#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:47:15 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179596 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/60/4506024.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_4506024
loop_
_publ_author_name
'Plonka, Anna M.'
'Banerjee, Debasis'
'Parise, John B.'
_publ_section_title
;
 Effect of Ligand Structural Isomerism in Formation of Calcium
 Coordination Networks
;
_journal_issue                   5
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2460
_journal_paper_doi               10.1021/cg300093h
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C33 H37 Ca3 N7 O16'
_chemical_formula_weight         907.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                98.257(2)
_cell_angle_beta                 111.863(2)
_cell_angle_gamma                107.785(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0501(3)
_cell_length_b                   13.9638(3)
_cell_length_c                   14.7073(3)
_cell_measurement_reflns_used    29343
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.8033
_cell_measurement_theta_min      3.1966
_cell_volume                     2092.18(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics
;
CrystalMaker (CrystalMaker, 2009) and Mercury (CCDC, 2010)
;
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4962
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54549
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro, Oxford Diffraction Ltd, 2010),
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.760
_refine_diff_density_min         -1.610
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0437
_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)+(0.0783P)²+1.9881P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                7482
_reflns_number_total             8526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300093h_si_002.cif
_cod_data_source_block           Ca3_5PDC_DMF
_cod_database_code               4506024
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.0000 0.0000 0.5000 0.02162(14) Uani 1 2 d S . .
Ca2 Ca 0.29920(4) 0.41956(3) 0.42279(3) 0.01877(11) Uani 1 1 d . . .
Ca3 Ca 0.0000 0.5000 0.0000 0.02985(17) Uani 1 2 d S . .
Ca4 Ca -0.46179(4) 0.06171(3) -0.13771(3) 0.01888(11) Uani 1 1 d . . .
O8 O -0.24180(15) 0.16187(13) -0.05908(12) 0.0294(4) Uani 1 1 d . . .
O2 O 0.25240(15) 0.31158(13) 0.51834(13) 0.0312(4) Uani 1 1 d . . .
O9 O 0.52385(16) 0.44612(13) 0.43037(12) 0.0319(4) Uani 1 1 d . . .
O6 O -0.31640(15) 0.01322(15) 0.22644(14) 0.0379(4) Uani 1 1 d . . .
O5 O -0.13578(16) 0.04385(14) 0.36380(13) 0.0357(4) Uani 1 1 d . . .
O4 O 0.84015(17) 0.46057(15) 0.83689(15) 0.0462(5) Uani 1 1 d . . .
O3 O 0.72685(17) 0.50314(16) 0.70457(15) 0.0493(6) Uani 1 1 d . . .
O1 O 0.15996(16) 0.16496(13) 0.54918(14) 0.0375(4) Uani 1 1 d . . .
C9 C -0.12223(19) 0.13839(16) 0.24397(16) 0.0213(4) Uani 1 1 d . . .
N2 N 0.07174(18) 0.28987(15) 0.28969(14) 0.0272(4) Uani 1 1 d . . .
C11 C -0.1015(2) 0.22520(17) 0.11840(16) 0.0231(4) Uani 1 1 d . . .
C14 C 0.0013(2) 0.21186(17) 0.31329(16) 0.0233(4) Uani 1 1 d . . .
H14 H 0.0365 0.2064 0.3794 0.028 Uiso 1 1 calc R . .
O7 O -0.09383(18) 0.32507(14) 0.00226(14) 0.0408(5) Uani 1 1 d . . .
C4 C 0.6147(2) 0.35918(17) 0.74394(17) 0.0251(5) Uani 1 1 d . . .
C3 C 0.4959(2) 0.34747(16) 0.66958(16) 0.0239(4) Uani 1 1 d . . .
H3 H 0.4905 0.3966 0.6334 0.029 Uiso 1 1 calc R . .
C2 C 0.3852(2) 0.26240(16) 0.64923(16) 0.0214(4) Uani 1 1 d . . .
C13 C 0.0193(2) 0.29582(18) 0.19382(17) 0.0273(5) Uani 1 1 d . . .
H13 H 0.0666 0.3505 0.1768 0.033 Uiso 1 1 calc R . .
C10 C -0.1729(2) 0.14470(17) 0.14441(16) 0.0237(4) Uani 1 1 d . . .
H10 H -0.2539 0.0955 0.0957 0.028 Uiso 1 1 calc R . .
C1 C 0.2554(2) 0.24434(16) 0.56576(16) 0.0224(4) Uani 1 1 d . . .
N1 N 0.51291(19) 0.20116(15) 0.77743(16) 0.0316(5) Uani 1 1 d . . .
O12 O 0.4417(2) 0.07409(13) 0.07407(14) 0.0384(4) Uani 1 1 d . . .
O10 O 0.35960(19) 0.29861(15) 0.32908(16) 0.0457(5) Uani 1 1 d . . .
C15 C 0.4687(2) 0.36661(18) 0.35332(18) 0.0278(5) Uani 1 1 d . . .
O11 O 0.5403(2) 0.16800(15) -0.00358(15) 0.0465(5) Uani 1 1 d . . .
C18 C 0.5518(2) 0.25773(18) 0.14865(18) 0.0295(5) Uani 1 1 d . . .
C16 C 0.5342(2) 0.35652(18) 0.28570(18) 0.0283(5) Uani 1 1 d . . .
C7 C 0.3985(2) 0.19077(17) 0.70498(18) 0.0277(5) Uani 1 1 d . . .
H7 H 0.3246 0.1331 0.6914 0.033 Uiso 1 1 calc R . .
C6 C 0.6189(2) 0.28488(18) 0.79675(18) 0.0303(5) Uani 1 1 d . . .
H6 H 0.6985 0.2933 0.8477 0.036 Uiso 1 1 calc R . .
C8 C -0.1968(2) 0.05836(17) 0.28092(17) 0.0243(4) Uani 1 1 d . . .
O16D O -0.4599(3) -0.0186(2) -0.29080(17) 0.0610(6) Uani 1 1 d . . .
C19 C 0.5077(2) 0.15802(18) 0.06666(18) 0.0293(5) Uani 1 1 d . . .
C5 C 0.7373(2) 0.44818(18) 0.76423(17) 0.0296(5) Uani 1 1 d . . .
C12 C -0.1500(2) 0.23870(17) 0.01189(17) 0.0246(4) Uani 1 1 d . . .
C17 C 0.4933(2) 0.26199(18) 0.21366(18) 0.0279(5) Uani 1 1 d . . .
H17 H 0.4277 0.2023 0.2089 0.033 Uiso 1 1 calc R . .
O13D O -0.0755(2) 0.0541(2) 0.61799(18) 0.0587(6) Uani 1 1 d . . .
O14D O 0.1824(2) 0.51223(19) 0.46536(19) 0.0607(6) Uani 1 1 d . . .
N3 N 0.6914(3) 0.44031(19) 0.2287(2) 0.0537(7) Uani 1 1 d . . .
C20 C 0.6495(3) 0.3483(2) 0.1596(2) 0.0447(7) Uani 1 1 d . . .
H20 H 0.6888 0.3451 0.1161 0.054 Uiso 1 1 calc R . .
C21 C 0.6336(3) 0.4429(2) 0.2903(2) 0.0399(6) Uani 1 1 d . . .
H21 H 0.6615 0.5062 0.3390 0.048 Uiso 1 1 calc R . .
O15D O 0.1313(3) 0.4489(2) -0.0613(2) 0.0729(7) Uani 1 1 d . . .
N7D N -0.5604(3) -0.1158(2) -0.4561(2) 0.0584(7) Uani 1 1 d . . .
C24D C 0.1062(4) 0.5487(3) 0.4155(4) 0.0712(11) Uani 1 1 d . . .
H24D H 0.0659 0.5203 0.3447 0.085 Uiso 1 1 calc R . .
N5D N 0.0774(3) 0.6211(2) 0.4512(3) 0.0665(9) Uani 1 1 d . . .
C33D C -0.1017(4) 0.0021(3) 0.6744(3) 0.0610(9) Uani 1 1 d . . .
N4D N -0.1031(4) 0.0403(3) 0.7603(2) 0.0749(10) Uani 1 1 d . . .
C27D C 0.1983(4) 0.4180(4) -0.0895(3) 0.0716(11) Uani 1 1 d . . .
H27D H 0.2007 0.4311 -0.1492 0.086 Uiso 1 1 calc R . .
N6D N 0.2673(5) 0.3690(5) -0.0471(4) 0.1167(18) Uani 1 1 d . . .
C26D C -0.0179(5) 0.6586(4) 0.3993(6) 0.123(2) Uani 1 1 d . . .
H26C H -0.0165 0.7139 0.4472 0.184 Uiso 1 1 calc R . .
H26A H -0.1020 0.6021 0.3679 0.184 Uiso 1 1 calc R . .
H26B H 0.0004 0.6850 0.3474 0.184 Uiso 1 1 calc R . .
C22D C -0.1323(6) -0.0259(5) 0.8231(4) 0.1066(19) Uani 1 1 d . . .
H22C H -0.1289 0.0161 0.8826 0.160 Uiso 1 1 calc R . .
H22B H -0.0695 -0.0570 0.8440 0.160 Uiso 1 1 calc R . .
H22A H -0.2176 -0.0803 0.7842 0.160 Uiso 1 1 calc R . .
C23D C -0.0748(9) 0.1524(5) 0.7963(5) 0.168(4) Uani 1 1 d . . .
H23C H -0.0804 0.1669 0.8599 0.253 Uiso 1 1 calc R . .
H23B H -0.1367 0.1705 0.7463 0.253 Uiso 1 1 calc R . .
H23A H 0.0112 0.1932 0.8063 0.253 Uiso 1 1 calc R . .
C25D C 0.1430(7) 0.6712(5) 0.5641(5) 0.113(2) Uani 1 1 d . . .
H25C H 0.1122 0.7241 0.5801 0.170 Uiso 1 1 calc R . .
H25B H 0.2352 0.7030 0.5869 0.170 Uiso 1 1 calc R . .
H25A H 0.1238 0.6188 0.5978 0.170 Uiso 1 1 calc R . .
C28D C 0.2562(6) 0.3386(5) 0.0457(5) 0.113 Uiso 1 1 d . . .
H28C H 0.3124 0.3026 0.0708 0.170 Uiso 1 1 calc R . .
H28A H 0.1681 0.2932 0.0262 0.170 Uiso 1 1 calc R . .
H28B H 0.2812 0.4008 0.0985 0.170 Uiso 1 1 calc R . .
C29D C 0.3429(6) 0.3315(5) -0.0870(5) 0.113 Uiso 1 1 d . . .
H29A H 0.3861 0.2971 -0.0423 0.170 Uiso 1 1 calc R . .
H29B H 0.4062 0.3896 -0.0915 0.170 Uiso 1 1 calc R . .
H29C H 0.2869 0.2825 -0.1539 0.170 Uiso 1 1 calc R . .
C31D C -0.4497(10) -0.1360(8) -0.4523(5) 0.113(3) Uani 0.675(5) 1 d P A 1
H31D H -0.4708 -0.1799 -0.5179 0.169 Uiso 0.675(5) 1 calc PR A 1
H31F H -0.4249 -0.1709 -0.4012 0.169 Uiso 0.675(5) 1 calc PR A 1
H31E H -0.3790 -0.0707 -0.4355 0.169 Uiso 0.675(5) 1 calc PR A 1
C30D C -0.5596(5) -0.0590(4) -0.3790(3) 0.0499(12) Uani 0.675(5) 1 d P A 1
H30D H -0.6338 -0.0465 -0.3871 0.060 Uiso 0.675(5) 1 calc PR A 1
C32D C -0.6744(7) -0.1542(6) -0.5612(4) 0.093(3) Uani 0.675(5) 1 d P A 1
H32C H -0.6574 -0.1946 -0.6091 0.139 Uiso 0.675(5) 1 calc PR A 1
H32A H -0.6867 -0.0950 -0.5828 0.139 Uiso 0.675(5) 1 calc PR A 1
H32B H -0.7514 -0.1973 -0.5582 0.139 Uiso 0.675(5) 1 calc PR A 1
C32' C -0.5810(17) -0.2011(13) -0.5249(13) 0.093 Uiso 0.325(5) 1 d P A 2
H32D H -0.6544 -0.2136 -0.5880 0.139 Uiso 0.325(5) 1 calc PR A 2
H32F H -0.5980 -0.2609 -0.4994 0.139 Uiso 0.325(5) 1 calc PR A 2
H32E H -0.5055 -0.1902 -0.5367 0.139 Uiso 0.325(5) 1 calc PR A 2
C30' C -0.4637(17) -0.0836(13) -0.3572(13) 0.093 Uiso 0.325(5) 1 d P A 2
H30' H -0.4010 -0.1121 -0.3414 0.111 Uiso 0.325(5) 1 calc PR A 2
C31' C -0.6583 -0.0676 -0.4673 0.093 Uiso 0.325(5) 1 d P A 2
H31C H -0.6235 -0.0079 -0.4088 0.139 Uiso 0.325(5) 1 calc PR A 2
H31B H -0.7362 -0.1185 -0.4720 0.139 Uiso 0.325(5) 1 calc PR A 2
H31A H -0.6779 -0.0454 -0.5282 0.139 Uiso 0.325(5) 1 calc PR A 2
H33D H -0.1209 -0.0827 0.6599 0.111 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'
O O 0.0106 0.0060 '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'
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
O1 Ca1 O1 180.0 2_556 .
O1 Ca1 O5 89.20(6) 2_556 2_556
O1 Ca1 O5 90.80(6) . 2_556
O1 Ca1 O5 90.80(6) 2_556 .
O1 Ca1 O5 89.20(6) . .
O5 Ca1 O5 180.0 2_556 .
O1 Ca1 O13D 92.27(8) 2_556 2_556
O1 Ca1 O13D 87.73(8) . 2_556
O5 Ca1 O13D 95.46(8) 2_556 2_556
O5 Ca1 O13D 84.54(8) . 2_556
O1 Ca1 O13D 87.73(8) 2_556 .
O1 Ca1 O13D 92.27(8) . .
O5 Ca1 O13D 84.54(8) 2_556 .
O5 Ca1 O13D 95.46(8) . .
O13D Ca1 O13D 179.999(1) 2_556 .
O1 Ca1 C33D 105.25(9) 2_556 2_556
O1 Ca1 C33D 74.75(9) . 2_556
O5 Ca1 C33D 108.65(8) 2_556 2_556
O5 Ca1 C33D 71.35(8) . 2_556
O13D Ca1 C33D 18.73(9) 2_556 2_556
O13D Ca1 C33D 161.28(9) . 2_556
O3 Ca2 O2 160.76(6) 2_666 .
O3 Ca2 O14D 83.60(9) 2_666 .
O2 Ca2 O14D 89.59(8) . .
O3 Ca2 O9 103.97(7) 2_666 2_666
O2 Ca2 O9 92.77(6) . 2_666
O14D Ca2 O9 81.77(8) . 2_666
O3 Ca2 O10 87.60(9) 2_666 .
O2 Ca2 O10 93.89(7) . .
O14D Ca2 O10 162.49(8) . .
O9 Ca2 O10 115.13(6) 2_666 .
O3 Ca2 N2 80.30(6) 2_666 .
O2 Ca2 N2 81.03(6) . .
O14D Ca2 N2 83.06(8) . .
O9 Ca2 N2 163.64(6) 2_666 .
O10 Ca2 N2 80.55(7) . .
O3 Ca2 O9 85.38(7) 2_666 .
O2 Ca2 O9 110.47(6) . .
O14D Ca2 O9 142.05(8) . .
O9 Ca2 O9 65.92(6) 2_666 .
O10 Ca2 O9 51.48(6) . .
N2 Ca2 O9 130.42(6) . .
O3 Ca2 C15 81.07(8) 2_666 .
O2 Ca2 C15 108.09(7) . .
O14D Ca2 C15 161.62(8) . .
O9 Ca2 C15 92.15(6) 2_666 .
O10 Ca2 C15 26.01(6) . .
N2 Ca2 C15 104.15(7) . .
O9 Ca2 C15 26.38(6) . .
O3 Ca2 Ca2 95.08(5) 2_666 2_666
O2 Ca2 Ca2 104.12(4) . 2_666
O14D Ca2 Ca2 113.93(7) . 2_666
O9 Ca2 Ca2 34.38(4) 2_666 2_666
O10 Ca2 Ca2 81.85(5) . 2_666
N2 Ca2 Ca2 161.97(5) . 2_666
O9 Ca2 Ca2 31.55(4) . 2_666
C15 Ca2 Ca2 57.82(5) . 2_666
O4 Ca3 O4 180.0 2_666 1_454
O4 Ca3 O15D 92.10(10) 2_666 2_565
O4 Ca3 O15D 87.90(10) 1_454 2_565
O4 Ca3 O15D 87.90(10) 2_666 .
O4 Ca3 O15D 92.10(10) 1_454 .
O15D Ca3 O15D 179.999(2) 2_565 .
O4 Ca3 O7 90.10(6) 2_666 2_565
O4 Ca3 O7 89.90(6) 1_454 2_565
O15D Ca3 O7 88.48(9) 2_565 2_565
O15D Ca3 O7 91.52(9) . 2_565
O4 Ca3 O7 89.90(6) 2_666 .
O4 Ca3 O7 90.10(6) 1_454 .
O15D Ca3 O7 91.52(9) 2_565 .
O15D Ca3 O7 88.48(9) . .
O7 Ca3 O7 180.0 2_565 .
O12 Ca4 O11 100.09(7) 2 1_455
O12 Ca4 O6 95.75(7) 2 2_455
O11 Ca4 O6 94.67(8) 1_455 2_455
O12 Ca4 O8 94.36(7) 2 .
O11 Ca4 O8 83.33(7) 1_455 .
O6 Ca4 O8 169.89(6) 2_455 .
O12 Ca4 O16D 91.57(8) 2 .
O11 Ca4 O16D 168.16(8) 1_455 .
O6 Ca4 O16D 86.18(8) 2_455 .
O8 Ca4 O16D 93.77(8) . .
O12 Ca4 N1 174.85(7) 2 1_454
O11 Ca4 N1 85.01(8) 1_455 1_454
O6 Ca4 N1 83.11(6) 2_455 1_454
O8 Ca4 N1 86.84(6) . 1_454
O16D Ca4 N1 83.36(8) . 1_454
C12 O8 Ca4 146.71(16) . .
C1 O2 Ca2 160.65(16) . .
C15 O9 Ca2 156.68(16) . 2_666
C15 O9 Ca2 88.32(14) . .
Ca2 O9 Ca2 114.08(6) 2_666 .
C8 O6 Ca4 174.98(19) . 2_455
C8 O5 Ca1 167.28(18) . .
C5 O4 Ca3 162.2(2) . 1_656
C5 O3 Ca2 171.0(2) . 2_666
C1 O1 Ca1 168.06(18) . .
C10 C9 C14 118.17(19) . .
C10 C9 C8 122.90(18) . .
C14 C9 C8 118.89(19) . .
C14 N2 C13 117.23(18) . .
C14 N2 Ca2 120.81(14) . .
C13 N2 Ca2 121.94(14) . .
C13 C11 C10 117.99(19) . .
C13 C11 C12 119.22(18) . .
C10 C11 C12 122.79(19) . .
N2 C14 C9 123.42(19) . .
N2 C14 H14 118.3 . .
C9 C14 H14 118.3 . .
C12 O7 Ca3 171.12(19) . .
C3 C4 C6 118.5(2) . .
C3 C4 C5 120.79(19) . .
C6 C4 C5 120.63(19) . .
C4 C3 C2 119.75(19) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C3 C2 C7 117.96(19) . .
C3 C2 C1 121.28(18) . .
C7 C2 C1 120.68(18) . .
N2 C13 C11 123.86(19) . .
N2 C13 H13 118.1 . .
C11 C13 H13 118.1 . .
C9 C10 C11 119.28(19) . .
C9 C10 H10 120.4 . .
C11 C10 H10 120.4 . .
O1 C1 O2 125.1(2) . .
O1 C1 C2 118.37(19) . .
O2 C1 C2 116.57(18) . .
C7 N1 C6 118.10(18) . .
C7 N1 Ca4 122.26(14) . 1_656
C6 N1 Ca4 119.28(14) . 1_656
C19 O12 Ca4 141.54(17) . 2
C15 O10 Ca2 93.39(14) . .
O10 C15 O9 122.4(2) . .
O10 C15 C16 118.9(2) . .
O9 C15 C16 118.6(2) . .
O10 C15 Ca2 60.60(13) . .
O9 C15 Ca2 65.30(12) . .
C16 C15 Ca2 157.81(17) . .
C19 O11 Ca4 137.68(17) . 1_655
C20 C18 C17 118.1(2) . .
C20 C18 C19 120.8(2) . .
C17 C18 C19 121.1(2) . .
C17 C16 C21 118.2(2) . .
C17 C16 C15 120.9(2) . .
C21 C16 C15 120.8(2) . .
N1 C7 C2 122.98(19) . .
N1 C7 H7 118.5 . .
C2 C7 H7 118.5 . .
N1 C6 C4 122.7(2) . .
N1 C6 H6 118.7 . .
C4 C6 H6 118.7 . .
O6 C8 O5 125.1(2) . .
O6 C8 C9 116.61(19) . .
O5 C8 C9 118.32(19) . .
C30' O16D C30D 59.7(9) . .
C30' O16D Ca4 161.1(8) . .
C30D O16D Ca4 124.4(3) . .
O12 C19 O11 126.0(2) . .
O12 C19 C18 118.0(2) . .
O11 C19 C18 116.0(2) . .
O4 C5 O3 125.1(2) . .
O4 C5 C4 118.61(19) . .
O3 C5 C4 116.31(19) . .
O7 C12 O8 125.4(2) . .
O7 C12 C11 117.34(19) . .
O8 C12 C11 117.23(18) . .
C16 C17 C18 119.0(2) . .
C16 C17 H17 120.5 . .
C18 C17 H17 120.5 . .
C33D O13D Ca1 123.5(2) . .
C24D O14D Ca2 133.0(3) . .
C21 N3 C20 116.8(2) . .
N3 C20 C18 124.1(2) . .
N3 C20 H20 117.9 . .
C18 C20 H20 117.9 . .
N3 C21 C16 123.7(2) . .
N3 C21 H21 118.1 . .
C16 C21 H21 118.1 . .
C27D O15D Ca3 175.9(3) . .
C30D N7D C32' 160.0(8) . .
C30D N7D C30' 55.7(8) . .
C32' N7D C30' 121.0(11) . .
C30D N7D C31D 122.9(5) . .
C32' N7D C31D 62.3(8) . .
C30' N7D C31D 68.2(8) . .
C30D N7D C31' 57.6(3) . .
C32' N7D C31' 123.7(8) . .
C30' N7D C31' 113.0(8) . .
C31D N7D C31' 163.7(5) . .
C30D N7D C32D 121.2(5) . .
C32' N7D C32D 60.5(8) . .
C30' N7D C32D 175.3(8) . .
C31D N7D C32D 115.5(5) . .
C31' N7D C32D 64.5(4) . .
O14D C24D N5D 126.7(4) . .
O14D C24D H24D 116.7 . .
N5D C24D H24D 116.7 . .
C24D N5D C26D 129.0(5) . .
C24D N5D C25D 118.4(4) . .
C26D N5D C25D 112.5(4) . .
O13D C33D N4D 125.2(4) . .
O13D C33D H33D 123.4(3) . .
N4D C33D H33D 111.4(3) . .
C33D N4D C22D 121.7(4) . .
C33D N4D C23D 120.4(4) . .
C22D N4D C23D 117.9(4) . .
O15D C27D N6D 127.4(4) . .
O15D C27D H27D 116.3 . .
N6D C27D H27D 116.3 . .
C27D N6D C29D 124.4(5) . .
C27D N6D C28D 117.2(4) . .
C29D N6D C28D 118.1(5) . .
N5D C26D H26C 109.5 . .
N5D C26D H26A 109.5 . .
H26C C26D H26A 109.5 . .
N5D C26D H26B 109.5 . .
H26C C26D H26B 109.5 . .
H26A C26D H26B 109.5 . .
N4D C22D H22C 109.5 . .
N4D C22D H22B 109.5 . .
H22C C22D H22B 109.5 . .
N4D C22D H22A 109.5 . .
H22C C22D H22A 109.5 . .
H22B C22D H22A 109.5 . .
N4D C23D H23C 109.5 . .
N4D C23D H23B 109.5 . .
H23C C23D H23B 109.5 . .
N4D C23D H23A 109.5 . .
H23C C23D H23A 109.5 . .
H23B C23D H23A 109.5 . .
N5D C25D H25C 109.5 . .
N5D C25D H25B 109.5 . .
H25C C25D H25B 109.5 . .
N5D C25D H25A 109.5 . .
H25C C25D H25A 109.5 . .
H25B C25D H25A 109.5 . .
N6D C28D H28C 109.5 . .
N6D C28D H28A 109.5 . .
H28C C28D H28A 109.5 . .
N6D C28D H28B 109.5 . .
H28C C28D H28B 109.5 . .
H28A C28D H28B 109.5 . .
N6D C29D H29A 109.5 . .
N6D C29D H29B 109.5 . .
H29A C29D H29B 109.5 . .
N6D C29D H29C 109.5 . .
H29A C29D H29C 109.5 . .
H29B C29D H29C 109.5 . .
N7D C31D H31D 109.5 . .
N7D C31D H31F 109.5 . .
H31D C31D H31F 109.5 . .
N7D C31D H31E 109.5 . .
H31D C31D H31E 109.5 . .
H31F C31D H31E 109.5 . .
N7D C30D O16D 122.4(4) . .
N7D C30D H30D 118.8 . .
O16D C30D H30D 118.8 . .
N7D C32D H32C 109.5 . .
N7D C32D H32A 109.5 . .
H32C C32D H32A 109.5 . .
N7D C32D H32B 109.5 . .
H32C C32D H32B 109.5 . .
H32A C32D H32B 109.5 . .
N7D C32' H32D 109.5 . .
N7D C32' H32F 109.5 . .
H32D C32' H32F 109.5 . .
N7D C32' H32E 109.5 . .
H32D C32' H32E 109.5 . .
H32F C32' H32E 109.5 . .
O16D C30' N7D 120.7(14) . .
O16D C30' H30' 119.7 . .
N7D C30' H30' 119.7 . .
N7D C31' H31C 109.5 . .
N7D C31' H31B 109.5 . .
H31C C31' H31B 109.5 . .
N7D C31' H31A 109.5 . .
H31C C31' H31A 109.5 . .
H31B C31' H31A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.3055(16) 2_556
Ca1 O1 2.3055(16) .
Ca1 O5 2.3638(16) 2_556
Ca1 O5 2.3639(16) .
Ca1 O13D 2.373(2) 2_556
Ca1 O13D 2.373(2) .
Ca1 C33D 3.229(3) 2_556
Ca2 O3 2.2632(17) 2_666
Ca2 O2 2.2903(15) .
Ca2 O14D 2.362(2) .
Ca2 O9 2.3857(16) 2_666
Ca2 O10 2.4721(19) .
Ca2 N2 2.5647(18) .
Ca2 O9 2.5745(17) .
Ca2 C15 2.833(2) .
Ca2 Ca2 4.1631(8) 2_666
Ca3 O4 2.3020(17) 2_666
Ca3 O4 2.3021(17) 1_454
Ca3 O15D 2.322(3) 2_565
Ca3 O15D 2.322(3) .
Ca3 O7 2.3686(16) 2_565
Ca3 O7 2.3686(16) .
Ca4 O12 2.2698(17) 2
Ca4 O11 2.2791(18) 1_455
Ca4 O6 2.2898(16) 2_455
Ca4 O8 2.3040(16) .
Ca4 O16D 2.378(2) .
Ca4 N1 2.4940(18) 1_454
O8 C12 1.248(3) .
O2 C1 1.249(3) .
O9 C15 1.259(3) .
O9 Ca2 2.3858(16) 2_666
O6 C8 1.248(3) .
O6 Ca4 2.2898(16) 2_455
O5 C8 1.250(3) .
O4 C5 1.240(3) .
O4 Ca3 2.3020(17) 1_656
O3 C5 1.243(3) .
O3 Ca2 2.2631(17) 2_666
O1 C1 1.243(3) .
C9 C10 1.389(3) .
C9 C14 1.394(3) .
C9 C8 1.509(3) .
N2 C14 1.338(3) .
N2 C13 1.340(3) .
C11 C13 1.388(3) .
C11 C10 1.389(3) .
C11 C12 1.517(3) .
C14 H14 0.9300 .
O7 C12 1.247(3) .
C4 C3 1.382(3) .
C4 C6 1.384(3) .
C4 C5 1.503(3) .
C3 C2 1.383(3) .
C3 H3 0.9300 .
C2 C7 1.391(3) .
C2 C1 1.502(3) .
C13 H13 0.9300 .
C10 H10 0.9300 .
N1 C7 1.341(3) .
N1 C6 1.342(3) .
N1 Ca4 2.4939(18) 1_656
O12 C19 1.245(3) .
O12 Ca4 2.2697(17) 2
O10 C15 1.244(3) .
C15 C16 1.498(3) .
O11 C19 1.246(3) .
O11 Ca4 2.2791(18) 1_655
C18 C20 1.379(4) .
C18 C17 1.388(3) .
C18 C19 1.504(3) .
C16 C17 1.386(3) .
C16 C21 1.389(3) .
C7 H7 0.9300 .
C6 H6 0.9300 .
O16D C30' 1.210(17) .
O16D C30D 1.289(5) .
C17 H17 0.9300 .
O13D C33D 1.242(4) .
O14D C24D 1.238(5) .
N3 C21 1.335(3) .
N3 C20 1.337(4) .
C20 H20 0.9300 .
C21 H21 0.9300 .
O15D C27D 1.193(5) .
N7D C30D 1.283(5) .
N7D C32' 1.338(16) .
N7D C30' 1.381(17) .
N7D C31D 1.428(8) .
N7D C31' 1.499(3) .
N7D C32D 1.514(7) .
C24D N5D 1.272(5) .
C24D H24D 0.9300 .
N5D C26D 1.415(5) .
N5D C25D 1.489(7) .
C33D N4D 1.307(5) .
C33D H33D 1.106(4) .
N4D C22D 1.456(6) .
N4D C23D 1.466(7) .
C27D N6D 1.278(6) .
C27D H27D 0.9300 .
N6D C29D 1.431(7) .
N6D C28D 1.526(7) .
C26D H26C 0.9600 .
C26D H26A 0.9600 .
C26D H26B 0.9600 .
C22D H22C 0.9600 .
C22D H22B 0.9600 .
C22D H22A 0.9600 .
C23D H23C 0.9600 .
C23D H23B 0.9600 .
C23D H23A 0.9600 .
C25D H25C 0.9600 .
C25D H25B 0.9600 .
C25D H25A 0.9600 .
C28D H28C 0.9600 .
C28D H28A 0.9600 .
C28D H28B 0.9600 .
C29D H29A 0.9600 .
C29D H29B 0.9600 .
C29D H29C 0.9600 .
C31D H31D 0.9600 .
C31D H31F 0.9600 .
C31D H31E 0.9600 .
C30D H30D 0.9300 .
C32D H32C 0.9600 .
C32D H32A 0.9600 .
C32D H32B 0.9600 .
C32' H32D 0.9600 .
C32' H32F 0.9600 .
C32' H32E 0.9600 .
C30' H30' 0.9300 .
C31' H31C 0.9600 .
C31' H31B 0.9600 .
C31' H31A 0.9600 .
