# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_[Mn(tpada)ClCa(OH2)3(MeOH)2]Cl
_database_code_depnum_ccdc_archive 'CCDC 995924'
_audit_update_record             
;
2014-04-07 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H39 Ca Cl2 Mn N4 O11.50'
_chemical_formula_weight         733.51

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'
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'
Cl Cl 0.1484 0.1585 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.7202(2)
_cell_length_b                   14.6163(3)
_cell_length_c                   13.0992(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.324(2)
_cell_angle_gamma                90.00
_cell_volume                     1666.79(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4093
_cell_measurement_theta_min      3.4065
_cell_measurement_theta_max      32.4143

_exptl_crystal_description       plate
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 -1 0.0306 -0.0000 -0.0003 -0.9997 0.0272 0.0446 0.0148
0 -1 0 0.0578 -0.0001 -1.0004 0.0003 0.0234 -0.0255 0.0341
0 1 0 0.0948 0.0001 1.0004 -0.0003 -0.0234 0.0255 -0.0341
0 0 1 0.0196 0.0000 0.0003 0.9997 -0.0272 -0.0446 -0.0148
-1 0 0 0.1558 -1.0001 -0.0024 0.0004 0.0610 -0.0141 -0.0522
1 0 0 0.1568 1.0001 0.0024 -0.0004 -0.0610 0.0141 0.0522
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             764
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.7929
_exptl_absorpt_correction_T_max  0.9625
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18389
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.41
_diffrn_reflns_theta_max         30.51
_reflns_number_total             10046
_reflns_number_gt                8219
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   44.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  179.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega   40.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  179.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
  3 omega  -18.00   42.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   57.0000  150.0000 60

#__ type_ start__ end____ width___ exp.time_
  4 omega  -53.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   37.0000  -60.0000 97

#__ type_ start__ end____ width___ exp.time_
  5 omega  -97.00  -48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000 -180.0000 49

#__ type_ start__ end____ width___ exp.time_
  6 omega    6.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   60.0000   22.0000 88

#__ type_ start__ end____ width___ exp.time_
  7 omega    1.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   37.0000  -60.0000 32

#__ type_ start__ end____ width___ exp.time_
  8 omega   61.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   37.0000  -60.0000 35

#__ type_ start__ end____ width___ exp.time_
  9 omega -100.00  -65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -37.0000  120.0000 35

;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0245P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(14)
_refine_ls_number_reflns         10046
_refine_ls_number_parameters     480
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0511
_refine_ls_wR_factor_ref         0.0848
_refine_ls_wR_factor_gt          0.0775
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.36007(4) 0.86908(3) 0.37912(3) 0.01497(9) Uani 1 1 d . . .
Ca1 Ca 0.37325(6) 1.04270(4) 0.16193(4) 0.01659(11) Uani 1 1 d . A .
Cl1 Cl 0.25606(8) 0.98772(5) 0.49705(5) 0.02246(15) Uani 1 1 d . . .
Cl2 Cl 0.55711(11) 0.34053(5) 0.14415(6) 0.0404(2) Uani 1 1 d . . .
O1 O 0.5217(2) 0.96507(13) 0.30246(15) 0.0182(4) Uani 1 1 d . . .
O2 O 0.7552(2) 1.03000(15) 0.31556(16) 0.0296(5) Uani 1 1 d . . .
O3 O 0.2259(2) 0.91496(13) 0.23350(14) 0.0188(4) Uani 1 1 d . . .
O4 O 0.0193(2) 0.88830(14) 0.12799(16) 0.0291(5) Uani 1 1 d . . .
N1 N 0.3658(3) 0.74387(17) 0.50544(17) 0.0200(5) Uani 1 1 d . . .
N2 N 0.5795(2) 0.87268(18) 0.47473(16) 0.0178(4) Uani 1 1 d . . .
N3 N 0.1338(3) 0.79539(15) 0.36847(19) 0.0184(5) Uani 1 1 d . . .
N4 N 0.4390(3) 0.74295(16) 0.29582(18) 0.0190(5) Uani 1 1 d . . .
C1 C 0.4601(3) 0.7755(2) 0.5958(2) 0.0264(7) Uani 1 1 d . . .
H1A H 0.4942 0.7221 0.6378 0.032 Uiso 1 1 calc R . .
H1B H 0.3974 0.8153 0.6382 0.032 Uiso 1 1 calc R . .
C2 C 0.5983(3) 0.8277(2) 0.5639(2) 0.0224(6) Uani 1 1 d . . .
C3 C 0.7341(4) 0.8338(2) 0.6236(2) 0.0298(7) Uani 1 1 d . . .
H3 H 0.7452 0.8022 0.6869 0.036 Uiso 1 1 calc R . .
C4 C 0.8537(3) 0.8861(2) 0.5904(2) 0.0310(7) Uani 1 1 d . . .
H4 H 0.9479 0.8905 0.6302 0.037 Uiso 1 1 calc R . .
C5 C 0.8334(3) 0.9320(2) 0.4978(2) 0.0248(6) Uani 1 1 d . . .
H5 H 0.9141 0.9677 0.4729 0.030 Uiso 1 1 calc R . .
C6 C 0.6941(3) 0.92479(19) 0.4425(2) 0.0184(6) Uani 1 1 d . . .
C7 C 0.6559(3) 0.97719(19) 0.3451(2) 0.0199(6) Uani 1 1 d . . .
C8 C 0.2064(3) 0.7263(2) 0.5308(2) 0.0250(7) Uani 1 1 d . . .
H8A H 0.1763 0.7711 0.5826 0.030 Uiso 1 1 calc R . .
H8B H 0.1994 0.6643 0.5607 0.030 Uiso 1 1 calc R . .
C9 C 0.0977(3) 0.7331(2) 0.4382(2) 0.0220(6) Uani 1 1 d . . .
C10 C -0.0362(4) 0.6819(2) 0.4252(3) 0.0297(7) Uani 1 1 d . . .
H10 H -0.0610 0.6377 0.4748 0.036 Uiso 1 1 calc R . .
C11 C -0.1325(4) 0.6957(2) 0.3399(3) 0.0368(8) Uani 1 1 d . . .
H11 H -0.2248 0.6615 0.3304 0.044 Uiso 1 1 calc R . .
C12 C -0.0944(3) 0.7598(2) 0.2679(3) 0.0299(7) Uani 1 1 d . . .
H12 H -0.1597 0.7707 0.2086 0.036 Uiso 1 1 calc R . .
C13 C 0.0412(3) 0.80737(19) 0.2849(2) 0.0203(6) Uani 1 1 d . . .
C14 C 0.0991(3) 0.8761(2) 0.2089(2) 0.0190(5) Uani 1 1 d . . .
C15 C 0.4373(4) 0.6635(2) 0.4604(2) 0.0301(7) Uani 1 1 d . . .
H15A H 0.3808 0.6083 0.4809 0.036 Uiso 1 1 calc R . .
H15B H 0.5437 0.6582 0.4905 0.036 Uiso 1 1 calc R . .
C16 C 0.4430(3) 0.66305(19) 0.3457(2) 0.0208(6) Uani 1 1 d . . .
C17 C 0.4618(4) 0.5808(2) 0.2950(3) 0.0301(7) Uani 1 1 d . . .
H17 H 0.4602 0.5245 0.3312 0.036 Uiso 1 1 calc R . .
C18 C 0.4828(5) 0.5817(2) 0.1917(3) 0.0437(10) Uani 1 1 d . . .
H18 H 0.4991 0.5263 0.1561 0.052 Uiso 1 1 calc R . .
C19 C 0.4798(4) 0.6637(3) 0.1409(3) 0.0386(9) Uani 1 1 d . . .
H19 H 0.4934 0.6659 0.0695 0.046 Uiso 1 1 calc R . .
C20 C 0.4570(3) 0.7422(2) 0.1948(2) 0.0269(7) Uani 1 1 d . . .
H20 H 0.4538 0.7988 0.1591 0.032 Uiso 1 1 calc R . .
O21 O 0.2493(2) 1.11000(15) 0.30352(18) 0.0250(5) Uani 1 1 d . . .
H1O H 0.256(4) 1.085(3) 0.358(3) 0.055(14) Uiso 1 1 d . . .
C21 C 0.0877(4) 1.1251(3) 0.2832(3) 0.0369(8) Uani 1 1 d . . .
H21A H 0.0693 1.1494 0.2138 0.055 Uiso 1 1 calc R . .
H21B H 0.0510 1.1692 0.3326 0.055 Uiso 1 1 calc R . .
H21C H 0.0325 1.0672 0.2893 0.055 Uiso 1 1 calc R . .
O22 O 0.5116(3) 0.94785(16) 0.05358(18) 0.0288(5) Uani 1 1 d . . .
H2O H 0.468(4) 0.928(3) 0.000(3) 0.036(11) Uiso 1 1 d . . .
C22 C 0.6732(4) 0.9310(3) 0.0599(3) 0.0392(8) Uani 1 1 d . . .
H22A H 0.7213 0.9647 0.0055 0.059 Uiso 1 1 calc R . .
H22B H 0.6920 0.8653 0.0518 0.059 Uiso 1 1 calc R . .
H22C H 0.7173 0.9513 0.1266 0.059 Uiso 1 1 calc R . .
O23 O 0.1771(3) 1.0167(2) 0.0361(2) 0.0380(7) Uani 1 1 d . . .
H1O3 H 0.127(7) 0.974(4) 0.057(4) 0.11(2) Uiso 1 1 d . . .
H2O3 H 0.152(8) 1.044(5) -0.002(6) 0.05(2) Uiso 0.671(6) 1 d P A 1
C23 C 0.1458(14) 1.0285(9) -0.0763(10) 0.048(3) Uani 0.329(6) 1 d P A 2
H23A H 0.1962 1.0843 -0.0988 0.072 Uiso 0.329(6) 1 calc PR A 2
H23B H 0.0348 1.0333 -0.0917 0.072 Uiso 0.329(6) 1 calc PR A 2
H23C H 0.1858 0.9756 -0.1123 0.072 Uiso 0.329(6) 1 calc PR A 2
O24 O 0.0725(5) 1.0601(4) -0.1551(3) 0.0623(17) Uani 0.671(6) 1 d P A 1
H4O H 0.1059 1.0131 -0.1833 0.093 Uiso 0.671(6) 1 calc PR A 1
C24 C -0.0870(7) 1.0653(6) -0.1738(5) 0.080(3) Uani 0.671(6) 1 d P A 1
H24A H -0.1303 1.1062 -0.1237 0.120 Uiso 0.671(6) 1 calc PR A 1
H24B H -0.1317 1.0041 -0.1680 0.120 Uiso 0.671(6) 1 calc PR A 1
H24C H -0.1105 1.0892 -0.2429 0.120 Uiso 0.671(6) 1 calc PR A 1
O25 O 0.3122(3) 1.18919(16) 0.0912(2) 0.0349(6) Uani 1 1 d . . .
H1O5 H 0.222(5) 1.210(3) 0.064(3) 0.061(14) Uiso 1 1 d . . .
H2O5 H 0.374(4) 1.230(2) 0.102(2) 0.025(10) Uiso 1 1 d . . .
O26 O 0.6031(3) 1.12764(17) 0.1705(2) 0.0304(5) Uani 1 1 d . . .
H1O6 H 0.612(5) 1.188(3) 0.158(3) 0.074(15) Uiso 1 1 d . . .
H2O6 H 0.669(4) 1.111(2) 0.214(2) 0.019(9) Uiso 1 1 d . . .
O31 O 1.0399(3) 0.2556(2) 0.0161(3) 0.0684(10) Uani 1 1 d . . .
H31O H 1.036(6) 0.295(3) -0.036(4) 0.081(18) Uiso 1 1 d . . .
C31 C 0.8938(14) 0.2075(10) 0.0154(11) 0.073(4) Uani 0.50 1 d P B 1
H31A H 0.9046 0.1531 0.0590 0.109 Uiso 0.50 1 calc PR B 1
H31B H 0.8627 0.1889 -0.0546 0.109 Uiso 0.50 1 calc PR B 1
H31C H 0.8155 0.2480 0.0414 0.109 Uiso 0.50 1 calc PR B 1
C31B C 0.937(4) 0.286(2) 0.086(2) 0.106(12) Uani 0.25 1 d PU B 2
H31D H 0.8473 0.3135 0.0497 0.159 Uiso 0.25 1 calc PR B 2
H31E H 0.9875 0.3318 0.1315 0.159 Uiso 0.25 1 calc PR B 2
H31F H 0.9042 0.2342 0.1272 0.159 Uiso 0.25 1 calc PR B 2
C31C C 0.896(3) 0.254(2) 0.0526(16) 0.048(6) Uani 0.25 1 d P B 3
H31G H 0.8866 0.3028 0.1025 0.071 Uiso 0.25 1 calc PR B 3
H31H H 0.8799 0.1944 0.0855 0.071 Uiso 0.25 1 calc PR B 3
H31I H 0.8193 0.2619 -0.0042 0.071 Uiso 0.25 1 calc PR B 3
O32 O 0.8165(4) 0.4314(3) 0.2797(3) 0.0530(18) Uani 0.643(8) 1 d P . .
O33 O 0.910(2) 0.3383(15) 0.2142(13) 0.102(10) Uani 0.200(10) 1 d P . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 N2 2.226(2) . ?
Mn1 N3 2.245(2) . ?
Mn1 O1 2.2646(19) . ?
Mn1 N4 2.269(2) . ?
Mn1 O3 2.280(2) . ?
Mn1 N1 2.466(2) . ?
Mn1 Cl1 2.5256(8) . ?
Mn1 Ca1 3.8190(6) . ?
Ca1 O23 2.337(3) . ?
Ca1 O26 2.355(2) . ?
Ca1 O22 2.364(2) . ?
Ca1 O25 2.381(2) . ?
Ca1 O21 2.410(2) . ?
Ca1 O1 2.465(2) . ?
Ca1 O3 2.4810(19) . ?
O1 C7 1.279(3) . ?
O2 C7 1.239(3) . ?
O3 C14 1.268(3) . ?
O4 C14 1.247(3) . ?
N1 C15 1.470(4) . ?
N1 C8 1.470(3) . ?
N1 C1 1.476(4) . ?
N2 C2 1.342(4) . ?
N2 C6 1.344(3) . ?
N3 C13 1.333(4) . ?
N3 C9 1.340(4) . ?
N4 C16 1.337(4) . ?
N4 C20 1.341(4) . ?
C1 C2 1.506(4) . ?
C2 C3 1.384(4) . ?
C3 C4 1.383(4) . ?
C4 C5 1.388(4) . ?
C5 C6 1.382(4) . ?
C6 C7 1.509(4) . ?
C8 C9 1.499(4) . ?
C9 C10 1.389(4) . ?
C10 C11 1.372(5) . ?
C11 C12 1.383(5) . ?
C12 C13 1.379(4) . ?
C13 C14 1.521(4) . ?
C15 C16 1.507(4) . ?
C16 C17 1.388(4) . ?
C17 C18 1.375(5) . ?
C18 C19 1.370(5) . ?
C19 C20 1.369(4) . ?
O21 C21 1.436(4) . ?
O22 C22 1.429(4) . ?
O23 C23 1.492(12) . ?
O24 C24 1.400(7) . ?
O31 C31C 1.37(2) . ?
O31 C31B 1.39(3) . ?
O31 C31 1.455(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Mn1 N3 140.35(9) . . ?
N2 Mn1 O1 72.42(8) . . ?
N3 Mn1 O1 146.84(8) . . ?
N2 Mn1 N4 90.86(9) . . ?
N3 Mn1 N4 82.56(8) . . ?
O1 Mn1 N4 94.36(7) . . ?
N2 Mn1 O3 147.83(8) . . ?
N3 Mn1 O3 71.50(8) . . ?
O1 Mn1 O3 75.48(7) . . ?
N4 Mn1 O3 89.54(8) . . ?
N2 Mn1 N1 69.92(8) . . ?
N3 Mn1 N1 70.68(8) . . ?
O1 Mn1 N1 140.21(7) . . ?
N4 Mn1 N1 74.03(8) . . ?
O3 Mn1 N1 140.28(8) . . ?
N2 Mn1 Cl1 88.11(6) . . ?
N3 Mn1 Cl1 91.25(6) . . ?
O1 Mn1 Cl1 95.78(5) . . ?
N4 Mn1 Cl1 168.98(6) . . ?
O3 Mn1 Cl1 97.17(5) . . ?
N1 Mn1 Cl1 95.34(6) . . ?
N2 Mn1 Ca1 109.97(6) . . ?
N3 Mn1 Ca1 109.68(6) . . ?
O1 Mn1 Ca1 37.97(5) . . ?
N4 Mn1 Ca1 99.12(6) . . ?
O3 Mn1 Ca1 38.50(5) . . ?
N1 Mn1 Ca1 173.11(6) . . ?
Cl1 Mn1 Ca1 91.54(2) . . ?
O23 Ca1 O26 134.86(10) . . ?
O23 Ca1 O22 81.90(10) . . ?
O26 Ca1 O22 82.84(9) . . ?
O23 Ca1 O25 74.56(11) . . ?
O26 Ca1 O25 73.42(9) . . ?
O22 Ca1 O25 113.83(9) . . ?
O23 Ca1 O21 105.47(9) . . ?
O26 Ca1 O21 99.60(8) . . ?
O22 Ca1 O21 165.58(8) . . ?
O25 Ca1 O21 80.34(9) . . ?
O23 Ca1 O1 141.57(9) . . ?
O26 Ca1 O1 78.37(8) . . ?
O22 Ca1 O1 85.08(7) . . ?
O25 Ca1 O1 143.16(8) . . ?
O21 Ca1 O1 81.54(7) . . ?
O23 Ca1 O3 76.72(9) . . ?
O26 Ca1 O3 146.81(8) . . ?
O22 Ca1 O3 94.53(8) . . ?
O25 Ca1 O3 135.63(8) . . ?
O21 Ca1 O3 75.59(7) . . ?
O1 Ca1 O3 68.44(6) . . ?
O23 Ca1 Mn1 111.42(8) . . ?
O26 Ca1 Mn1 112.17(7) . . ?
O22 Ca1 Mn1 95.51(6) . . ?
O25 Ca1 Mn1 150.66(7) . . ?
O21 Ca1 Mn1 70.35(6) . . ?
O1 Ca1 Mn1 34.41(4) . . ?
O3 Ca1 Mn1 34.90(5) . . ?
C7 O1 Mn1 117.99(17) . . ?
C7 O1 Ca1 133.62(18) . . ?
Mn1 O1 Ca1 107.62(7) . . ?
C14 O3 Mn1 118.56(17) . . ?
C14 O3 Ca1 134.78(18) . . ?
Mn1 O3 Ca1 106.59(7) . . ?
C15 N1 C8 112.3(2) . . ?
C15 N1 C1 110.0(2) . . ?
C8 N1 C1 111.3(2) . . ?
C15 N1 Mn1 108.45(16) . . ?
C8 N1 Mn1 107.39(17) . . ?
C1 N1 Mn1 107.13(17) . . ?
C2 N2 C6 119.7(2) . . ?
C2 N2 Mn1 122.39(19) . . ?
C6 N2 Mn1 117.85(18) . . ?
C13 N3 C9 119.6(2) . . ?
C13 N3 Mn1 118.42(18) . . ?
C9 N3 Mn1 121.6(2) . . ?
C16 N4 C20 118.2(2) . . ?
C16 N4 Mn1 118.34(18) . . ?
C20 N4 Mn1 122.5(2) . . ?
N1 C1 C2 110.7(2) . . ?
N2 C2 C3 121.2(3) . . ?
N2 C2 C1 115.5(3) . . ?
C3 C2 C1 123.2(3) . . ?
C4 C3 C2 119.6(3) . . ?
C3 C4 C5 118.8(3) . . ?
C6 C5 C4 119.0(3) . . ?
N2 C6 C5 121.7(3) . . ?
N2 C6 C7 114.9(2) . . ?
C5 C6 C7 123.3(3) . . ?
O2 C7 O1 126.0(3) . . ?
O2 C7 C6 117.2(3) . . ?
O1 C7 C6 116.8(2) . . ?
N1 C8 C9 111.5(2) . . ?
N3 C9 C10 120.8(3) . . ?
N3 C9 C8 115.8(3) . . ?
C10 C9 C8 123.4(3) . . ?
C11 C10 C9 119.4(3) . . ?
C10 C11 C12 119.7(3) . . ?
C13 C12 C11 118.0(3) . . ?
N3 C13 C12 122.6(3) . . ?
N3 C13 C14 114.6(2) . . ?
C12 C13 C14 122.8(3) . . ?
O4 C14 O3 126.0(3) . . ?
O4 C14 C13 117.4(2) . . ?
O3 C14 C13 116.6(2) . . ?
N1 C15 C16 116.3(2) . . ?
N4 C16 C17 121.6(3) . . ?
N4 C16 C15 118.8(2) . . ?
C17 C16 C15 119.5(3) . . ?
C18 C17 C16 119.2(3) . . ?
C19 C18 C17 119.2(3) . . ?
C20 C19 C18 118.8(3) . . ?
N4 C20 C19 123.0(3) . . ?
C21 O21 Ca1 113.55(19) . . ?
C22 O22 Ca1 127.1(2) . . ?
C23 O23 Ca1 139.6(5) . . ?
C31C O31 C31B 30.5(15) . . ?
C31C O31 C31 34.0(10) . . ?
C31B O31 C31 64.0(14) . . ?

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
O21 H1O Cl1 0.80(4) 2.31(4) 3.100(2) 169(4) .
O22 H2O Cl2 0.83(4) 2.28(4) 3.057(2) 156(3) 2_655
O23 H1O3 O4 0.82(6) 1.84(6) 2.657(4) 169(6) .
O23 H1O3 O3 0.82(6) 2.56(6) 2.992(4) 114(5) .
O23 H2O3 O24 0.67(7) 2.10(8) 2.691(5) 149(8) .
O24 H4O O32 0.84 1.89 2.707(6) 163.0 2_655
O24 H4O O33 0.84 2.59 3.34(2) 149.2 2_655
O25 H1O5 O31 0.90(4) 1.80(4) 2.698(4) 176(4) 1_465
O25 H2O5 Cl2 0.80(3) 2.32(3) 3.124(3) 175(3) 1_565
O26 H1O6 Cl2 0.90(5) 2.29(5) 3.154(3) 162(4) 1_565
O26 H2O6 O2 0.82(3) 1.90(3) 2.668(3) 154(3) .
O31 H31O O4 0.89(5) 1.87(5) 2.734(4) 164(4) 2_645
O33 H31E O31 1.31 1.95 3.134(19) 146.6 .

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.074
####################################################################### 
# 
# 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_[Ca(tpada)(OH2)2]2
_database_code_depnum_ccdc_archive 'CCDC 995925'
_audit_update_record             
;
2014-04-07 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H50.40 Ca2 N8 O17.20'
_chemical_formula_weight         998.65

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'
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.1802(5)
_cell_length_b                   23.6482(6)
_cell_length_c                   10.2620(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.840(5)
_cell_angle_gamma                90.00
_cell_volume                     2259.69(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2661
_cell_measurement_theta_min      3.3682
_cell_measurement_theta_max      32.3784

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -1 0 0.0549 0.0000 -1.0000 -0.0000 0.0082 0.0275 -0.0086
0 1 0 0.0549 -0.0000 1.0000 0.0000 -0.0082 -0.0275 0.0086
0 1 1 0.1417 0.0000 1.0000 1.0000 -0.0797 -0.0120 -0.0103
0 0 -1 0.1384 -0.0000 -0.0000 -1.0000 0.0715 -0.0155 0.0189
0 0 0 0.0860 -0.5000 0.0000 0.5000 -0.0271 0.0164 0.0266
0 0 0 0.0860 0.5000 -0.0000 -0.5000 0.0271 -0.0164 -0.0266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1048
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8551
_exptl_absorpt_correction_T_max  0.9641
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11187
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.37
_diffrn_reflns_theta_max         28.28
_reflns_number_total             5512
_reflns_number_gt                4033
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    7.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   57.0000  120.0000 79

#__ type_ start__ end____ width___ exp.time_
  2 omega  -17.00    9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   19.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
  3 omega   64.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   19.0000  -90.0000 28

#__ type_ start__ end____ width___ exp.time_
  4 omega  -43.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -68.0000  -35.0000 81

#__ type_ start__ end____ width___ exp.time_
  5 omega  -47.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -19.0000   90.0000 25

;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0309P)²+0.4458P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5512
_refine_ls_number_parameters     426
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.0916
_refine_ls_wR_factor_gt          0.0817
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.36397(4) 0.436691(16) 0.90633(4) 0.02240(10) Uani 1 1 d . . .
O1 O 0.38011(13) 0.53266(5) 1.00576(13) 0.0223(3) Uani 1 1 d . . .
O2 O 0.27525(16) 0.59625(6) 1.0924(2) 0.0500(5) Uani 1 1 d . . .
O3 O 0.44935(14) 0.41890(5) 1.16005(14) 0.0239(3) Uani 1 1 d . . .
O4 O 0.46629(15) 0.36666(5) 1.34807(14) 0.0274(3) Uani 1 1 d . . .
N1 N 0.12495(17) 0.38401(7) 0.70734(18) 0.0261(4) Uani 1 1 d . . .
N2 N 0.12366(16) 0.48164(6) 0.86264(16) 0.0200(3) Uani 1 1 d . . .
N3 N 0.28032(17) 0.34430(6) 0.97699(18) 0.0252(4) Uani 1 1 d . . .
N4 N 0.06400(18) 0.32593(7) 0.39894(18) 0.0304(4) Uani 1 1 d . . .
C1 C -0.0041(2) 0.39969(9) 0.7307(2) 0.0294(5) Uani 1 1 d . . .
H1A H -0.092(2) 0.3912(9) 0.649(2) 0.033(6) Uiso 1 1 d . . .
H1B H -0.009(2) 0.3761(9) 0.806(2) 0.032(6) Uiso 1 1 d . . .
C2 C -0.0034(2) 0.46040(8) 0.77310(19) 0.0241(4) Uani 1 1 d . . .
C3 C -0.1289(2) 0.49194(10) 0.7290(2) 0.0321(5) Uani 1 1 d . . .
H3 H -0.216(2) 0.4771(9) 0.659(2) 0.038(6) Uiso 1 1 d . . .
C4 C -0.1253(2) 0.54511(10) 0.7850(2) 0.0335(5) Uani 1 1 d . . .
H4 H -0.209(2) 0.5663(9) 0.756(2) 0.032(6) Uiso 1 1 d . . .
C5 C 0.0030(2) 0.56604(9) 0.8828(2) 0.0278(4) Uani 1 1 d . . .
H5 H 0.015(2) 0.6023(9) 0.927(2) 0.030(6) Uiso 1 1 d . . .
C6 C 0.1258(2) 0.53341(8) 0.9167(2) 0.0217(4) Uani 1 1 d . . .
C7 C 0.2718(2) 0.55578(8) 1.0134(2) 0.0243(4) Uani 1 1 d . . .
C8 C 0.1478(2) 0.32271(9) 0.7262(2) 0.0294(5) Uani 1 1 d . . .
H8A H 0.063(2) 0.3000(9) 0.670(2) 0.028(5) Uiso 1 1 d . . .
H8B H 0.226(2) 0.3110(8) 0.691(2) 0.022(5) Uiso 1 1 d . . .
C9 C 0.2002(2) 0.30613(8) 0.8813(2) 0.0263(4) Uani 1 1 d . . .
C10 C 0.1696(2) 0.25331(9) 0.9217(2) 0.0305(5) Uani 1 1 d . . .
H10 H 0.110(2) 0.2287(9) 0.853(2) 0.041(6) Uiso 1 1 d . . .
C11 C 0.2209(2) 0.23981(9) 1.0635(3) 0.0323(5) Uani 1 1 d . . .
H11 H 0.202(2) 0.2051(10) 1.096(2) 0.036(6) Uiso 1 1 d . . .
C12 C 0.3025(2) 0.27920(8) 1.1635(2) 0.0288(5) Uani 1 1 d . . .
H12 H 0.340(2) 0.2725(8) 1.258(2) 0.021(5) Uiso 1 1 d . . .
C13 C 0.3304(2) 0.33072(8) 1.1157(2) 0.0243(4) Uani 1 1 d . . .
C14 C 0.4229(2) 0.37568(8) 1.2172(2) 0.0225(4) Uani 1 1 d . . .
C15 C 0.1151(2) 0.40358(9) 0.5661(2) 0.0283(5) Uani 1 1 d . . .
H15A H 0.0902(19) 0.4433(8) 0.5576(19) 0.017(5) Uiso 1 1 d . . .
H15B H 0.210(2) 0.4009(8) 0.561(2) 0.020(5) Uiso 1 1 d . . .
C16 C 0.0105(2) 0.37181(8) 0.4384(2) 0.0258(4) Uani 1 1 d . . .
C17 C -0.1311(2) 0.38866(9) 0.3666(2) 0.0280(5) Uani 1 1 d . . .
H17 H -0.163(2) 0.4218(9) 0.396(2) 0.024(5) Uiso 1 1 d . . .
C18 C -0.2206(2) 0.35731(10) 0.2509(2) 0.0323(5) Uani 1 1 d . . .
H18 H -0.318(2) 0.3700(9) 0.199(2) 0.033(6) Uiso 1 1 d . . .
C19 C -0.1668(2) 0.31013(9) 0.2112(2) 0.0336(5) Uani 1 1 d . . .
H19 H -0.226(2) 0.2878(9) 0.131(2) 0.033(6) Uiso 1 1 d . . .
C20 C -0.0251(2) 0.29589(9) 0.2867(2) 0.0328(5) Uani 1 1 d . . .
H20 H 0.015(2) 0.2628(9) 0.263(2) 0.028(6) Uiso 1 1 d . . .
O11 O 0.36148(16) 0.49367(6) 0.70860(16) 0.0267(3) Uani 1 1 d . . .
H1O1 H 0.414(3) 0.5220(11) 0.741(3) 0.054(8) Uiso 1 1 d . . .
H2O1 H 0.399(3) 0.4755(12) 0.658(3) 0.063(9) Uiso 1 1 d . . .
O12 O 0.46021(18) 0.36536(7) 0.80019(19) 0.0365(4) Uani 1 1 d . . .
H1O2 H 0.437(3) 0.3491(13) 0.722(3) 0.076(10) Uiso 1 1 d . . .
H2O2 H 0.554(3) 0.3747(12) 0.835(3) 0.074(10) Uiso 1 1 d . . .
O13 O 0.36604(18) 0.30815(6) 0.52925(17) 0.0312(3) Uani 1 1 d . . .
H1O3 H 0.272(3) 0.3134(11) 0.486(3) 0.065(9) Uiso 1 1 d . . .
H2O3 H 0.401(3) 0.3231(12) 0.474(3) 0.075(11) Uiso 1 1 d . . .
O14 O 0.3846(4) 0.19194(11) 0.4134(4) 0.0516(12) Uani 0.601(5) 1 d PD . .
O15 O 0.5304(10) 0.4382(5) 0.5827(15) 0.035(2) Uani 0.53(3) 1 d P A 1
H2O5 H 0.599(7) 0.428(3) 0.655(8) 0.10(3) Uiso 0.53(3) 1 d P A 1
O15B O 0.4888(16) 0.4548(5) 0.5279(17) 0.038(2) Uani 0.47(3) 1 d P A 2
H3O5 H 0.474(7) 0.480(2) 0.487(7) 0.04(2) Uiso 0.47(3) 1 d P A 2
H1O5 H 0.505(4) 0.4229(16) 0.491(4) 0.092(12) Uiso 1 1 d . . .
H1O4 H 0.329(4) 0.1656(14) 0.416(5) 0.054(14) Uiso 0.601(5) 1 d PD . .
H2O4 H 0.379(4) 0.2209(12) 0.459(4) 0.051(14) Uiso 0.601(5) 1 d PD . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O12 2.4196(16) . ?
Ca1 O3 2.4253(14) . ?
Ca1 O11 2.4273(15) . ?
Ca1 O1 2.4664(13) . ?
Ca1 O1 2.4954(13) 3_667 ?
Ca1 N2 2.5355(16) . ?
Ca1 N3 2.5543(16) . ?
Ca1 N1 2.7616(16) . ?
Ca1 Ca1 4.0035(8) 3_667 ?
O1 C7 1.261(2) . ?
O1 Ca1 2.4954(13) 3_667 ?
O2 C7 1.246(2) . ?
O3 C14 1.261(2) . ?
O4 C14 1.251(2) . ?
N1 C8 1.468(3) . ?
N1 C1 1.475(3) . ?
N1 C15 1.486(3) . ?
N2 C6 1.341(2) . ?
N2 C2 1.345(2) . ?
N3 C9 1.341(2) . ?
N3 C13 1.343(3) . ?
N4 C20 1.345(3) . ?
N4 C16 1.348(2) . ?
C1 C2 1.499(3) . ?
C2 C3 1.388(3) . ?
C3 C4 1.377(3) . ?
C4 C5 1.378(3) . ?
C5 C6 1.388(3) . ?
C6 C7 1.510(3) . ?
C8 C9 1.511(3) . ?
C9 C10 1.391(3) . ?
C10 C11 1.370(3) . ?
C11 C12 1.387(3) . ?
C12 C13 1.385(3) . ?
C13 C14 1.519(3) . ?
C15 C16 1.512(3) . ?
C16 C17 1.386(3) . ?
C17 C18 1.384(3) . ?
C18 C19 1.375(3) . ?
C19 C20 1.376(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O12 Ca1 O3 109.13(5) . . ?
O12 Ca1 O11 83.11(6) . . ?
O3 Ca1 O11 150.67(5) . . ?
O12 Ca1 O1 148.91(5) . . ?
O3 Ca1 O1 77.32(4) . . ?
O11 Ca1 O1 79.13(5) . . ?
O12 Ca1 O1 79.15(5) . 3_667 ?
O3 Ca1 O1 78.08(4) . 3_667 ?
O11 Ca1 O1 78.32(5) . 3_667 ?
O1 Ca1 O1 72.42(5) . 3_667 ?
O12 Ca1 N2 138.59(6) . . ?
O3 Ca1 N2 99.44(5) . . ?
O11 Ca1 N2 86.34(5) . . ?
O1 Ca1 N2 65.52(5) . . ?
O1 Ca1 N2 137.21(5) 3_667 . ?
O12 Ca1 N3 76.91(5) . . ?
O3 Ca1 N3 64.08(5) . . ?
O11 Ca1 N3 145.10(5) . . ?
O1 Ca1 N3 130.07(5) . . ?
O1 Ca1 N3 124.40(5) 3_667 . ?
N2 Ca1 N3 90.01(5) . . ?
O12 Ca1 N1 75.45(5) . . ?
O3 Ca1 N1 122.81(5) . . ?
O11 Ca1 N1 85.64(5) . . ?
O1 Ca1 N1 127.77(5) . . ?
O1 Ca1 N1 151.34(5) 3_667 . ?
N2 Ca1 N1 63.87(5) . . ?
N3 Ca1 N1 61.89(5) . . ?
O12 Ca1 Ca1 114.22(4) . 3_667 ?
O3 Ca1 Ca1 74.69(3) . 3_667 ?
O11 Ca1 Ca1 75.98(4) . 3_667 ?
O1 Ca1 Ca1 36.45(3) . 3_667 ?
O1 Ca1 Ca1 35.96(3) 3_667 3_667 ?
N2 Ca1 Ca1 101.66(4) . 3_667 ?
N3 Ca1 Ca1 138.48(4) . 3_667 ?
N1 Ca1 Ca1 157.56(4) . 3_667 ?
C7 O1 Ca1 120.73(11) . . ?
C7 O1 Ca1 131.51(12) . 3_667 ?
Ca1 O1 Ca1 107.58(5) . 3_667 ?
C14 O3 Ca1 126.07(12) . . ?
C8 N1 C1 109.32(16) . . ?
C8 N1 C15 112.39(15) . . ?
C1 N1 C15 111.52(17) . . ?
C8 N1 Ca1 107.60(12) . . ?
C1 N1 Ca1 110.04(11) . . ?
C15 N1 Ca1 105.83(11) . . ?
C6 N2 C2 118.31(16) . . ?
C6 N2 Ca1 117.15(12) . . ?
C2 N2 Ca1 123.84(12) . . ?
C9 N3 C13 118.27(17) . . ?
C9 N3 Ca1 122.81(13) . . ?
C13 N3 Ca1 118.58(12) . . ?
C20 N4 C16 117.90(18) . . ?
N1 C1 C2 112.82(17) . . ?
N2 C2 C3 121.77(19) . . ?
N2 C2 C1 116.51(17) . . ?
C3 C2 C1 121.61(18) . . ?
C4 C3 C2 119.3(2) . . ?
C3 C4 C5 119.3(2) . . ?
C4 C5 C6 118.37(19) . . ?
N2 C6 C5 122.78(18) . . ?
N2 C6 C7 116.04(16) . . ?
C5 C6 C7 121.14(17) . . ?
O2 C7 O1 125.33(18) . . ?
O2 C7 C6 117.27(17) . . ?
O1 C7 C6 117.39(16) . . ?
N1 C8 C9 111.40(16) . . ?
N3 C9 C10 122.0(2) . . ?
N3 C9 C8 116.61(18) . . ?
C10 C9 C8 121.41(18) . . ?
C11 C10 C9 119.4(2) . . ?
C10 C11 C12 119.1(2) . . ?
C13 C12 C11 118.4(2) . . ?
N3 C13 C12 122.80(19) . . ?
N3 C13 C14 115.07(17) . . ?
C12 C13 C14 122.12(19) . . ?
O4 C14 O3 126.05(18) . . ?
O4 C14 C13 117.95(17) . . ?
O3 C14 C13 116.00(17) . . ?
N1 C15 C16 115.90(17) . . ?
N4 C16 C17 122.12(19) . . ?
N4 C16 C15 115.57(17) . . ?
C17 C16 C15 122.30(19) . . ?
C18 C17 C16 119.0(2) . . ?
C19 C18 C17 119.1(2) . . ?
C18 C19 C20 119.0(2) . . ?
N4 C20 C19 122.9(2) . . ?

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
O11 H1O1 O3 0.84(3) 1.94(3) 2.775(2) 172(3) 3_667
O11 H2O1 O15B 0.87(3) 1.96(3) 2.812(5) 165(3) .
O11 H2O1 O15 0.87(3) 2.00(3) 2.853(5) 166(3) .
O12 H1O2 O13 0.84(3) 2.05(3) 2.885(2) 176(3) .
O12 H2O2 O2 0.90(3) 1.73(3) 2.625(2) 170(3) 3_667
O12 H2O2 O1 0.90(3) 2.65(3) 3.132(2) 114(2) 3_667
O13 H1O3 N4 0.89(3) 1.96(3) 2.845(2) 178(3) .
O13 H2O3 O4 0.85(3) 1.97(3) 2.819(2) 172(3) 1_554
O15 H2O5 O2 0.82(7) 2.45(7) 3.219(17) 156(6) 3_667
O15B H3O5 O15B 0.71(6) 1.61(5) 2.25(3) 149(7) 3_666
O14 H1O4 O2 0.848(19) 1.94(2) 2.774(3) 169(4) 2_546
O14 H2O4 O13 0.844(19) 2.21(2) 3.030(3) 165(4) .

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.054
