#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/64/4336416.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_4336416
loop_
_publ_author_name
'Wei Yi'
'Haiyan Ma'
_publ_contact_author_address
;
        Laboratory of Organometallic Chemistry
        East China University of Science and Technology
        130 Meilong Road, P.O.Box 310#
        200237,Shanghai
        P. R. China
;
_publ_contact_author_email       haiyanma@ecust.edu.cn
_publ_contact_author_fax         '0086 21 64253519'
_publ_contact_author_name        'Haiyan Ma'
_publ_contact_author_phone       '0086 21 64253519'
_publ_section_title
;
 Magnesium and Calcium Complexes Containing Biphenyl-Based Tridentate
 Iminophenolate Ligands for Ring-Opening Polymerization of rac-Lactide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11821
_journal_page_last               11835
_journal_paper_doi               10.1021/ic4012668
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C60.5 H65 Ca N2 O4'
_chemical_formula_weight         924.23
_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                112.018(5)
_cell_angle_beta                 96.288(6)
_cell_angle_gamma                107.016(5)
_cell_formula_units_Z            2
_cell_length_a                   13.118(4)
_cell_length_b                   13.922(5)
_cell_length_c                   17.106(5)
_cell_measurement_reflns_used    647
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.533
_cell_measurement_theta_min      2.460
_cell_volume                     2683.4(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0775
_diffrn_reflns_av_sigmaI/netI    0.1794
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11270
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        3.90
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.9743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         9311
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.2089
_refine_ls_R_factor_gt           0.0918
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1457P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2405
_refine_ls_wR_factor_ref         0.2983
_reflns_number_gt                3049
_reflns_number_total             9311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4012668_si_002_1.cif
_cod_data_source_block           a10322c
_cod_original_cell_volume        2683.5(15)
_cod_original_formula_sum        'C60.50 H65 Ca N2 O4'
_cod_database_code               4336416
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ca1 Ca 0.05488(11) 0.90168(11) 0.21915(9) 0.0564(4) Uani 1 1 d .
N1 N -0.0814(4) 0.7317(4) 0.2131(3) 0.0579(14) Uani 1 1 d .
N2 N -0.0102(4) 1.0581(4) 0.2401(3) 0.0556(13) Uani 1 1 d .
O1 O 0.1518(3) 0.8132(3) 0.2561(3) 0.0620(12) Uani 1 1 d .
O2 O -0.0536(4) 0.8110(4) 0.0710(3) 0.0708(13) Uani 1 1 d .
O3 O 0.1716(3) 1.0118(3) 0.1798(3) 0.0659(12) Uani 1 1 d .
O4 O 0.0681(4) 1.0072(4) 0.3805(3) 0.0736(14) Uani 1 1 d .
C1 C 0.1445(5) 0.7446(5) 0.2904(4) 0.0566(17) Uani 1 1 d .
C2 C 0.2432(5) 0.7410(5) 0.3353(4) 0.0549(16) Uani 1 1 d .
C3 C 0.2302(6) 0.6679(6) 0.3741(4) 0.0656(19) Uani 1 1 d .
H3 H 0.2935 0.6661 0.4029 0.079 Uiso 1 1 calc R
C4 C 0.1299(6) 0.5977(6) 0.3728(5) 0.069(2) Uani 1 1 d .
C5 C 0.0361(6) 0.5977(5) 0.3265(4) 0.0621(18) Uani 1 1 d .
H5 H -0.0322 0.5470 0.3202 0.075 Uiso 1 1 calc R
C6 C 0.0426(5) 0.6724(5) 0.2894(4) 0.0547(16) Uani 1 1 d .
C7 C -0.0621(5) 0.6681(5) 0.2473(4) 0.0590(18) Uani 1 1 d .
H7 H -0.1239 0.6119 0.2445 0.071 Uiso 1 1 calc R
C8 C 0.1229(7) 0.5216(7) 0.4181(6) 0.104(3) Uani 1 1 d .
H8A H 0.1619 0.4731 0.3946 0.156 Uiso 1 1 calc R
H8B H 0.0472 0.4781 0.4090 0.156 Uiso 1 1 calc R
H8C H 0.1553 0.5655 0.4793 0.156 Uiso 1 1 calc R
C9 C 0.3559(5) 0.8144(5) 0.3375(5) 0.0653(19) Uani 1 1 d .
C10 C 0.3729(7) 0.9383(6) 0.3863(6) 0.102(3) Uani 1 1 d .
H10A H 0.3225 0.9563 0.3541 0.153 Uiso 1 1 calc R
H10B H 0.4470 0.9832 0.3922 0.153 Uiso 1 1 calc R
H10C H 0.3596 0.9527 0.4429 0.153 Uiso 1 1 calc R
C11 C 0.3695(6) 0.7890(6) 0.2442(5) 0.082(2) Uani 1 1 d .
H11A H 0.3671 0.7140 0.2162 0.123 Uiso 1 1 calc R
H11B H 0.4389 0.8395 0.2464 0.123 Uiso 1 1 calc R
H11C H 0.3110 0.7977 0.2118 0.123 Uiso 1 1 calc R
C12 C 0.4494(6) 0.7970(7) 0.3869(6) 0.095(3) Uani 1 1 d .
H12A H 0.4464 0.8188 0.4466 0.142 Uiso 1 1 calc R
H12B H 0.5190 0.8413 0.3839 0.142 Uiso 1 1 calc R
H12C H 0.4409 0.7200 0.3608 0.142 Uiso 1 1 calc R
C13 C -0.1953(5) 0.7048(5) 0.1761(5) 0.0632(18) Uani 1 1 d .
C14 C -0.2634(6) 0.7306(7) 0.2313(6) 0.087(2) Uani 1 1 d .
H14 H -0.2363 0.7621 0.2914 0.104 Uiso 1 1 calc R
C15 C -0.3735(6) 0.7083(7) 0.1950(7) 0.090(3) Uani 1 1 d .
H15 H -0.4201 0.7248 0.2311 0.108 Uiso 1 1 calc R
C16 C -0.4114(7) 0.6635(8) 0.1088(7) 0.106(3) Uani 1 1 d .
H16 H -0.4839 0.6515 0.0856 0.128 Uiso 1 1 calc R
C17 C -0.3460(6) 0.6347(6) 0.0536(6) 0.089(2) Uani 1 1 d .
H17 H -0.3754 0.6005 -0.0062 0.107 Uiso 1 1 calc R
C18 C -0.2359(5) 0.6564(5) 0.0869(5) 0.0636(19) Uani 1 1 d .
C19 C -0.1655(6) 0.6225(6) 0.0274(4) 0.0652(19) Uani 1 1 d .
C20 C -0.1872(6) 0.5099(6) -0.0253(5) 0.083(2) Uani 1 1 d .
H20 H -0.2465 0.4559 -0.0225 0.099 Uiso 1 1 calc R
C21 C -0.1233(8) 0.4775(8) -0.0808(5) 0.095(3) Uani 1 1 d .
H21 H -0.1389 0.4025 -0.1147 0.114 Uiso 1 1 calc R
C22 C -0.0347(8) 0.5579(8) -0.0860(6) 0.100(3) Uani 1 1 d .
H22 H 0.0099 0.5366 -0.1226 0.120 Uiso 1 1 calc R
C23 C -0.0135(7) 0.6680(7) -0.0371(5) 0.085(2) Uani 1 1 d .
H23 H 0.0441 0.7217 -0.0419 0.102 Uiso 1 1 calc R
C24 C -0.0777(6) 0.7003(6) 0.0198(5) 0.0667(19) Uani 1 1 d .
C25 C -0.0650(7) 0.8740(7) 0.0239(5) 0.101(3) Uani 1 1 d .
H25A H -0.0220 0.8636 -0.0185 0.151 Uiso 1 1 calc R
H25B H -0.0396 0.9513 0.0633 0.151 Uiso 1 1 calc R
H25C H -0.1409 0.8496 -0.0051 0.151 Uiso 1 1 calc R
C26 C 0.3519(7) 1.0696(6) 0.1037(6) 0.085(3) Uani 1 1 d .
C27 C 0.4089(8) 1.0420(8) 0.1727(7) 0.130(4) Uani 1 1 d .
H27A H 0.4712 1.1063 0.2121 0.195 Uiso 1 1 calc R
H27B H 0.4330 0.9818 0.1441 0.195 Uiso 1 1 calc R
H27C H 0.3577 1.0207 0.2046 0.195 Uiso 1 1 calc R
C28 C 0.2745(8) 0.9648(6) 0.0291(6) 0.113(3) Uani 1 1 d .
H28A H 0.2150 0.9295 0.0487 0.170 Uiso 1 1 calc R
H28B H 0.3131 0.9155 0.0067 0.170 Uiso 1 1 calc R
H28C H 0.2460 0.9821 -0.0160 0.170 Uiso 1 1 calc R
C29 C 0.4437(8) 1.1245(7) 0.0675(7) 0.145(5) Uani 1 1 d .
H29A H 0.4115 1.1378 0.0213 0.217 Uiso 1 1 calc R
H29B H 0.4832 1.0760 0.0457 0.217 Uiso 1 1 calc R
H29C H 0.4935 1.1938 0.1132 0.217 Uiso 1 1 calc R
C30 C 0.2938(5) 1.1478(5) 0.1467(4) 0.0577(17) Uani 1 1 d .
C31 C 0.3265(6) 1.2542(6) 0.1569(4) 0.067(2) Uani 1 1 d .
H31 H 0.3891 1.2798 0.1387 0.080 Uiso 1 1 calc R
C32 C 0.2738(6) 1.3300(6) 0.1927(4) 0.0660(19) Uani 1 1 d .
C33 C 0.1833(5) 1.2908(5) 0.2190(4) 0.0588(17) Uani 1 1 d .
H33 H 0.1460 1.3378 0.2427 0.071 Uiso 1 1 calc R
C34 C 0.1430(5) 1.1807(5) 0.2117(4) 0.0510(16) Uani 1 1 d .
C35 C 0.2017(5) 1.1102(5) 0.1794(4) 0.0538(16) Uani 1 1 d .
C36 C 0.3207(6) 1.4482(5) 0.2044(5) 0.083(2) Uani 1 1 d .
H36A H 0.2743 1.4872 0.2291 0.125 Uiso 1 1 calc R
H36B H 0.3247 1.4490 0.1490 0.125 Uiso 1 1 calc R
H36C H 0.3932 1.4839 0.2427 0.125 Uiso 1 1 calc R
C37 C 0.0460(5) 1.1510(5) 0.2410(4) 0.0562(17) Uani 1 1 d .
H37 H 0.0192 1.2079 0.2644 0.067 Uiso 1 1 calc R
C38 C -0.1016(6) 1.0570(6) 0.2798(5) 0.0638(19) Uani 1 1 d .
C39 C -0.2077(7) 0.9978(7) 0.2252(6) 0.090(2) Uani 1 1 d .
H39 H -0.2164 0.9572 0.1660 0.108 Uiso 1 1 calc R
C40 C -0.2987(8) 0.9981(9) 0.2566(9) 0.119(4) Uani 1 1 d .
H40 H -0.3691 0.9608 0.2199 0.142 Uiso 1 1 calc R
C41 C -0.2812(9) 1.0574(10) 0.3472(11) 0.130(5) Uani 1 1 d .
H41 H -0.3419 1.0589 0.3706 0.156 Uiso 1 1 calc R
C42 C -0.1797(9) 1.1119(8) 0.4011(6) 0.096(3) Uani 1 1 d .
H42 H -0.1721 1.1492 0.4606 0.116 Uiso 1 1 calc R
C43 C -0.0847(6) 1.1137(6) 0.3694(5) 0.068(2) Uani 1 1 d .
C44 C 0.0248(7) 1.1732(6) 0.4260(5) 0.0665(19) Uani 1 1 d .
C45 C 0.0607(10) 1.2848(8) 0.4804(6) 0.096(3) Uani 1 1 d .
H45 H 0.0135 1.3228 0.4786 0.115 Uiso 1 1 calc R
C46 C 0.1616(11) 1.3421(8) 0.5366(7) 0.120(4) Uani 1 1 d .
H46 H 0.1811 1.4165 0.5745 0.145 Uiso 1 1 calc R
C47 C 0.2346(9) 1.2886(10) 0.5370(6) 0.115(3) Uani 1 1 d .
H47 H 0.3055 1.3289 0.5727 0.138 Uiso 1 1 calc R
C48 C 0.2053(8) 1.1780(8) 0.4861(6) 0.098(3) Uani 1 1 d .
H48 H 0.2548 1.1423 0.4880 0.118 Uiso 1 1 calc R
C49 C 0.1020(7) 1.1203(6) 0.4323(5) 0.070(2) Uani 1 1 d .
C50 C 0.0792(9) 0.9439(7) 0.4287(5) 0.114(3) Uani 1 1 d .
H50A H 0.1426 0.9236 0.4211 0.171 Uiso 1 1 calc R
H50B H 0.0146 0.8779 0.4078 0.171 Uiso 1 1 calc R
H50C H 0.0877 0.9879 0.4894 0.171 Uiso 1 1 calc R
C51 C 0.4494(11) 0.5533(11) 0.4810(8) 0.181(5) Uiso 1 1 d D
H51A H 0.4073 0.5884 0.4636 0.217 Uiso 1 1 calc R
C52 C 0.4156(12) 0.4437(11) 0.4290(9) 0.183(5) Uiso 1 1 d D
H52A H 0.3564 0.4133 0.3809 0.220 Uiso 1 1 calc R
C53 C 0.4643(13) 0.3736(12) 0.4433(10) 0.213(6) Uiso 1 1 d D
C54 C 0.445(2) 0.2578(14) 0.3900(17) 0.277(18) Uiso 0.50 1 d PD
H54A H 0.3808 0.2274 0.3430 0.416 Uiso 0.50 1 calc PR
H54B H 0.4334 0.2171 0.4249 0.416 Uiso 0.50 1 calc PR
H54C H 0.5074 0.2522 0.3669 0.416 Uiso 0.50 1 calc PR
C55 C 0.3376(8) 0.6096(8) 0.7136(6) 0.173(5) Uiso 1 1 d GD
H55A H 0.3624 0.5978 0.6631 0.208 Uiso 1 1 calc R
C56 C 0.3720(7) 0.5703(7) 0.7706(7) 0.195(6) Uiso 1 1 d GD
H56A H 0.4200 0.5321 0.7586 0.234 Uiso 1 1 calc R
C57 C 0.3352(8) 0.5879(8) 0.8455(7) 0.224(7) Uiso 1 1 d GD
H57A H 0.3584 0.5614 0.8839 0.268 Uiso 1 1 calc R
C58 C 0.2640(8) 0.6446(8) 0.8633(6) 0.209(6) Uiso 1 1 d GD
H58A H 0.2393 0.6564 0.9137 0.251 Uiso 1 1 calc R
C59 C 0.2297(7) 0.6838(7) 0.8062(7) 0.190(5) Uiso 1 1 d GD
H59A H 0.1817 0.7221 0.8182 0.228 Uiso 1 1 calc R
C60 C 0.2664(8) 0.6663(7) 0.7314(6) 0.247(8) Uiso 1 1 d GD
C61 C 0.217(2) 0.705(2) 0.6734(14) 0.51(2) Uiso 1 1 d D
H61A H 0.1698 0.7419 0.7007 0.769 Uiso 1 1 calc R
H61B H 0.1740 0.6431 0.6194 0.769 Uiso 1 1 calc R
H61C H 0.2737 0.7566 0.6625 0.769 Uiso 1 1 calc R
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'
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
O3 Ca1 O1 102.85(16) . .
O3 Ca1 O2 87.24(16) . .
O1 Ca1 O2 115.90(17) . .
O3 Ca1 N1 160.37(18) . .
O1 Ca1 N1 74.41(17) . .
O2 Ca1 N1 77.01(17) . .
O3 Ca1 N2 74.86(17) . .
O1 Ca1 N2 155.99(17) . .
O2 Ca1 N2 88.02(17) . .
N1 Ca1 N2 115.61(18) . .
O3 Ca1 O4 108.20(16) . .
O1 Ca1 O4 87.94(16) . .
O2 Ca1 O4 148.50(17) . .
N1 Ca1 O4 91.23(17) . .
N2 Ca1 O4 70.69(16) . .
C7 N1 C13 115.2(5) . .
C7 N1 Ca1 126.3(4) . .
C13 N1 Ca1 118.2(4) . .
C37 N2 C38 116.2(5) . .
C37 N2 Ca1 125.2(4) . .
C38 N2 Ca1 115.7(4) . .
C1 O1 Ca1 140.1(4) . .
C24 O2 C25 114.3(5) . .
C24 O2 Ca1 122.0(4) . .
C25 O2 Ca1 120.6(4) . .
C35 O3 Ca1 143.3(4) . .
C49 O4 C50 113.5(6) . .
C49 O4 Ca1 130.5(4) . .
C50 O4 Ca1 112.2(4) . .
O1 C1 C6 122.6(6) . .
O1 C1 C2 120.4(6) . .
C6 C1 C2 116.9(6) . .
C3 C2 C1 117.9(6) . .
C3 C2 C9 122.1(6) . .
C1 C2 C9 120.0(6) . .
C4 C3 C2 124.7(7) . .
C4 C3 H3 117.7 . .
C2 C3 H3 117.7 . .
C3 C4 C5 117.2(6) . .
C3 C4 C8 121.3(7) . .
C5 C4 C8 121.4(7) . .
C4 C5 C6 121.1(6) . .
C4 C5 H5 119.4 . .
C6 C5 H5 119.4 . .
C5 C6 C1 121.9(6) . .
C5 C6 C7 115.6(6) . .
C1 C6 C7 122.4(6) . .
N1 C7 C6 129.1(6) . .
N1 C7 H7 115.5 . .
C6 C7 H7 115.5 . .
C4 C8 H8A 109.5 . .
C4 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C4 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C2 C9 C10 110.8(6) . .
C2 C9 C12 111.8(6) . .
C10 C9 C12 105.8(6) . .
C2 C9 C11 110.4(6) . .
C10 C9 C11 109.8(6) . .
C12 C9 C11 108.1(6) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C9 C11 H11A 109.5 . .
C9 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C9 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C9 C12 H12A 109.5 . .
C9 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C9 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C18 C13 C14 120.6(7) . .
C18 C13 N1 120.2(6) . .
C14 C13 N1 119.1(7) . .
C13 C14 C15 119.0(8) . .
C13 C14 H14 120.5 . .
C15 C14 H14 120.5 . .
C16 C15 C14 120.0(8) . .
C16 C15 H15 120.0 . .
C14 C15 H15 120.0 . .
C15 C16 C17 121.6(8) . .
C15 C16 H16 119.2 . .
C17 C16 H16 119.2 . .
C16 C17 C18 120.3(8) . .
C16 C17 H17 119.9 . .
C18 C17 H17 119.9 . .
C13 C18 C17 118.5(7) . .
C13 C18 C19 120.9(6) . .
C17 C18 C19 120.5(7) . .
C24 C19 C20 117.2(7) . .
C24 C19 C18 121.6(6) . .
C20 C19 C18 121.1(7) . .
C21 C20 C19 121.7(8) . .
C21 C20 H20 119.1 . .
C19 C20 H20 119.1 . .
C20 C21 C22 119.6(8) . .
C20 C21 H21 120.2 . .
C22 C21 H21 120.2 . .
C23 C22 C21 119.8(8) . .
C23 C22 H22 120.1 . .
C21 C22 H22 120.1 . .
C22 C23 C24 120.3(8) . .
C22 C23 H23 119.9 . .
C24 C23 H23 119.9 . .
O2 C24 C19 118.7(7) . .
O2 C24 C23 120.0(6) . .
C19 C24 C23 121.3(7) . .
O2 C25 H25A 109.5 . .
O2 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
O2 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C28 C26 C30 112.1(7) . .
C28 C26 C29 107.1(7) . .
C30 C26 C29 111.5(6) . .
C28 C26 C27 110.1(7) . .
C30 C26 C27 109.3(7) . .
C29 C26 C27 106.6(8) . .
C26 C27 H27A 109.5 . .
C26 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C26 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C26 C28 H28A 109.5 . .
C26 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C26 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C26 C29 H29A 109.5 . .
C26 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C26 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C31 C30 C35 117.3(6) . .
C31 C30 C26 122.6(6) . .
C35 C30 C26 120.1(6) . .
C30 C31 C32 125.7(6) . .
C30 C31 H31 117.2 . .
C32 C31 H31 117.2 . .
C33 C32 C31 115.9(6) . .
C33 C32 C36 123.1(7) . .
C31 C32 C36 120.9(6) . .
C32 C33 C34 122.6(6) . .
C32 C33 H33 118.7 . .
C34 C33 H33 118.7 . .
C35 C34 C33 119.2(6) . .
C35 C34 C37 124.7(5) . .
C33 C34 C37 116.1(6) . .
O3 C35 C34 120.0(5) . .
O3 C35 C30 121.0(6) . .
C34 C35 C30 119.0(6) . .
C32 C36 H36A 109.5 . .
C32 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
C32 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
N2 C37 C34 130.0(6) . .
N2 C37 H37 115.0 . .
C34 C37 H37 115.0 . .
C43 C38 C39 121.1(7) . .
C43 C38 N2 121.1(6) . .
C39 C38 N2 117.8(7) . .
C40 C39 C38 121.6(9) . .
C40 C39 H39 119.2 . .
C38 C39 H39 119.2 . .
C39 C40 C41 117.0(10) . .
C39 C40 H40 121.5 . .
C41 C40 H40 121.5 . .
C42 C41 C40 122.2(10) . .
C42 C41 H41 118.9 . .
C40 C41 H41 118.9 . .
C41 C42 C43 121.4(9) . .
C41 C42 H42 119.3 . .
C43 C42 H42 119.3 . .
C38 C43 C42 116.5(8) . .
C38 C43 C44 121.2(6) . .
C42 C43 C44 122.2(8) . .
C45 C44 C49 115.2(8) . .
C45 C44 C43 121.9(8) . .
C49 C44 C43 122.9(7) . .
C46 C45 C44 123.3(10) . .
C46 C45 H45 118.4 . .
C44 C45 H45 118.4 . .
C45 C46 C47 119.2(10) . .
C45 C46 H46 120.4 . .
C47 C46 H46 120.4 . .
C48 C47 C46 121.3(10) . .
C48 C47 H47 119.3 . .
C46 C47 H47 119.3 . .
C47 C48 C49 118.9(10) . .
C47 C48 H48 120.6 . .
C49 C48 H48 120.6 . .
C48 C49 O4 120.8(8) . .
C48 C49 C44 122.0(8) . .
O4 C49 C44 117.2(7) . .
O4 C50 H50A 109.5 . .
O4 C50 H50B 109.5 . .
H50A C50 H50B 109.5 . .
O4 C50 H50C 109.5 . .
H50A C50 H50C 109.5 . .
H50B C50 H50C 109.5 . .
C52 C51 C53 133.5(14) . 2_666
C52 C51 H51A 113.2 . .
C53 C51 H51A 113.2 2_666 .
C51 C52 C53 123.6(14) . .
C51 C52 H52A 118.2 . .
C53 C52 H52A 118.2 . .
C52 C53 C51 102.9(13) . 2_666
C52 C53 C54 130.2(15) . .
C51 C53 C54 126.4(14) 2_666 .
C53 C54 H54A 109.5 . .
C53 C54 H54B 109.5 . .
H54A C54 H54B 109.5 . .
C53 C54 H54C 109.5 . .
H54A C54 H54C 109.5 . .
H54B C54 H54C 109.5 . .
C60 C55 C56 120.0 . .
C60 C55 H55A 120.0 . .
C56 C55 H55A 120.0 . .
C57 C56 C55 120.0 . .
C57 C56 H56A 120.0 . .
C55 C56 H56A 120.0 . .
C58 C57 C56 120.0 . .
C58 C57 H57A 120.0 . .
C56 C57 H57A 120.0 . .
C59 C58 C57 120.0 . .
C59 C58 H58A 120.0 . .
C57 C58 H58A 120.0 . .
C60 C59 C58 120.0 . .
C60 C59 H59A 120.0 . .
C58 C59 H59A 120.0 . .
C59 C60 C55 120.0 . .
C59 C60 C61 114.1(10) . .
C55 C60 C61 125.8(10) . .
C60 C61 H61A 109.5 . .
C60 C61 H61B 109.5 . .
H61A C61 H61B 109.5 . .
C60 C61 H61C 109.5 . .
H61A C61 H61C 109.5 . .
H61B C61 H61C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O3 2.184(4) .
Ca1 O1 2.203(5) .
Ca1 O2 2.408(5) .
Ca1 N1 2.471(5) .
Ca1 N2 2.483(5) .
Ca1 O4 2.552(5) .
N1 C7 1.294(7) .
N1 C13 1.436(8) .
N2 C37 1.282(7) .
N2 C38 1.440(8) .
O1 C1 1.284(7) .
O2 C24 1.373(7) .
O2 C25 1.422(8) .
O3 C35 1.313(7) .
O4 C49 1.385(8) .
O4 C50 1.439(8) .
C1 C6 1.412(8) .
C1 C2 1.455(8) .
C2 C3 1.391(8) .
C2 C9 1.519(9) .
C3 C4 1.383(9) .
C3 H3 0.9300 .
C4 C5 1.388(9) .
C4 C8 1.519(9) .
C5 C6 1.396(8) .
C5 H5 0.9300 .
C6 C7 1.454(9) .
C7 H7 0.9300 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 C10 1.542(9) .
C9 C12 1.542(9) .
C9 C11 1.542(10) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 C18 1.382(9) .
C13 C14 1.391(9) .
C14 C15 1.402(10) .
C14 H14 0.9300 .
C15 C16 1.334(11) .
C15 H15 0.9300 .
C16 C17 1.372(11) .
C16 H16 0.9300 .
C17 C18 1.392(9) .
C17 H17 0.9300 .
C18 C19 1.488(9) .
C19 C24 1.387(9) .
C19 C20 1.405(9) .
C20 C21 1.372(11) .
C20 H20 0.9300 .
C21 C22 1.396(11) .
C21 H21 0.9300 .
C22 C23 1.366(10) .
C22 H22 0.9300 .
C23 C24 1.389(9) .
C23 H23 0.9300 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C26 C28 1.497(10) .
C26 C30 1.521(9) .
C26 C29 1.549(10) .
C26 C27 1.555(12) .
C27 H27A 0.9600 .
C27 H27B 0.9600 .
C27 H27C 0.9600 .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C30 C31 1.352(8) .
C30 C35 1.430(8) .
C31 C32 1.416(9) .
C31 H31 0.9300 .
C32 C33 1.353(8) .
C32 C36 1.503(9) .
C33 C34 1.418(8) .
C33 H33 0.9300 .
C34 C35 1.412(8) .
C34 C37 1.424(8) .
C36 H36A 0.9600 .
C36 H36B 0.9600 .
C36 H36C 0.9600 .
C37 H37 0.9300 .
C38 C43 1.393(9) .
C38 C39 1.399(10) .
C39 C40 1.361(11) .
C39 H39 0.9300 .
C40 C41 1.411(14) .
C40 H40 0.9300 .
C41 C42 1.347(13) .
C41 H41 0.9300 .
C42 C43 1.410(10) .
C42 H42 0.9300 .
C43 C44 1.444(10) .
C44 C45 1.376(10) .
C44 C49 1.433(10) .
C45 C46 1.356(13) .
C45 H45 0.9300 .
C46 C47 1.375(14) .
C46 H46 0.9300 .
C47 C48 1.361(12) .
C47 H47 0.9300 .
C48 C49 1.365(11) .
C48 H48 0.9300 .
C50 H50A 0.9600 .
C50 H50B 0.9600 .
C50 H50C 0.9600 .
C51 C52 1.348(8) .
C51 C53 1.418(9) 2_666
C51 H51A 0.9300 .
C52 C53 1.388(9) .
C52 H52A 0.9300 .
C53 C51 1.418(9) 2_666
C53 C54 1.450(14) .
C54 H54A 0.9600 .
C54 H54B 0.9600 .
C54 H54C 0.9600 .
C55 C60 1.379(5) .
C55 C56 1.379(5) .
C55 H55A 0.9300 .
C56 C57 1.379(5) .
C56 H56A 0.9300 .
C57 C58 1.379(5) .
C57 H57A 0.9300 .
C58 C59 1.379(5) .
C58 H58A 0.9300 .
C59 C60 1.379(5) .
C59 H59A 0.9300 .
C60 C61 1.475(13) .
C61 H61A 0.9600 .
C61 H61B 0.9600 .
C61 H61C 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O3 Ca1 N1 C7 100.5(7) . .
O1 Ca1 N1 C7 16.0(5) . .
O2 Ca1 N1 C7 137.9(5) . .
N2 Ca1 N1 C7 -140.7(5) . .
O4 Ca1 N1 C7 -71.6(5) . .
O3 Ca1 N1 C13 -86.2(7) . .
O1 Ca1 N1 C13 -170.7(5) . .
O2 Ca1 N1 C13 -48.8(5) . .
N2 Ca1 N1 C13 32.6(5) . .
O4 Ca1 N1 C13 101.7(5) . .
O3 Ca1 N2 C37 -14.4(5) . .
O1 Ca1 N2 C37 73.2(7) . .
O2 Ca1 N2 C37 -102.1(5) . .
N1 Ca1 N2 C37 -176.7(5) . .
O4 Ca1 N2 C37 101.5(5) . .
O3 Ca1 N2 C38 -174.7(5) . .
O1 Ca1 N2 C38 -87.0(6) . .
O2 Ca1 N2 C38 97.7(5) . .
N1 Ca1 N2 C38 23.1(5) . .
O4 Ca1 N2 C38 -58.7(5) . .
O3 Ca1 O1 C1 173.3(6) . .
O2 Ca1 O1 C1 -93.5(6) . .
N1 Ca1 O1 C1 -26.8(6) . .
N2 Ca1 O1 C1 91.7(7) . .
O4 Ca1 O1 C1 65.1(6) . .
O3 Ca1 O2 C24 119.8(5) . .
O1 Ca1 O2 C24 16.9(5) . .
N1 Ca1 O2 C24 -48.4(5) . .
N2 Ca1 O2 C24 -165.2(5) . .
O4 Ca1 O2 C24 -118.8(5) . .
O3 Ca1 O2 C25 -39.4(6) . .
O1 Ca1 O2 C25 -142.3(5) . .
N1 Ca1 O2 C25 152.4(6) . .
N2 Ca1 O2 C25 35.6(5) . .
O4 Ca1 O2 C25 82.0(6) . .
O1 Ca1 O3 C35 -145.8(7) . .
O2 Ca1 O3 C35 98.2(7) . .
N1 Ca1 O3 C35 134.6(7) . .
N2 Ca1 O3 C35 9.5(7) . .
O4 Ca1 O3 C35 -53.7(7) . .
O3 Ca1 O4 C49 25.2(6) . .
O1 Ca1 O4 C49 128.0(6) . .
O2 Ca1 O4 C49 -90.9(7) . .
N1 Ca1 O4 C49 -157.6(6) . .
N2 Ca1 O4 C49 -40.8(6) . .
O3 Ca1 O4 C50 -130.8(5) . .
O1 Ca1 O4 C50 -27.9(5) . .
O2 Ca1 O4 C50 113.1(6) . .
N1 Ca1 O4 C50 46.4(5) . .
N2 Ca1 O4 C50 163.2(6) . .
Ca1 O1 C1 C6 23.4(10) . .
Ca1 O1 C1 C2 -154.6(5) . .
O1 C1 C2 C3 177.6(6) . .
C6 C1 C2 C3 -0.4(9) . .
O1 C1 C2 C9 -3.3(9) . .
C6 C1 C2 C9 178.6(6) . .
C1 C2 C3 C4 0.3(10) . .
C9 C2 C3 C4 -178.8(7) . .
C2 C3 C4 C5 2.6(11) . .
C2 C3 C4 C8 -179.0(6) . .
C3 C4 C5 C6 -5.5(10) . .
C8 C4 C5 C6 176.2(6) . .
C4 C5 C6 C1 5.6(10) . .
C4 C5 C6 C7 -176.4(6) . .
O1 C1 C6 C5 179.6(6) . .
C2 C1 C6 C5 -2.4(9) . .
O1 C1 C6 C7 1.6(10) . .
C2 C1 C6 C7 179.7(6) . .
C13 N1 C7 C6 179.9(6) . .
Ca1 N1 C7 C6 -6.7(10) . .
C5 C6 C7 N1 174.8(6) . .
C1 C6 C7 N1 -7.2(11) . .
C3 C2 C9 C10 -117.9(7) . .
C1 C2 C9 C10 63.1(8) . .
C3 C2 C9 C12 -0.1(9) . .
C1 C2 C9 C12 -179.2(6) . .
C3 C2 C9 C11 120.3(7) . .
C1 C2 C9 C11 -58.7(8) . .
C7 N1 C13 C18 -107.4(7) . .
Ca1 N1 C13 C18 78.6(7) . .
C7 N1 C13 C14 74.1(8) . .
Ca1 N1 C13 C14 -99.9(7) . .
C18 C13 C14 C15 -1.0(11) . .
N1 C13 C14 C15 177.5(6) . .
C13 C14 C15 C16 -0.2(13) . .
C14 C15 C16 C17 2.2(14) . .
C15 C16 C17 C18 -2.9(14) . .
C14 C13 C18 C17 0.3(11) . .
N1 C13 C18 C17 -178.1(6) . .
C14 C13 C18 C19 -176.3(7) . .
N1 C13 C18 C19 5.2(10) . .
C16 C17 C18 C13 1.6(12) . .
C16 C17 C18 C19 178.2(7) . .
C13 C18 C19 C24 -69.4(9) . .
C17 C18 C19 C24 114.0(8) . .
C13 C18 C19 C20 112.4(8) . .
C17 C18 C19 C20 -64.2(10) . .
C24 C19 C20 C21 1.3(11) . .
C18 C19 C20 C21 179.6(7) . .
C19 C20 C21 C22 -0.5(13) . .
C20 C21 C22 C23 -1.2(14) . .
C21 C22 C23 C24 2.0(14) . .
C25 O2 C24 C19 -116.9(7) . .
Ca1 O2 C24 C19 82.7(7) . .
C25 O2 C24 C23 64.2(9) . .
Ca1 O2 C24 C23 -96.2(7) . .
C20 C19 C24 O2 -179.3(6) . .
C18 C19 C24 O2 2.4(10) . .
C20 C19 C24 C23 -0.5(11) . .
C18 C19 C24 C23 -178.8(7) . .
C22 C23 C24 O2 177.7(7) . .
C22 C23 C24 C19 -1.2(13) . .
C28 C26 C30 C31 -124.9(8) . .
C29 C26 C30 C31 -4.8(11) . .
C27 C26 C30 C31 112.7(8) . .
C28 C26 C30 C35 56.0(10) . .
C29 C26 C30 C35 176.1(7) . .
C27 C26 C30 C35 -66.4(8) . .
C35 C30 C31 C32 -3.8(11) . .
C26 C30 C31 C32 177.1(7) . .
C30 C31 C32 C33 0.3(11) . .
C30 C31 C32 C36 177.3(7) . .
C31 C32 C33 C34 0.2(10) . .
C36 C32 C33 C34 -176.6(6) . .
C32 C33 C34 C35 2.8(10) . .
C32 C33 C34 C37 -179.1(6) . .
Ca1 O3 C35 C34 -2.9(10) . .
Ca1 O3 C35 C30 176.9(5) . .
C33 C34 C35 O3 173.6(6) . .
C37 C34 C35 O3 -4.3(10) . .
C33 C34 C35 C30 -6.2(9) . .
C37 C34 C35 C30 175.9(6) . .
C31 C30 C35 O3 -173.2(6) . .
C26 C30 C35 O3 5.9(10) . .
C31 C30 C35 C34 6.6(9) . .
C26 C30 C35 C34 -174.3(7) . .
C38 N2 C37 C34 176.4(6) . .
Ca1 N2 C37 C34 16.2(10) . .
C35 C34 C37 N2 -4.3(11) . .
C33 C34 C37 N2 177.7(6) . .
C37 N2 C38 C43 -69.1(8) . .
Ca1 N2 C38 C43 93.0(6) . .
C37 N2 C38 C39 110.5(7) . .
Ca1 N2 C38 C39 -87.5(6) . .
C43 C38 C39 C40 3.7(12) . .
N2 C38 C39 C40 -175.9(7) . .
C38 C39 C40 C41 -2.4(14) . .
C39 C40 C41 C42 0.1(16) . .
C40 C41 C42 C43 0.8(15) . .
C39 C38 C43 C42 -2.6(10) . .
N2 C38 C43 C42 177.0(6) . .
C39 C38 C43 C44 178.8(7) . .
N2 C38 C43 C44 -1.6(10) . .
C41 C42 C43 C38 0.4(12) . .
C41 C42 C43 C44 179.0(8) . .
C38 C43 C44 C45 122.8(8) . .
C42 C43 C44 C45 -55.7(10) . .
C38 C43 C44 C49 -59.7(9) . .
C42 C43 C44 C49 121.8(8) . .
C49 C44 C45 C46 -0.2(12) . .
C43 C44 C45 C46 177.5(8) . .
C44 C45 C46 C47 3.5(15) . .
C45 C46 C47 C48 -4.2(16) . .
C46 C47 C48 C49 1.6(15) . .
C47 C48 C49 O4 -178.9(7) . .
C47 C48 C49 C44 1.8(12) . .
C50 O4 C49 C48 55.3(9) . .
Ca1 O4 C49 C48 -100.4(8) . .
C50 O4 C49 C44 -125.3(7) . .
Ca1 O4 C49 C44 79.0(7) . .
C45 C44 C49 C48 -2.5(10) . .
C43 C44 C49 C48 179.9(7) . .
C45 C44 C49 O4 178.2(6) . .
C43 C44 C49 O4 0.5(10) . .
C53 C51 C52 C53 1(3) 2_666 .
C51 C52 C53 C51 -1(2) . 2_666
C51 C52 C53 C54 -174(2) . .
C60 C55 C56 C57 0.0 . .
C55 C56 C57 C58 0.0 . .
C56 C57 C58 C59 0.0 . .
C57 C58 C59 C60 0.0 . .
C58 C59 C60 C55 0.0 . .
C58 C59 C60 C61 175.7(14) . .
C56 C55 C60 C59 0.0 . .
C56 C55 C60 C61 -175.2(16) . .
