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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CdCEPPA_publ
_database_code_depnum_ccdc_archive 'CCDC 1993189'
loop_
_audit_author_name
_audit_author_address
'Rosario Mercedes Perez Colodrero'
;Universidad de Malaga
Spain
;
_audit_update_record             
;
2020-11-19 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_pd_block_id                     
2020-11-19T09:38|CdCEPPA|Cd-phosphinate|D8_Advance

_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2020-11-19T09:38

#=============================================================================
# 5. OVERALL REFINEMENT & COMPUTING DETAILS

_refine_special_details          
; ?
;
_pd_proc_ls_special_details      
; ?
;

# The following items are used to identify the programs used.
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_ls_weighting_scheme      ?
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_number_constraints    ?

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?

#==============================================================================
# 6. SAMPLE PREPARATION DATA

# (In the unusual case where multiple samples are used in a single
#  Rietveld study, this information should be moved into the phase
#  blocks)

# The following three fields describe the preparation of the material.
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

_pd_char_colour                  white # use ICDD colour descriptions
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.02
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     134
_refine_ls_goodness_of_fit_all   2.66
_refine_ls_number_restraints     50
_refine_ls_matrix_type           full
#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C18 Cd O8 P2'

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C18 Cd O8 P2'
_chemical_compound_source        ? # for minerals and
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_exptl_crystal_description       Polycrystalline

_diffrn_ambient_temperature      298
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x+1/2,+y+1/2,-z+1/2
-1 -x,-y,-z
-2 +x+1/2,-y+1/2,+z+1/2

_exptl_crystal_F_000             ?
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?

_cell_measurement_temperature    298

_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   CdCEPPA
_cell_length_a                   14.9484(4)
_cell_length_b                   5.51968(13)
_cell_length_c                   23.7152(5)
_cell_angle_alpha                90.0
_cell_angle_beta                 95.4112(18)
_cell_angle_gamma                90.0
_cell_volume                     1948.03(9)

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Cd Cd1 0.7502(6) -0.3806(5) 1.0000(5) 1.0 Uiso 0.0226(10) 4
P P1 0.8336(12) 0.1053(28) 1.0861(6) 1.0 Uiso 0.0327(21) 4
P P2 0.6715(12) 0.1158(28) 0.9139(6) 1.0 Uiso 0.0327(21) 4
C C1 0.8551(24) 0.136(6) 1.1628(7) 1.0 Uiso 0.0052(16) 4
C C2 0.8952(24) -0.062(5) 1.1934(10) 1.0 Uiso 0.0052(16) 4
C C3 0.9196(19) -0.033(5) 1.2512(10) 1.0 Uiso 0.0052(16) 4
C C4 0.8854(25) 0.163(5) 1.2797(7) 1.0 Uiso 0.0052(16) 4
C C5 0.8416(27) 0.353(5) 1.2499(10) 1.0 Uiso 0.0052(16) 4
C C6 0.8274(24) 0.343(5) 1.1910(10) 1.0 Uiso 0.0052(16) 4
C C7 0.9402(16) 0.197(5) 1.0628(18) 1.0 Uiso 0.0052(16) 4
C C8 0.9721(16) 0.444(5) 1.0830(15) 1.0 Uiso 0.0052(16) 4
C C9 1.0671(18) 0.512(6) 1.0728(15) 1.0 Uiso 0.0052(16) 4
C C10 0.6587(22) 0.153(5) 0.8373(7) 1.0 Uiso 0.0052(16) 4
C C11 0.6089(20) -0.012(4) 0.8017(11) 1.0 Uiso 0.0052(16) 4
C C12 0.6113(19) 0.011(4) 0.7434(10) 1.0 Uiso 0.0052(16) 4
C C13 0.6328(20) 0.238(5) 0.7216(7) 1.0 Uiso 0.0052(16) 4
C C14 0.6679(20) 0.421(4) 0.7584(11) 1.0 Uiso 0.0052(16) 4
C C15 0.6953(18) 0.361(5) 0.8143(10) 1.0 Uiso 0.0052(16) 4
C C16 0.5631(14) 0.158(5) 0.9405(16) 1.0 Uiso 0.0052(16) 4
C C17 0.5107(17) 0.363(6) 0.9112(14) 1.0 Uiso 0.0052(16) 4
C C18 0.4225(20) 0.441(5) 0.9317(14) 1.0 Uiso 0.0052(16) 4
O O1 0.8155(16) -0.1642(29) 1.0736(11) 1.0 Uiso 0.0052(16) 4
O O2 0.7597(16) 0.278(4) 1.0646(11) 1.0 Uiso 0.0052(16) 4
O O3 1.0953(18) 0.695(4) 1.0998(11) 1.0 Uiso 0.0052(16) 4
O O4 1.0989(19) 0.384(4) 1.0364(12) 1.0 Uiso 0.0052(16) 4
O O5 0.7038(15) -0.1426(31) 0.9273(10) 1.0 Uiso 0.0052(16) 4
O O6 0.7362(17) 0.314(4) 0.9349(12) 1.0 Uiso 0.0052(16) 4
O O7 0.4015(21) 0.3055(35) 0.9700(11) 1.0 Uiso 0.0052(16) 4
O O8 0.3909(17) 0.634(4) 0.9112(11) 1.0 Uiso 0.0052(16) 4
_chemical_formula_weight         518.55
_cell_formula_units_Z            4

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O1 2.260(25) . 1_555 N
Cd1 O2 2.424(22) . 1_545 N
Cd1 O4 2.490(28) . -1_757 N
Cd1 O5 2.225(22) . 1_555 N
Cd1 O6 2.280(23) . 1_545 N
Cd1 O7 2.475(30) . -1_657 N
P1 C1 1.826(6) . 1_555 N
P1 C7 1.807(7) . 1_555 N
P1 O1 1.536(6) . 1_555 N
P1 O2 1.511(6) . 1_555 N
P2 C10 1.820(6) . 1_555 N
P2 C16 1.809(6) . 1_555 N
P2 O5 1.529(6) . 1_555 N
P2 O6 1.515(6) . 1_555 N
C1 P1 1.826(6) . 1_555 N
C1 C2 1.415(6) . 1_555 N
C1 C6 1.407(6) . 1_555 N
C2 C1 1.415(6) . 1_555 N
C2 C3 1.394(6) . 1_555 N
C3 C2 1.394(6) . 1_555 N
C3 C4 1.398(7) . 1_555 N
C4 C3 1.398(7) . 1_555 N
C4 C5 1.395(6) . 1_555 N
C5 C4 1.395(6) . 1_555 N
C5 C6 1.393(6) . 1_555 N
C6 C1 1.407(6) . 1_555 N
C6 C5 1.393(6) . 1_555 N
C7 P1 1.807(7) . 1_555 N
C7 C8 1.508(7) . 1_555 N
C8 C7 1.508(7) . 1_555 N
C8 C9 1.510(7) . 1_555 N
C9 C8 1.510(7) . 1_555 N
C9 O3 1.249(7) . 1_555 N
C9 O4 1.241(7) . 1_555 N
C10 P2 1.820(6) . 1_555 N
C10 C11 1.4047(20) . 1_555 N
C10 C15 1.4045(20) . 1_555 N
C11 C10 1.4047(20) . 1_555 N
C11 C12 1.3921(19) . 1_555 N
C12 C11 1.3921(19) . 1_555 N
C12 C13 1.4037(20) . 1_555 N
C13 C12 1.4037(20) . 1_555 N
C13 C14 1.4033(20) . 1_555 N
C14 C13 1.4033(20) . 1_555 N
C14 C15 1.3911(19) . 1_555 N
C15 C10 1.4045(20) . 1_555 N
C15 C14 1.3911(19) . 1_555 N
C16 P2 1.809(6) . 1_555 N
C16 C17 1.506(7) . 1_555 N
C17 C16 1.506(7) . 1_555 N
C17 C18 1.511(7) . 1_555 N
C18 C17 1.511(7) . 1_555 N
C18 O7 1.239(7) . 1_555 N
C18 O8 1.248(7) . 1_555 N
O1 Cd1 2.260(25) . 1_555 N
O1 P1 1.536(6) . 1_555 N
O2 Cd1 2.424(22) . 1_565 N
O2 P1 1.511(6) . 1_555 N
O3 C9 1.249(7) . 1_555 N
O4 Cd1 2.490(28) . -1_757 N
O4 C9 1.241(7) . 1_555 N
O5 Cd1 2.225(22) . 1_555 N
O5 P2 1.529(6) . 1_555 N
O6 Cd1 2.280(23) . 1_565 N
O6 P2 1.515(6) . 1_555 N
O7 Cd1 2.475(30) . -1_657 N
O7 C18 1.239(7) . 1_555 N
O8 C18 1.248(7) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 O2 85.9(8) 1_555 . 1_545 N
O1 Cd1 O5 111.5(5) 1_555 . 1_555 N
O1 Cd1 O6 156.8(9) 1_555 . 1_545 N
O2 Cd1 O5 160.7(8) 1_545 . 1_555 N
O2 Cd1 O6 81.4(5) 1_545 . 1_545 N
O5 Cd1 O6 84.8(8) 1_555 . 1_545 N
C1 P1 C7 101.6(17) 1_555 . 1_555 N
C1 P1 O1 107.1(8) 1_555 . 1_555 N
C1 P1 O2 109.5(8) 1_555 . 1_555 N
C7 P1 O1 110.8(12) 1_555 . 1_555 N
C7 P1 O2 111.0(8) 1_555 . 1_555 N
O1 P1 O2 115.8(9) 1_555 . 1_555 N
C10 P2 C16 108.7(16) 1_555 . 1_555 N
C10 P2 O5 108.2(8) 1_555 . 1_555 N
C10 P2 O6 104.5(14) 1_555 . 1_555 N
C16 P2 O5 108.9(8) 1_555 . 1_555 N
C16 P2 O6 110.9(8) 1_555 . 1_555 N
O5 P2 O6 115.3(9) 1_555 . 1_555 N
P1 C1 C2 117.8(15) 1_555 . 1_555 N
P1 C1 C6 121.1(15) 1_555 . 1_555 N
C2 C1 C6 121.0(5) 1_555 . 1_555 N
C1 C2 C3 118.3(6) 1_555 . 1_555 N
C2 C3 C4 119.4(7) 1_555 . 1_555 N
C3 C4 C5 120.9(6) 1_555 . 1_555 N
C4 C5 C6 119.9(6) 1_555 . 1_555 N
C1 C6 C5 119.0(6) 1_555 . 1_555 N
P1 C7 C8 114.6(18) 1_555 . 1_555 N
C7 C8 C9 116.6(20) 1_555 . 1_555 N
C8 C9 O3 113.4(23) 1_555 . 1_555 N
C8 C9 O4 113.5(23) 1_555 . 1_555 N
O3 C9 O4 132.9(16) 1_555 . 1_555 N
P2 C10 C11 121.9(19) 1_555 . 1_555 N
P2 C10 C15 118.1(19) 1_555 . 1_555 N
C11 C10 C15 119.88(5) 1_555 . 1_555 N
C10 C11 C12 118.40(20) 1_555 . 1_555 N
C11 C12 C13 118.46(20) 1_555 . 1_555 N
C12 C13 C14 119.88(5) 1_555 . 1_555 N
C13 C14 C15 118.58(20) 1_555 . 1_555 N
C10 C15 C14 118.48(20) 1_555 . 1_555 N
P2 C16 C17 112.3(17) 1_555 . 1_555 N
C16 C17 C18 119.7(20) 1_555 . 1_555 N
C17 C18 O7 110.7(23) 1_555 . 1_555 N
C17 C18 O8 115.3(21) 1_555 . 1_555 N
O7 C18 O8 133.6(16) 1_555 . 1_555 N
Cd1 O1 P1 135.8(13) 1_555 . 1_555 N
Cd1 O2 P1 134.5(15) 1_565 . 1_555 N
Cd1 O5 P2 141.3(14) 1_555 . 1_555 N
Cd1 O6 P2 140.5(16) 1_565 . 1_555 N

# Powder diffraction data for histogram  1
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
; ?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a~1~'
_diffrn_radiation_wavelength     0.7093
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'D8 ADVANCE (Bruker AXS) diffractometer'
_diffrn_source_target            ?
_diffrn_measurement_device_type  'D8 ADVANCE (Bruker AXS) diffractometer'
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             ? # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       ?
_computing_data_reduction        ?

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     ?

# The following item is used for angular dispersive measurements only.

_diffrn_radiation_monochromator  ?

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          ?
_pd_instr_dist_mono/spec         ?
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         ?

# 10. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;

_pd_spec_mount_mode              ? # options are 'reflection'
# or 'transmission'

_pd_spec_shape                   ? # options are 'cylinder'
# 'flat_sheet' or 'irregular'


loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Mg 0.0 0.050 0.037 5.42040 2.82750 2.17350 79.2611 1.22690 0.38080 2.30730
7.19370 0.85840 International_Tables_Vol_C
Cd 4.0 -0.777 1.215 19.2214 0.59460 17.6444 6.90890 4.46100 24.7008 1.60290
87.4825 5.06940 International_Tables_Vol_C
P 8.0 0.102 0.095 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080
68.1645 1.11490 International_Tables_Vol_C
C 72.0 0.003 0.002 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
O 32.0 0.011 0.006 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
_diffrn_radiation_polarisn_ratio ?
_pd_proc_ls_prof_R_factor        0.0553
_pd_proc_ls_prof_wR_factor       0.0738
_pd_proc_ls_prof_wR_expected     0.0294
_refine_ls_R_Fsqd_factor         0.06502

_pd_proc_ls_background_function  
;   GSAS Background function number 7 with 36 terms.
 Linear interpolation
      1:    108344.     2:    84301.6     3:    70778.6     4:    67580.1    
      5:    61861.6     6:    58491.0     7:    61001.7     8:    44289.3    
      9:    38190.8    10:    32575.9    11:    32833.1    12:    27239.9    
     13:    23819.2    14:    23527.1    15:    20192.8    16:    21393.4    
     17:    24261.5    18:    18843.2    19:    20516.0    20:    21815.5    
     21:    17926.5    22:    22366.5    23:    18514.5    24:    18571.0    
     25:    17913.8    26:    19638.1    27:    17158.9    28:    16520.6    
     29:    13901.2    30:    15592.4    31:    11828.6    32:    10555.6    
     33:    7709.71    34:    3284.43    35:    1016.58    36:   -2442.94    
;

_exptl_absorpt_process_details   
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_T_max  1.00000
_pd_proc_ls_pref_orient_corr     
;   March-Dollase
 AXIS  1 Ratio=   0.99445  h= 0.000  k= 0.000  l= 1.000
 Prefered orientation correction range: Min=   0.99168, Max=   1.01685
;

_pd_proc_ls_profile_function     
;
 CW Profile function number 3 with  19 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 #1(GU)   =    0.000 #2(GV)   =    0.000 #3(GW)   =    1.890
 #4(GP)   =    0.000 #5(LX)   =    0.000 #6(LY)   =   17.184
 #7(S/L)  =   0.0132 #8(H/L)  =   0.0142
 #9(trns) =     0.00 #10(shft)=   0.0000
 #11(stec)=     0.00 #12(ptec)=     0.00 #13(sfec)=     0.00
 #14(L11) =    0.000 #15(L22) =    0.000 #16(L33) =    0.000
 #17(L12) =    0.000 #18(L13) =    0.000 #19(L23) =    0.000
 Peak tails are ignored  where the intensity is below 0.0030 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_peak_cutoff          0.00300
_pd_proc_info_datetime           2020-11-19T09:38:44
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        4.0
_pd_meas_2theta_range_max        44.99
_pd_meas_2theta_range_inc        0.01
_pd_proc_2theta_range_min        3.99924
_pd_proc_2theta_range_max        44.98923
_pd_proc_2theta_range_inc        0.01
_pd_meas_number_of_points        4100
_pd_proc_number_of_points        4100

_reflns_number_total             1830
_reflns_limit_h_min              0
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              5
_reflns_limit_l_min              -23
_reflns_limit_l_max              22
_reflns_d_resolution_high        1.037
_reflns_d_resolution_low         7.441

#--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#
####################################################################### 
# 
# 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_S1_publ
_database_code_depnum_ccdc_archive 'CCDC 1993190'
loop_
_audit_author_name
_audit_author_address
'Rosario Mercedes Perez Colodrero'
;Universidad de Malaga
Spain
;
_audit_update_record             
;
2020-11-19 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_pd_block_id                     2020-04-28T16:52|S1|S1_Ilia|Mythen

_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2020-04-28T16:52

#=============================================================================
# 5. OVERALL REFINEMENT & COMPUTING DETAILS

_refine_special_details          
; ?
;
_pd_proc_ls_special_details      
; ?
;

# The following items are used to identify the programs used.
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_ls_weighting_scheme      ?
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_number_constraints    ?

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?

#==============================================================================
# 6. SAMPLE PREPARATION DATA

# (In the unusual case where multiple samples are used in a single
#  Rietveld study, this information should be moved into the phase
#  blocks)

# The following three fields describe the preparation of the material.
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

_pd_char_colour                  pink # use ICDD colour descriptions
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     133
_refine_ls_goodness_of_fit_all   11.53
_refine_ls_number_restraints     78
_refine_ls_matrix_type           full
#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C36 Co4 O20 P4, 4(O)'

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C36 Co4 O24 P4'
_chemical_compound_source        ? # for minerals and
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_exptl_crystal_description       polycrystalline

_diffrn_ambient_temperature      298
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/a'
_space_group_name_Hall           '-P 2yab'
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x+1/2,+y+1/2,-z
-1 -x,-y,-z
-2 +x+1/2,-y+1/2,+z

_exptl_crystal_F_000             ?
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?

_cell_measurement_temperature    298

_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   'from C:/gsas/MyWork/Ilia/S1/S1-Ilia.cif'
_cell_length_a                   9.39192(24)
_cell_length_b                   23.4056(6)
_cell_length_c                   10.51984(25)
_cell_angle_alpha                90.0
_cell_angle_beta                 95.5626(19)
_cell_angle_gamma                90.0
_cell_volume                     2301.62(10)

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Co Co1 0.0 0.0 0.0 1.0 Uiso 0.0193(18) 2
Co Co2 0.0 0.0 0.5 1.0 Uiso 0.0193(18) 2
Co Co3 -0.2123(7) -0.01947(27) 0.2317(7) 1.0 Uiso 0.0193(18) 4
P P1 -0.0115(15) 0.0933(5) 0.2608(14) 1.0 Uiso 0.015(4) 4
O O11 -0.1002(25) 0.0482(9) 0.1766(21) 1.0 Uiso 0.0088(24) 4
O O21 0.0726(26) 0.0664(8) 0.3736(20) 1.0 Uiso 0.0088(24) 4
C C11 0.1418(33) 0.1294(13) 0.1982(34) 1.0 Uiso 0.0088(24) 4
C C21 0.270(4) 0.0957(14) 0.1643(31) 1.0 Uiso 0.0088(24) 4
C C31 0.286(4) 0.0886(15) 0.0132(31) 1.0 Uiso 0.0088(24) 4
O O31 0.3400(28) 0.1262(11) -0.0499(25) 1.0 Uiso 0.0088(24) 4
O O41 0.1802(27) 0.0582(10) -0.0383(23) 1.0 Uiso 0.0088(24) 4
C C41b -0.1452(35) 0.1446(14) 0.299(4) 1.0 Uiso 0.0088(24) 4
C C51b -0.263(4) 0.1440(15) 0.2129(32) 1.0 Uiso 0.0088(24) 4
C C61b -0.378(4) 0.1842(17) 0.232(4) 1.0 Uiso 0.0088(24) 4
C C71b -0.357(4) 0.2266(14) 0.325(4) 1.0 Uiso 0.0088(24) 4
C C81b -0.239(4) 0.2213(15) 0.4133(31) 1.0 Uiso 0.0088(24) 4
C C91b -0.121(4) 0.1896(17) 0.393(4) 1.0 Uiso 0.0088(24) 4
P P2 -0.0965(15) 0.0862(6) -0.2528(13) 1.0 Uiso 0.015(4) 4
O O12 -0.1487(25) 0.0478(9) -0.1400(21) 1.0 Uiso 0.0088(24) 4
O O22 -0.0279(23) -0.0579(9) 0.3136(19) 1.0 Uiso 0.0088(24) 4
C C12 -0.2721(31) 0.0935(13) -0.3334(32) 1.0 Uiso 0.0088(24) 4
C C22 -0.356(4) 0.0444(14) 0.6066(30) 1.0 Uiso 0.0088(24) 4
C C32 -0.3442(34) 0.0450(16) 0.4514(32) 1.0 Uiso 0.0088(24) 4
O O32 -0.2307(19) 0.0160(11) 0.4289(23) 1.0 Uiso 0.0088(24) 4
O O42 -0.4535(27) 0.0557(10) 0.3835(25) 1.0 Uiso 0.0088(24) 4
C C42b -0.037(4) 0.1547(11) -0.192(4) 1.0 Uiso 0.0088(24) 4
C C52b -0.124(4) 0.1857(16) -0.113(4) 1.0 Uiso 0.0088(24) 4
C C62b -0.072(4) 0.2415(14) -0.0805(35) 1.0 Uiso 0.0088(24) 4
C C72b 0.518(4) 0.2289(12) 0.845(4) 1.0 Uiso 0.0088(24) 4
C C82b 0.108(4) 0.2406(15) 0.770(4) 1.0 Uiso 0.0088(24) 4
C C92b 0.085(4) 0.1828(15) -0.239(4) 1.0 Uiso 0.0088(24) 4
O Ow1 -0.4025(27) 0.0138(10) 0.1618(22) 1.0 Uiso 0.0088(24) 4
O Ow2 -0.3552(25) -0.0850(9) 0.2785(25) 1.0 Uiso 0.0088(24) 4
O Ow3 -0.3327(27) -0.1154(10) 0.5275(25) 1.0 Uiso 0.0088(24) 4
O Ow4 0.5899(27) 0.0706(10) 0.9394(24) 1.0 Uiso 0.0088(24) 4
_chemical_formula_weight         1175.96
_cell_formula_units_Z            2

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O11 2.439(21) . 1_555 N
Co1 O11 2.439(21) . -1_555 N
Co1 O41 2.240(22) . 1_555 N
Co1 O41 2.240(22) . -1_555 N
Co1 O12 2.230(21) . 1_555 N
Co1 O12 2.230(21) . -1_555 N
Co2 O21 2.196(17) . 1_555 N
Co2 O21 2.196(17) . -1_556 N
Co2 O22 2.378(17) . 1_555 N
Co2 O22 2.378(17) . -1_556 N
Co2 O32 2.254(17) . 1_555 N
Co2 O32 2.254(17) . -1_556 N
Co3 O11 2.017(20) . 1_555 N
Co3 O41 2.274(24) . -1_555 N
Co3 O22 2.065(21) . 1_555 N
Co3 O32 2.257(23) . 1_555 N
Co3 Ow1 2.021(24) . 1_555 N
Co3 Ow2 2.127(21) . 1_555 N
P1 O11 1.566(19) . 1_555 N
P1 O21 1.499(19) . 1_555 N
P1 C11 1.845(25) . 1_555 N
P1 C41b 1.810(22) . 1_555 N
O11 Co1 2.439(21) . 1_555 N
O11 Co3 2.017(20) . 1_555 N
O11 P1 1.566(19) . 1_555 N
O21 Co2 2.196(17) . 1_555 N
O21 P1 1.499(19) . 1_555 N
C11 P1 1.845(25) . 1_555 N
C11 C21 1.511(28) . 1_555 N
C21 C11 1.511(28) . 1_555 N
C21 C31 1.620(28) . 1_555 N
C31 C21 1.620(28) . 1_555 N
C31 O31 1.238(26) . 1_555 N
C31 O41 1.298(27) . 1_555 N
O31 C31 1.238(26) . 1_555 N
O41 Co1 2.240(22) . 1_555 N
O41 Co3 2.274(24) . -1_555 N
O41 C31 1.298(27) . 1_555 N
C41b P1 1.810(22) . 1_555 N
C41b C51b 1.361(27) . 1_555 N
C41b C91b 1.446(26) . 1_555 N
C51b C41b 1.361(27) . 1_555 N
C51b C61b 1.460(28) . 1_555 N
C61b C51b 1.460(28) . 1_555 N
C61b C71b 1.391(27) . 1_555 N
C71b C61b 1.391(27) . 1_555 N
C71b C81b 1.389(27) . 1_555 N
C81b C71b 1.389(27) . 1_555 N
C81b C91b 1.364(29) . 1_555 N
C91b C41b 1.446(26) . 1_555 N
C91b C81b 1.364(29) . 1_555 N
P2 O12 1.604(20) . 1_555 N
P2 O22 1.535(18) . -1_555 N
P2 C12 1.788(24) . 1_555 N
P2 C42b 1.793(22) . 1_555 N
O12 Co1 2.230(21) . 1_555 N
O12 P2 1.604(20) . 1_555 N
O22 Co2 2.378(17) . 1_555 N
O22 Co3 2.065(21) . 1_555 N
O22 P2 1.535(18) . -1_555 N
C12 P2 1.788(24) . 1_555 N
C12 C22 1.500(27) . 1_554 N
C22 C12 1.500(27) . 1_556 N
C22 C32 1.648(28) . 1_555 N
C32 C22 1.648(28) . 1_555 N
C32 O32 1.305(26) . 1_555 N
C32 O42 1.218(25) . 1_555 N
O32 Co2 2.254(17) . 1_555 N
O32 Co3 2.257(23) . 1_555 N
O32 C32 1.305(26) . 1_555 N
O42 C32 1.218(25) . 1_555 N
C42b P2 1.793(22) . 1_555 N
C42b C52b 1.416(26) . 1_555 N
C42b C92b 1.453(26) . 1_555 N
C52b C42b 1.416(26) . 1_555 N
C52b C62b 1.423(28) . 1_555 N
C62b C52b 1.423(28) . 1_555 N
C62b C72b 1.396(28) . -2_454 N
C72b C62b 1.396(28) . -2_556 N
C72b C82b 1.406(27) . -2_555 N
C82b C72b 1.406(27) . -2_455 N
C82b C92b 1.371(27) . 1_556 N
C92b C42b 1.453(26) . 1_555 N
C92b C82b 1.371(27) . 1_554 N
Ow1 Co3 2.021(24) . 1_555 N
Ow2 Co3 2.127(21) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Co3 O22 91.3(9) 1_555 . 1_555 N
O11 Co3 Ow1 93.5(10) 1_555 . 1_555 N
O11 Co3 Ow2 172.3(10) 1_555 . 1_555 N
O22 Co3 Ow1 174.9(10) 1_555 . 1_555 N
O22 Co3 Ow2 96.4(9) 1_555 . 1_555 N
Ow1 Co3 Ow2 78.8(9) 1_555 . 1_555 N
O11 P1 O21 112.0(16) 1_555 . 1_555 N
O11 P1 C11 119.9(17) 1_555 . 1_555 N
O11 P1 C41b 103.4(17) 1_555 . 1_555 N
O21 P1 C11 96.1(15) 1_555 . 1_555 N
O21 P1 C41b 115.2(18) 1_555 . 1_555 N
C11 P1 C41b 111.0(17) 1_555 . 1_555 N
Co3 O11 P1 129.1(15) 1_555 . 1_555 N
P1 C11 C21 120.8(24) 1_555 . 1_555 N
C11 C21 C31 116.0(29) 1_555 . 1_555 N
C21 C31 O31 122.4(30) 1_555 . 1_555 N
C21 C31 O41 108.9(26) 1_555 . 1_555 N
O31 C31 O41 120.1(32) 1_555 . 1_555 N
P1 C41b C51b 112.4(28) 1_555 . 1_555 N
P1 C41b C91b 124.7(29) 1_555 . 1_555 N
C51b C41b C91b 121.7(23) 1_555 . 1_555 N
C41b C51b C61b 117.8(22) 1_555 . 1_555 N
C51b C61b C71b 120.2(25) 1_555 . 1_555 N
C61b C71b C81b 116.9(24) 1_555 . 1_555 N
C71b C81b C91b 123.6(26) 1_555 . 1_555 N
C41b C91b C81b 115.4(24) 1_555 . 1_555 N
O12 P2 O22 111.5(15) 1_555 . -1_555 N
O12 P2 C12 94.1(16) 1_555 . 1_555 N
O12 P2 C42b 110.1(17) 1_555 . 1_555 N
O22 P2 C12 123.2(16) -1_555 . 1_555 N
O22 P2 C42b 108.2(16) -1_555 . 1_555 N
C12 P2 C42b 108.8(17) 1_555 . 1_555 N
Co3 O22 P2 131.0(14) 1_555 . -1_555 N
P2 C12 C22 123.5(25) 1_555 . 1_554 N
C12 C22 C32 109.0(27) 1_556 . 1_555 N
C22 C32 O32 108.2(26) 1_555 . 1_555 N
C22 C32 O42 116.6(30) 1_555 . 1_555 N
O32 C32 O42 131.1(32) 1_555 . 1_555 N
P2 C42b C52b 119.4(27) 1_555 . 1_555 N
P2 C42b C92b 120.8(28) 1_555 . 1_555 N
C52b C42b C92b 119.0(21) 1_555 . 1_555 N
C42b C52b C62b 114.2(23) 1_555 . 1_555 N
C52b C62b C72b 122.1(28) 1_555 . -2_564 N
C62b C72b C82b 119.7(26) -2_666 . -2_665 N
C72b C82b C92b 116.1(24) -2_565 . 1_556 N
C42b C92b C82b 123.2(24) 1_555 . 1_554 N

# Powder diffraction data for histogram  1
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
; ?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4124
_diffrn_source                   synchrotron
_diffrn_source_type              'BL04-MSPD (Alba synchrotron)'
_diffrn_source_target            ?
_diffrn_measurement_device_type  'BL04-MSPD (Alba synchrotron)'
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             ? # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       ?
_computing_data_reduction        ?

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     ?

# The following item is used for angular dispersive measurements only.

_diffrn_radiation_monochromator  ?

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          ?
_pd_instr_dist_mono/spec         ?
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         ?

# 10. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;

_pd_spec_mount_mode              ? # options are 'reflection'
# or 'transmission'

_pd_spec_shape                   ? # options are 'cylinder'
# 'flat_sheet' or 'irregular'


loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Co 8.0 0.213 0.354 12.2841 4.27910 7.34090 0.27840 4.00340 13.5359 2.34880
71.1692 1.01180 International_Tables_Vol_C
P 8.0 0.035 0.031 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080
68.1645 1.11490 International_Tables_Vol_C
O 48.0 0.002 0.002 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
C 72.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
_diffrn_radiation_polarisn_ratio 1.0
_pd_proc_ls_prof_R_factor        0.0794
_pd_proc_ls_prof_wR_factor       0.1066
_pd_proc_ls_prof_wR_expected     0.0097
_refine_ls_R_Fsqd_factor         0.15531

_pd_proc_ls_background_function  
;   GSAS Background function number 7 with 20 terms.
 Linear interpolation
      1:    126.361     2:    91.5906     3:    74.6021     4:    69.6256    
      5:    70.0491     6:    63.4089     7:    52.0356     8:    39.1737    
      9:    43.4772    10:    33.2126    11:    31.6297    12:    33.5042    
     13:    26.7971    14:    32.1393    15:    35.1304    16:    33.6033    
     17:    31.4787    18:    33.4288    19:    28.1571    20:    26.2462    
;

_exptl_absorpt_process_details   
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_T_max  1.00000
_pd_proc_ls_pref_orient_corr     
;   March-Dollase
 AXIS  1 Ratio=   0.91455  h= 0.000  k= 1.000  l= 0.000
 Prefered orientation correction range: Min=   0.87461, Max=   1.30730
;

_pd_proc_ls_profile_function     
;
 CW Profile function number 3 with  19 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 #1(GU)   =   70.447 #2(GV)   =   -4.051 #3(GW)   =    0.460
 #4(GP)   =    0.000 #5(LX)   =    0.328 #6(LY)   =    0.000
 #7(S/L)  =   0.0027 #8(H/L)  =   0.0067
 #9(trns) =     0.00 #10(shft)=   0.0000
 #11(stec)=     0.00 #12(ptec)=     0.00 #13(sfec)=     0.00
 #14(L11) =    0.000 #15(L22) =    0.000 #16(L33) =    0.000
 #17(L12) =    0.000 #18(L13) =    0.000 #19(L23) =    0.000
 Peak tails are ignored  where the intensity is below 0.0020 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_peak_cutoff          0.00200
_pd_proc_info_datetime           2020-04-28T16:52:58
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        0.32586
_pd_meas_2theta_range_max        44.54586
_pd_meas_2theta_range_inc        0.006
_pd_proc_2theta_range_min        0.3295
_pd_proc_2theta_range_max        44.5495
_pd_proc_2theta_range_inc        0.006
_pd_meas_number_of_points        7371
_pd_proc_number_of_points        7371

_reflns_number_total             1441
_reflns_limit_h_min              0
_reflns_limit_h_max              7
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              -8
_reflns_limit_l_max              8
_reflns_d_resolution_high        1.187
_reflns_d_resolution_low         11.703

#--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#
####################################################################### 
# 
# 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_CaCEPPA_publ
_database_code_depnum_ccdc_archive 'CCDC 1993191'
loop_
_audit_author_name
_audit_author_address
'Rosario Mercedes Perez Colodrero'
;Universidad de Malaga
Spain
;
_audit_update_record             
;
2020-11-19 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_pd_block_id                     2020-03-23T17:31|CaCEPPA|CaCEPPA|D8_Advance

_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2020-03-23T17:31

#=============================================================================
# 5. OVERALL REFINEMENT & COMPUTING DETAILS

_refine_special_details          
; ?
;
_pd_proc_ls_special_details      
; ?
;

# The following items are used to identify the programs used.
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_ls_weighting_scheme      ?
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_number_constraints    ?

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?

#==============================================================================
# 6. SAMPLE PREPARATION DATA

# (In the unusual case where multiple samples are used in a single
#  Rietveld study, this information should be moved into the phase
#  blocks)

# The following three fields describe the preparation of the material.
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

_pd_char_colour                  white # use ICDD colour descriptions
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     138
_refine_ls_goodness_of_fit_all   3.45
_refine_ls_number_restraints     71
_refine_ls_matrix_type           full
#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '2(C9 O4 P), Ca'

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C18 Ca O8 P2'
_chemical_compound_source        ? # for minerals and
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_exptl_crystal_description       polycrystalline

_diffrn_ambient_temperature      298
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P n'
_space_group_name_Hall           'P -2yac'
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 +x+1/2,-y,+z+1/2

_exptl_crystal_F_000             ?
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?

_cell_measurement_temperature    298

_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   
'from C:/GSAS/MyWork/CaCEPPA_ILIA/CaCEPPA_LB/C18H20O8P2Ca_best1.cif'
_cell_length_a                   14.4949(7)
_cell_length_b                   5.76901(27)
_cell_length_c                   12.9059(5)
_cell_angle_alpha                90.0
_cell_angle_beta                 113.4324(23)
_cell_angle_gamma                90.0
_cell_volume                     990.20(9)

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Ca Ca1 0.8338(11) 0.3656(11) 0.12794 1.0 Uiso 0.0127(12) 2
P P1 0.8352(8) 0.8749(18) -0.0557(7) 1.0 Uiso 0.0127(12) 2
P P2 0.8365(7) 0.8608(18) 0.3076(7) 1.0 Uiso 0.0127(12) 2
C C1 0.8956(15) 0.8925(26) -0.1552(14) 1.0 Uiso 0.0100(17) 2
C C2 0.9255(17) 1.1092(24) -0.1816(16) 1.0 Uiso 0.0100(17) 2
C C3 0.9499(17) 1.1201(31) -0.2766(16) 1.0 Uiso 0.0100(17) 2
C C4 0.9912(18) 0.921(4) -0.3042(18) 1.0 Uiso 0.0100(17) 2
C C5 0.9645(18) 0.7046(32) -0.2750(16) 1.0 Uiso 0.0100(17) 2
C C6 0.9387(16) 0.6937(24) -0.1809(16) 1.0 Uiso 0.0100(17) 2
C C7 0.7084(9) 0.7856(34) -0.1402(19) 1.0 Uiso 0.0100(17) 2
C C8 0.6925(14) 0.5424(30) -0.1867(19) 1.0 Uiso 0.0100(17) 2
C C9 0.5912(12) 0.514(5) -0.2811(20) 1.0 Uiso 0.0100(17) 2
C C10 0.7665(12) 0.8683(31) 0.3971(13) 1.0 Uiso 0.0100(17) 2
C C11 0.6814(13) 0.7265(32) 0.3712(13) 1.0 Uiso 0.0100(17) 2
C C12 0.6434(14) 0.6936(33) 0.4544(17) 1.0 Uiso 0.0100(17) 2
C C13 0.6611(16) 0.865(4) 0.5367(17) 1.0 Uiso 0.0100(17) 2
C C14 0.7449(16) 1.0103(31) 0.5614(12) 1.0 Uiso 0.0100(17) 2
C C15 0.7835(13) 1.0420(26) 0.4786(15) 1.0 Uiso 0.0100(17) 2
C C16 0.9651(8) 0.830(4) 0.4060(17) 1.0 Uiso 0.0100(17) 2
C C17 0.9831(14) 0.615(5) 0.4775(19) 1.0 Uiso 0.0100(17) 2
C C18 1.0836(12) 0.499(4) 0.5102(22) 1.0 Uiso 0.0100(17) 2
O O1 0.8924(14) 0.6924(27) 0.0326(13) 1.0 Uiso 0.0100(17) 2
O O2 0.8405(15) 1.1155(23) -0.0038(14) 1.0 Uiso 0.0100(17) 2
O O3 0.5748(16) 0.384(4) -0.3628(15) 1.0 Uiso 0.0100(17) 2
O O4 0.5218(15) 0.630(4) -0.2755(17) 1.0 Uiso 0.0100(17) 2
O O5 0.8005(15) 0.6456(26) 0.2336(14) 1.0 Uiso 0.0100(17) 2
O O6 0.8169(16) 1.0802(25) 0.2379(15) 1.0 Uiso 0.0100(17) 2
O O7 1.1490(15) 0.619(4) 0.4961(17) 1.0 Uiso 0.0100(17) 2
O O8 1.1073(15) 0.3413(31) 0.5829(16) 1.0 Uiso 0.0100(17) 2
_chemical_formula_weight         446.22
_cell_formula_units_Z            2

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.573(18) . 1_555 N
Ca1 O2 2.262(14) . 1_545 N
Ca1 O4 2.506(25) . 2_565 N
Ca1 O5 2.286(16) . 1_555 N
Ca1 O6 2.250(14) . 1_545 N
Ca1 O7 2.540(24) . 2_464 N
P1 C1 1.822(7) . 1_555 N
P1 C7 1.799(8) . 1_555 N
P1 O1 1.530(8) . 1_555 N
P1 O2 1.529(8) . 1_555 N
P2 C10 1.817(7) . 1_555 N
P2 C16 1.798(8) . 1_555 N
P2 O5 1.527(8) . 1_555 N
P2 O6 1.513(8) . 1_555 N
C1 P1 1.822(7) . 1_555 N
C1 C2 1.408(4) . 1_555 N
C1 C6 1.408(4) . 1_555 N
C2 C1 1.408(4) . 1_555 N
C2 C3 1.406(4) . 1_555 N
C3 C2 1.406(4) . 1_555 N
C3 C4 1.405(4) . 1_555 N
C4 C3 1.405(4) . 1_555 N
C4 C5 1.403(4) . 1_555 N
C5 C4 1.403(4) . 1_555 N
C5 C6 1.407(4) . 1_555 N
C6 C1 1.408(4) . 1_555 N
C6 C5 1.407(4) . 1_555 N
C7 P1 1.799(8) . 1_555 N
C7 C8 1.507(8) . 1_555 N
C8 C7 1.507(8) . 1_555 N
C8 C9 1.497(8) . 1_555 N
C9 C8 1.497(8) . 1_555 N
C9 O3 1.237(8) . 1_555 N
C9 O4 1.233(8) . 1_555 N
C10 P2 1.817(7) . 1_555 N
C10 C11 1.405(4) . 1_555 N
C10 C15 1.402(4) . 1_555 N
C11 C10 1.405(4) . 1_555 N
C11 C12 1.401(4) . 1_555 N
C12 C11 1.401(4) . 1_555 N
C12 C13 1.399(4) . 1_555 N
C13 C12 1.399(4) . 1_555 N
C13 C14 1.403(4) . 1_555 N
C14 C13 1.403(4) . 1_555 N
C14 C15 1.402(4) . 1_555 N
C15 C10 1.402(4) . 1_555 N
C15 C14 1.402(4) . 1_555 N
C16 P2 1.798(8) . 1_555 N
C16 C17 1.508(9) . 1_555 N
C17 C16 1.508(9) . 1_555 N
C17 C18 1.504(8) . 1_555 N
C18 C17 1.504(8) . 1_555 N
C18 O7 1.245(8) . 1_555 N
C18 O8 1.251(8) . 1_555 N
O1 Ca1 2.573(18) . 1_555 N
O1 P1 1.530(8) . 1_555 N
O2 Ca1 2.262(14) . 1_565 N
O2 P1 1.529(8) . 1_555 N
O3 C9 1.237(8) . 1_555 N
O3 O4 2.134(14) . 1_555 N
O4 Ca1 2.506(25) . 2_464 N
O4 C9 1.233(8) . 1_555 N
O4 O3 2.134(14) . 1_555 N
O5 Ca1 2.286(16) . 1_555 N
O5 P2 1.527(8) . 1_555 N
O6 Ca1 2.250(14) . 1_565 N
O6 P2 1.513(8) . 1_555 N
O7 Ca1 2.540(24) . 2_565 N
O7 C18 1.245(8) . 1_555 N
O7 O8 2.172(15) . 1_555 N
O8 C18 1.251(8) . 1_555 N
O8 O7 2.172(15) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O2 89.2(6) 1_555 . 1_545 N
O1 Ca1 O4 74.3(7) 1_555 . 2_565 N
O1 Ca1 O5 87.5(5) 1_555 . 1_555 N
O1 Ca1 O6 167.8(9) 1_555 . 1_545 N
O1 Ca1 O7 96.6(7) 1_555 . 2_464 N
O2 Ca1 O4 91.0(9) 1_545 . 2_565 N
O2 Ca1 O5 169.1(8) 1_545 . 1_555 N
O2 Ca1 O6 93.2(6) 1_545 . 1_545 N
O2 Ca1 O7 82.4(7) 1_545 . 2_464 N
O4 Ca1 O5 98.2(8) 2_565 . 1_555 N
O4 Ca1 O6 93.6(8) 2_565 . 1_545 N
O4 Ca1 O7 168.9(8) 2_565 . 2_464 N
O5 Ca1 O6 92.3(7) 1_555 . 1_545 N
O5 Ca1 O7 87.6(8) 1_555 . 2_464 N
O6 Ca1 O7 95.6(9) 1_545 . 2_464 N
C1 P1 C7 104.4(8) 1_555 . 1_555 N
C1 P1 O1 107.0(8) 1_555 . 1_555 N
C1 P1 O2 107.6(8) 1_555 . 1_555 N
C7 P1 O1 112.0(9) 1_555 . 1_555 N
C7 P1 O2 112.7(9) 1_555 . 1_555 N
O1 P1 O2 112.4(9) 1_555 . 1_555 N
C10 P2 C16 103.8(8) 1_555 . 1_555 N
C10 P2 O5 106.2(8) 1_555 . 1_555 N
C10 P2 O6 109.8(9) 1_555 . 1_555 N
C16 P2 O5 111.3(8) 1_555 . 1_555 N
C16 P2 O6 113.5(9) 1_555 . 1_555 N
O5 P2 O6 111.8(9) 1_555 . 1_555 N
P1 C1 C2 120.0(8) 1_555 . 1_555 N
P1 C1 C6 120.2(8) 1_555 . 1_555 N
C2 C1 C6 117.2(5) 1_555 . 1_555 N
C1 C2 C3 117.3(5) 1_555 . 1_555 N
C2 C3 C4 117.7(5) 1_555 . 1_555 N
C3 C4 C5 117.9(5) 1_555 . 1_555 N
C4 C5 C6 117.9(5) 1_555 . 1_555 N
C1 C6 C5 117.5(5) 1_555 . 1_555 N
P1 C7 C8 117.8(10) 1_555 . 1_555 N
C7 C8 C9 111.8(11) 1_555 . 1_555 N
C8 C9 O3 123.6(13) 1_555 . 1_555 N
C8 C9 O4 116.9(11) 1_555 . 1_555 N
O3 C9 O4 119.5(12) 1_555 . 1_555 N
P2 C10 C11 119.6(8) 1_555 . 1_555 N
P2 C10 C15 121.2(8) 1_555 . 1_555 N
C11 C10 C15 118.1(4) 1_555 . 1_555 N
C10 C11 C12 118.1(4) 1_555 . 1_555 N
C11 C12 C13 118.5(5) 1_555 . 1_555 N
C12 C13 C14 118.4(5) 1_555 . 1_555 N
C13 C14 C15 118.5(4) 1_555 . 1_555 N
C10 C15 C14 118.3(4) 1_555 . 1_555 N
P2 C16 C17 113.0(10) 1_555 . 1_555 N
C16 C17 C18 116.9(15) 1_555 . 1_555 N
C17 C18 O7 114.8(13) 1_555 . 1_555 N
C17 C18 O8 118.8(14) 1_555 . 1_555 N
O7 C18 O8 121.0(15) 1_555 . 1_555 N
Ca1 O1 P1 132.5(12) 1_555 . 1_555 N
Ca1 O2 P1 153.9(12) 1_565 . 1_555 N
Ca1 O4 C9 136.7(16) 2_464 . 1_555 N
Ca1 O5 P2 147.9(12) 1_555 . 1_555 N
Ca1 O6 P2 161.0(14) 1_565 . 1_555 N
Ca1 O7 C18 125.7(15) 2_565 . 1_555 N

# Powder diffraction data for histogram  1
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
; ?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a~1~'
_diffrn_radiation_wavelength     0.7093
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'D8 ADVANCE (Bruker AXS) diffractometer'
_diffrn_source_target            ?
_diffrn_measurement_device_type  'D8 ADVANCE (Bruker AXS) diffractometer'
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             ? # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       ?
_computing_data_reduction        ?

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     ?

# The following item is used for angular dispersive measurements only.

_diffrn_radiation_monochromator  ?

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          ?
_pd_instr_dist_mono/spec         ?
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         ?

# 10. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;

_pd_spec_mount_mode              ? # options are 'reflection'
# or 'transmission'

_pd_spec_shape                   ? # options are 'cylinder'
# 'flat_sheet' or 'irregular'


loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Ca 2.0 0.228 0.309 8.62660 10.4421 7.38730 0.65990 1.58990 85.7484 1.02110
178.437 1.37510 International_Tables_Vol_C
P 4.0 0.102 0.095 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080
68.1645 1.11490 International_Tables_Vol_C
C 36.0 0.003 0.002 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
O 16.0 0.011 0.006 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
_diffrn_radiation_polarisn_ratio ?
_pd_proc_ls_prof_R_factor        0.0780
_pd_proc_ls_prof_wR_factor       0.1042
_pd_proc_ls_prof_wR_expected     0.0312
_refine_ls_R_Fsqd_factor         0.08885

_pd_proc_ls_background_function  
;   GSAS Background function number 1 with 36 terms.
 Shifted Chebyshev function of 1st kind
      1:    32310.7     2:   -27377.5     3:    15662.6     4:   -8801.99    
      5:    3014.28     6:    374.821     7:   -1434.26     8:    2880.47    
      9:   -3383.79    10:    2306.89    11:   -1219.18    12:    548.902    
     13:    943.813    14:   -1515.65    15:    1253.30    16:   -263.257    
     17:   -457.581    18:    794.515    19:    98.6653    20:   -971.156    
     21:    713.685    22:   -541.675    23:    72.8548    24:   -120.618    
     25:    260.650    26:   -487.586    27:    559.983    28:   -551.099    
     29:   -313.852    30:    822.731    31:   -599.576    32:   -356.942    
     33:    401.067    34:   -382.759    35:    84.6699    36:   -83.1854    
;

_exptl_absorpt_process_details   
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_T_max  1.00000
# Extinction correction
_pd_proc_ls_pref_orient_corr     
;   March-Dollase
 AXIS  1 Ratio=   1.20033  h= 1.000  k= 0.000  l= 0.000
 Prefered orientation correction range: Min=   0.57823, Max=   1.31507
;

_pd_proc_ls_profile_function     
;
 CW Profile function number 4 with  21 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 Microstrain broadening by P.W. Stephens,  (1999). J. Appl. Cryst.,32,281-289.
 #1(GU)   =    0.000 #2(GV)   =    0.000 #3(GW)   =    3.621
 #4(GP)   =    0.000 #5(LX)   =    2.167 #6(ptec) =     0.00
 #7(trns) =     0.00 #8(shft) =   0.0000 #9(sfec) =     0.00
 #10(S/L) =   0.0047 #11(H/L) =   0.0070 #12(eta) =   0.3572
 #13(S400 ) =  5.2E-03 #14(S040 ) =  2.0E-01 #15(S004 ) =  3.7E-02
 #16(S220 ) =  1.1E-01 #17(S202 ) = -9.5E-03 #18(S022 ) =  4.6E-02
 #19(S301 ) = -8.8E-04 #20(S103 ) =  0.0E+00 #21(S121 ) =  1.0E-01
 Peak tails are ignored  where the intensity is below 0.0030 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_peak_cutoff          0.00300
_pd_proc_info_datetime           2020-03-23T17:31:22
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        3.0
_pd_meas_2theta_range_max        50.0
_pd_meas_2theta_range_inc        0.01
_pd_proc_2theta_range_min        3.00226
_pd_proc_2theta_range_max        50.00226
_pd_proc_2theta_range_inc        0.01
_pd_meas_number_of_points        4701
_pd_proc_number_of_points        4701

_reflns_number_total             1751
_reflns_limit_h_min              0
_reflns_limit_h_max              17
_reflns_limit_k_min              0
_reflns_limit_k_max              6
_reflns_limit_l_min              -15
_reflns_limit_l_max              14
_reflns_d_resolution_high        0.839
_reflns_d_resolution_low         7.488

#--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#
