7_665 ?
Ca1 O3 2.803(2) 8 ?
Ca1 O3 2.803(2) 9_655 ?
Ca1 P1 3.2029(10) 8 ?
Ca1 P1 3.2029(10) 9_655 ?
Ca1 P1 3.2029(10) 7_665 ?
Ca2 F1 2.309(4) . ?
Ca2 F1 2.309(4) 10_556 ?
Ca2 O3 2.345(2) 9 ?
Ca2 O3 2.345(2) 6 ?
Ca2 O2 2.368(3) 3_565 ?
Ca2 O3 2.497(2) 10_556 ?
Ca2 O3 2.497(2) . ?
Ca2 O1 2.679(3) 2 ?
Ca2 P1 3.0747(13) . ?
Ca2 P1 3.2513(12) 2 ?
Ca2 P1 3.4873(13) 3_565 ?
P1 O3 1.533(2) . ?
P1 O3 1.533(2) 10_556 ?
P1 O1 1.537(3) . ?
P1 O2 1.541(3) . ?
F1 F1 0.26(13) 10_556 ?

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 Ca1 O1 74.62(8) 2_655 3_665 ?
O1 Ca1 O1 74.62(8) 2_655 . ?
O1 Ca1 O1 74.62(8) 3_665 . ?
O1 Ca1 O2 92.66(7) 2_655 8 ?
O1 Ca1 O2 154.44(10) 3_665 8 ?
O1 Ca1 O2 124.00(10) . 8 ?
O1 Ca1 O2 124.00(10) 2_655 9_655 ?
O1 Ca1 O2 92.66(8) 3_665 9_655 ?
O1 Ca1 O2 154.44(10) . 9_655 ?
O2 Ca1 O2 75.95(9) 8 9_655 ?
O1 Ca1 O2 154.44(10) 2_655 7_665 ?
O1 Ca1 O2 124.00(10) 3_665 7_665 ?
O1 Ca1 O2 92.66(7) . 7_665 ?
O2 Ca1 O2 75.95(9) 8 7_665 ?
O2 Ca1 O2 75.95(9) 9_655 7_665 ?
O1 Ca1 O3 142.27(8) 2_655 7_665 ?
O1 Ca1 O3 68.78(8) 3_665 7_665 ?
O1 Ca1 O3 86.99(9) . 7_665 ?
O2 Ca1 O3 124.63(8) 8 7_665 ?
O2 Ca1 O3 67.62(8) 9_655 7_665 ?
O2 Ca1 O3 56.05(8) 7_665 7_665 ?
O1 Ca1 O3 86.99(9) 2_655 8 ?
O1 Ca1 O3 142.27(8) 3_665 8 ?
O1 Ca1 O3 68.78(8) . 8 ?
O2 Ca1 O3 56.05(8) 8 8 ?
O2 Ca1 O3 124.63(8) 9_655 8 ?
O2 Ca1 O3 67.62(8) 7_665 8 ?
O3 Ca1 O3 116.98(3) 7_665 8 ?
O1 Ca1 O3 68.78(8) 2_655 9_655 ?
O1 Ca1 O3 86.99(9) 3_665 9_655 ?
O1 Ca1 O3 142.27(8) . 9_655 ?
O2 Ca1 O3 67.62(8) 8 9_655 ?
O2 Ca1 O3 56.05(8) 9_655 9_655 ?
O2 Ca1 O3 124.63(8) 7_665 9_655 ?
O3 Ca1 O3 116.98(3) 7_665 9_655 ?
O3 Ca1 O3 116.98(3) 8 9_655 ?
O1 Ca1 P1 93.11(7) 2_655 8 ?
O1 Ca1 P1 166.65(6) 3_665 8 ?
O1 Ca1 P1 97.34(7) . 8 ?
O2 Ca1 P1 27.80(7) 8 8 ?
O2 Ca1 P1 98.69(6) 9_655 8 ?
O2 Ca1 P1 66.15(7) 7_665 8 ?
O3 Ca1 P1 122.18(5) 7_665 8 ?
O3 Ca1 P1 28.60(4) 8 8 ?
O3 Ca1 P1 93.51(5) 9_655 8 ?
O1 Ca1 P1 97.34(7) 2_655 9_655 ?
O1 Ca1 P1 93.11(7) 3_665 9_655 ?
O1 Ca1 P1 166.65(6) . 9_655 ?
O2 Ca1 P1 66.15(7) 8 9_655 ?
O2 Ca1 P1 27.80(7) 9_655 9_655 ?
O2 Ca1 P1 98.69(6) 7_665 9_655 ?
O3 Ca1 P1 93.51(5) 7_665 9_655 ?
O3 Ca1 P1 122.18(5) 8 9_655 ?
O3 Ca1 P1 28.60(4) 9_655 9_655 ?
P1 Ca1 P1 93.68(2) 8 9_655 ?
O1 Ca1 P1 166.65(6) 2_655 7_665 ?
O1 Ca1 P1 97.34(7) 3_665 7_665 ?
O1 Ca1 P1 93.11(7) . 7_665 ?
O2 Ca1 P1 98.69(6) 8 7_665 ?
O2 Ca1 P1 66.15(7) 9_655 7_665 ?
O2 Ca1 P1 27.80(7) 7_665 7_665 ?
O3 Ca1 P1 28.60(4) 7_665 7_665 ?
O3 Ca1 P1 93.51(5) 8 7_665 ?
O3 Ca1 P1 122.18(5) 9_655 7_665 ?
P1 Ca1 P1 93.68(2) 8 7_665 ?
P1 Ca1 P1 93.68(2) 9_655 7_665 ?
F1 Ca2 F1 6(3) . 10_556 ?
F1 Ca2 O3 105.9(16) . 9 ?
F1 Ca2 O3 99.7(16) 10_556 9 ?
F1 Ca2 O3 99.7(16) . 6 ?
F1 Ca2 O3 105.9(16) 10_556 6 ?
O3 Ca2 O3 140.01(13) 9 6 ?
F1 Ca2 O2 152.0(2) . 3_565 ?
F1 Ca2 O2 152.0(2) 10_556 3_565 ?
O3 Ca2 O2 85.73(6) 9 3_565 ?
O3 Ca2 O2 85.73(6) 6 3_565 ?
F1 Ca2 O3 80.0(8) . 10_556 ?
F1 Ca2 O3 83.3(8) 10_556 10_556 ?
O3 Ca2 O3 136.04(8) 9 10_556 ?
O3 Ca2 O3 77.95(5) 6 10_556 ?
O2 Ca2 O3 74.27(9) 3_565 10_556 ?
F1 Ca2 O3 83.3(8) . . ?
F1 Ca2 O3 80.0(8) 10_556 . ?
O3 Ca2 O3 77.96(5) 9 . ?
O3 Ca2 O3 136.04(8) 6 . ?
O2 Ca2 O3 74.27(9) 3_565 . ?
O3 Ca2 O3 59.21(9) 10_556 . ?
F1 Ca2 O1 106.88(8) . 2 ?
F1 Ca2 O1 106.88(8) 10_556 2 ?
O3 Ca2 O1 71.72(6) 9 2 ?
O3 Ca2 O1 71.72(6) 6 2 ?
O2 Ca2 O1 100.90(11) 3_565 2 ?
O3 Ca2 O1 149.59(5) 10_556 2 ?
O3 Ca2 O1 149.59(5) . 2 ?
F1 Ca2 P1 82.87(3) . . ?
F1 Ca2 P1 82.87(3) 10_556 . ?
O3 Ca2 P1 106.62(6) 9 . ?
O3 Ca2 P1 106.62(6) 6 . ?
O2 Ca2 P1 69.34(9) 3_565 . ?
O3 Ca2 P1 29.70(5) 10_556 . ?
O3 Ca2 P1 29.70(5) . . ?
O1 Ca2 P1 170.24(7) 2 . ?
F1 Ca2 P1 78.94(4) . 2 ?
F1 Ca2 P1 78.94(4) 10_556 2 ?
O3 Ca2 P1 77.69(5) 9 2 ?
O3 Ca2 P1 77.69(5) 6 2 ?
O2 Ca2 P1 128.88(9) 3_565 2 ?
O3 Ca2 P1 144.41(5) 10_556 2 ?
O3 Ca2 P1 144.41(5) . 2 ?
O1 Ca2 P1 27.98(7) 2 2 ?
P1 Ca2 P1 161.78(4) . 2 ?
F1 Ca2 P1 172.7(7) . 3_565 ?
F1 Ca2 P1 172.7(7) 10_556 3_565 ?
O3 Ca2 P1 79.03(6) 9 3_565 ?
O3 Ca2 P1 79.03(6) 6 3_565 ?
O2 Ca2 P1 21.25(8) 3_565 3_565 ?
O3 Ca2 P1 92.68(6) 10_556 3_565 ?
O3 Ca2 P1 92.68(6) . 3_565 ?
O1 Ca2 P1 79.65(7) 2 3_565 ?
P1 Ca2 P1 90.59(4) . 3_565 ?
P1 Ca2 P1 107.63(4) 2 3_565 ?
F1 Ca2 Ca1 130.2(9) . 1_455 ?
F1 Ca2 Ca1 126.6(10) 10_556 1_455 ?
O3 Ca2 Ca1 44.37(6) 9 1_455 ?
O3 Ca2 Ca1 95.71(7) 6 1_455 ?
O2 Ca2 Ca1 75.78(8) 3_565 1_455 ?
O3 Ca2 Ca1 149.75(6) 10_556 1_455 ?
O3 Ca2 Ca1 115.83(5) . 1_455 ?
O1 Ca2 Ca1 36.39(4) 2 1_455 ?
P1 Ca2 Ca1 136.44(3) . 1_455 ?
P1 Ca2 Ca1 58.61(2) 2 1_455 ?
P1 Ca2 Ca1 57.09(2) 3_565 1_455 ?
O3 P1 O3 107.16(17) . 10_556 ?
O3 P1 O1 110.98(11) . . ?
O3 P1 O1 110.98(11) 10_556 . ?
O3 P1 O2 108.09(12) . . ?
O3 P1 O2 108.09(12) 10_556 . ?
O1 P1 O2 111.37(18) . . ?
O3 P1 Ca2 53.81(8) . . ?
O3 P1 Ca2 53.81(8) 10_556 . ?
O1 P1 Ca2 133.06(13) . . ?
O2 P1 Ca2 115.57(13) . . ?
O3 P1 Ca1 112.55(9) . 4_665 ?
O3 P1 Ca1 61.05(10) 10_556 4_665 ?
O1 P1 Ca1 136.01(8) . 4_665 ?
O2 P1 Ca1 47.93(8) . 4_665 ?
Ca2 P1 Ca1 80.14(3) . 4_665 ?
O3 P1 Ca1 61.06(10) . 7_665 ?
O3 P1 Ca1 112.55(9) 10_556 7_665 ?
O1 P1 Ca1 136.01(8) . 7_665 ?
O2 P1 Ca1 47.93(8) . 7_665 ?
Ca2 P1 Ca1 80.14(3) . 7_665 ?
Ca1 P1 Ca1 65.23(4) 4_665 7_665 ?
O3 P1 Ca2 79.57(10) . 3 ?
O3 P1 Ca2 79.57(10) 10_556 3 ?
O1 P1 Ca2 54.84(13) . 3 ?
O2 P1 Ca2 166.21(13) . 3 ?
Ca2 P1 Ca2 78.22(4) . 3 ?
Ca1 P1 Ca2 140.56(2) 4_665 3 ?
Ca1 P1 Ca2 140.56(2) 7_665 3 ?
O3 P1 Ca2 122.66(9) . 2_665 ?
O3 P1 Ca2 122.66(9) 10_556 2_665 ?
O1 P1 Ca2 77.53(13) . 2_665 ?
O2 P1 Ca2 33.84(12) . 2_665 ?
Ca2 P1 Ca2 149.41(4) . 2_665 ?
Ca1 P1 Ca2 74.20(2) 4_665 2_665 ?
Ca1 P1 Ca2 74.20(2) 7_665 2_665 ?
Ca2 P1 Ca2 132.37(4) 3 2_665 ?
P1 O1 Ca1 129.54(9) . 10_556 ?
P1 O1 Ca1 129.54(9) . . ?
Ca1 O1 Ca1 91.16(10) 10_556 . ?
P1 O1 Ca2 97.18(15) . 3 ?
Ca1 O1 Ca2 102.06(10) 10_556 3 ?
Ca1 O1 Ca2 102.06(10) . 3 ?
P1 O2 Ca2 124.91(18) . 2_665 ?
P1 O2 Ca1 104.26(12) . 7_665 ?
Ca2 O2 Ca1 113.92(10) 2_665 7_665 ?
P1 O2 Ca1 104.26(12) . 4_665 ?
Ca2 O2 Ca1 113.92(10) 2_665 4_665 ?
Ca1 O2 Ca1 89.45(11) 7_665 4_665 ?
P1 O3 Ca2 142.06(12) . 8 ?
P1 O3 Ca2 96.49(10) . . ?
Ca2 O3 Ca2 117.42(9) 8 . ?
P1 O3 Ca1 90.34(11) . 7_665 ?
Ca2 O3 Ca1 99.82(8) 8 7_665 ?
Ca2 O3 Ca1 99.23(8) . 7_665 ?
F1 F1 Ca2 86.8(17) 10_556 2 ?
F1 F1 Ca2 86.8(16) 10_556 3 ?
Ca2 F1 Ca2 119.7(3) 2 3 ?
F1 F1 Ca2 86.8(16) 10_556 . ?
Ca2 F1 Ca2 119.7(3) 2 . ?
Ca2 F1 Ca2 119.7(3) 3 . ?

_refine_diff_density_max         0.590
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.176




# start Validation Reply Form

_vrf_PLAT029_Ap1quarterdegP1_1_V2_0m_a
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low 0.820.  
RESPONSE: The experiment was done in a diamond anvil cell, so this 
level of completeness is acceptable.
;
_vrf_PLAT911_Ap1quarterdegP1_1_V2_0m_a
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600  
RESPONSE: The experiment was done in a diamond anvil cell, with 
rotion along a single axis. This restricts the amound of recprocal
space probed.
;
# end Validation Reply Form
