#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/42/2214219.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2214219
loop_
_publ_author_name
'Xi-Shi Tai'
'Jie Yin'
' Ming-Yang Hao'
_publ_section_title
;
 Tetrakis(1,10-phenanthroline)calcium(II) bis(perchlorate)
 4-(dimethylamino)benzaldehyde disolvate
;
_journal_coeditor_code           HB2432
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1827
_journal_page_last               m1827
_journal_paper_doi               10.1107/S1600536807027055
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ca (C12 H8 N2)4] (Cl O4)2, 2C9 H11 N O'
_chemical_formula_moiety         'C48 H32 Ca N8 2+, 2(Cl O4 -), 2(C9 H11 N O)'
_chemical_formula_sum            'C66 H54 Ca Cl2 N10 O10'
_chemical_formula_weight         1258.17
_chemical_name_systematic
;
Tetrakis(1,10-phenanthroline)calcium(II) bis(perchlorate)
4-(dimethylamino)benzaldehyde disolvate
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.455(3)
_cell_length_b                   17.455(3)
_cell_length_c                   38.952(3)
_cell_measurement_reflns_used    2661
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.49
_cell_measurement_theta_min      2.66
_cell_volume                     11868(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1033
_diffrn_reflns_av_sigmaI/netI    0.1287
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            29937
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5232
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.562
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.2233
_refine_ls_R_factor_gt           0.0785
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1079P)²+113.9196P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1998
_refine_ls_wR_factor_ref         0.3877
_reflns_number_gt                1808
_reflns_number_total             5234
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2432.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2214219
_cod_database_fobs_code          2214219
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Ca Ca1 0.0000 0.7500 0.12539(6) 0.0351(6) Uani d S 1
Cl Cl1 0.5000 0.7500 0.02830(9) 0.0715(11) Uani d S 1
Cl Cl2 0.0000 0.2500 0.02789(8) 0.0603(10) Uani d S 1
N N1 -0.0545(4) 0.8700(4) 0.15864(19) 0.0474(19) Uani d . 1
N N2 0.0017(4) 0.8820(4) 0.09279(19) 0.0452(19) Uani d . 1
N N3 0.1283(4) 0.7490(4) 0.09188(19) 0.0452(19) Uani d . 1
N N4 0.1188(4) 0.8022(4) 0.15835(19) 0.0462(19) Uani d . 1
N N5 0.2086(6) 0.0408(6) 0.1909(3) 0.086(3) Uani d . 1
O O1 0.2703(8) -0.0671(6) 0.0342(3) 0.153(5) Uani d . 1
O O2 0.5000 0.7500 0.0637(3) 0.114(4) Uani d S 1
O O3 0.5413(15) 0.8168(15) 0.0180(6) 0.107(7) Uani d P 0.50
O O4 0.4339(13) 0.741(2) 0.0105(5) 0.103(7) Uani d P 0.50
O O5 0.5532(14) 0.6898(15) 0.0198(5) 0.110(7) Uani d P 0.50
O O6 0.0000 0.2500 0.0636(3) 0.094(4) Uani d S 1
O O7 0.0611(13) 0.2976(13) 0.0161(5) 0.092(6) Uani d P 0.50
O O8 -0.0639(12) 0.3007(11) 0.0189(4) 0.091(5) Uani d P 0.50
O O9 -0.0071(17) 0.1840(12) 0.0108(5) 0.089(6) Uani d P 0.50
C C1 -0.0806(6) 0.8672(6) 0.1906(3) 0.060(3) Uani d . 1
H H1 -0.0858 0.8191 0.2006 0.072 Uiso calc R 1
C C2 -0.1006(6) 0.9302(7) 0.2101(3) 0.068(3) Uani d . 1
H H2 -0.1174 0.9248 0.2326 0.082 Uiso calc R 1
C C3 -0.0950(6) 1.0007(7) 0.1951(3) 0.071(3) Uani d . 1
H H3 -0.1092 1.0441 0.2074 0.085 Uiso calc R 1
C C4 -0.0685(6) 1.0082(6) 0.1618(3) 0.055(3) Uani d . 1
C C5 -0.0482(5) 0.9408(5) 0.1440(3) 0.044(2) Uani d . 1
C C6 -0.0206(5) 0.9465(5) 0.1093(3) 0.044(2) Uani d . 1
C C7 -0.0164(5) 1.0191(6) 0.0936(3) 0.055(3) Uani d . 1
C C8 0.0096(6) 1.0232(7) 0.0594(3) 0.067(3) Uani d . 1
H H8 0.0132 1.0702 0.0483 0.080 Uiso calc R 1
C C9 0.0293(6) 0.9581(7) 0.0431(3) 0.065(3) Uani d . 1
H H9 0.0455 0.9595 0.0203 0.078 Uiso calc R 1
C C10 0.0251(5) 0.8889(6) 0.0604(2) 0.052(2) Uani d . 1
H H10 0.0394 0.8447 0.0488 0.062 Uiso calc R 1
C C11 -0.0615(6) 1.0812(6) 0.1450(4) 0.069(3) Uani d . 1
H H11 -0.0741 1.1257 0.1569 0.083 Uiso calc R 1
C C12 -0.0371(6) 1.0860(6) 0.1124(3) 0.068(3) Uani d . 1
H H12 -0.0335 1.1337 0.1019 0.082 Uiso calc R 1
C C13 0.1337(6) 0.7300(6) 0.0587(2) 0.055(3) Uani d . 1
H H13 0.0893 0.7150 0.0473 0.066 Uiso calc R 1
C C14 0.2021(7) 0.7315(6) 0.0403(3) 0.065(3) Uani d . 1
H H14 0.2027 0.7218 0.0168 0.078 Uiso calc R 1
C C15 0.2674(7) 0.7476(6) 0.0573(3) 0.067(3) Uani d . 1
H H15 0.3139 0.7458 0.0458 0.080 Uiso calc R 1
C C16 0.2660(6) 0.7666(6) 0.0918(3) 0.060(3) Uani d . 1
C C17 0.1935(5) 0.7696(5) 0.1083(3) 0.044(2) Uani d . 1
C C18 0.1890(5) 0.7927(5) 0.1433(3) 0.048(2) Uani d . 1
C C19 0.2581(6) 0.8087(6) 0.1616(3) 0.062(3) Uani d . 1
C C20 0.2527(7) 0.8315(7) 0.1959(3) 0.080(4) Uani d . 1
H H20 0.2968 0.8404 0.2087 0.096 Uiso calc R 1
C C21 0.1828(7) 0.8407(6) 0.2104(3) 0.072(3) Uani d . 1
H H21 0.1783 0.8566 0.2331 0.087 Uiso calc R 1
C C22 0.1170(6) 0.8257(6) 0.1907(3) 0.060(3) Uani d . 1
H H22 0.0694 0.8326 0.2010 0.072 Uiso calc R 1
C C23 0.3336(6) 0.7822(6) 0.1108(4) 0.070(3) Uani d . 1
H H23 0.3811 0.7797 0.1000 0.084 Uiso calc R 1
C C24 0.3295(6) 0.8005(7) 0.1442(4) 0.076(3) Uani d . 1
H H24 0.3746 0.8081 0.1564 0.091 Uiso calc R 1
C C25 0.3071(10) -0.0484(7) 0.0583(4) 0.112(6) Uani d . 1
H H25 0.3600 -0.0476 0.0555 0.135 Uiso calc R 1
C C26 0.2777(10) -0.0262(7) 0.0920(4) 0.093(5) Uani d . 1
C C27 0.2001(9) -0.0254(7) 0.1016(5) 0.104(6) Uani d . 1
H H27 0.1632 -0.0407 0.0858 0.124 Uiso calc R 1
C C28 0.1778(8) -0.0032(8) 0.1332(4) 0.092(5) Uani d . 1
H H28 0.1258 -0.0030 0.1383 0.110 Uiso calc R 1
C C29 0.2297(7) 0.0196(6) 0.1587(4) 0.069(3) Uani d . 1
C C30 0.3079(7) 0.0191(6) 0.1488(3) 0.073(3) Uani d . 1
H H30 0.3448 0.0349 0.1645 0.087 Uiso calc R 1
C C31 0.3309(7) -0.0042(7) 0.1166(3) 0.081(4) Uani d . 1
H H31 0.3828 -0.0052 0.1112 0.097 Uiso calc R 1
C C32 0.1287(8) 0.0439(9) 0.2004(4) 0.130(6) Uani d . 1
H H32A 0.1014 0.0753 0.1843 0.196 Uiso calc R 1
H H32B 0.1239 0.0653 0.2230 0.196 Uiso calc R 1
H H32C 0.1076 -0.0069 0.2002 0.196 Uiso calc R 1
C C33 0.2644(8) 0.0570(8) 0.2170(4) 0.103(4) Uani d . 1
H H33A 0.2985 0.0141 0.2193 0.154 Uiso calc R 1
H H33B 0.2388 0.0659 0.2384 0.154 Uiso calc R 1
H H33C 0.2931 0.1017 0.2107 0.154 Uiso calc R 1
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N3 Ca1 N3 6_464 . 119.5(3)
N3 Ca1 N4 6_464 . 159.1(2)
N3 Ca1 N4 . . 64.0(2)
N3 Ca1 N4 6_464 6_464 64.0(2)
N3 Ca1 N4 . 6_464 159.1(2)
N4 Ca1 N4 . 6_464 120.9(3)
N3 Ca1 N2 6_464 6_464 75.7(2)
N3 Ca1 N2 . 6_464 76.2(2)
N4 Ca1 N2 . 6_464 123.6(2)
N4 Ca1 N2 6_464 6_464 85.5(2)
N3 Ca1 N2 6_464 . 76.2(2)
N3 Ca1 N2 . . 75.7(2)
N4 Ca1 N2 . . 85.5(2)
N4 Ca1 N2 6_464 . 123.6(2)
N2 Ca1 N2 6_464 . 122.3(3)
N3 Ca1 N1 6_464 . 86.0(2)
N3 Ca1 N1 . . 124.3(2)
N4 Ca1 N1 . . 76.6(2)
N4 Ca1 N1 6_464 . 75.5(2)
N2 Ca1 N1 6_464 . 158.0(2)
N2 Ca1 N1 . . 63.0(2)
N3 Ca1 N1 6_464 6_464 124.3(2)
N3 Ca1 N1 . 6_464 86.0(2)
N4 Ca1 N1 . 6_464 75.5(2)
N4 Ca1 N1 6_464 6_464 76.6(2)
N2 Ca1 N1 6_464 6_464 63.0(2)
N2 Ca1 N1 . 6_464 158.0(2)
N1 Ca1 N1 . 6_464 121.3(3)
O4 Cl1 O4 . 6_564 118.4(19)
O4 Cl1 O2 . . 120.8(9)
O4 Cl1 O2 6_564 . 120.8(9)
O4 Cl1 O3 . 6_564 48.1(11)
O4 Cl1 O3 6_564 6_564 112.3(13)
O2 Cl1 O3 . 6_564 106.3(9)
O4 Cl1 O3 . . 112.3(13)
O4 Cl1 O3 6_564 . 48.1(11)
O2 Cl1 O3 . . 106.3(9)
O3 Cl1 O3 6_564 . 147.3(18)
O4 Cl1 O5 . . 110.4(13)
O4 Cl1 O5 6_564 . 54.4(12)
O2 Cl1 O5 . . 103.2(9)
O3 Cl1 O5 6_564 . 70.5(12)
O3 Cl1 O5 . . 101.9(13)
O4 Cl1 O5 . 6_564 54.4(12)
O4 Cl1 O5 6_564 6_564 110.4(13)
O2 Cl1 O5 . 6_564 103.2(9)
O3 Cl1 O5 6_564 6_564 101.9(13)
O3 Cl1 O5 . 6_564 70.5(12)
O5 Cl1 O5 . 6_564 153.6(17)
O9 Cl2 O9 . 6_454 120.2(17)
O9 Cl2 O6 . . 119.9(9)
O9 Cl2 O6 6_454 . 119.9(9)
O9 Cl2 O7 . 6_454 43.0(10)
O9 Cl2 O7 6_454 6_454 114.3(11)
O6 Cl2 O7 . 6_454 108.7(8)
O9 Cl2 O7 . . 114.3(11)
O9 Cl2 O7 6_454 . 43.0(10)
O6 Cl2 O7 . . 108.7(8)
O7 Cl2 O7 6_454 . 142.6(17)
O9 Cl2 O8 . 6_454 55.4(11)
O9 Cl2 O8 6_454 6_454 109.4(12)
O6 Cl2 O8 . 6_454 103.8(7)
O7 Cl2 O8 6_454 6_454 98.1(11)
O7 Cl2 O8 . 6_454 73.0(11)
O9 Cl2 O8 . . 109.4(12)
O9 Cl2 O8 6_454 . 55.4(11)
O6 Cl2 O8 . . 103.8(7)
O7 Cl2 O8 6_454 . 73.0(11)
O7 Cl2 O8 . . 98.1(11)
O8 Cl2 O8 6_454 . 152.5(14)
C1 N1 C5 . . 117.0(8)
C1 N1 Ca1 . . 123.7(6)
C5 N1 Ca1 . . 118.9(6)
C10 N2 C6 . . 117.6(8)
C10 N2 Ca1 . . 122.7(6)
C6 N2 Ca1 . . 119.7(6)
C13 N3 C17 . . 117.7(8)
C13 N3 Ca1 . . 123.3(6)
C17 N3 Ca1 . . 119.0(6)
C22 N4 C18 . . 117.9(8)
C22 N4 Ca1 . . 123.9(6)
C18 N4 Ca1 . . 117.3(6)
C29 N5 C33 . . 121.6(11)
C29 N5 C32 . . 120.6(12)
C33 N5 C32 . . 117.8(13)
O4 O3 Cl1 6_564 . 62.5(17)
O4 O3 O5 6_564 6_564 109(2)
Cl1 O3 O5 . 6_564 55.1(11)
O3 O4 O5 6_564 6_564 134(3)
O3 O4 Cl1 6_564 . 69.3(18)
O5 O4 Cl1 6_564 . 66.2(15)
O4 O5 Cl1 6_564 . 59.4(14)
O4 O5 O3 6_564 6_564 103(2)
Cl1 O5 O3 . 6_564 54.4(11)
O9 O7 Cl2 6_454 . 63.7(19)
O9 O7 O8 6_454 6_454 111(3)
Cl2 O7 O8 . 6_454 54.5(10)
O9 O8 Cl2 6_454 . 57.3(12)
O9 O8 O7 6_454 6_454 99.3(15)
Cl2 O8 O7 . 6_454 52.5(9)
O7 O9 O8 6_454 6_454 140(3)
O7 O9 Cl2 6_454 . 73(2)
O8 O9 Cl2 6_454 . 67.4(14)
N1 C1 C2 . . 125.0(10)
N1 C1 H1 . . 117.5
C2 C1 H1 . . 117.5
C3 C2 C1 . . 117.7(11)
C3 C2 H2 . . 121.2
C1 C2 H2 . . 121.2
C2 C3 C4 . . 120.6(10)
C2 C3 H3 . . 119.7
C4 C3 H3 . . 119.7
C3 C4 C5 . . 117.7(10)
C3 C4 C11 . . 122.6(10)
C5 C4 C11 . . 119.7(10)
N1 C5 C4 . . 122.0(9)
N1 C5 C6 . . 118.8(8)
C4 C5 C6 . . 119.2(9)
N2 C6 C7 . . 121.7(9)
N2 C6 C5 . . 119.1(8)
C7 C6 C5 . . 119.2(9)
C8 C7 C6 . . 118.3(10)
C8 C7 C12 . . 121.7(10)
C6 C7 C12 . . 120.0(11)
C9 C8 C7 . . 119.1(10)
C9 C8 H8 . . 120.5
C7 C8 H8 . . 120.5
C8 C9 C10 . . 119.4(10)
C8 C9 H9 . . 120.3
C10 C9 H9 . . 120.3
N2 C10 C9 . . 123.9(10)
N2 C10 H10 . . 118.0
C9 C10 H10 . . 118.0
C12 C11 C4 . . 120.8(10)
C12 C11 H11 . . 119.6
C4 C11 H11 . . 119.6
C11 C12 C7 . . 121.1(10)
C11 C12 H12 . . 119.4
C7 C12 H12 . . 119.4
N3 C13 C14 . . 123.6(10)
N3 C13 H13 . . 118.2
C14 C13 H13 . . 118.2
C15 C14 C13 . . 118.3(10)
C15 C14 H14 . . 120.8
C13 C14 H14 . . 120.8
C14 C15 C16 . . 120.9(10)
C14 C15 H15 . . 119.5
C16 C15 H15 . . 119.5
C15 C16 C23 . . 122.6(11)
C15 C16 C17 . . 117.7(10)
C23 C16 C17 . . 119.7(11)
N3 C17 C18 . . 118.8(8)
N3 C17 C16 . . 121.5(9)
C18 C17 C16 . . 119.6(9)
N4 C18 C17 . . 119.7(8)
N4 C18 C19 . . 121.1(10)
C17 C18 C19 . . 119.2(10)
C20 C19 C24 . . 122.9(11)
C20 C19 C18 . . 118.5(11)
C24 C19 C18 . . 118.6(11)
C21 C20 C19 . . 119.5(11)
C21 C20 H20 . . 120.2
C19 C20 H20 . . 120.2
C20 C21 C22 . . 119.2(11)
C20 C21 H21 . . 120.4
C22 C21 H21 . . 120.4
N4 C22 C21 . . 123.7(10)
N4 C22 H22 . . 118.1
C21 C22 H22 . . 118.1
C24 C23 C16 . . 120.5(11)
C24 C23 H23 . . 119.7
C16 C23 H23 . . 119.7
C23 C24 C19 . . 122.2(11)
C23 C24 H24 . . 118.9
C19 C24 H24 . . 118.9
O1 C25 C26 . . 126.6(18)
O1 C25 H25 . . 116.7
C26 C25 H25 . . 116.7
C31 C26 C27 . . 117.4(14)
C31 C26 C25 . . 117.2(16)
C27 C26 C25 . . 125.4(14)
C28 C27 C26 . . 121.6(13)
C28 C27 H27 . . 119.2
C26 C27 H27 . . 119.2
C27 C28 C29 . . 122.8(14)
C27 C28 H28 . . 118.6
C29 C28 H28 . . 118.6
N5 C29 C28 . . 123.8(12)
N5 C29 C30 . . 121.0(11)
C28 C29 C30 . . 115.2(13)
C31 C30 C29 . . 122.0(12)
C31 C30 H30 . . 119.0
C29 C30 H30 . . 119.0
C30 C31 C26 . . 120.9(13)
C30 C31 H31 . . 119.5
C26 C31 H31 . . 119.5
N5 C32 H32A . . 109.5
N5 C32 H32B . . 109.5
H32A C32 H32B . . 109.5
N5 C32 H32C . . 109.5
H32A C32 H32C . . 109.5
H32B C32 H32C . . 109.5
N5 C33 H33A . . 109.5
N5 C33 H33B . . 109.5
H33A C33 H33B . . 109.5
N5 C33 H33C . . 109.5
H33A C33 H33C . . 109.5
H33B C33 H33C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ca1 N3 6_464 2.593(7) ?
Ca1 N3 . 2.593(7) y
Ca1 N4 . 2.604(7) y
Ca1 N4 6_464 2.604(7) ?
Ca1 N2 6_464 2.631(7) ?
Ca1 N2 . 2.631(7) y
Ca1 N1 . 2.641(7) y
Ca1 N1 6_464 2.641(7) ?
Cl1 O4 . 1.36(2) ?
Cl1 O4 6_564 1.36(2) ?
Cl1 O2 . 1.377(13) ?
Cl1 O3 6_564 1.43(2) ?
Cl1 O3 . 1.43(2) ?
Cl1 O5 . 1.44(2) ?
Cl1 O5 6_564 1.44(2) ?
Cl2 O9 . 1.34(2) ?
Cl2 O9 6_454 1.34(2) ?
Cl2 O6 . 1.389(11) ?
Cl2 O7 6_454 1.43(2) ?
Cl2 O7 . 1.43(2) ?
Cl2 O8 6_454 1.466(19) ?
Cl2 O8 . 1.466(19) ?
N1 C1 . 1.325(11) ?
N1 C5 . 1.366(11) ?
N2 C10 . 1.331(11) ?
N2 C6 . 1.353(11) ?
N3 C13 . 1.338(11) ?
N3 C17 . 1.354(11) ?
N4 C22 . 1.326(11) ?
N4 C18 . 1.368(11) ?
N5 C29 . 1.356(16) ?
N5 C33 . 1.436(15) ?
N5 C32 . 1.445(15) ?
O1 C25 . 1.183(15) ?
O3 O4 6_564 1.14(3) ?
O3 O5 6_564 1.66(3) ?
O4 O3 6_564 1.14(3) ?
O4 O5 6_564 1.28(3) ?
O5 O4 6_564 1.28(3) ?
O5 O3 6_564 1.66(3) ?
O7 O9 6_454 1.02(2) ?
O7 O8 6_454 1.72(3) ?
O8 O9 6_454 1.31(3) ?
O8 O7 6_454 1.72(3) ?
O9 O7 6_454 1.02(2) ?
O9 O8 6_454 1.31(3) ?
C1 C2 . 1.382(13) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.365(15) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.385(14) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.410(12) ?
C4 C11 . 1.437(14) ?
C5 C6 . 1.438(13) ?
C6 C7 . 1.409(12) ?
C7 C8 . 1.407(14) ?
C7 C12 . 1.426(14) ?
C8 C9 . 1.348(14) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.385(13) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 C12 . 1.341(15) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C13 C14 . 1.393(13) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.349(15) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.382(14) ?
C15 H15 . 0.9300 ?
C16 C23 . 1.418(15) ?
C16 C17 . 1.422(13) ?
C17 C18 . 1.421(13) ?
C18 C19 . 1.432(13) ?
C19 C20 . 1.396(15) ?
C19 C24 . 1.425(15) ?
C20 C21 . 1.354(15) ?
C20 H20 . 0.9300 ?
C21 C22 . 1.405(14) ?
C21 H21 . 0.9300 ?
C22 H22 . 0.9300 ?
C23 C24 . 1.343(16) ?
C23 H23 . 0.9300 ?
C24 H24 . 0.9300 ?
C25 C26 . 1.46(2) ?
C25 H25 . 0.9300 ?
C26 C31 . 1.386(16) ?
C26 C27 . 1.41(2) ?
C27 C28 . 1.35(2) ?
C27 H27 . 0.9300 ?
C28 C29 . 1.403(16) ?
C28 H28 . 0.9300 ?
C29 C30 . 1.419(15) ?
C30 C31 . 1.380(16) ?
C30 H30 . 0.9300 ?
C31 H31 . 0.9300 ?
C32 H32A . 0.9600 ?
C32 H32B . 0.9600 ?
C32 H32C . 0.9600 ?
C33 H33A . 0.9600 ?
C33 H33B . 0.9600 ?
C33 H33C . 0.9600 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N3 Ca1 N1 C1 6_464 . 105.0(8)
N3 Ca1 N1 C1 . . -131.6(7)
N4 Ca1 N1 C1 . . -86.6(8)
N4 Ca1 N1 C1 6_464 . 40.8(7)
N2 Ca1 N1 C1 6_464 . 71.7(10)
N2 Ca1 N1 C1 . . -178.5(8)
N1 Ca1 N1 C1 6_464 . -23.2(7)
N3 Ca1 N1 C5 6_464 . -82.6(6)
N3 Ca1 N1 C5 . . 40.8(7)
N4 Ca1 N1 C5 . . 85.8(6)
N4 Ca1 N1 C5 6_464 . -146.8(7)
N2 Ca1 N1 C5 6_464 . -115.9(8)
N2 Ca1 N1 C5 . . -6.1(6)
N1 Ca1 N1 C5 6_464 . 149.2(7)
N3 Ca1 N2 C10 6_464 . -84.1(7)
N3 Ca1 N2 C10 . . 41.8(7)
N4 Ca1 N2 C10 . . 106.2(7)
N4 Ca1 N2 C10 6_464 . -129.3(7)
N2 Ca1 N2 C10 6_464 . -21.3(6)
N1 Ca1 N2 C10 . . -176.7(8)
N1 Ca1 N2 C10 6_464 . 76.3(10)
N3 Ca1 N2 C6 6_464 . 97.0(6)
N3 Ca1 N2 C6 . . -137.0(6)
N4 Ca1 N2 C6 . . -72.7(6)
N4 Ca1 N2 C6 6_464 . 51.9(7)
N2 Ca1 N2 C6 6_464 . 159.9(7)
N1 Ca1 N2 C6 . . 4.5(6)
N1 Ca1 N2 C6 6_464 . -102.6(8)
N3 Ca1 N3 C13 6_464 . -17.2(6)
N4 Ca1 N3 C13 . . -173.8(8)
N4 Ca1 N3 C13 6_464 . 77.0(10)
N2 Ca1 N3 C13 6_464 . 47.2(7)
N2 Ca1 N3 C13 . . -81.9(7)
N1 Ca1 N3 C13 . . -124.0(7)
N1 Ca1 N3 C13 6_464 . 110.4(7)
N3 Ca1 N3 C17 6_464 . 161.9(7)
N4 Ca1 N3 C17 . . 5.2(6)
N4 Ca1 N3 C17 6_464 . -103.9(9)
N2 Ca1 N3 C17 6_464 . -133.7(6)
N2 Ca1 N3 C17 . . 97.2(6)
N1 Ca1 N3 C17 . . 55.0(7)
N1 Ca1 N3 C17 6_464 . -70.6(6)
N3 Ca1 N4 C22 6_464 . 77.3(10)
N3 Ca1 N4 C22 . . -177.5(8)
N4 Ca1 N4 C22 6_464 . -20.6(7)
N2 Ca1 N4 C22 6_464 . -127.4(7)
N2 Ca1 N4 C22 . . 106.3(7)
N1 Ca1 N4 C22 . . 43.0(7)
N1 Ca1 N4 C22 6_464 . -84.8(7)
N3 Ca1 N4 C18 6_464 . -114.1(8)
N3 Ca1 N4 C18 . . -8.9(6)
N4 Ca1 N4 C18 6_464 . 148.0(7)
N2 Ca1 N4 C18 6_464 . 41.1(7)
N2 Ca1 N4 C18 . . -85.1(6)
N1 Ca1 N4 C18 . . -148.4(6)
N1 Ca1 N4 C18 6_464 . 83.8(6)
O4 Cl1 O3 O4 . 6_564 -109(3)
O2 Cl1 O3 O4 . 6_564 117.0(16)
O3 Cl1 O3 O4 6_564 6_564 -63.0(16)
O5 Cl1 O3 O4 . 6_564 9(2)
O5 Cl1 O3 O4 6_564 6_564 -144(2)
O4 Cl1 O3 O5 . 6_564 35.6(13)
O4 Cl1 O3 O5 6_564 6_564 144(2)
O2 Cl1 O3 O5 . 6_564 -98.6(10)
O3 Cl1 O3 O5 6_564 6_564 81.4(10)
O5 Cl1 O3 O5 . 6_564 153.7(17)
O4 Cl1 O4 O3 6_564 6_564 95.4(19)
O2 Cl1 O4 O3 . 6_564 -84.6(19)
O3 Cl1 O4 O3 . 6_564 148.7(19)
O5 Cl1 O4 O3 . 6_564 36(2)
O5 Cl1 O4 O3 6_564 6_564 -169(2)
O4 Cl1 O4 O5 6_564 6_564 -95.7(16)
O2 Cl1 O4 O5 . 6_564 84.3(16)
O3 Cl1 O4 O5 6_564 6_564 169(2)
O3 Cl1 O4 O5 . 6_564 -42.4(17)
O5 Cl1 O4 O5 . 6_564 -155.4(17)
O4 Cl1 O5 O4 . 6_564 111(2)
O2 Cl1 O5 O4 . 6_564 -118.6(13)
O3 Cl1 O5 O4 6_564 6_564 138.5(18)
O3 Cl1 O5 O4 . 6_564 -8.4(18)
O5 Cl1 O5 O4 6_564 6_564 61.4(13)
O4 Cl1 O5 O3 . 6_564 -27.5(14)
O4 Cl1 O5 O3 6_564 6_564 -138.5(18)
O2 Cl1 O5 O3 . 6_564 102.9(10)
O3 Cl1 O5 O3 . 6_564 -146.9(19)
O5 Cl1 O5 O3 6_564 6_564 -77.1(10)
O9 Cl2 O7 O9 . 6_454 109(3)
O6 Cl2 O7 O9 . 6_454 -114.1(17)
O7 Cl2 O7 O9 6_454 6_454 65.9(17)
O8 Cl2 O7 O9 6_454 6_454 147(2)
O8 Cl2 O7 O9 . 6_454 -7(2)
O9 Cl2 O7 O8 . 6_454 -37.8(11)
O9 Cl2 O7 O8 6_454 6_454 -147(2)
O6 Cl2 O7 O8 . 6_454 99.1(8)
O7 Cl2 O7 O8 6_454 6_454 -80.9(8)
O8 Cl2 O7 O8 . 6_454 -153.3(14)
O9 Cl2 O8 O9 . 6_454 -114(2)
O6 Cl2 O8 O9 . 6_454 117.0(11)
O7 Cl2 O8 O9 6_454 6_454 -137.3(14)
O7 Cl2 O8 O9 . 6_454 5.4(16)
O8 Cl2 O8 O9 6_454 6_454 -63.0(11)
O9 Cl2 O8 O7 . 6_454 23.3(13)
O9 Cl2 O8 O7 6_454 6_454 137.3(14)
O6 Cl2 O8 O7 . 6_454 -105.7(9)
O7 Cl2 O8 O7 . 6_454 142.7(17)
O8 Cl2 O8 O7 6_454 6_454 74.3(9)
O9 Cl2 O9 O7 6_454 6_454 -94.2(19)
O6 Cl2 O9 O7 . 6_454 85.8(19)
O7 Cl2 O9 O7 . 6_454 -142.5(19)
O8 Cl2 O9 O7 6_454 6_454 172(2)
O8 Cl2 O9 O7 . 6_454 -34(2)
O9 Cl2 O9 O8 6_454 6_454 93.7(12)
O6 Cl2 O9 O8 . 6_454 -86.3(12)
O7 Cl2 O9 O8 6_454 6_454 -172(2)
O7 Cl2 O9 O8 . 6_454 45.4(14)
O8 Cl2 O9 O8 . 6_454 154.1(13)
C5 N1 C1 C2 . . -0.9(15)
Ca1 N1 C1 C2 . . 171.6(8)
N1 C1 C2 C3 . . 1.7(17)
C1 C2 C3 C4 . . -1.4(16)
C2 C3 C4 C5 . . 0.4(15)
C2 C3 C4 C11 . . -179.9(10)
C1 N1 C5 C4 . . -0.2(13)
Ca1 N1 C5 C4 . . -173.1(6)
C1 N1 C5 C6 . . -179.7(8)
Ca1 N1 C5 C6 . . 7.4(10)
C3 C4 C5 N1 . . 0.4(14)
C11 C4 C5 N1 . . -179.3(9)
C3 C4 C5 C6 . . 179.9(9)
C11 C4 C5 C6 . . 0.2(13)
C10 N2 C6 C7 . . -2.7(12)
Ca1 N2 C6 C7 . . 176.2(6)
C10 N2 C6 C5 . . 178.3(8)
Ca1 N2 C6 C5 . . -2.8(10)
N1 C5 C6 N2 . . -3.1(12)
C4 C5 C6 N2 . . 177.4(8)
N1 C5 C6 C7 . . 177.8(8)
C4 C5 C6 C7 . . -1.7(12)
N2 C6 C7 C8 . . 2.0(13)
C5 C6 C7 C8 . . -179.0(8)
N2 C6 C7 C12 . . -177.0(8)
C5 C6 C7 C12 . . 2.0(13)
C6 C7 C8 C9 . . 0.1(14)
C12 C7 C8 C9 . . 179.2(10)
C7 C8 C9 C10 . . -1.4(15)
C6 N2 C10 C9 . . 1.4(14)
Ca1 N2 C10 C9 . . -177.5(7)
C8 C9 C10 N2 . . 0.7(16)
C3 C4 C11 C12 . . -178.6(11)
C5 C4 C11 C12 . . 1.1(16)
C4 C11 C12 C7 . . -0.8(17)
C8 C7 C12 C11 . . -179.8(10)
C6 C7 C12 C11 . . -0.8(15)
C17 N3 C13 C14 . . -1.0(14)
Ca1 N3 C13 C14 . . 178.0(7)
N3 C13 C14 C15 . . 5.0(15)
C13 C14 C15 C16 . . -3.9(16)
C14 C15 C16 C23 . . 178.6(10)
C14 C15 C16 C17 . . -0.9(15)
C13 N3 C17 C18 . . 177.8(8)
Ca1 N3 C17 C18 . . -1.3(10)
C13 N3 C17 C16 . . -4.0(13)
Ca1 N3 C17 C16 . . 176.9(6)
C15 C16 C17 N3 . . 5.0(14)
C23 C16 C17 N3 . . -174.5(9)
C15 C16 C17 C18 . . -176.8(9)
C23 C16 C17 C18 . . 3.7(14)
C22 N4 C18 C17 . . -178.3(8)
Ca1 N4 C18 C17 . . 12.4(10)
C22 N4 C18 C19 . . -1.0(13)
Ca1 N4 C18 C19 . . -170.3(7)
N3 C17 C18 N4 . . -7.5(13)
C16 C17 C18 N4 . . 174.2(8)
N3 C17 C18 C19 . . 175.0(8)
C16 C17 C18 C19 . . -3.2(13)
N4 C18 C19 C20 . . 2.4(14)
C17 C18 C19 C20 . . 179.8(9)
N4 C18 C19 C24 . . -177.7(9)
C17 C18 C19 C24 . . -0.3(14)
C24 C19 C20 C21 . . 177.7(11)
C18 C19 C20 C21 . . -2.4(17)
C19 C20 C21 C22 . . 1.0(18)
C18 N4 C22 C21 . . -0.5(14)
Ca1 N4 C22 C21 . . 168.0(8)
C20 C21 C22 N4 . . 0.5(17)
C15 C16 C23 C24 . . 179.9(11)
C17 C16 C23 C24 . . -0.7(16)
C16 C23 C24 C19 . . -3.0(18)
C20 C19 C24 C23 . . -176.6(12)
C18 C19 C24 C23 . . 3.5(17)
O1 C25 C26 C31 . . -178.4(13)
O1 C25 C26 C27 . . 2(2)
C31 C26 C27 C28 . . 1.0(19)
C25 C26 C27 C28 . . -179.1(13)
C26 C27 C28 C29 . . -1(2)
C33 N5 C29 C28 . . 174.2(11)
C32 N5 C29 C28 . . -2.5(18)
C33 N5 C29 C30 . . -5.5(17)
C32 N5 C29 C30 . . 177.7(11)
C27 C28 C29 N5 . . -178.7(12)
C27 C28 C29 C30 . . 1.1(18)
N5 C29 C30 C31 . . 178.2(11)
C28 C29 C30 C31 . . -1.6(16)
C29 C30 C31 C26 . . 1.8(18)
C27 C26 C31 C30 . . -1.4(17)
C25 C26 C31 C30 . . 178.7(11)
