#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/17/4501742.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4501742
loop_
_publ_author_name
'Clark, Thomas E.'
'Martin, Adam'
'Makha, Mohamed'
'Sobolev, Alexandre N.'
'Su, Dian'
'Rohrs, Henry W.'
'Gross, Michael L.'
'Raston, Colin L.'
_publ_section_title
;
 Layered Calcium Structures of p-Phosphonic Acid O-Methyl-Calix[6]arene.
;
_journal_issue                   7
_journal_name_full               'Crystal growth & design'
_journal_page_first              3211
_journal_page_last               3217
_journal_paper_doi               10.1021/cg1003484
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C48 H46 O24 P6, Ca4, 26.5(H2 O)'
_chemical_formula_sum            'C48 H99 Ca4 O50.5 P6'
_chemical_formula_weight         1830.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.047(7)
_cell_angle_beta                 95.814(5)
_cell_angle_gamma                108.467(6)
_cell_formula_units_Z            1
_cell_length_a                   11.4113(7)
_cell_length_b                   12.9903(9)
_cell_length_c                   15.4684(11)
_cell_measurement_reflns_used    3480
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.1
_cell_measurement_theta_min      3.12
_cell_volume                     1951.6(3)
_computing_cell_refinement
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_molecular_graphics    'X-Seed 2.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_sigmaI/netI    0.1485
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22732
_diffrn_reflns_theta_full        67.30
_diffrn_reflns_theta_max         67.30
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    4.520
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             961
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0250P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                3372
_reflns_number_total             6828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg1003484_si_004.cif
_cod_data_source_block           Complex5c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1951.6(2)
_cod_original_formula_sum        'C48 H99 Ca4 O50.50 P6'
_cod_database_code               4501742
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ca1 Ca 0.66179(10) 0.59052(9) 0.46310(8) 0.0247(3) Uani 1 1 d .
Ca2 Ca -0.01197(10) 0.29131(9) 0.49953(8) 0.0246(3) Uani 1 1 d .
O01W O 0.6239(3) 0.7225(3) 0.5975(3) 0.0329(10) Uani 1 1 d .
H011 H 0.6587 0.7989 0.6264 0.049 Uiso 1 1 d .
H012 H 0.5591 0.6991 0.6182 0.049 Uiso 1 1 d .
O02W O 0.5765(3) 0.4810(3) 0.5675(3) 0.0292(9) Uani 1 1 d .
H021 H 0.5950 0.4190 0.5512 0.044 Uiso 1 1 d .
H022 H 0.6015 0.5202 0.6285 0.044 Uiso 1 1 d .
O03W O -0.1950(3) 0.1271(3) 0.3905(3) 0.0326(10) Uani 1 1 d .
H031 H -0.2258 0.0618 0.3961 0.049 Uiso 1 1 d .
H032 H -0.2541 0.1334 0.3572 0.049 Uiso 1 1 d .
O04W O -0.0792(4) 0.1965(3) 0.6001(3) 0.0440(11) Uani 1 1 d .
H041 H -0.0374 0.2411 0.6585 0.066 Uiso 1 1 d .
H042 H -0.1583 0.1764 0.5979 0.066 Uiso 1 1 d .
O05W O 0.1755(3) 0.4041(3) 0.6345(2) 0.0269(9) Uani 1 1 d .
H051 H 0.1933 0.4794 0.6613 0.040 Uiso 1 1 d .
H052 H 0.1724 0.3786 0.6778 0.040 Uiso 1 1 d .
O06W O 0.1314(4) 0.1863(3) 0.4663(3) 0.0523(12) Uani 1 1 d .
H061 H 0.1267 0.1524 0.4065 0.078 Uiso 1 1 d .
H062 H 0.1410 0.1405 0.4914 0.078 Uiso 1 1 d .
O07W O 0.6425(3) 0.2845(3) 0.5142(3) 0.0349(10) Uani 1 1 d .
H071 H 0.6257 0.2513 0.4531 0.052 Uiso 1 1 d .
H072 H 0.7225 0.3244 0.5360 0.052 Uiso 1 1 d .
O08W O 0.3592(4) 0.0431(3) 0.2929(3) 0.0446(11) Uani 1 1 d .
H081 H 0.4359 0.0780 0.2927 0.067 Uiso 1 1 d .
H082 H 0.3593 0.0083 0.3298 0.067 Uiso 1 1 d .
O09W O 0.1069(4) 0.0489(3) 0.2777(3) 0.0539(13) Uani 1 1 d .
H091 H 0.0411 -0.0159 0.2483 0.081 Uiso 1 1 d .
H092 H 0.1726 0.0316 0.2749 0.081 Uiso 1 1 d .
O10W O 0.3329(4) -0.0803(4) 0.4073(3) 0.0618(14) Uani 1 1 d .
H101 H 0.3439 -0.0240 0.4620 0.093 Uiso 1 1 d .
H102 H 0.3916 -0.1068 0.4107 0.093 Uiso 1 1 d .
O11W O 0.1319(4) 0.1338(3) 0.7772(3) 0.0494(12) Uani 1 1 d .
H111 H 0.1751 0.1079 0.8056 0.074 Uiso 1 1 d .
H112 H 0.1576 0.1331 0.7274 0.074 Uiso 1 1 d .
O12W O 0.0421(5) 0.3119(4) 0.7877(3) 0.0759(17) Uani 1 1 d .
H121 H 0.0744 0.2650 0.7967 0.114 Uiso 1 1 d .
H122 H 0.1008 0.3816 0.8092 0.114 Uiso 1 1 d .
O13W O 0.1852(4) 0.5452(4) 0.8582(3) 0.0624(14) Uani 1 1 d .
H131 H 0.1939 0.5992 0.9135 0.094 Uiso 1 1 d .
H132 H 0.1994 0.5781 0.8200 0.094 Uiso 1 1 d .
O1 O 0.7575(3) 0.2684(3) -0.0359(3) 0.0265(9) Uani 1 1 d .
C10 C 0.8431(5) 0.2090(5) -0.0699(5) 0.0407(17) Uani 1 1 d .
H10A H 0.9045 0.2205 -0.0146 0.061 Uiso 1 1 calc R
H10B H 0.8890 0.2435 -0.1090 0.061 Uiso 1 1 calc R
H10C H 0.7937 0.1228 -0.1091 0.061 Uiso 1 1 calc R
C11 C 0.6651(5) 0.2559(4) -0.1097(4) 0.0223(12) Uani 1 1 d .
C12 C 0.5490(5) 0.1635(4) -0.1414(4) 0.0187(12) Uani 1 1 d .
C13 C 0.4599(5) 0.1515(4) -0.2165(4) 0.0232(13) Uani 1 1 d .
H13 H 0.3796 0.0858 -0.2414 0.028 Uiso 1 1 calc R
C14 C 0.4860(5) 0.2336(4) -0.2558(4) 0.0230(13) Uani 1 1 d .
C15 C 0.6022(5) 0.3305(4) -0.2185(4) 0.0249(13) Uani 1 1 d .
H15 H 0.6191 0.3880 -0.2443 0.030 Uiso 1 1 calc R
C16 C 0.6942(5) 0.3451(4) -0.1445(4) 0.0232(12) Uani 1 1 d .
P1 P 0.37689(16) 0.20629(13) -0.36217(12) 0.0383(4) Uani 1 1 d .
O11 O 0.3850(3) 0.3187(3) -0.3673(3) 0.0415(11) Uani 1 1 d .
O12 O 0.4459(4) 0.1464(4) -0.4482(3) 0.0574(13) Uani 1 1 d .
H12 H 0.5060 0.2017 -0.4510 0.086 Uiso 1 1 calc R
O13 O 0.2576(4) 0.1077(3) -0.3845(3) 0.0486(12) Uani 1 1 d .
C1 C 0.5126(5) 0.0757(4) -0.0977(4) 0.0211(12) Uani 1 1 d .
H1B H 0.5868 0.0559 -0.0827 0.025 Uiso 1 1 calc R
H1A H 0.4429 0.0004 -0.1454 0.025 Uiso 1 1 calc R
C2 C 0.1626(4) 0.1431(4) 0.0697(4) 0.0236(13) Uani 1 1 d .
H2A H 0.1149 0.1107 0.0019 0.028 Uiso 1 1 calc R
H2B H 0.1211 0.0861 0.0958 0.028 Uiso 1 1 calc R
O2 O 0.2573(3) 0.0577(3) -0.1019(2) 0.0237(9) Uani 1 1 d .
C20 C 0.1792(5) -0.0667(4) -0.1361(4) 0.0286(14) Uani 1 1 d .
H20A H 0.1230 -0.0952 -0.1996 0.043 Uiso 1 1 calc R
H20C H 0.1275 -0.0774 -0.0910 0.043 Uiso 1 1 calc R
H20B H 0.2335 -0.1129 -0.1414 0.043 Uiso 1 1 calc R
C21 C 0.3406(5) 0.1095(4) -0.0113(4) 0.0221(13) Uani 1 1 d .
C22 C 0.3008(5) 0.1525(4) 0.0725(4) 0.0183(12) Uani 1 1 d .
C23 C 0.3884(5) 0.2096(4) 0.1604(4) 0.0198(12) Uani 1 1 d .
H23 H 0.3610 0.2388 0.2175 0.024 Uiso 1 1 calc R
C24 C 0.5181(5) 0.2258(4) 0.1676(4) 0.0225(13) Uani 1 1 d .
C25 C 0.5532(5) 0.1835(4) 0.0838(4) 0.0217(13) Uani 1 1 d .
H25 H 0.6405 0.1955 0.0875 0.026 Uiso 1 1 calc R
C26 C 0.4693(5) 0.1239(4) -0.0065(4) 0.0173(12) Uani 1 1 d .
P2 P 0.62607(13) 0.29474(11) 0.28563(10) 0.0219(3) Uani 1 1 d .
O21 O 0.6202(3) 0.1967(3) 0.3182(2) 0.0252(9) Uani 1 1 d .
O22 O 0.7592(3) 0.3545(3) 0.2726(2) 0.0246(9) Uani 1 1 d .
O23 O 0.5841(3) 0.3883(3) 0.3529(2) 0.0225(8) Uani 1 1 d .
O3 O 0.2012(3) 0.3182(3) 0.0007(3) 0.0288(9) Uani 1 1 d .
C30 C 0.3310(5) 0.3802(5) 0.0017(4) 0.0341(15) Uani 1 1 d .
H30A H 0.3406 0.3545 -0.0644 0.051 Uiso 1 1 calc R
H30C H 0.3886 0.3613 0.0392 0.051 Uiso 1 1 calc R
H30B H 0.3521 0.4672 0.0312 0.051 Uiso 1 1 calc R
C31 C 0.1752(5) 0.3479(4) 0.0914(4) 0.0218(12) Uani 1 1 d .
C32 C 0.1630(5) 0.4583(4) 0.1398(4) 0.0227(13) Uani 1 1 d .
C33 C 0.1346(4) 0.4814(4) 0.2287(4) 0.0240(13) Uani 1 1 d .
H33 H 0.1251 0.5550 0.2627 0.029 Uiso 1 1 calc R
C34 C 0.1197(4) 0.4018(4) 0.2697(4) 0.0201(12) Uani 1 1 d .
C35 C 0.1306(4) 0.2920(4) 0.2175(4) 0.0208(12) Uani 1 1 d .
H35 H 0.1205 0.2358 0.2443 0.025 Uiso 1 1 calc R
C36 C 0.1557(4) 0.2646(4) 0.1276(4) 0.0183(12) Uani 1 1 d .
P3 P 0.08090(13) 0.43939(12) 0.38464(10) 0.0223(3) Uani 1 1 d .
O33 O 0.1588(3) 0.4112(3) 0.4514(2) 0.0237(8) Uani 1 1 d .
O32 O -0.0575(3) 0.3477(3) 0.3675(2) 0.0242(9) Uani 1 1 d .
H32 H -0.1103 0.3597 0.3345 0.036 Uiso 1 1 calc R
O31 O 0.0913(3) 0.5674(3) 0.4224(2) 0.0266(9) Uani 1 1 d .
C3 C 0.1788(5) 0.5502(4) 0.1000(4) 0.0234(13) Uani 1 1 d .
H3A H 0.1685 0.5100 0.0296 0.028 Uiso 1 1 calc R
H3B H 0.1101 0.5811 0.1105 0.028 Uiso 1 1 calc R
O00W O 0.0000 0.0000 0.5000 0.087(5) Uiso 0.50 2 d SP
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O01W Ca1 O11 93.09(13) . 2_665
O01W Ca1 O33 95.24(12) . 2_666
O11 Ca1 O33 138.46(13) 2_665 2_666
O01W Ca1 O23 142.02(13) . .
O11 Ca1 O23 102.14(13) 2_665 .
O33 Ca1 O23 95.82(11) 2_666 .
O01W Ca1 O02W 74.83(12) . 2_666
O11 Ca1 O02W 78.37(12) 2_665 2_666
O33 Ca1 O02W 142.96(12) 2_666 2_666
O23 Ca1 O02W 74.53(11) . 2_666
O01W Ca1 O05W 138.24(12) . 2_666
O11 Ca1 O05W 74.63(12) 2_665 2_666
O33 Ca1 O05W 72.20(11) 2_666 2_666
O23 Ca1 O05W 79.67(11) . 2_666
O02W Ca1 O05W 137.41(12) 2_666 2_666
O01W Ca1 O02W 70.52(11) . .
O11 Ca1 O02W 145.63(13) 2_665 .
O33 Ca1 O02W 74.65(11) 2_666 .
O23 Ca1 O02W 77.66(11) . .
O02W Ca1 O02W 68.38(12) 2_666 .
O05W Ca1 O02W 137.27(10) 2_666 .
O01W Ca1 O06W 72.95(12) . 2_666
O11 Ca1 O06W 75.07(13) 2_665 2_666
O33 Ca1 O06W 68.80(11) 2_666 2_666
O23 Ca1 O06W 144.52(12) . 2_666
O02W Ca1 O06W 136.53(11) 2_666 2_666
O05W Ca1 O06W 65.36(11) 2_666 2_666
O02W Ca1 O06W 124.58(12) . 2_666
O01W Ca1 Ca2 105.09(9) . 2_666
O11 Ca1 Ca2 97.92(10) 2_665 2_666
O33 Ca1 Ca2 40.70(8) 2_666 2_666
O23 Ca1 Ca2 106.93(8) . 2_666
O02W Ca1 Ca2 176.26(9) 2_666 2_666
O05W Ca1 Ca2 40.75(8) 2_666 2_666
O02W Ca1 Ca2 115.21(8) . 2_666
O06W Ca1 Ca2 40.95(7) 2_666 2_666
O01W Ca1 Ca1 68.87(9) . 2_666
O11 Ca1 Ca1 112.83(10) 2_665 2_666
O33 Ca1 Ca1 108.12(9) 2_666 2_666
O23 Ca1 Ca1 73.15(9) . 2_666
O02W Ca1 Ca1 34.88(8) 2_666 2_666
O05W Ca1 Ca1 152.74(9) 2_666 2_666
O02W Ca1 Ca1 33.50(7) . 2_666
O06W Ca1 Ca1 141.26(10) 2_666 2_666
Ca2 Ca1 Ca1 148.70(5) 2_666 2_666
O31 Ca2 O03W 103.19(13) 2_566 .
O31 Ca2 O04W 88.65(14) 2_566 .
O03W Ca2 O04W 80.31(14) . .
O31 Ca2 O06W 160.24(14) 2_566 .
O03W Ca2 O06W 95.45(13) . .
O04W Ca2 O06W 88.08(14) . .
O31 Ca2 O05W 87.13(12) 2_566 .
O03W Ca2 O05W 158.12(12) . .
O04W Ca2 O05W 80.71(13) . .
O06W Ca2 O05W 73.11(13) . .
O31 Ca2 O33 100.14(12) 2_566 .
O03W Ca2 O33 124.02(13) . .
O04W Ca2 O33 150.38(13) . .
O06W Ca2 O33 74.10(12) . .
O05W Ca2 O33 71.64(11) . .
O31 Ca2 O32 81.75(11) 2_566 .
O03W Ca2 O32 75.99(12) . .
O04W Ca2 O32 151.57(13) . .
O06W Ca2 O32 109.46(13) . .
O05W Ca2 O32 125.10(11) . .
O33 Ca2 O32 58.05(11) . .
O31 Ca2 P3 86.60(9) 2_566 .
O03W Ca2 P3 103.73(10) . .
O04W Ca2 P3 174.36(11) . .
O06W Ca2 P3 95.37(11) . .
O05W Ca2 P3 96.00(9) . .
O33 Ca2 P3 28.71(8) . .
O32 Ca2 P3 30.12(8) . .
O31 Ca2 Ca1 114.52(10) 2_566 2_666
O03W Ca2 Ca1 139.93(10) . 2_666
O04W Ca2 Ca1 112.44(10) . 2_666
O06W Ca2 Ca1 49.70(9) . 2_666
O05W Ca2 Ca1 42.43(8) . 2_666
O33 Ca2 Ca1 38.32(7) . 2_666
O32 Ca2 Ca1 95.86(8) . 2_666
P3 Ca2 Ca1 67.03(4) . 2_666
O31 Ca2 H041 82.1 2_566 .
O03W Ca2 H041 96.6 . .
O04W Ca2 H041 16.5 . .
O06W Ca2 H041 89.4 . .
O05W Ca2 H041 65.4 . .
O33 Ca2 H041 136.8 . .
O32 Ca2 H041 160.1 . .
P3 Ca2 H041 158.6 . .
Ca1 Ca2 H041 101.3 2_666 .
Ca1 O01W H011 129.3 . .
Ca1 O01W H012 121.2 . .
H011 O01W H012 108.4 . .
Ca1 O02W Ca1 111.62(12) 2_666 .
Ca1 O02W H021 107.2 2_666 .
Ca1 O02W H021 107.7 . .
Ca1 O02W H022 103.1 2_666 .
Ca1 O02W H022 118.3 . .
H021 O02W H022 108.4 . .
Ca2 O03W H031 123.0 . .
Ca2 O03W H032 123.9 . .
H031 O03W H032 108.4 . .
Ca2 O04W H041 111.1 . .
Ca2 O04W H042 114.0 . .
H041 O04W H042 108.5 . .
Ca2 O05W Ca1 96.82(12) . 2_666
Ca2 O05W H051 114.4 . .
Ca1 O05W H051 97.1 2_666 .
Ca2 O05W H052 113.7 . .
Ca1 O05W H052 125.5 2_666 .
H051 O05W H052 108.4 . .
Ca2 O06W Ca1 89.35(12) . 2_666
Ca2 O06W H061 112.5 . .
Ca1 O06W H061 105.0 2_666 .
Ca2 O06W H062 124.7 . .
Ca1 O06W H062 114.2 2_666 .
H061 O06W H062 108.4 . .
H071 O07W H072 108.4 . .
H081 O08W H082 108.4 . .
H091 O09W H092 108.4 . .
H101 O10W H102 108.4 . .
H111 O11W H112 108.4 . .
H121 O12W H122 108.4 . .
H131 O13W H132 108.4 . .
C11 O1 C10 113.9(4) . .
O1 C10 H10A 109.5 . .
O1 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
O1 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C12 C11 O1 119.4(4) . .
C12 C11 C16 122.6(5) . .
O1 C11 C16 117.9(4) . .
C11 C12 C13 118.2(5) . .
C11 C12 C1 123.0(5) . .
C13 C12 C1 118.9(4) . .
C14 C13 C12 121.2(5) . .
C14 C13 H13 119.4 . .
C12 C13 H13 119.4 . .
C13 C14 C15 119.4(5) . .
C13 C14 P1 120.2(4) . .
C15 C14 P1 120.1(4) . .
C16 C15 C14 121.3(5) . .
C16 C15 H15 119.4 . .
C14 C15 H15 119.4 . .
C15 C16 C11 117.2(5) . .
C15 C16 C3 123.5(5) . 2_665
C11 C16 C3 119.3(5) . 2_665
O13 P1 O11 123.2(2) . .
O13 P1 O12 102.6(3) . .
O11 P1 O12 103.5(2) . .
O13 P1 C14 111.5(2) . .
O11 P1 C14 111.8(2) . .
O12 P1 C14 100.9(2) . .
P1 O11 Ca1 146.9(3) . 2_665
P1 O12 H12 109.5 . .
C12 C1 C26 112.9(4) . .
C12 C1 H1B 109.0 . .
C26 C1 H1B 109.0 . .
C12 C1 H1A 109.0 . .
C26 C1 H1A 109.0 . .
H1B C1 H1A 107.8 . .
C36 C2 C22 112.2(4) . .
C36 C2 H2A 109.2 . .
C22 C2 H2A 109.2 . .
C36 C2 H2B 109.2 . .
C22 C2 H2B 109.2 . .
H2A C2 H2B 107.9 . .
C21 O2 C20 115.0(4) . .
O2 C20 H20A 109.5 . .
O2 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
O2 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
H20C C20 H20B 109.5 . .
C22 C21 O2 121.3(5) . .
C22 C21 C26 120.5(5) . .
O2 C21 C26 118.1(5) . .
C23 C22 C21 119.3(5) . .
C23 C22 C2 118.8(5) . .
C21 C22 C2 121.8(4) . .
C22 C23 C24 121.6(5) . .
C22 C23 H23 119.2 . .
C24 C23 H23 119.2 . .
C25 C24 C23 117.2(5) . .
C25 C24 P2 123.7(4) . .
C23 C24 P2 119.1(4) . .
C24 C25 C26 123.8(5) . .
C24 C25 H25 118.1 . .
C26 C25 H25 118.1 . .
C25 C26 C21 117.6(5) . .
C25 C26 C1 121.8(4) . .
C21 C26 C1 120.6(4) . .
O23 P2 O21 111.8(2) . .
O23 P2 O22 111.04(19) . .
O21 P2 O22 112.11(18) . .
O23 P2 C24 107.7(2) . .
O21 P2 C24 108.3(2) . .
O22 P2 C24 105.5(2) . .
P2 O23 Ca1 141.71(19) . .
C31 O3 C30 114.9(4) . .
O3 C30 H30A 109.5 . .
O3 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
O3 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
H30C C30 H30B 109.5 . .
C36 C31 O3 118.0(4) . .
C36 C31 C32 122.1(5) . .
O3 C31 C32 119.7(4) . .
C33 C32 C31 117.0(5) . .
C33 C32 C3 119.6(4) . .
C31 C32 C3 123.5(5) . .
C34 C33 C32 122.6(5) . .
C34 C33 H33 118.7 . .
C32 C33 H33 118.7 . .
C33 C34 C35 118.0(5) . .
C33 C34 P3 119.2(4) . .
C35 C34 P3 122.7(4) . .
C36 C35 C34 120.9(5) . .
C36 C35 H35 119.5 . .
C34 C35 H35 119.5 . .
C31 C36 C35 119.2(5) . .
C31 C36 C2 120.2(5) . .
C35 C36 C2 120.6(4) . .
O31 P3 O33 115.6(2) . .
O31 P3 O32 113.02(19) . .
O33 P3 O32 101.51(19) . .
O31 P3 C34 107.2(2) . .
O33 P3 C34 111.9(2) . .
O32 P3 C34 107.3(2) . .
O31 P3 Ca2 119.59(15) . .
O33 P3 Ca2 51.04(13) . .
O32 P3 Ca2 52.19(12) . .
C34 P3 Ca2 133.03(16) . .
P3 O33 Ca1 158.8(2) . 2_666
P3 O33 Ca2 100.25(16) . .
Ca1 O33 Ca2 100.98(12) 2_666 .
P3 O32 Ca2 97.69(16) . .
P3 O32 H32 109.5 . .
Ca2 O32 H32 147.1 . .
P3 O31 Ca2 148.7(2) . 2_566
C16 C3 C32 113.9(4) 2_665 .
C16 C3 H3A 108.8 2_665 .
C32 C3 H3A 108.8 . .
C16 C3 H3B 108.8 2_665 .
C32 C3 H3B 108.8 . .
H3A C3 H3B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O01W 2.328(4) .
Ca1 O11 2.329(3) 2_665
Ca1 O33 2.333(3) 2_666
Ca1 O23 2.335(3) .
Ca1 O02W 2.508(3) 2_666
Ca1 O05W 2.510(4) 2_666
Ca1 O02W 2.598(4) .
Ca1 O06W 2.817(4) 2_666
Ca1 Ca2 3.6930(15) 2_666
Ca1 Ca1 4.223(2) 2_666
Ca2 O31 2.293(3) 2_566
Ca2 O03W 2.350(4) .
Ca2 O04W 2.368(4) .
Ca2 O06W 2.420(4) .
Ca2 O05W 2.428(4) .
Ca2 O33 2.453(3) .
Ca2 O32 2.475(3) .
Ca2 P3 3.1046(17) .
Ca2 Ca1 3.6930(15) 2_666
Ca2 H041 2.7897 .
O01W H011 0.8498 .
O01W H012 0.8496 .
O02W Ca1 2.508(3) 2_666
O02W H021 0.8497 .
O02W H022 0.8499 .
O03W H031 0.8495 .
O03W H032 0.8498 .
O04W H041 0.8497 .
O04W H042 0.8495 .
O05W Ca1 2.510(4) 2_666
O05W H051 0.8490 .
O05W H052 0.8510 .
O06W Ca1 2.817(4) 2_666
O06W H061 0.8494 .
O06W H062 0.8500 .
O07W H071 0.8499 .
O07W H072 0.8497 .
O08W H081 0.8498 .
O08W H082 0.8498 .
O09W H091 0.8500 .
O09W H092 0.8498 .
O10W H101 0.8497 .
O10W H102 0.8498 .
O11W H111 0.8500 .
O11W H112 0.8495 .
O12W H121 0.8499 .
O12W H122 0.8497 .
O13W H131 0.8498 .
O13W H132 0.8498 .
O1 C11 1.396(6) .
O1 C10 1.450(6) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.362(7) .
C11 C16 1.415(7) .
C12 C13 1.390(6) .
C12 C1 1.505(6) .
C13 C14 1.384(6) .
C13 H13 0.9500 .
C14 C15 1.385(7) .
C14 P1 1.804(5) .
C15 C16 1.385(7) .
C15 H15 0.9500 .
C16 C3 1.507(7) 2_665
P1 O13 1.442(4) .
P1 O11 1.466(3) .
P1 O12 1.679(4) .
O11 Ca1 2.329(3) 2_665
O12 H12 0.8400 .
C1 C26 1.516(6) .
C1 H1B 0.9900 .
C1 H1A 0.9900 .
C2 C36 1.527(6) .
C2 C22 1.538(6) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
O2 C21 1.392(6) .
O2 C20 1.427(5) .
C20 H20A 0.9800 .
C20 H20C 0.9800 .
C20 H20B 0.9800 .
C21 C22 1.391(7) .
C21 C26 1.410(6) .
C22 C23 1.377(6) .
C23 C24 1.414(6) .
C23 H23 0.9500 .
C24 C25 1.362(7) .
C24 P2 1.808(5) .
C25 C26 1.384(6) .
C25 H25 0.9500 .
P2 O23 1.519(3) .
P2 O21 1.522(3) .
P2 O22 1.543(3) .
O3 C31 1.399(6) .
O3 C30 1.439(6) .
C30 H30A 0.9800 .
C30 H30C 0.9800 .
C30 H30B 0.9800 .
C31 C36 1.364(7) .
C31 C32 1.406(6) .
C32 C33 1.389(7) .
C32 C3 1.507(6) .
C33 C34 1.379(6) .
C33 H33 0.9500 .
C34 C35 1.403(6) .
C34 P3 1.800(5) .
C35 C36 1.385(7) .
C35 H35 0.9500 .
P3 O31 1.501(3) .
P3 O33 1.516(3) .
P3 O32 1.572(3) .
O33 Ca1 2.332(3) 2_666
O32 H32 0.8400 .
O31 Ca2 2.293(3) 2_566
C3 C16 1.507(7) 2_665
C3 H3A 0.9900 .
C3 H3B 0.9900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O01W H011 O08W 0.85 2.05 2.805(5) 147.4 2_666
O01W H011 O09W 0.85 2.63 3.271(5) 133.3 2_666
O01W H012 O23 0.85 1.87 2.708(5) 166.6 2_666
O02W H021 O07W 0.85 1.89 2.743(4) 177.7 .
O03W H031 O13 0.85 2.05 2.866(5) 161.2 2
O03W H032 O21 0.85 2.01 2.828(4) 161.4 1_455
O04W H041 O12W 0.85 1.84 2.681(6) 169.5 .
O04W H042 O10W 0.85 1.96 2.777(5) 160.0 2_556
O05W H051 O22 0.85 1.87 2.715(4) 175.9 2_666
O05W H052 O12W 0.85 2.58 3.327(6) 147.3 .
O06W H061 O09W 0.85 1.88 2.717(6) 168.5 .
O06W H062 O00W 0.85 2.07 2.680(4) 127.7 .
O06W H062 O13 0.85 2.47 3.236(6) 150.6 1_556
O07W H071 O21 0.85 1.92 2.761(5) 169.1 .
O07W H072 O31 0.85 2.01 2.858(5) 171.9 2_666
O08W H081 O21 0.85 2.07 2.902(5) 166.6 .
O08W H082 O10W 0.85 1.94 2.779(6) 171.7 .
O09W H091 O11W 0.85 1.97 2.775(5) 158.3 2_556
O09W H092 O08W 0.85 2.07 2.892(5) 163.1 .
O10W H101 O12 0.85 1.98 2.720(6) 145.2 1_556
O10W H102 O12 0.85 2.16 2.994(6) 168.6 2_655
O11W H111 O2 0.85 2.04 2.875(5) 166.6 1_556
O11W H112 O13 0.85 2.15 2.972(6) 162.9 1_556
O12W H121 O11W 0.85 1.95 2.771(5) 163.5 .
O12W H122 O13W 0.85 1.83 2.657(6) 162.4 .
O13W H131 O1 0.85 1.90 2.736(5) 170.1 2_666
O13W H132 O22 0.85 1.97 2.812(5) 174.9 2_666
O12 H12 O07W 0.84 1.85 2.662(6) 162.8 1_554
O32 H32 O22 0.84 1.65 2.476(4) 165.2 1_455
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O01W Ca1 O02W Ca1 80.89(14) . 2_666
O11 Ca1 O02W Ca1 15.5(3) 2_665 2_666
O33 Ca1 O02W Ca1 -177.71(16) 2_666 2_666
O23 Ca1 O02W Ca1 -78.05(13) . 2_666
O02W Ca1 O02W Ca1 0.0 2_666 2_666
O05W Ca1 O02W Ca1 -137.56(15) 2_666 2_666
O06W Ca1 O02W Ca1 132.45(13) 2_666 2_666
Ca2 Ca1 O02W Ca1 178.86(9) 2_666 2_666
O31 Ca2 O05W Ca1 -132.12(12) 2_566 2_666
O03W Ca2 O05W Ca1 108.7(3) . 2_666
O04W Ca2 O05W Ca1 138.78(14) . 2_666
O06W Ca2 O05W Ca1 47.97(13) . 2_666
O33 Ca2 O05W Ca1 -30.44(10) . 2_666
O32 Ca2 O05W Ca1 -54.28(16) . 2_666
P3 Ca2 O05W Ca1 -45.84(9) . 2_666
O31 Ca2 O06W Ca1 -41.3(5) 2_566 2_666
O03W Ca2 O06W Ca1 157.97(12) . 2_666
O04W Ca2 O06W Ca1 -121.95(14) . 2_666
O05W Ca2 O06W Ca1 -41.08(11) . 2_666
O33 Ca2 O06W Ca1 34.10(11) . 2_666
O32 Ca2 O06W Ca1 80.93(13) . 2_666
P3 Ca2 O06W Ca1 53.58(10) . 2_666
C10 O1 C11 C12 92.6(5) . .
C10 O1 C11 C16 -91.1(5) . .
O1 C11 C12 C13 -178.4(4) . .
C16 C11 C12 C13 5.4(7) . .
O1 C11 C12 C1 2.7(7) . .
C16 C11 C12 C1 -173.4(4) . .
C11 C12 C13 C14 -2.4(7) . .
C1 C12 C13 C14 176.5(4) . .
C12 C13 C14 C15 -1.1(7) . .
C12 C13 C14 P1 172.6(4) . .
C13 C14 C15 C16 1.8(8) . .
P1 C14 C15 C16 -171.9(4) . .
C14 C15 C16 C11 1.0(7) . .
C14 C15 C16 C3 -178.9(5) . 2_665
C12 C11 C16 C15 -4.7(7) . .
O1 C11 C16 C15 179.1(4) . .
C12 C11 C16 C3 175.2(5) . 2_665
O1 C11 C16 C3 -1.0(7) . 2_665
C13 C14 P1 O13 11.2(5) . .
C15 C14 P1 O13 -175.2(4) . .
C13 C14 P1 O11 153.5(4) . .
C15 C14 P1 O11 -32.9(5) . .
C13 C14 P1 O12 -97.1(4) . .
C15 C14 P1 O12 76.5(4) . .
O13 P1 O11 Ca1 -59.5(6) . 2_665
O12 P1 O11 Ca1 55.6(5) . 2_665
C14 P1 O11 Ca1 163.4(4) . 2_665
C11 C12 C1 C26 81.5(6) . .
C13 C12 C1 C26 -97.4(5) . .
C20 O2 C21 C22 -83.8(5) . .
C20 O2 C21 C26 99.9(5) . .
O2 C21 C22 C23 -176.1(4) . .
C26 C21 C22 C23 0.0(7) . .
O2 C21 C22 C2 1.2(7) . .
C26 C21 C22 C2 177.3(4) . .
C36 C2 C22 C23 50.8(6) . .
C36 C2 C22 C21 -126.5(5) . .
C21 C22 C23 C24 0.1(7) . .
C2 C22 C23 C24 -177.3(4) . .
C22 C23 C24 C25 0.6(7) . .
C22 C23 C24 P2 -176.9(3) . .
C23 C24 C25 C26 -1.6(7) . .
P2 C24 C25 C26 175.8(3) . .
C24 C25 C26 C21 1.7(7) . .
C24 C25 C26 C1 -178.4(4) . .
C22 C21 C26 C25 -0.9(6) . .
O2 C21 C26 C25 175.3(4) . .
C22 C21 C26 C1 179.3(4) . .
O2 C21 C26 C1 -4.5(6) . .
C12 C1 C26 C25 -92.8(5) . .
C12 C1 C26 C21 87.0(5) . .
C25 C24 P2 O23 148.4(4) . .
C23 C24 P2 O23 -34.3(4) . .
C25 C24 P2 O21 -90.5(4) . .
C23 C24 P2 O21 86.9(4) . .
C25 C24 P2 O22 29.7(4) . .
C23 C24 P2 O22 -152.9(3) . .
O21 P2 O23 Ca1 113.4(3) . .
O22 P2 O23 Ca1 -12.7(4) . .
C24 P2 O23 Ca1 -127.7(3) . .
O01W Ca1 O23 P2 -154.6(3) . .
O11 Ca1 O23 P2 94.0(3) 2_665 .
O33 Ca1 O23 P2 -48.4(3) 2_666 .
O02W Ca1 O23 P2 168.1(3) 2_666 .
O05W Ca1 O23 P2 22.3(3) 2_666 .
O02W Ca1 O23 P2 -121.2(3) . .
O06W Ca1 O23 P2 12.7(4) 2_666 .
Ca2 Ca1 O23 P2 -8.3(3) 2_666 .
Ca1 Ca1 O23 P2 -155.6(3) 2_666 .
C30 O3 C31 C36 -108.0(5) . .
C30 O3 C31 C32 75.4(6) . .
C36 C31 C32 C33 2.3(7) . .
O3 C31 C32 C33 178.7(4) . .
C36 C31 C32 C3 -177.5(5) . .
O3 C31 C32 C3 -1.1(7) . .
C31 C32 C33 C34 0.6(7) . .
C3 C32 C33 C34 -179.6(4) . .
C32 C33 C34 C35 -1.7(8) . .
C32 C33 C34 P3 -179.2(4) . .
C33 C34 C35 C36 0.1(7) . .
P3 C34 C35 C36 177.5(4) . .
O3 C31 C36 C35 179.6(4) . .
C32 C31 C36 C35 -3.9(8) . .
O3 C31 C36 C2 0.0(7) . .
C32 C31 C36 C2 176.5(4) . .
C34 C35 C36 C31 2.6(7) . .
C34 C35 C36 C2 -177.7(4) . .
C22 C2 C36 C31 76.1(6) . .
C22 C2 C36 C35 -103.5(5) . .
C33 C34 P3 O31 -8.4(5) . .
C35 C34 P3 O31 174.2(4) . .
C33 C34 P3 O33 -136.2(4) . .
C35 C34 P3 O33 46.4(5) . .
C33 C34 P3 O32 113.3(4) . .
C35 C34 P3 O32 -64.1(4) . .
C33 C34 P3 Ca2 167.3(3) . .
C35 C34 P3 Ca2 -10.1(5) . .
O31 Ca2 P3 O31 18.0(2) 2_566 .
O03W Ca2 P3 O31 120.74(18) . .
O06W Ca2 P3 O31 -142.29(19) . .
O05W Ca2 P3 O31 -68.76(18) . .
O33 Ca2 P3 O31 -100.4(2) . .
O32 Ca2 P3 O31 97.4(2) . .
Ca1 Ca2 P3 O31 -100.48(16) 2_666 .
O31 Ca2 P3 O33 118.40(19) 2_566 .
O03W Ca2 P3 O33 -138.84(19) . .
O06W Ca2 P3 O33 -41.88(19) . .
O05W Ca2 P3 O33 31.65(18) . .
O32 Ca2 P3 O33 -162.2(2) . .
Ca1 Ca2 P3 O33 -0.07(16) 2_666 .
O31 Ca2 P3 O32 -79.40(18) 2_566 .
O03W Ca2 P3 O32 23.35(17) . .
O06W Ca2 P3 O32 120.32(18) . .
O05W Ca2 P3 O32 -166.15(17) . .
O33 Ca2 P3 O32 162.2(2) . .
Ca1 Ca2 P3 O32 162.13(16) 2_666 .
O31 Ca2 P3 C34 -157.3(2) 2_566 .
O03W Ca2 P3 C34 -54.5(2) . .
O06W Ca2 P3 C34 42.4(2) . .
O05W Ca2 P3 C34 116.0(2) . .
O33 Ca2 P3 C34 84.3(3) . .
O32 Ca2 P3 C34 -77.9(3) . .
Ca1 Ca2 P3 C34 84.2(2) 2_666 .
O31 P3 O33 Ca1 -71.8(6) . 2_666
O32 P3 O33 Ca1 165.4(5) . 2_666
C34 P3 O33 Ca1 51.3(6) . 2_666
Ca2 P3 O33 Ca1 179.7(7) . 2_666
O31 P3 O33 Ca2 108.4(2) . .
O32 P3 O33 Ca2 -14.27(19) . .
C34 P3 O33 Ca2 -128.38(19) . .
O31 Ca2 O33 P3 -63.13(18) 2_566 .
O03W Ca2 O33 P3 50.5(2) . .
O04W Ca2 O33 P3 -168.6(2) . .
O06W Ca2 O33 P3 136.29(19) . .
O05W Ca2 O33 P3 -146.64(19) . .
O32 Ca2 O33 P3 10.42(14) . .
Ca1 Ca2 O33 P3 179.9(2) 2_666 .
O31 Ca2 O33 Ca1 116.98(13) 2_566 2_666
O03W Ca2 O33 Ca1 -129.42(13) . 2_666
O04W Ca2 O33 Ca1 11.5(3) . 2_666
O06W Ca2 O33 Ca1 -43.61(14) . 2_666
O05W Ca2 O33 Ca1 33.46(11) . 2_666
O32 Ca2 O33 Ca1 -169.48(16) . 2_666
P3 Ca2 O33 Ca1 -179.9(2) . 2_666
O31 P3 O32 Ca2 -110.45(18) . .
O33 P3 O32 Ca2 14.04(19) . .
C34 P3 O32 Ca2 131.54(17) . .
O31 Ca2 O32 P3 97.49(16) 2_566 .
O03W Ca2 O32 P3 -156.62(17) . .
O04W Ca2 O32 P3 169.0(2) . .
O06W Ca2 O32 P3 -65.71(18) . .
O05W Ca2 O32 P3 16.9(2) . .
O33 Ca2 O32 P3 -9.97(13) . .
Ca1 Ca2 O32 P3 -16.50(14) 2_666 .
O33 P3 O31 Ca2 -94.5(4) . 2_566
O32 P3 O31 Ca2 21.9(5) . 2_566
C34 P3 O31 Ca2 139.9(4) . 2_566
Ca2 P3 O31 Ca2 -36.5(5) . 2_566
C33 C32 C3 C16 78.0(6) . 2_665
C31 C32 C3 C16 -102.2(6) . 2_665
