#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:48:25 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178917 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/46/4114604.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_4114604
loop_
_publ_author_name
'Akira Onoda'
'Yusuke Yamada'
'Taka-aki Okamura'
'Mototsugu Doi'
'Hitoshi Yamamoto'
'Norikazu Ueyama'
_publ_section_title
;
 Synthesis of Zigzag-Chain and Cyclic-Octanuclear Calcium Complexes and
 Hexanuclear Bulky Aryl-Phosphate Sodium Complexes with Ortho-Amide
 Groups: Structural Transformation Involving a Network of Inter- and
 Intramolecular Hydrogen Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1052
_journal_page_last               1059
_journal_paper_doi               10.1021/ja011457r
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C208 H278 Ca8 N32 O87 P8 '
_chemical_formula_sum            'C208 H278 Ca8 N32 O87 P8'
_chemical_formula_weight         5187.02
_chemical_name_systematic
; 
[Ca8(O3POC6H3(NHCOPh)2)8(H2O)12(dmf)8]-8(DMF)-11(H2O)
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      85
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Fri Aug 31 10:24:09 2001'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   29.8134(5)
_cell_length_b                   29.8134(5)
_cell_length_c                   16.9925(3)
_cell_measurement_reflns_used    89508
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     15103.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR88 (Burla, 1989)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1454
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17887
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    0.260
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             5452
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         17290
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.805
_refine_ls_R_factor_all          0.2491
_refine_ls_R_factor_gt           0.1052
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1680P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2860
_refine_ls_wR_factor_ref         0.3395
_reflns_number_gt                3918
_reflns_number_total             17290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011457r_5.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4114604
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -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 0.30846(4) 0.38026(4) 0.35111(9) 0.0931(5) Uani 1 1 d .
Ca2 Ca 0.38409(4) 0.30138(4) 0.24734(9) 0.0971(5) Uani 1 1 d .
P1 P 0.31370(6) 0.39277(6) 0.17319(13) 0.1005(6) Uani 1 1 d .
P2 P 0.39493(6) 0.30609(6) 0.42616(13) 0.0956(6) Uani 1 1 d .
O1 O 0.2859(3) 0.5863(2) 0.2110(6) 0.238(4) Uani 1 1 d .
O2 O 0.3955(2) 0.4684(3) -0.0798(4) 0.185(3) Uani 1 1 d .
O3 O 0.4993(4) 0.2910(3) 0.6871(6) 0.217(4) Uani 1 1 d .
O4 O 0.5183(2) 0.4576(2) 0.3984(4) 0.186(3) Uani 1 1 d .
O10 O 0.33599(14) 0.44134(14) 0.1487(3) 0.1057(14) Uani 1 1 d .
O11 O 0.30277(17) 0.36836(16) 0.0984(3) 0.1256(16) Uani 1 1 d .
O12 O 0.27411(13) 0.40505(15) 0.2242(3) 0.1073(14) Uani 1 1 d .
O13 O 0.35016(13) 0.37180(13) 0.2239(3) 0.0995(13) Uani 1 1 d .
O20 O 0.44543(13) 0.32254(12) 0.4526(3) 0.1007(13) Uani 1 1 d .
O21 O 0.36870(15) 0.29723(14) 0.5004(3) 0.1149(14) Uani 1 1 d .
O22 O 0.37708(12) 0.34356(13) 0.3752(3) 0.0977(12) Uani 1 1 d .
O23 O 0.23429(12) 0.40500(14) 0.3753(3) 0.1012(13) Uani 1 1 d .
O31 O 0.34632(16) 0.44724(17) 0.3734(4) 0.146(2) Uani 1 1 d .
O32 O 0.2965(6) 0.3038(3) 0.3117(13) 0.303(15) Uani 0.532(17) 1 d P
O33 O 0.29935(17) 0.3589(2) 0.4839(3) 0.157(2) Uani 1 1 d .
O41 O 0.45762(17) 0.32197(16) 0.2299(4) 0.145(2) Uani 1 1 d .
O42 O 0.3186(5) 0.2606(7) 0.2753(12) 0.299(17) Uani 0.468(17) 1 d P
O43 O 0.3641(2) 0.29391(17) 0.1139(4) 0.154(2) Uani 1 1 d .
O51 O 0.3475(10) 0.6978(10) 0.4362(17) 0.520(19) Uiso 0.773(10) 1 d PD
O61 O 0.6241(8) 0.3549(8) -0.0645(19) 0.494(18) Uiso 0.678(11) 1 d PD
O71 O 0.2500 0.2500 0.1666(16) 0.342(12) Uiso 1 4 d S
O72 O 0.2500 0.2500 0.4141(14) 0.295(10) Uiso 1 4 d S
O73 O 0.2500 0.7500 0.5000 0.55(2) Uiso 1 4 d S
O74 O 0.6380(10) 0.4356(10) 0.1457(16) 0.628(17) Uiso 1 1 d .
O75 O 0.5954(16) 0.1943(15) 0.757(3) 0.91(3) Uiso 1 1 d .
N1 N 0.2843(2) 0.5107(2) 0.2063(5) 0.139(3) Uani 1 1 d .
H1 H 0.2833 0.4867 0.2343 0.167 Uiso 1 1 calc R
N2 N 0.3471(3) 0.4265(3) -0.0114(4) 0.143(2) Uani 1 1 d .
H2 H 0.3390 0.3999 0.0020 0.172 Uiso 1 1 calc R
N3 N 0.4419(3) 0.3025(3) 0.6109(5) 0.150(3) Uani 1 1 d .
H3 H 0.4180 0.2905 0.5916 0.180 Uiso 1 1 calc R
N4 N 0.46022(19) 0.40939(17) 0.4023(5) 0.116(2) Uani 1 1 d .
H4 H 0.4399 0.3963 0.3747 0.139 Uiso 1 1 calc R
N5 N 0.3816(4) 0.5011(5) 0.4444(11) 0.316(9) Uani 1 1 d D
N6 N 0.5270(5) 0.3388(2) 0.1802(11) 0.304(9) Uani 1 1 d D
N7 N 0.3935(6) 0.6666(5) 0.4888(10) 0.247(7) Uiso 0.773(10) 1 d PD
N8 N 0.6008(5) 0.4186(7) -0.1136(12) 0.267(9) Uiso 0.678(11) 1 d PD
C1A C 0.2774(2) 0.5500(2) 0.3318(4) 0.152(4) Uani 1 1 d G
C2A C 0.26043(17) 0.51350(16) 0.3730(6) 0.140(3) Uani 1 1 d G
H11 H 0.2516 0.4878 0.3461 0.169 Uiso 1 1 calc R
C3A C 0.25673(19) 0.5153(2) 0.4545(6) 0.156(4) Uani 1 1 d G
H12 H 0.2454 0.4909 0.4821 0.187 Uiso 1 1 calc R
C4A C 0.2700(2) 0.5537(3) 0.4947(5) 0.193(5) Uani 1 1 d G
H13 H 0.2675 0.5549 0.5492 0.232 Uiso 1 1 calc R
C5A C 0.2869(2) 0.5902(2) 0.4535(6) 0.241(8) Uani 1 1 d G
H14 H 0.2957 0.6159 0.4804 0.289 Uiso 1 1 calc R
C6A C 0.2906(2) 0.58841(17) 0.3720(6) 0.212(7) Uani 1 1 d G
H15 H 0.3019 0.6129 0.3444 0.255 Uiso 1 1 calc R
C1B C 0.4121(3) 0.3939(4) -0.0691(6) 0.191(5) Uani 1 1 d G
C2B C 0.4000(4) 0.3522(5) -0.0389(6) 0.297(10) Uani 1 1 d G
H16 H 0.3747 0.3496 -0.0074 0.357 Uiso 1 1 calc R
C3B C 0.4258(5) 0.3146(4) -0.0560(8) 0.46(2) Uani 1 1 d G
H17 H 0.4177 0.2868 -0.0358 0.554 Uiso 1 1 calc R
C4B C 0.4637(5) 0.3186(4) -0.1032(8) 0.330(12) Uani 1 1 d G
H18 H 0.4809 0.2934 -0.1146 0.396 Uiso 1 1 calc R
C5B C 0.4758(3) 0.3602(5) -0.1333(6) 0.275(10) Uani 1 1 d G
H19 H 0.5011 0.3629 -0.1649 0.330 Uiso 1 1 calc R
C6B C 0.4500(4) 0.3979(3) -0.1163(5) 0.203(5) Uani 1 1 d G
H20 H 0.4581 0.4257 -0.1364 0.243 Uiso 1 1 calc R
C1C C 0.4502(6) 0.2316(3) 0.6747(7) 0.246(8) Uani 1 1 d G
C2C C 0.4088(6) 0.2157(5) 0.6496(7) 0.44(2) Uani 1 1 d G
H21 H 0.3908 0.2334 0.6174 0.530 Uiso 1 1 calc R
C3C C 0.3942(5) 0.1735(6) 0.6728(9) 0.63(4) Uani 1 1 d G
H22 H 0.3665 0.1629 0.6561 0.755 Uiso 1 1 calc R
C4C C 0.4211(7) 0.1471(3) 0.7210(9) 0.78(5) Uani 1 1 d G
H23 H 0.4113 0.1188 0.7365 0.930 Uiso 1 1 calc R
C5C C 0.4625(6) 0.1629(5) 0.7460(7) 0.432(18) Uani 1 1 d GU
H24 H 0.4805 0.1453 0.7783 0.519 Uiso 1 1 calc R
C6C C 0.4771(4) 0.2052(6) 0.7229(7) 0.307(11) Uani 1 1 d G
H25 H 0.5048 0.2158 0.7396 0.368 Uiso 1 1 calc R
C1D C 0.4835(2) 0.44336(17) 0.2778(4) 0.116(3) Uani 1 1 d G
C2D C 0.44598(15) 0.43004(16) 0.2353(5) 0.127(3) Uani 1 1 d G
H26 H 0.4219 0.4166 0.2610 0.152 Uiso 1 1 calc R
C3D C 0.4444(2) 0.4368(2) 0.1544(5) 0.149(3) Uani 1 1 d G
H27 H 0.4192 0.4279 0.1260 0.178 Uiso 1 1 calc R
C4D C 0.4803(3) 0.4570(2) 0.1160(4) 0.167(4) Uani 1 1 d G
H28 H 0.4792 0.4615 0.0619 0.201 Uiso 1 1 calc R
C5D C 0.5178(2) 0.47028(19) 0.1585(5) 0.175(5) Uani 1 1 d G
H29 H 0.5419 0.4837 0.1329 0.210 Uiso 1 1 calc R
C6D C 0.51945(15) 0.46347(18) 0.2394(5) 0.148(4) Uani 1 1 d G
H30 H 0.5446 0.4724 0.2678 0.178 Uiso 1 1 calc R
C11 C 0.31446(18) 0.4694(2) 0.0959(5) 0.122(3) Uani 1 1 d G
C12 C 0.2887(2) 0.5048(2) 0.1238(5) 0.137(3) Uani 1 1 d G
C13 C 0.26902(19) 0.53463(19) 0.0712(7) 0.177(5) Uani 1 1 d G
H5 H 0.2518 0.5584 0.0899 0.212 Uiso 1 1 calc R
C14 C 0.2751(2) 0.5290(3) -0.0093(6) 0.198(5) Uani 1 1 d G
H6 H 0.2619 0.5489 -0.0445 0.237 Uiso 1 1 calc R
C15 C 0.3008(3) 0.4935(3) -0.0372(4) 0.180(4) Uani 1 1 d G
H7 H 0.3049 0.4897 -0.0910 0.216 Uiso 1 1 calc R
C16 C 0.32051(19) 0.4637(2) 0.0154(5) 0.139(3) Uani 1 1 d G
C17 C 0.2817(3) 0.5494(4) 0.2446(8) 0.161(4) Uani 1 1 d .
C18 C 0.3834(4) 0.4309(5) -0.0554(6) 0.155(4) Uani 1 1 d .
C21 C 0.45137(16) 0.35615(15) 0.5083(4) 0.110(2) Uani 1 1 d G
C22 C 0.45178(19) 0.34611(16) 0.5881(4) 0.132(3) Uani 1 1 d G
C23 C 0.4614(2) 0.3794(2) 0.6428(3) 0.154(3) Uani 1 1 d G
H8 H 0.4617 0.3727 0.6962 0.184 Uiso 1 1 calc R
C24 C 0.47062(19) 0.4228(2) 0.6175(4) 0.153(4) Uani 1 1 d G
H9 H 0.4771 0.4451 0.6541 0.183 Uiso 1 1 calc R
C25 C 0.47021(17) 0.43287(14) 0.5377(5) 0.146(3) Uani 1 1 d G
H10 H 0.4764 0.4619 0.5208 0.175 Uiso 1 1 calc R
C26 C 0.46058(16) 0.39954(19) 0.4830(3) 0.109(2) Uani 1 1 d G
C27 C 0.4652(6) 0.2784(4) 0.6580(8) 0.182(5) Uani 1 1 d .
C28 C 0.4884(3) 0.4374(3) 0.3627(7) 0.132(3) Uani 1 1 d .
C31 C 0.3564(6) 0.4622(6) 0.4454(11) 0.284(9) Uiso 1 1 d D
H31 H 0.3474 0.4480 0.4914 0.341 Uiso 1 1 calc R
C32 C 0.3885(9) 0.5256(8) 0.3754(14) 0.429(18) Uiso 1 1 d D
H32 H 0.3846 0.5063 0.3307 0.515 Uiso 1 1 calc R
H33 H 0.4184 0.5375 0.3753 0.515 Uiso 1 1 calc R
H34 H 0.3673 0.5497 0.3728 0.515 Uiso 1 1 calc R
C33 C 0.3815(8) 0.5246(8) 0.5207(13) 0.465(17) Uiso 1 1 d D
H35 H 0.4090 0.5185 0.5481 0.558 Uiso 1 1 calc R
H36 H 0.3566 0.5143 0.5517 0.558 Uiso 1 1 calc R
H37 H 0.3787 0.5563 0.5120 0.558 Uiso 1 1 calc R
C41 C 0.4773(6) 0.3282(5) 0.1683(9) 0.219(6) Uiso 1 1 d .
H38 H 0.4637 0.3267 0.1192 0.263 Uiso 1 1 calc R
C42 C 0.5456(7) 0.3522(7) 0.1053(10) 0.361(11) Uiso 1 1 d D
H39 H 0.5609 0.3803 0.1111 0.433 Uiso 1 1 calc R
H40 H 0.5219 0.3552 0.0674 0.433 Uiso 1 1 calc R
H41 H 0.5665 0.3298 0.0877 0.433 Uiso 1 1 calc R
C43 C 0.5452(9) 0.3425(9) 0.2598(15) 0.47(2) Uiso 1 1 d D
H42 H 0.5497 0.3735 0.2726 0.559 Uiso 1 1 calc R
H43 H 0.5734 0.3270 0.2624 0.559 Uiso 1 1 calc R
H44 H 0.5246 0.3293 0.2966 0.559 Uiso 1 1 calc R
C51 C 0.3521(7) 0.6905(8) 0.5102(17) 0.352(14) Uiso 0.773(10) 1 d PD
H45 H 0.3365 0.6971 0.5561 0.553 Uiso 0.773(10) 1 calc PR
C52 C 0.4195(8) 0.6587(8) 0.4156(13) 0.343(13) Uiso 0.773(10) 1 d PD
H46 H 0.4356 0.6309 0.4199 0.386 Uiso 0.773(10) 1 calc PR
H47 H 0.4404 0.6828 0.4079 0.386 Uiso 0.773(10) 1 calc PR
H48 H 0.3994 0.6573 0.3715 0.386 Uiso 0.773(10) 1 calc PR
C53 C 0.4187(6) 0.6464(6) 0.5482(11) 0.252(9) Uiso 0.773(10) 1 d PD
H49 H 0.3990 0.6366 0.5895 0.395 Uiso 0.773(10) 1 calc PR
H50 H 0.4398 0.6676 0.5688 0.395 Uiso 0.773(10) 1 calc PR
H51 H 0.4344 0.6210 0.5270 0.395 Uiso 0.773(10) 1 calc PR
C61 C 0.6146(7) 0.3754(9) -0.1248(18) 0.51(3) Uiso 0.678(11) 1 d PD
H52 H 0.6166 0.3625 -0.1745 0.676 Uiso 0.678(11) 1 calc PR
C62 C 0.5954(9) 0.4428(7) -0.0422(17) 0.361(16) Uiso 0.678(11) 1 d PD
H53 H 0.6234 0.4434 -0.0142 0.534 Uiso 0.678(11) 1 calc PR
H54 H 0.5730 0.4285 -0.0103 0.534 Uiso 0.678(11) 1 calc PR
H55 H 0.5862 0.4730 -0.0538 0.534 Uiso 0.678(11) 1 calc PR
C63 C 0.5953(8) 0.4272(9) -0.1960(14) 0.327(14) Uiso 0.678(11) 1 d PD
H56 H 0.6102 0.4043 -0.2257 0.567 Uiso 0.678(11) 1 calc PR
H57 H 0.6081 0.4559 -0.2086 0.567 Uiso 0.678(11) 1 calc PR
H58 H 0.5640 0.4274 -0.2088 0.567 Uiso 0.678(11) 1 calc PR
H59 H 0.2928(16) 0.2655(18) 0.353(3) 0.089 Uiso 1 1 d .
H60 H 0.2944(16) 0.2340(18) 0.235(3) 0.089 Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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
O31 Ca1 O22 87.08(15) . .
O31 Ca1 O33 97.5(2) . .
O22 Ca1 O33 78.98(17) . .
O31 Ca1 O23 99.06(16) . .
O22 Ca1 O23 157.80(17) . .
O33 Ca1 O23 79.07(17) . .
O31 Ca1 O32 158.9(6) . .
O22 Ca1 O32 74.8(4) . .
O33 Ca1 O32 89.6(5) . .
O23 Ca1 O32 101.8(5) . .
O31 Ca1 O12 94.9(2) . .
O22 Ca1 O12 130.03(15) . .
O33 Ca1 O12 149.04(16) . .
O23 Ca1 O12 71.01(15) . .
O32 Ca1 O12 88.8(4) . .
O31 Ca1 O13 89.21(19) . .
O22 Ca1 O13 70.89(15) . .
O33 Ca1 O13 148.73(16) . .
O23 Ca1 O13 130.11(16) . .
O32 Ca1 O13 74.8(6) . .
O12 Ca1 O13 59.25(14) . .
O31 Ca1 O42 156.3(3) . 3
O22 Ca1 O42 112.4(2) . 3
O33 Ca1 O42 99.4(3) . 3
O23 Ca1 O42 68.3(2) . 3
O32 Ca1 O42 37.7(4) . 3
O12 Ca1 O42 62.4(3) . 3
O12 Ca1 Ca2 38.86(9) . 3
O13 Ca1 Ca2 91.77(11) . 3
O41 Ca2 O43 98.2(2) . .
O42 Ca2 O43 86.3(5) . .
O41 Ca2 O13 98.59(16) . .
O42 Ca2 O13 97.9(7) . .
O43 Ca2 O13 79.25(17) . .
O41 Ca2 O12 88.90(17) . 4
O42 Ca2 O12 76.2(5) . 4
O43 Ca2 O12 79.47(17) . 4
O13 Ca2 O12 158.24(17) . 4
O41 Ca2 O23 89.3(2) . 4
O42 Ca2 O23 79.1(7) . 4
O43 Ca2 O23 149.37(16) . 4
O13 Ca2 O23 129.14(15) . 4
O12 Ca2 O23 70.98(14) 4 4
O41 Ca2 O22 93.25(19) . .
O42 Ca2 O22 90.8(3) . .
O43 Ca2 O22 148.94(16) . .
O13 Ca2 O22 70.52(14) . .
O12 Ca2 O22 129.74(16) 4 .
O23 Ca2 O22 58.86(13) 4 .
O41 Ca2 O32 157.4(3) . .
O42 Ca2 O32 33.7(4) . .
O43 Ca2 O32 98.1(4) . .
O13 Ca2 O32 69.4(2) . .
O12 Ca2 O32 109.4(2) 4 .
O23 Ca2 O32 84.6(3) 4 .
O22 Ca2 O32 65.0(3) . .
O21 P2 O22 115.2(3) . .
O21 P2 O23 116.2(2) . 4
O22 P2 O23 109.3(3) . 4
O21 P2 O20 107.4(3) . .
O22 P2 O20 105.0(2) . .
O23 P2 O20 102.2(2) 4 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O31 2.325(5) .
Ca1 O22 2.356(4) .
Ca1 O33 2.360(6) .
Ca1 O23 2.367(4) .
Ca1 O32 2.402(11) .
Ca1 O12 2.499(5) .
Ca1 O13 2.506(4) .
Ca1 P1 3.050(3) .
Ca1 O42 3.05(3) 3
Ca1 Ca2 3.7044(17) .
Ca1 Ca2 3.7211(18) 3
Ca2 O41 2.296(5) .
Ca2 O42 2.349(10) .
Ca2 O43 2.355(6) .
Ca2 O13 2.364(4) .
Ca2 O12 2.369(4) 4
Ca2 O23 2.499(5) 4
Ca2 O22 2.519(4) .
Ca2 O32 2.83(2) .
Ca2 P2 3.059(3) .
Ca2 C41 3.190(19) .
Ca2 Ca1 3.7212(18) 4
P1 O11 1.501(5) .
P1 O12 1.510(4) .
P1 O13 1.521(4) .
P1 O10 1.647(4) .
P2 O21 1.507(5) .
P2 O22 1.510(4) .
P2 O23 1.512(4) 4
P2 O20 1.646(4) .
O1 C17 1.245(11) .
O2 C18 1.245(12) .
O3 C27 1.191(13) .
O4 C28 1.235(9) .
O10 C11 1.384(6) .
O12 Ca2 2.369(4) 3
O20 C21 1.389(5) .
O23 P2 1.512(4) 3
O23 Ca2 2.499(5) 3
O31 C31 1.336(19) .
O32 O42 1.57(2) .
O32 H59 1.34(5) .
O41 C41 1.216(15) .
O42 Ca1 3.05(3) 4
O42 H60 1.28(5) .
O51 C51 1.284(18) .
O61 C61 1.226(19) .
N1 C17 1.328(11) .
N1 C12 1.418(9) .
N1 H1 0.8600 .
N2 C18 1.320(11) .
N2 C16 1.437(9) .
N2 H2 0.8600 .
N3 C27 1.280(14) .
N3 C22 1.389(8) .
N3 H3 0.8600 .
N4 C28 1.363(9) .
N4 C26 1.403(8) .
N4 H4 0.8600 .
N5 C31 1.381(13) .
N5 C32 1.396(16) .
N5 C33 1.473(16) .
N6 C42 1.445(14) .
N6 C43 1.462(17) .
N6 C41 1.526(18) .
N7 C53 1.395(14) .
N7 C51 1.469(16) .
N7 C52 1.485(15) .
N8 C61 1.365(17) .
N8 C62 1.421(16) .
N8 C63 1.433(17) .
C1A C2A 1.3900 .
C1A C6A 1.3900 .
C1A C17 1.487(13) .
C2A C3A 1.3900 .
C2A H11 0.9300 .
C3A C4A 1.3900 .
C3A H12 0.9300 .
C4A C5A 1.3900 .
C4A H13 0.9300 .
C5A C6A 1.3900 .
C5A H14 0.9300 .
C6A H15 0.9300 .
C1B C2B 1.3900 .
C1B C6B 1.3900 .
C1B C18 1.418(12) .
C2B C3B 1.3900 .
C2B H16 0.9300 .
C3B C4B 1.3900 .
C3B H17 0.9300 .
C4B C5B 1.3900 .
C4B H18 0.9300 .
C5B C6B 1.3900 .
C5B H19 0.9300 .
C6B H20 0.9300 .
C1C C2C 1.3900 .
C1C C6C 1.3900 .
C1C C27 1.491(15) .
C2C C3C 1.3900 .
C2C H21 0.9300 .
C3C C4C 1.3900 .
C3C H22 0.9300 .
C4C C5C 1.3900 .
C4C H23 0.9300 .
C5C C6C 1.3900 .
C5C H24 0.9300 .
C6C H25 0.9300 .
C1D C2D 1.3900 .
C1D C6D 1.3900 .
C1D C28 1.461(11) .
C2D C3D 1.3900 .
C2D H26 0.9300 .
C3D C4D 1.3900 .
C3D H27 0.9300 .
C4D C5D 1.3900 .
C4D H28 0.9300 .
C5D C6D 1.3900 .
C5D H29 0.9300 .
C6D H30 0.9300 .
C11 C12 1.3900 .
C11 C16 1.3900 .
C12 C13 1.3900 .
C13 C14 1.3900 .
C13 H5 0.9300 .
C14 C15 1.3900 .
C14 H6 0.9300 .
C15 C16 1.3900 .
C15 H7 0.9300 .
C21 C22 1.3900 .
C21 C26 1.3900 .
C22 C23 1.3900 .
C23 C24 1.3900 .
C23 H8 0.9300 .
C24 C25 1.3900 .
C24 H9 0.9300 .
C25 C26 1.3900 .
C25 H10 0.9300 .
C31 H31 0.9300 .
C32 H32 0.9600 .
C32 H33 0.9600 .
C32 H34 0.9600 .
C33 H35 0.9600 .
C33 H36 0.9600 .
C33 H37 0.9600 .
C41 H38 0.9300 .
C42 H39 0.9600 .
C42 H40 0.9600 .
C42 H41 0.9600 .
C43 H42 0.9600 .
C43 H43 0.9600 .
C43 H44 0.9600 .
C51 H45 0.9300 .
C52 H46 0.9600 .
C52 H47 0.9600 .
C52 H48 0.9600 .
C53 H49 0.9600 .
C53 H50 0.9600 .
C53 H51 0.9600 .
C61 H52 0.9300 .
C62 H53 0.9600 .
C62 H54 0.9600 .
C62 H55 0.9600 .
C63 H56 0.9600 .
C63 H57 0.9600 .
C63 H58 0.9600 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N(1) H(1) O(10) . 0.860 2.533 2.757(8) 95.896 no
N(1) H(1) O(12) . 0.860 2.455 3.178(8) 142.125 no
N(2) H(2) O(11) . 0.860 2.176 2.869(8) 137.562 no
N(3) H(3) O(21) . 0.860 2.146 2.883(9) 143.528 no
N(4) H(4) O(20) . 0.860 2.571 2.762(6) 93.610 no
N(4) H(4) O(22) . 0.860 2.445 3.195(6) 146.108 no
N(1) H(1) O(41) 3_555 0.860 3.256 3.565(8) 104.078 no
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
C17 N1 C12 C13 -33.2(10)
C18 N2 C16 C15 58.5(10)
C18 N2 C16 C11 -121.9(8)
C27 N3 C22 C23 -50.6(13)
C27 N3 C22 C21 130.1(11)
C28 N4 C26 C25 37.9(8)
