# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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_3333
_database_code_depnum_ccdc_archive 'CCDC 1897617'
loop_
_audit_author_name
_audit_author_address
KCaPOF
;Shihezi University
China
;
_audit_update_record             
;
2019-02-16 deposited with the CCDC.	2019-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca F K2 O4 P'
_chemical_formula_weight         232.25

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.661(3)
_cell_length_b                   5.8589(16)
_cell_length_c                   7.325(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     543.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    10680
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      22.48

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.839
_exptl_crystal_F_000             456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    2.931
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2849
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         3.213
_diffrn_reflns_theta_max         27.619
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             695
_reflns_number_gt                650
_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-2013 (Sheldrick, 2013)'
_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)+14.3729P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         695
_refine_ls_number_parameters     53
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0727
_refine_ls_wR_factor_ref         0.1735
_refine_ls_wR_factor_gt          0.1725
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_restrained_S_all      1.247
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001

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 0.57096(16) 0.2500 0.2022(3) 0.0104(6) Uani 1 2 d S T P . .
K1 K 0.6876(2) 0.7500 0.9961(4) 0.0240(7) Uani 1 2 d S T P . .
K2 K 0.5740(2) 0.2500 -0.2910(4) 0.0210(7) Uani 1 2 d S T P . .
P1 P 0.66143(19) 0.7500 0.4882(3) 0.0068(6) Uani 1 2 d S T P . .
F1 F 0.5000 0.0000 0.0000 0.0163(14) Uani 1 2 d S . P . .
O1 O 0.5985(7) 0.7500 0.6647(13) 0.026(2) Uani 1 2 d S T P . .
O2 O 0.6323(5) 0.5360(10) 0.3799(9) 0.0259(15) Uani 1 1 d . . . . .
O3 O 0.7804(6) 0.7500 0.5254(14) 0.026(2) Uani 1 2 d S T 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 O2 2.260(6) . ?
Ca1 O2 2.260(6) 7_565 ?
Ca1 F1 2.2683(16) . ?
Ca1 F1 2.2683(16) 3_655 ?
Ca1 O3 2.284(8) 2_664 ?
Ca1 O1 2.357(9) 5_666 ?
Ca1 K2 3.5177(19) 5_655 ?
Ca1 K2 3.5177(19) 5_665 ?
Ca1 K1 3.581(3) 5_666 ?
Ca1 K1 3.611(2) 1_554 ?
Ca1 K1 3.611(2) 1_544 ?
Ca1 K2 3.613(4) . ?
K1 O1 2.677(10) . ?
K1 F1 2.791(2) 3_656 ?
K1 F1 2.791(2) 1_566 ?
K1 O2 2.955(7) 8_766 ?
K1 O2 2.955(7) 2_665 ?
K1 O3 2.9651(17) 2_675 ?
K1 O3 2.9651(16) 2_665 ?
K1 O2 3.157(7) 7_576 ?
K1 O2 3.157(7) 1_556 ?
K1 K2 3.397(4) 2_666 ?
K1 P1 3.498(2) 2_675 ?
K1 P1 3.498(2) 2_665 ?
K2 F1 2.751(2) 3_655 ?
K2 F1 2.751(2) . ?
K2 O3 2.961(10) 2_664 ?
K2 O1 2.9636(15) 1_554 ?
K2 O1 2.9636(15) 1_544 ?
K2 O2 2.969(7) 3_645 ?
K2 O2 2.969(7) 5_665 ?
K2 O2 3.027(7) 7_564 ?
K2 O2 3.027(7) 1_554 ?
K2 P1 3.312(4) 5_665 ?
K2 K1 3.398(4) 2_663 ?
K2 Ca1 3.5177(19) 5_655 ?
P1 O1 1.519(9) . ?
P1 O2 1.529(6) 7_575 ?
P1 O2 1.529(6) . ?
P1 O3 1.531(8) . ?
P1 K2 3.312(4) 5_665 ?
P1 K1 3.498(2) 2_674 ?
P1 K1 3.498(2) 2_664 ?
P1 K2 3.524(2) 1_566 ?
P1 K2 3.524(2) 1_556 ?
P1 K1 3.620(4) 1_554 ?
F1 Ca1 2.2683(16) 5_655 ?
F1 K2 2.751(2) 5_655 ?
F1 K1 2.790(2) 1_544 ?
F1 K1 2.790(2) 5_666 ?
O1 Ca1 2.356(8) 5_666 ?
O1 K2 2.9636(15) 1_566 ?
O1 K2 2.9636(15) 1_556 ?
O2 K1 2.955(7) 2_664 ?
O2 K2 2.969(7) 5_665 ?
O2 K2 3.027(7) 1_556 ?
O2 K1 3.157(7) 1_554 ?
O3 Ca1 2.284(8) 2_665 ?
O3 K2 2.961(10) 2_665 ?
O3 K1 2.9651(16) 2_674 ?
O3 K1 2.9651(16) 2_664 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ca1 O2 95.7(3) . 7_565 ?
O2 Ca1 F1 172.35(18) . . ?
O2 Ca1 F1 91.91(17) 7_565 . ?
O2 Ca1 F1 91.91(17) . 3_655 ?
O2 Ca1 F1 172.35(18) 7_565 3_655 ?
F1 Ca1 F1 80.44(7) . 3_655 ?
O2 Ca1 O3 92.5(2) . 2_664 ?
O2 Ca1 O3 92.5(2) 7_565 2_664 ?
F1 Ca1 O3 87.5(2) . 2_664 ?
F1 Ca1 O3 87.5(2) 3_655 2_664 ?
O2 Ca1 O1 94.3(2) . 5_666 ?
O2 Ca1 O1 94.3(2) 7_565 5_666 ?
F1 Ca1 O1 84.8(2) . 5_666 ?
F1 Ca1 O1 84.8(2) 3_655 5_666 ?
O3 Ca1 O1 169.9(4) 2_664 5_666 ?
O2 Ca1 K2 133.65(19) . 5_655 ?
O2 Ca1 K2 56.98(16) 7_565 5_655 ?
F1 Ca1 K2 51.42(5) . 5_655 ?
F1 Ca1 K2 116.87(8) 3_655 5_655 ?
O3 Ca1 K2 122.33(6) 2_664 5_655 ?
O1 Ca1 K2 56.53(5) 5_666 5_655 ?
O2 Ca1 K2 56.98(16) . 5_665 ?
O2 Ca1 K2 133.65(19) 7_565 5_665 ?
F1 Ca1 K2 116.87(8) . 5_665 ?
F1 Ca1 K2 51.42(5) 3_655 5_665 ?
O3 Ca1 K2 122.33(6) 2_664 5_665 ?
O1 Ca1 K2 56.53(5) 5_666 5_665 ?
K2 Ca1 K2 112.77(9) 5_655 5_665 ?
O2 Ca1 K1 123.21(16) . 5_666 ?
O2 Ca1 K1 123.21(16) 7_565 5_666 ?
F1 Ca1 K1 51.19(5) . 5_666 ?
F1 Ca1 K1 51.19(5) 3_655 5_666 ?
O3 Ca1 K1 121.5(3) 2_664 5_666 ?
O1 Ca1 K1 48.4(3) 5_666 5_666 ?
K2 Ca1 K1 66.30(6) 5_655 5_666 ?
K2 Ca1 K1 66.30(6) 5_665 5_666 ?
O2 Ca1 K1 59.92(18) . 1_554 ?
O2 Ca1 K1 134.58(17) 7_565 1_554 ?
F1 Ca1 K1 114.39(8) . 1_554 ?
F1 Ca1 K1 50.60(5) 3_655 1_554 ?
O3 Ca1 K1 54.99(6) 2_664 1_554 ?
O1 Ca1 K1 123.04(8) 5_666 1_554 ?
K2 Ca1 K1 165.08(9) 5_655 1_554 ?
K2 Ca1 K1 67.36(5) 5_665 1_554 ?
K1 Ca1 K1 101.79(6) 5_666 1_554 ?
O2 Ca1 K1 134.58(17) . 1_544 ?
O2 Ca1 K1 59.91(18) 7_565 1_544 ?
F1 Ca1 K1 50.60(5) . 1_544 ?
F1 Ca1 K1 114.39(8) 3_655 1_544 ?
O3 Ca1 K1 54.99(6) 2_664 1_544 ?
O1 Ca1 K1 123.04(8) 5_666 1_544 ?
K2 Ca1 K1 67.36(5) 5_655 1_544 ?
K2 Ca1 K1 165.08(9) 5_665 1_544 ?
K1 Ca1 K1 101.79(6) 5_666 1_544 ?
K1 Ca1 K1 108.44(9) 1_554 1_544 ?
O2 Ca1 K2 124.93(18) . . ?
O2 Ca1 K2 124.92(18) 7_565 . ?
F1 Ca1 K2 49.57(5) . . ?
F1 Ca1 K2 49.57(5) 3_655 . ?
O3 Ca1 K2 54.9(3) 2_664 . ?
O1 Ca1 K2 115.1(3) 5_666 . ?
K2 Ca1 K2 100.99(6) 5_655 . ?
K2 Ca1 K2 100.99(6) 5_665 . ?
K1 Ca1 K2 66.68(8) 5_666 . ?
K1 Ca1 K2 65.02(6) 1_554 . ?
K1 Ca1 K2 65.02(6) 1_544 . ?
O1 K1 F1 69.54(16) . 3_656 ?
O1 K1 F1 69.54(16) . 1_566 ?
F1 K1 F1 63.32(6) 3_656 1_566 ?
O1 K1 O2 93.7(2) . 8_766 ?
F1 K1 O2 163.21(17) 3_656 8_766 ?
F1 K1 O2 111.23(12) 1_566 8_766 ?
O1 K1 O2 93.7(2) . 2_665 ?
F1 K1 O2 111.23(12) 3_656 2_665 ?
F1 K1 O2 163.21(17) 1_566 2_665 ?
O2 K1 O2 69.1(2) 8_766 2_665 ?
O1 K1 O3 97.1(2) . 2_675 ?
F1 K1 O3 129.35(17) 3_656 2_675 ?
F1 K1 O3 66.23(15) 1_566 2_675 ?
O2 K1 O3 49.86(19) 8_766 2_675 ?
O2 K1 O3 118.4(2) 2_665 2_675 ?
O1 K1 O3 97.1(2) . 2_665 ?
F1 K1 O3 66.23(15) 3_656 2_665 ?
F1 K1 O3 129.35(17) 1_566 2_665 ?
O2 K1 O3 118.4(2) 8_766 2_665 ?
O2 K1 O3 49.86(19) 2_665 2_665 ?
O3 K1 O3 162.2(4) 2_675 2_665 ?
O1 K1 O2 135.57(19) . 7_576 ?
F1 K1 O2 90.61(14) 3_656 7_576 ?
F1 K1 O2 66.03(12) 1_566 7_576 ?
O2 K1 O2 101.68(14) 8_766 7_576 ?
O2 K1 O2 130.76(19) 2_665 7_576 ?
O3 K1 O2 64.7(2) 2_675 7_576 ?
O3 K1 O2 111.0(2) 2_665 7_576 ?
O1 K1 O2 135.57(19) . 1_556 ?
F1 K1 O2 66.03(12) 3_656 1_556 ?
F1 K1 O2 90.61(14) 1_566 1_556 ?
O2 K1 O2 130.76(19) 8_766 1_556 ?
O2 K1 O2 101.68(14) 2_665 1_556 ?
O3 K1 O2 111.0(2) 2_675 1_556 ?
O3 K1 O2 64.7(2) 2_665 1_556 ?
O2 K1 O2 46.8(2) 7_576 1_556 ?
O1 K1 K2 142.2(2) . 2_666 ?
F1 K1 K2 138.72(8) 3_656 2_666 ?
F1 K1 K2 138.72(8) 1_566 2_666 ?
O2 K1 K2 56.40(14) 8_766 2_666 ?
O2 K1 K2 56.40(14) 2_665 2_666 ?
O3 K1 K2 81.11(18) 2_675 2_666 ?
O3 K1 K2 81.11(18) 2_665 2_666 ?
O2 K1 K2 77.78(13) 7_576 2_666 ?
O2 K1 K2 77.78(13) 1_556 2_666 ?
O1 K1 P1 102.43(12) . 2_675 ?
F1 K1 P1 154.79(7) 3_656 2_675 ?
F1 K1 P1 91.47(4) 1_566 2_675 ?
O2 K1 P1 25.68(11) 8_766 2_675 ?
O2 K1 P1 92.77(14) 2_665 2_675 ?
O3 K1 P1 25.75(15) 2_675 2_675 ?
O3 K1 P1 138.93(18) 2_665 2_675 ?
O2 K1 P1 78.66(12) 7_576 2_675 ?
O2 K1 P1 117.94(14) 1_556 2_675 ?
K2 K1 P1 61.45(6) 2_666 2_675 ?
O1 K1 P1 102.43(12) . 2_665 ?
F1 K1 P1 91.47(4) 3_656 2_665 ?
F1 K1 P1 154.79(7) 1_566 2_665 ?
O2 K1 P1 92.77(14) 8_766 2_665 ?
O2 K1 P1 25.68(12) 2_665 2_665 ?
O3 K1 P1 138.93(18) 2_675 2_665 ?
O3 K1 P1 25.75(15) 2_665 2_665 ?
O2 K1 P1 117.94(14) 7_576 2_665 ?
O2 K1 P1 78.66(12) 1_556 2_665 ?
K2 K1 P1 61.45(6) 2_666 2_665 ?
P1 K1 P1 113.72(10) 2_675 2_665 ?
F1 K2 F1 64.34(6) 3_655 . ?
F1 K2 O3 66.76(14) 3_655 2_664 ?
F1 K2 O3 66.76(14) . 2_664 ?
F1 K2 O1 66.05(17) 3_655 1_554 ?
F1 K2 O1 130.30(18) . 1_554 ?
O3 K2 O1 91.2(2) 2_664 1_554 ?
F1 K2 O1 130.30(18) 3_655 1_544 ?
F1 K2 O1 66.05(17) . 1_544 ?
O3 K2 O1 91.2(2) 2_664 1_544 ?
O1 K2 O1 162.6(3) 1_554 1_544 ?
F1 K2 O2 95.46(15) 3_655 3_645 ?
F1 K2 O2 69.24(13) . 3_645 ?
O3 K2 O2 135.97(19) 2_664 3_645 ?
O1 K2 O2 119.0(2) 1_554 3_645 ?
O1 K2 O2 69.5(2) 1_544 3_645 ?
F1 K2 O2 69.24(13) 3_655 5_665 ?
F1 K2 O2 95.46(15) . 5_665 ?
O3 K2 O2 135.97(19) 2_664 5_665 ?
O1 K2 O2 69.5(2) 1_554 5_665 ?
O1 K2 O2 119.0(2) 1_544 5_665 ?
O2 K2 O2 49.9(2) 3_645 5_665 ?
F1 K2 O2 174.19(16) 3_655 7_564 ?
F1 K2 O2 113.91(11) . 7_564 ?
O3 K2 O2 118.14(18) 2_664 7_564 ?
O1 K2 O2 115.8(2) 1_554 7_564 ?
O1 K2 O2 48.7(2) 1_544 7_564 ?
O2 K2 O2 78.82(19) 3_645 7_564 ?
O2 K2 O2 105.88(14) 5_665 7_564 ?
F1 K2 O2 113.91(11) 3_655 1_554 ?
F1 K2 O2 174.19(16) . 1_554 ?
O3 K2 O2 118.14(18) 2_664 1_554 ?
O1 K2 O2 48.7(2) 1_554 1_554 ?
O1 K2 O2 115.8(2) 1_544 1_554 ?
O2 K2 O2 105.88(14) 3_645 1_554 ?
O2 K2 O2 78.82(18) 5_665 1_554 ?
O2 K2 O2 67.2(2) 7_564 1_554 ?
F1 K2 P1 91.80(8) 3_655 5_665 ?
F1 K2 P1 91.80(8) . 5_665 ?
O3 K2 P1 154.34(19) 2_664 5_665 ?
O1 K2 P1 92.7(2) 1_554 5_665 ?
O1 K2 P1 92.7(2) 1_544 5_665 ?
O2 K2 P1 27.48(11) 3_645 5_665 ?
O2 K2 P1 27.48(11) 5_665 5_665 ?
O2 K2 P1 82.66(13) 7_564 5_665 ?
O2 K2 P1 82.66(13) 1_554 5_665 ?
F1 K2 K1 131.16(9) 3_655 2_663 ?
F1 K2 K1 131.16(9) . 2_663 ?
O3 K2 K1 78.83(18) 2_664 2_663 ?
O1 K2 K1 81.77(16) 1_554 2_663 ?
O1 K2 K1 81.77(16) 1_544 2_663 ?
O2 K2 K1 132.91(16) 3_645 2_663 ?
O2 K2 K1 132.91(16) 5_665 2_663 ?
O2 K2 K1 54.40(13) 7_564 2_663 ?
O2 K2 K1 54.40(13) 1_554 2_663 ?
P1 K2 K1 126.83(11) 5_665 2_663 ?
F1 K2 Ca1 97.02(7) 3_655 5_655 ?
F1 K2 Ca1 40.14(4) . 5_655 ?
O3 K2 Ca1 100.36(10) 2_664 5_655 ?
O1 K2 Ca1 153.89(19) 1_554 5_655 ?
O1 K2 Ca1 41.55(16) 1_544 5_655 ?
O2 K2 Ca1 39.65(11) 3_645 5_655 ?
O2 K2 Ca1 86.17(13) 5_665 5_655 ?
O2 K2 Ca1 79.26(12) 7_564 5_655 ?
O2 K2 Ca1 137.36(14) 1_554 5_655 ?
P1 K2 Ca1 67.12(5) 5_665 5_655 ?
K1 K2 Ca1 123.26(4) 2_663 5_655 ?
O1 P1 O2 108.4(3) . 7_575 ?
O1 P1 O2 108.4(3) . . ?
O2 P1 O2 110.2(5) 7_575 . ?
O1 P1 O3 111.4(6) . . ?
O2 P1 O3 109.3(3) 7_575 . ?
O2 P1 O3 109.3(3) . . ?
O1 P1 K2 84.2(4) . 5_665 ?
O2 P1 K2 63.7(2) 7_575 5_665 ?
O2 P1 K2 63.7(2) . 5_665 ?
O3 P1 K2 164.4(4) . 5_665 ?
O1 P1 K1 105.8(2) . 2_674 ?
O2 P1 K1 56.9(2) 7_575 2_674 ?
O2 P1 K1 145.8(3) . 2_674 ?
O3 P1 K1 57.27(7) . 2_674 ?
K2 P1 K1 119.93(6) 5_665 2_674 ?
O1 P1 K1 105.8(2) . 2_664 ?
O2 P1 K1 145.8(3) 7_575 2_664 ?
O2 P1 K1 56.9(2) . 2_664 ?
O3 P1 K1 57.27(7) . 2_664 ?
K2 P1 K1 119.93(6) 5_665 2_664 ?
K1 P1 K1 113.72(10) 2_674 2_664 ?
O1 P1 K2 56.26(5) . 1_566 ?
O2 P1 K2 58.7(3) 7_575 1_566 ?
O2 P1 K2 147.6(3) . 1_566 ?
O3 P1 K2 103.1(2) . 1_566 ?
K2 P1 K2 85.26(7) 5_665 1_566 ?
K1 P1 K2 57.86(6) 2_674 1_566 ?
K1 P1 K2 149.32(10) 2_664 1_566 ?
O1 P1 K2 56.26(5) . 1_556 ?
O2 P1 K2 147.6(3) 7_575 1_556 ?
O2 P1 K2 58.7(3) . 1_556 ?
O3 P1 K2 103.1(2) . 1_556 ?
K2 P1 K2 85.26(7) 5_665 1_556 ?
K1 P1 K2 149.32(10) 2_674 1_556 ?
K1 P1 K2 57.86(6) 2_664 1_556 ?
K2 P1 K2 112.44(10) 1_566 1_556 ?
O1 P1 K1 153.6(4) . 1_554 ?
O2 P1 K1 60.3(3) 7_575 1_554 ?
O2 P1 K1 60.4(3) . 1_554 ?
O3 P1 K1 95.0(4) . 1_554 ?
K2 P1 K1 69.40(8) 5_665 1_554 ?
K1 P1 K1 88.08(7) 2_674 1_554 ?
K1 P1 K1 88.08(7) 2_664 1_554 ?
K2 P1 K1 119.05(5) 1_566 1_554 ?
K2 P1 K1 119.05(5) 1_556 1_554 ?
O1 P1 K1 36.8(4) . . ?
O2 P1 K1 122.6(3) 7_575 . ?
O2 P1 K1 122.6(3) . . ?
O3 P1 K1 74.7(4) . . ?
K2 P1 K1 120.94(9) 5_665 . ?
K1 P1 K1 86.28(7) 2_674 . ?
K1 P1 K1 86.28(7) 2_664 . ?
K2 P1 K1 64.59(6) 1_566 . ?
K2 P1 K1 64.59(6) 1_556 . ?
K1 P1 K1 169.66(10) 1_554 . ?
Ca1 F1 Ca1 180.0 5_655 . ?
Ca1 F1 K2 88.44(7) 5_655 . ?
Ca1 F1 K2 91.56(7) . . ?
Ca1 F1 K2 91.56(7) 5_655 5_655 ?
Ca1 F1 K2 88.44(7) . 5_655 ?
K2 F1 K2 180.0 . 5_655 ?
Ca1 F1 K1 89.51(7) 5_655 1_544 ?
Ca1 F1 K1 90.49(7) . 1_544 ?
K2 F1 K1 88.95(7) . 1_544 ?
K2 F1 K1 91.05(7) 5_655 1_544 ?
Ca1 F1 K1 90.49(7) 5_655 5_666 ?
Ca1 F1 K1 89.51(7) . 5_666 ?
K2 F1 K1 91.05(7) . 5_666 ?
K2 F1 K1 88.95(7) 5_655 5_666 ?
K1 F1 K1 180.00(5) 1_544 5_666 ?
P1 O1 Ca1 146.1(6) . 5_666 ?
P1 O1 K1 123.4(5) . . ?
Ca1 O1 K1 90.5(3) 5_666 . ?
P1 O1 K2 98.51(17) . 1_566 ?
Ca1 O1 K2 81.93(16) 5_666 1_566 ?
K1 O1 K2 86.8(2) . 1_566 ?
P1 O1 K2 98.51(17) . 1_556 ?
Ca1 O1 K2 81.93(16) 5_666 1_556 ?
K1 O1 K2 86.8(2) . 1_556 ?
K2 O1 K2 162.6(3) 1_566 1_556 ?
P1 O2 Ca1 171.9(4) . . ?
P1 O2 K1 97.4(3) . 2_664 ?
Ca1 O2 K1 90.6(2) . 2_664 ?
P1 O2 K2 88.8(3) . 5_665 ?
Ca1 O2 K2 83.37(18) . 5_665 ?
K1 O2 K2 168.9(2) 2_664 5_665 ?
P1 O2 K2 95.7(3) . 1_556 ?
Ca1 O2 K2 88.0(2) . 1_556 ?
K1 O2 K2 69.20(16) 2_664 1_556 ?
K2 O2 K2 101.18(18) 5_665 1_556 ?
P1 O2 K1 94.8(3) . 1_554 ?
Ca1 O2 K1 81.8(2) . 1_554 ?
K1 O2 K1 108.09(19) 2_664 1_554 ?
K2 O2 K1 80.34(17) 5_665 1_554 ?
K2 O2 K1 169.4(2) 1_556 1_554 ?
P1 O3 Ca1 155.7(6) . 2_665 ?
P1 O3 K2 118.2(5) . 2_665 ?
Ca1 O3 K2 86.0(3) 2_665 2_665 ?
P1 O3 K1 96.98(16) . 2_674 ?
Ca1 O3 K1 85.90(16) 2_665 2_674 ?
K2 O3 K1 81.9(2) 2_665 2_674 ?
P1 O3 K1 96.98(16) . 2_664 ?
Ca1 O3 K1 85.90(16) 2_665 2_664 ?
K2 O3 K1 81.9(2) 2_665 2_664 ?
K1 O3 K1 162.2(4) 2_674 2_664 ?

_refine_diff_density_max         1.095
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.219

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1897618'
loop_
_audit_author_name
_audit_author_address
KCaPOF
;Shihezi University
China
;
_audit_update_record             
;
2019-02-16 deposited with the CCDC.	2019-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca F O4 P Rb2'
_chemical_formula_weight         324.99

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.895(9)
_cell_length_b                   5.970(4)
_cell_length_c                   7.436(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     572.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    991
_cell_measurement_theta_min      4.18
_cell_measurement_theta_max      27.74

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      3.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.771
_exptl_crystal_F_000             600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    18.226
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3378
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.160
_diffrn_reflns_theta_max         27.788
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             737
_reflns_number_gt                635
_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-2013 (Sheldrick, 2013)'
_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)+(0.0245P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0053(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         737
_refine_ls_number_parameters     53
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_ref         0.0504
_refine_ls_wR_factor_gt          0.0468
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
Rb1 Rb 0.07626(3) 0.2500 0.70148(6) 0.01459(15) Uani 1 2 d S T P . .
Rb2 Rb 0.31204(3) 0.2500 0.48947(6) 0.01509(15) Uani 1 2 d S T P . .
P1 P 0.34141(9) 0.2500 0.98358(15) 0.0072(2) Uani 1 2 d S T P . .
Ca1 Ca 0.07383(6) 0.2500 0.20021(12) 0.0080(2) Uani 1 2 d S T P . .
F1 F 0.0000 0.0000 0.0000 0.0128(6) Uani 1 2 d S . P . .
O1 O 0.36490(16) 0.0403(3) 0.8712(3) 0.0152(5) Uani 1 1 d . . . . .
O2 O 0.4112(2) 0.2500 1.1513(5) 0.0158(7) Uani 1 2 d S T P . .
O3 O 0.2268(2) 0.2500 1.0371(4) 0.0151(7) Uani 1 2 d S T 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
Rb1 F1 2.8498(15) 3_556 ?
Rb1 F1 2.8498(15) 1_556 ?
Rb1 O2 3.013(2) 2_554 ?
Rb1 O2 3.013(2) 2_564 ?
Rb1 O1 3.048(3) 6_557 ?
Rb1 O1 3.048(3) 4_456 ?
Rb1 O1 3.100(3) 2_554 ?
Rb1 O1 3.100(3) 8_665 ?
Rb1 O3 3.162(4) . ?
Rb1 P1 3.326(2) 6_557 ?
Rb1 O2 3.378(4) 6_557 ?
Rb1 P1 3.558(2) 2_554 ?
Rb2 O2 2.821(4) 1_554 ?
Rb2 F1 2.8475(16) 4 ?
Rb2 F1 2.8475(16) 2 ?
Rb2 O1 2.997(3) 2_554 ?
Rb2 O1 2.997(3) 8_665 ?
Rb2 O3 3.047(2) 2_554 ?
Rb2 O3 3.047(2) 2_564 ?
Rb2 O1 3.177(3) . ?
Rb2 O1 3.177(3) 7_565 ?
Rb2 O3 3.539(4) 1_554 ?
Rb2 P1 3.582(2) 2_554 ?
Rb2 P1 3.582(2) 2_564 ?
P1 O3 1.531(3) . ?
P1 O1 1.535(2) 7_565 ?
P1 O1 1.535(2) . ?
P1 O2 1.538(3) . ?
P1 Rb1 3.326(2) 6_657 ?
P1 Rb1 3.558(2) 2_565 ?
P1 Rb1 3.558(2) 2 ?
P1 Rb2 3.582(2) 2 ?
P1 Rb2 3.582(2) 2_565 ?
P1 Rb2 3.781(3) 1_556 ?
Ca1 O1 2.290(2) 8_665 ?
Ca1 O1 2.290(2) 2_554 ?
Ca1 F1 2.3131(12) . ?
Ca1 F1 2.3131(12) 3 ?
Ca1 O3 2.315(3) 1_554 ?
Ca1 O2 2.370(3) 6_557 ?
Ca1 Rb1 3.632(2) 5_556 ?
Ca1 Rb1 3.632(2) 5_566 ?
Ca1 Rb2 3.659(2) 6_556 ?
Ca1 Rb2 3.679(2) 2_564 ?
Ca1 Rb2 3.6786(19) 2_554 ?
Ca1 Rb1 3.709(3) 1_554 ?
F1 Ca1 2.3130(12) 5 ?
F1 Rb2 2.8475(16) 6_556 ?
F1 Rb2 2.8475(16) 2_554 ?
F1 Rb1 2.8499(15) 1_554 ?
F1 Rb1 2.8499(15) 5_556 ?
O1 Ca1 2.290(2) 2 ?
O1 Rb2 2.997(2) 2 ?
O1 Rb1 3.048(3) 6_657 ?
O1 Rb1 3.100(3) 2 ?
O2 Ca1 2.370(3) 6_657 ?
O2 Rb2 2.821(4) 1_556 ?
O2 Rb1 3.013(2) 2_565 ?
O2 Rb1 3.013(2) 2 ?
O2 Rb1 3.378(4) 6_657 ?
O3 Ca1 2.315(3) 1_556 ?
O3 Rb2 3.047(2) 2 ?
O3 Rb2 3.047(2) 2_565 ?
O3 Rb2 3.539(4) 1_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
F1 Rb1 F1 63.16(5) 3_556 1_556 ?
F1 Rb1 O2 129.34(7) 3_556 2_554 ?
F1 Rb1 O2 66.17(7) 1_556 2_554 ?
F1 Rb1 O2 66.17(7) 3_556 2_564 ?
F1 Rb1 O2 129.34(6) 1_556 2_564 ?
O2 Rb1 O2 164.49(12) 2_554 2_564 ?
F1 Rb1 O1 92.57(6) 3_556 6_557 ?
F1 Rb1 O1 67.33(5) 1_556 6_557 ?
O2 Rb1 O1 67.60(8) 2_554 6_557 ?
O2 Rb1 O1 115.66(7) 2_564 6_557 ?
F1 Rb1 O1 67.33(5) 3_556 4_456 ?
F1 Rb1 O1 92.57(6) 1_556 4_456 ?
O2 Rb1 O1 115.66(7) 2_554 4_456 ?
O2 Rb1 O1 67.60(8) 2_564 4_456 ?
O1 Rb1 O1 48.51(9) 6_557 4_456 ?
F1 Rb1 O1 173.86(4) 3_556 2_554 ?
F1 Rb1 O1 114.12(6) 1_556 2_554 ?
O2 Rb1 O1 48.30(8) 2_554 2_554 ?
O2 Rb1 O1 116.28(8) 2_564 2_554 ?
O1 Rb1 O1 81.29(7) 6_557 2_554 ?
O1 Rb1 O1 107.94(5) 4_456 2_554 ?
F1 Rb1 O1 114.12(6) 3_556 8_665 ?
F1 Rb1 O1 173.86(4) 1_556 8_665 ?
O2 Rb1 O1 116.28(8) 2_554 8_665 ?
O2 Rb1 O1 48.30(8) 2_564 8_665 ?
O1 Rb1 O1 107.94(5) 6_557 8_665 ?
O1 Rb1 O1 81.29(7) 4_456 8_665 ?
O1 Rb1 O1 67.98(9) 2_554 8_665 ?
F1 Rb1 O3 66.23(6) 3_556 . ?
F1 Rb1 O3 66.23(6) 1_556 . ?
O2 Rb1 O3 93.72(6) 2_554 . ?
O2 Rb1 O3 93.72(6) 2_564 . ?
O1 Rb1 O3 133.56(6) 6_557 . ?
O1 Rb1 O3 133.56(6) 4_456 . ?
O1 Rb1 O3 118.36(7) 2_554 . ?
O1 Rb1 O3 118.36(7) 8_665 . ?
F1 Rb1 P1 90.46(4) 3_556 6_557 ?
F1 Rb1 P1 90.46(4) 1_556 6_557 ?
O2 Rb1 P1 89.86(6) 2_554 6_557 ?
O2 Rb1 P1 89.86(6) 2_564 6_557 ?
O1 Rb1 P1 27.43(4) 6_557 6_557 ?
O1 Rb1 P1 27.43(4) 4_456 6_557 ?
O1 Rb1 P1 83.98(5) 2_554 6_557 ?
O1 Rb1 P1 83.98(5) 8_665 6_557 ?
O3 Rb1 P1 152.31(6) . 6_557 ?
F1 Rb1 O2 112.80(6) 3_556 6_557 ?
F1 Rb1 O2 112.80(6) 1_556 6_557 ?
O2 Rb1 O2 86.42(6) 2_554 6_557 ?
O2 Rb1 O2 86.42(6) 2_564 6_557 ?
O1 Rb1 O2 45.47(6) 6_557 6_557 ?
O1 Rb1 O2 45.47(6) 4_456 6_557 ?
O1 Rb1 O2 62.55(7) 2_554 6_557 ?
O1 Rb1 O2 62.55(7) 8_665 6_557 ?
O3 Rb1 O2 178.82(8) . 6_557 ?
P1 Rb1 O2 26.51(6) 6_557 6_557 ?
F1 Rb1 P1 153.755(19) 3_556 2_554 ?
F1 Rb1 P1 91.05(5) 1_556 2_554 ?
O2 Rb1 P1 25.37(6) 2_554 2_554 ?
O2 Rb1 P1 139.36(7) 2_564 2_554 ?
O1 Rb1 P1 80.87(6) 6_557 2_554 ?
O1 Rb1 P1 122.04(5) 4_456 2_554 ?
O1 Rb1 P1 25.48(4) 2_554 2_554 ?
O1 Rb1 P1 92.02(6) 8_665 2_554 ?
O3 Rb1 P1 100.16(5) . 2_554 ?
P1 Rb1 P1 94.77(3) 6_557 2_554 ?
O2 Rb1 P1 80.46(5) 6_557 2_554 ?
O2 Rb2 F1 68.82(6) 1_554 4 ?
O2 Rb2 F1 68.82(6) 1_554 2 ?
F1 Rb2 F1 63.22(5) 4 2 ?
O2 Rb2 O1 94.80(7) 1_554 2_554 ?
F1 Rb2 O1 163.57(5) 4 2_554 ?
F1 Rb2 O1 110.67(6) 2 2_554 ?
O2 Rb2 O1 94.80(7) 1_554 8_665 ?
F1 Rb2 O1 110.67(6) 4 8_665 ?
F1 Rb2 O1 163.57(5) 2 8_665 ?
O1 Rb2 O1 70.66(9) 2_554 8_665 ?
O2 Rb2 O3 100.26(6) 1_554 2_554 ?
F1 Rb2 O3 130.54(6) 4 2_554 ?
F1 Rb2 O3 67.86(7) 2 2_554 ?
O1 Rb2 O3 48.90(7) 2_554 2_554 ?
O1 Rb2 O3 118.39(8) 8_665 2_554 ?
O2 Rb2 O3 100.26(6) 1_554 2_564 ?
F1 Rb2 O3 67.86(7) 4 2_564 ?
F1 Rb2 O3 130.54(6) 2 2_564 ?
O1 Rb2 O3 118.39(8) 2_554 2_564 ?
O1 Rb2 O3 48.90(7) 8_665 2_564 ?
O3 Rb2 O3 156.78(12) 2_554 2_564 ?
O2 Rb2 O1 134.37(7) 1_554 . ?
F1 Rb2 O1 89.96(4) 4 . ?
F1 Rb2 O1 65.56(4) 2 . ?
O1 Rb2 O1 101.40(5) 2_554 . ?
O1 Rb2 O1 130.80(6) 8_665 . ?
O3 Rb2 O1 62.95(7) 2_554 . ?
O3 Rb2 O1 108.50(8) 2_564 . ?
O2 Rb2 O1 134.37(7) 1_554 7_565 ?
F1 Rb2 O1 65.56(4) 4 7_565 ?
F1 Rb2 O1 89.96(4) 2 7_565 ?
O1 Rb2 O1 130.80(6) 2_554 7_565 ?
O1 Rb2 O1 101.40(5) 8_665 7_565 ?
O3 Rb2 O1 108.50(8) 2_554 7_565 ?
O3 Rb2 O1 62.95(7) 2_564 7_565 ?
O1 Rb2 O1 46.42(8) . 7_565 ?
O2 Rb2 O3 45.06(9) 1_554 1_554 ?
F1 Rb2 O3 106.89(5) 4 1_554 ?
F1 Rb2 O3 106.89(5) 2 1_554 ?
O1 Rb2 O3 58.98(6) 2_554 1_554 ?
O1 Rb2 O3 58.98(6) 8_665 1_554 ?
O3 Rb2 O3 93.41(6) 2_554 1_554 ?
O3 Rb2 O3 93.41(6) 2_564 1_554 ?
O1 Rb2 O3 156.36(4) . 1_554 ?
O1 Rb2 O3 156.36(4) 7_565 1_554 ?
O2 Rb2 P1 103.86(4) 1_554 2_554 ?
F1 Rb2 P1 155.154(18) 4 2_554 ?
F1 Rb2 P1 91.93(6) 2 2_554 ?
O1 Rb2 P1 25.02(4) 2_554 2_554 ?
O1 Rb2 P1 93.31(7) 8_665 2_554 ?
O3 Rb2 P1 25.08(6) 2_554 2_554 ?
O3 Rb2 P1 136.64(7) 2_564 2_554 ?
O1 Rb2 P1 78.52(5) . 2_554 ?
O1 Rb2 P1 117.26(5) 7_565 2_554 ?
O3 Rb2 P1 79.44(3) 1_554 2_554 ?
O2 Rb2 P1 103.86(4) 1_554 2_564 ?
F1 Rb2 P1 91.93(6) 4 2_564 ?
F1 Rb2 P1 155.154(18) 2 2_564 ?
O1 Rb2 P1 93.31(7) 2_554 2_564 ?
O1 Rb2 P1 25.02(4) 8_665 2_564 ?
O3 Rb2 P1 136.64(7) 2_554 2_564 ?
O3 Rb2 P1 25.08(6) 2_564 2_564 ?
O1 Rb2 P1 117.26(5) . 2_564 ?
O1 Rb2 P1 78.52(5) 7_565 2_564 ?
O3 Rb2 P1 79.44(3) 1_554 2_564 ?
P1 Rb2 P1 112.91(6) 2_554 2_564 ?
O3 P1 O1 109.39(11) . 7_565 ?
O3 P1 O1 109.39(11) . . ?
O1 P1 O1 109.28(18) 7_565 . ?
O3 P1 O2 110.74(19) . . ?
O1 P1 O2 109.01(12) 7_565 . ?
O1 P1 O2 109.01(12) . . ?
O3 P1 Rb1 170.64(14) . 6_657 ?
O1 P1 Rb1 66.13(9) 7_565 6_657 ?
O1 P1 Rb1 66.13(9) . 6_657 ?
O2 P1 Rb1 78.62(14) . 6_657 ?
O3 P1 Rb1 99.76(7) . 2_565 ?
O1 P1 Rb1 60.32(10) 7_565 2_565 ?
O1 P1 Rb1 150.81(10) . 2_565 ?
O2 P1 Rb1 57.06(3) . 2_565 ?
Rb1 P1 Rb1 85.23(3) 6_657 2_565 ?
O3 P1 Rb1 99.76(7) . 2 ?
O1 P1 Rb1 150.81(10) 7_565 2 ?
O1 P1 Rb1 60.32(10) . 2 ?
O2 P1 Rb1 57.06(3) . 2 ?
Rb1 P1 Rb1 85.23(3) 6_657 2 ?
Rb1 P1 Rb1 114.04(6) 2_565 2 ?
O3 P1 Rb2 57.55(4) . 2 ?
O1 P1 Rb2 142.69(10) 7_565 2 ?
O1 P1 Rb2 55.66(9) . 2 ?
O2 P1 Rb2 108.26(7) . 2 ?
Rb1 P1 Rb2 120.53(3) 6_657 2 ?
Rb1 P1 Rb2 149.14(4) 2_565 2 ?
Rb1 P1 Rb2 57.32(4) 2 2 ?
O3 P1 Rb2 57.55(4) . 2_565 ?
O1 P1 Rb2 55.66(9) 7_565 2_565 ?
O1 P1 Rb2 142.68(10) . 2_565 ?
O2 P1 Rb2 108.26(7) . 2_565 ?
Rb1 P1 Rb2 120.53(3) 6_657 2_565 ?
Rb1 P1 Rb2 57.32(4) 2_565 2_565 ?
Rb1 P1 Rb2 149.14(4) 2 2_565 ?
Rb2 P1 Rb2 112.91(6) 2 2_565 ?
O3 P1 Rb2 99.19(13) . . ?
O1 P1 Rb2 58.60(9) 7_565 . ?
O1 P1 Rb2 58.60(9) . . ?
O2 P1 Rb2 150.07(14) . . ?
Rb1 P1 Rb2 71.45(4) 6_657 . ?
Rb1 P1 Rb2 118.92(3) 2_565 . ?
Rb1 P1 Rb2 118.92(3) 2 . ?
Rb2 P1 Rb2 87.45(2) 2 . ?
Rb2 P1 Rb2 87.45(2) 2_565 . ?
O3 P1 Rb2 69.17(13) . 1_556 ?
O1 P1 Rb2 124.13(9) 7_565 1_556 ?
O1 P1 Rb2 124.13(9) . 1_556 ?
O2 P1 Rb2 41.57(13) . 1_556 ?
Rb1 P1 Rb2 120.19(4) 6_657 1_556 ?
Rb1 P1 Rb2 64.97(3) 2_565 1_556 ?
Rb1 P1 Rb2 64.97(3) 2 1_556 ?
Rb2 P1 Rb2 86.13(2) 2 1_556 ?
Rb2 P1 Rb2 86.13(2) 2_565 1_556 ?
Rb2 P1 Rb2 168.36(4) . 1_556 ?
O3 P1 Rb1 46.61(13) . . ?
O1 P1 Rb1 83.32(10) 7_565 . ?
O1 P1 Rb1 83.32(10) . . ?
O2 P1 Rb1 157.35(14) . . ?
Rb1 P1 Rb1 124.03(6) 6_657 . ?
Rb1 P1 Rb1 119.50(3) 2_565 . ?
Rb1 P1 Rb1 119.50(3) 2 . ?
Rb2 P1 Rb1 62.32(3) 2 . ?
Rb2 P1 Rb1 62.32(3) 2_565 . ?
Rb2 P1 Rb1 52.58(3) . . ?
Rb2 P1 Rb1 115.78(4) 1_556 . ?
O1 Ca1 O1 98.35(12) 8_665 2_554 ?
O1 Ca1 F1 170.99(6) 8_665 . ?
O1 Ca1 F1 90.64(7) 2_554 . ?
O1 Ca1 F1 90.64(7) 8_665 3 ?
O1 Ca1 F1 170.99(6) 2_554 3 ?
F1 Ca1 F1 80.37(6) . 3 ?
O1 Ca1 O3 89.83(9) 8_665 1_554 ?
O1 Ca1 O3 89.83(9) 2_554 1_554 ?
F1 Ca1 O3 90.77(8) . 1_554 ?
F1 Ca1 O3 90.77(8) 3 1_554 ?
O1 Ca1 O2 92.67(9) 8_665 6_557 ?
O1 Ca1 O2 92.67(9) 2_554 6_557 ?
F1 Ca1 O2 86.31(8) . 6_557 ?
F1 Ca1 O2 86.31(8) 3 6_557 ?
O3 Ca1 O2 176.18(12) 1_554 6_557 ?
O1 Ca1 Rb1 133.95(7) 8_665 5_556 ?
O1 Ca1 Rb1 56.64(7) 2_554 5_556 ?
F1 Ca1 Rb1 51.68(4) . 5_556 ?
F1 Ca1 Rb1 116.14(5) 3 5_556 ?
O3 Ca1 Rb1 124.01(3) 1_554 5_556 ?
O2 Ca1 Rb1 55.58(3) 6_557 5_556 ?
O1 Ca1 Rb1 56.64(7) 8_665 5_566 ?
O1 Ca1 Rb1 133.95(7) 2_554 5_566 ?
F1 Ca1 Rb1 116.14(5) . 5_566 ?
F1 Ca1 Rb1 51.68(4) 3 5_566 ?
O3 Ca1 Rb1 124.01(3) 1_554 5_566 ?
O2 Ca1 Rb1 55.58(3) 6_557 5_566 ?
Rb1 Ca1 Rb1 110.55(6) 5_556 5_566 ?
O1 Ca1 Rb2 122.17(6) 8_665 6_556 ?
O1 Ca1 Rb2 122.17(6) 2_554 6_556 ?
F1 Ca1 Rb2 51.11(2) . 6_556 ?
F1 Ca1 Rb2 51.11(2) 3 6_556 ?
O3 Ca1 Rb2 125.74(10) 1_554 6_556 ?
O2 Ca1 Rb2 50.44(9) 6_557 6_556 ?
Rb1 Ca1 Rb2 65.54(3) 5_556 6_556 ?
Rb1 Ca1 Rb2 65.54(3) 5_566 6_556 ?
O1 Ca1 Rb2 58.97(7) 8_665 2_564 ?
O1 Ca1 Rb2 135.45(7) 2_554 2_564 ?
F1 Ca1 Rb2 114.46(6) . 2_564 ?
F1 Ca1 Rb2 50.72(4) 3 2_564 ?
O3 Ca1 Rb2 55.67(3) 1_554 2_564 ?
O2 Ca1 Rb2 123.54(3) 6_557 2_564 ?
Rb1 Ca1 Rb2 164.99(3) 5_556 2_564 ?
Rb1 Ca1 Rb2 68.41(5) 5_566 2_564 ?
Rb2 Ca1 Rb2 101.83(3) 6_556 2_564 ?
O1 Ca1 Rb2 135.45(7) 8_665 2_554 ?
O1 Ca1 Rb2 58.97(7) 2_554 2_554 ?
F1 Ca1 Rb2 50.72(4) . 2_554 ?
F1 Ca1 Rb2 114.46(6) 3 2_554 ?
O3 Ca1 Rb2 55.67(3) 1_554 2_554 ?
O2 Ca1 Rb2 123.54(3) 6_557 2_554 ?
Rb1 Ca1 Rb2 68.41(5) 5_556 2_554 ?
Rb1 Ca1 Rb2 164.99(3) 5_566 2_554 ?
Rb2 Ca1 Rb2 101.83(3) 6_556 2_554 ?
Rb2 Ca1 Rb2 108.48(5) 2_564 2_554 ?
O1 Ca1 Rb1 123.53(6) 8_665 1_554 ?
O1 Ca1 Rb1 123.53(6) 2_554 1_554 ?
F1 Ca1 Rb1 50.20(3) . 1_554 ?
F1 Ca1 Rb1 50.20(3) 3 1_554 ?
O3 Ca1 Rb1 57.93(9) 1_554 1_554 ?
O2 Ca1 Rb1 118.25(9) 6_557 1_554 ?
Rb1 Ca1 Rb1 101.87(2) 5_556 1_554 ?
Rb1 Ca1 Rb1 101.87(2) 5_566 1_554 ?
Rb2 Ca1 Rb1 67.81(3) 6_556 1_554 ?
Rb2 Ca1 Rb1 64.57(3) 2_564 1_554 ?
Rb2 Ca1 Rb1 64.57(3) 2_554 1_554 ?
Ca1 F1 Ca1 180.00(4) 5 . ?
Ca1 F1 Rb2 90.32(4) 5 6_556 ?
Ca1 F1 Rb2 89.68(4) . 6_556 ?
Ca1 F1 Rb2 89.68(4) 5 2_554 ?
Ca1 F1 Rb2 90.32(4) . 2_554 ?
Rb2 F1 Rb2 180.0 6_556 2_554 ?
Ca1 F1 Rb1 88.78(6) 5 1_554 ?
Ca1 F1 Rb1 91.22(5) . 1_554 ?
Rb2 F1 Rb1 92.33(3) 6_556 1_554 ?
Rb2 F1 Rb1 87.67(3) 2_554 1_554 ?
Ca1 F1 Rb1 91.22(6) 5 5_556 ?
Ca1 F1 Rb1 88.78(5) . 5_556 ?
Rb2 F1 Rb1 87.67(3) 6_556 5_556 ?
Rb2 F1 Rb1 92.33(3) 2_554 5_556 ?
Rb1 F1 Rb1 180.000(16) 1_554 5_556 ?
P1 O1 Ca1 170.86(13) . 2 ?
P1 O1 Rb2 99.31(11) . 2 ?
Ca1 O1 Rb2 89.31(8) 2 2 ?
P1 O1 Rb1 86.44(10) . 6_657 ?
Ca1 O1 Rb1 84.48(7) 2 6_657 ?
Rb2 O1 Rb1 166.03(8) 2 6_657 ?
P1 O1 Rb1 94.20(11) . 2 ?
Ca1 O1 Rb1 86.12(8) 2 2 ?
Rb2 O1 Rb1 68.33(6) 2 2 ?
Rb1 O1 Rb1 98.71(7) 6_657 2 ?
P1 O1 Rb2 97.04(11) . . ?
Ca1 O1 Rb2 82.88(8) 2 . ?
Rb2 O1 Rb2 109.07(7) 2 . ?
Rb1 O1 Rb2 82.61(6) 6_657 . ?
Rb1 O1 Rb2 168.75(7) 2 . ?
P1 O2 Ca1 153.6(2) . 6_657 ?
P1 O2 Rb2 117.22(17) . 1_556 ?
Ca1 O2 Rb2 89.19(12) 6_657 1_556 ?
P1 O2 Rb1 97.57(6) . 2_565 ?
Ca1 O2 Rb1 83.97(6) 6_657 2_565 ?
Rb2 O2 Rb1 85.06(7) 1_556 2_565 ?
P1 O2 Rb1 97.57(6) . 2 ?
Ca1 O2 Rb1 83.97(6) 6_657 2 ?
Rb2 O2 Rb1 85.06(7) 1_556 2 ?
Rb1 O2 Rb1 164.49(12) 2_565 2 ?
P1 O2 Rb1 74.87(14) . 6_657 ?
Ca1 O2 Rb1 78.72(10) 6_657 6_657 ?
Rb2 O2 Rb1 167.91(11) 1_556 6_657 ?
Rb1 O2 Rb1 93.58(6) 2_565 6_657 ?
Rb1 O2 Rb1 93.58(6) 2 6_657 ?
P1 O3 Ca1 163.5(2) . 1_556 ?
P1 O3 Rb2 97.37(6) . 2 ?
Ca1 O3 Rb2 85.47(6) 1_556 2 ?
P1 O3 Rb2 97.37(6) . 2_565 ?
Ca1 O3 Rb2 85.47(6) 1_556 2_565 ?
Rb2 O3 Rb2 156.78(12) 2 2_565 ?
P1 O3 Rb1 112.79(16) . . ?
Ca1 O3 Rb1 83.72(11) 1_556 . ?
Rb2 O3 Rb1 78.89(6) 2 . ?
Rb2 O3 Rb1 78.89(6) 2_565 . ?
P1 O3 Rb2 86.98(14) . 1_556 ?
Ca1 O3 Rb2 76.51(10) 1_556 1_556 ?
Rb2 O3 Rb2 99.30(6) 2 1_556 ?
Rb2 O3 Rb2 99.30(6) 2_565 1_556 ?
Rb1 O3 Rb2 160.23(10) . 1_556 ?

_refine_diff_density_max         1.016
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.152

_shelxl_version_number           2013-2

