#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:35:20 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180146 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/43/7104348.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_7104348
loop_
_publ_author_name
'Barrett, Anthony G M'
'Crimmin, Mark R'
'Hill, Michael S'
'Hitchcock, Peter B'
'Lomas, Sarah L'
'Procopiou, Panayiotis A'
'Suntharalingam, Kogularamanan'
_publ_section_title
;
 Catalytic 2,3,4-hexatriene formation by terminal alkyne coupling at
 calcium.
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2299
_journal_page_last               2301
_journal_paper_doi               10.1039/b818848c
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         'C66 H92 Ca2 N4 O2, C7 H8'
_chemical_formula_sum            'C73 H100 Ca2 N4 O2'
_chemical_formula_weight         1145.73
_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                91.5190(10)
_cell_angle_beta                 104.5370(10)
_cell_angle_gamma                115.6400(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2296(2)
_cell_length_b                   14.3726(3)
_cell_length_c                   21.2865(4)
_cell_measurement_reflns_used    28675
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_volume                     3489.52(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo & Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54730
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.9531
_exptl_absorpt_correction_T_min  0.9018
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         13704
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0497
_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)+(0.0554P)²+1.8004P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                10031
_reflns_number_total             13704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b818848c.txt
_cod_data_source_block           jul1207
_cod_database_code               7104348
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 0.61643(4) 0.61165(3) 0.57158(2) 0.02857(12) Uani 1 1 d . . .
Ca1B Ca 0.53472(4) 0.14818(3) 0.99711(2) 0.02558(12) Uani 1 1 d . . .
O1 O 0.74896(14) 0.56567(13) 0.65702(8) 0.0396(4) Uani 1 1 d . . .
O1B O 0.57722(15) 0.25311(12) 1.10274(8) 0.0365(4) Uani 1 1 d . . .
N1 N 0.77792(15) 0.76727(14) 0.56947(9) 0.0284(4) Uani 1 1 d . . .
N2 N 0.60474(15) 0.71512(14) 0.65303(9) 0.0265(4) Uani 1 1 d . . .
N1B N 0.67039(15) 0.29444(14) 0.96591(9) 0.0278(4) Uani 1 1 d . . .
N2B N 0.40940(15) 0.21246(14) 0.93954(8) 0.0258(4) Uani 1 1 d . . .
C1 C 0.84014(19) 0.84194(18) 0.62091(11) 0.0321(5) Uani 1 1 d . . .
C2 C 0.8074(2) 0.84680(19) 0.67886(11) 0.0336(5) Uani 1 1 d . . .
H2 H 0.8698 0.8932 0.7153 0.040 Uiso 1 1 calc R . .
C3 C 0.69899(19) 0.79522(17) 0.69230(10) 0.0290(5) Uani 1 1 d . . .
C4 C 0.9546(2) 0.9326(2) 0.62018(13) 0.0520(7) Uani 1 1 d . . .
H4A H 0.9705 0.9233 0.5785 0.078 Uiso 0.50 1 calc PR . .
H4B H 1.0184 0.9352 0.6567 0.078 Uiso 0.50 1 calc PR . .
H4C H 0.9489 0.9981 0.6249 0.078 Uiso 0.50 1 calc PR . .
H4D H 0.9880 0.9811 0.6615 0.078 Uiso 0.50 1 calc PR . .
H4E H 0.9401 0.9692 0.5834 0.078 Uiso 0.50 1 calc PR . .
H4F H 1.0096 0.9063 0.6152 0.078 Uiso 0.50 1 calc PR . .
C5 C 0.6933(2) 0.8377(2) 0.75648(12) 0.0425(6) Uani 1 1 d . . .
H5A H 0.6148 0.7971 0.7613 0.064 Uiso 0.50 1 calc PR . .
H5B H 0.7097 0.9110 0.7566 0.064 Uiso 0.50 1 calc PR . .
H5C H 0.7516 0.8324 0.7931 0.064 Uiso 0.50 1 calc PR . .
H5D H 0.7693 0.8966 0.7794 0.064 Uiso 0.50 1 calc PR . .
H5E H 0.6744 0.7826 0.7841 0.064 Uiso 0.50 1 calc PR . .
H5F H 0.6325 0.8613 0.7476 0.064 Uiso 0.50 1 calc PR . .
C6 C 0.81385(19) 0.77825(17) 0.51026(11) 0.0297(5) Uani 1 1 d . . .
C7 C 0.7854(2) 0.83995(18) 0.46630(11) 0.0331(5) Uani 1 1 d . . .
C8 C 0.8175(2) 0.8460(2) 0.40847(12) 0.0387(6) Uani 1 1 d . . .
H8 H 0.7984 0.8876 0.3784 0.046 Uiso 1 1 calc R . .
C9 C 0.8760(2) 0.7931(2) 0.39387(13) 0.0431(6) Uani 1 1 d . . .
H9 H 0.8988 0.7995 0.3546 0.052 Uiso 1 1 calc R . .
C10 C 0.9011(2) 0.7310(2) 0.43642(13) 0.0443(6) Uani 1 1 d . . .
H10 H 0.9401 0.6935 0.4258 0.053 Uiso 1 1 calc R . .
C11 C 0.8709(2) 0.7214(2) 0.49498(12) 0.0364(6) Uani 1 1 d . . .
C12 C 0.7197(2) 0.8996(2) 0.47833(13) 0.0444(6) Uani 1 1 d . . .
H12 H 0.7099 0.8924 0.5233 0.053 Uiso 1 1 calc R . .
C13 C 0.5977(3) 0.8535(2) 0.42862(16) 0.0575(8) Uani 1 1 d . . .
H13A H 0.6054 0.8629 0.3843 0.086 Uiso 1 1 calc R . .
H13B H 0.5542 0.8893 0.4392 0.086 Uiso 1 1 calc R . .
H13C H 0.5554 0.7788 0.4305 0.086 Uiso 1 1 calc R . .
C14 C 0.7875(3) 1.0167(2) 0.47515(17) 0.0655(9) Uani 1 1 d . . .
H14A H 0.8662 1.0453 0.5063 0.098 Uiso 1 1 calc R . .
H14B H 0.7458 1.0536 0.4865 0.098 Uiso 1 1 calc R . .
H14C H 0.7938 1.0257 0.4306 0.098 Uiso 1 1 calc R . .
C15 C 0.9028(3) 0.6527(2) 0.54065(15) 0.0526(7) Uani 1 1 d . . .
H15 H 0.8524 0.6362 0.5709 0.063 Uiso 1 1 calc R . .
C16 C 1.0291(3) 0.7102(4) 0.5827(3) 0.1201(19) Uani 1 1 d . . .
H16A H 1.0807 0.7315 0.5543 0.180 Uiso 1 1 calc R . .
H16B H 1.0479 0.6641 0.6113 0.180 Uiso 1 1 calc R . .
H16C H 1.0404 0.7723 0.6096 0.180 Uiso 1 1 calc R . .
C17 C 0.8778(4) 0.5483(3) 0.5035(2) 0.0927(14) Uani 1 1 d . . .
H17A H 0.7944 0.5105 0.4791 0.139 Uiso 1 1 calc R . .
H17B H 0.8983 0.5062 0.5349 0.139 Uiso 1 1 calc R . .
H17C H 0.9247 0.5618 0.4727 0.139 Uiso 1 1 calc R . .
C18 C 0.49361(19) 0.68170(17) 0.66547(10) 0.0283(5) Uani 1 1 d . . .
C19 C 0.4302(2) 0.7393(2) 0.64828(12) 0.0377(6) Uani 1 1 d . . .
C20 C 0.3188(2) 0.7011(2) 0.65640(14) 0.0500(7) Uani 1 1 d . . .
H20 H 0.2759 0.7400 0.6456 0.060 Uiso 1 1 calc R . .
C21 C 0.2692(2) 0.6082(3) 0.67975(15) 0.0547(8) Uani 1 1 d . . .
H21 H 0.1929 0.5833 0.6848 0.066 Uiso 1 1 calc R . .
C22 C 0.3309(2) 0.5520(2) 0.69569(14) 0.0479(7) Uani 1 1 d . . .
H22 H 0.2962 0.4877 0.7113 0.057 Uiso 1 1 calc R . .
C23 C 0.4438(2) 0.58721(19) 0.68946(11) 0.0342(5) Uani 1 1 d . . .
C24 C 0.4780(3) 0.8393(2) 0.61944(14) 0.0486(7) Uani 1 1 d . . .
H24 H 0.5624 0.8606 0.6236 0.058 Uiso 1 1 calc R . .
C25 C 0.4127(3) 0.8211(3) 0.54647(15) 0.0683(9) Uani 1 1 d . . .
H25A H 0.4193 0.7651 0.5233 0.102 Uiso 1 1 calc R . .
H25B H 0.4471 0.8855 0.5280 0.102 Uiso 1 1 calc R . .
H25C H 0.3299 0.8012 0.5412 0.102 Uiso 1 1 calc R . .
C26 C 0.4708(4) 0.9286(3) 0.65567(17) 0.0758(10) Uani 1 1 d . . .
H26A H 0.3884 0.9120 0.6490 0.114 Uiso 1 1 calc R . .
H26B H 0.5097 0.9933 0.6385 0.114 Uiso 1 1 calc R . .
H26C H 0.5097 0.9378 0.7027 0.114 Uiso 1 1 calc R . .
C27 C 0.5079(2) 0.52197(19) 0.70826(13) 0.0402(6) Uani 1 1 d . . .
H27 H 0.5843 0.5568 0.6979 0.048 Uiso 1 1 calc R . .
C28 C 0.5350(3) 0.5155(3) 0.78151(14) 0.0609(8) Uani 1 1 d . . .
H28A H 0.5818 0.5861 0.8066 0.091 Uiso 1 1 calc R . .
H28B H 0.5790 0.4751 0.7919 0.091 Uiso 1 1 calc R . .
H28C H 0.4615 0.4811 0.7931 0.091 Uiso 1 1 calc R . .
C29 C 0.4400(3) 0.4122(2) 0.66875(16) 0.0608(8) Uani 1 1 d . . .
H29A H 0.3666 0.3746 0.6800 0.091 Uiso 1 1 calc R . .
H29B H 0.4874 0.3747 0.6792 0.091 Uiso 1 1 calc R . .
H29C H 0.4224 0.4168 0.6217 0.091 Uiso 1 1 calc R . .
C30 C 0.5599(2) 0.41831(19) 0.52015(13) 0.0417(6) Uani 1 1 d . . .
C31 C 0.6374(2) 0.43151(19) 0.56982(13) 0.0403(6) Uani 1 1 d . . .
C32 C 0.7302(2) 0.4638(2) 0.63249(13) 0.0455(6) Uani 1 1 d . . .
H32A H 0.7051 0.4145 0.6635 0.055 Uiso 1 1 calc R . .
H32B H 0.8027 0.4666 0.6257 0.055 Uiso 1 1 calc R . .
C33 C 0.8405(3) 0.6118(3) 0.71749(15) 0.0619(8) Uani 1 1 d . . .
H33A H 0.8190 0.5691 0.7516 0.093 Uiso 1 1 calc R . .
H33B H 0.8518 0.6823 0.7306 0.093 Uiso 1 1 calc R . .
H33C H 0.9133 0.6156 0.7117 0.093 Uiso 1 1 calc R . .
C1B C 0.6617(2) 0.38236(17) 0.95985(11) 0.0313(5) Uani 1 1 d . . .
C2B C 0.5577(2) 0.39123(17) 0.95335(11) 0.0318(5) Uani 1 1 d . . .
H2B H 0.5679 0.4608 0.9595 0.038 Uiso 1 1 calc R . .
C3B C 0.44094(19) 0.31312(17) 0.93910(10) 0.0283(5) Uani 1 1 d . . .
C4B C 0.7675(2) 0.4826(2) 0.95886(15) 0.0486(7) Uani 1 1 d . . .
H4B1 H 0.8354 0.4691 0.9637 0.073 Uiso 0.50 1 calc PR . .
H4B2 H 0.7845 0.5356 0.9952 0.073 Uiso 0.50 1 calc PR . .
H4B3 H 0.7508 0.5079 0.9170 0.073 Uiso 0.50 1 calc PR . .
H4B4 H 0.7451 0.5393 0.9536 0.073 Uiso 0.50 1 calc PR . .
H4B5 H 0.7959 0.4728 0.9221 0.073 Uiso 0.50 1 calc PR . .
H4B6 H 0.8297 0.5005 1.0003 0.073 Uiso 0.50 1 calc PR . .
C5B C 0.3486(2) 0.3517(2) 0.92032(13) 0.0415(6) Uani 1 1 d . . .
H5B1 H 0.2705 0.2924 0.9114 0.062 Uiso 0.50 1 calc PR . .
H5B2 H 0.3551 0.3849 0.8809 0.062 Uiso 0.50 1 calc PR . .
H5B3 H 0.3608 0.4025 0.9565 0.062 Uiso 0.50 1 calc PR . .
H5B4 H 0.3871 0.4275 0.9212 0.062 Uiso 0.50 1 calc PR . .
H5B5 H 0.3025 0.3350 0.9516 0.062 Uiso 0.50 1 calc PR . .
H5B6 H 0.2968 0.3174 0.8760 0.062 Uiso 0.50 1 calc PR . .
C6B C 0.77185(19) 0.28706(17) 0.95890(11) 0.0303(5) Uani 1 1 d . . .
C7B C 0.7753(2) 0.26132(19) 0.89555(12) 0.0359(6) Uani 1 1 d . . .
C8B C 0.8709(2) 0.2481(2) 0.88935(14) 0.0471(7) Uani 1 1 d . . .
H8B H 0.8749 0.2317 0.8468 0.056 Uiso 1 1 calc R . .
C9B C 0.9597(2) 0.2583(2) 0.94360(15) 0.0507(7) Uani 1 1 d . . .
H9B H 1.0244 0.2493 0.9384 0.061 Uiso 1 1 calc R . .
C10B C 0.9541(2) 0.2815(2) 1.00543(14) 0.0474(7) Uani 1 1 d . . .
H10B H 1.0151 0.2876 1.0427 0.057 Uiso 1 1 calc R . .
C11B C 0.8614(2) 0.2964(2) 1.01449(12) 0.0377(6) Uani 1 1 d . . .
C12B C 0.6786(2) 0.2477(2) 0.83430(12) 0.0431(6) Uani 1 1 d . . .
H12B H 0.6142 0.2521 0.8487 0.052 Uiso 1 1 calc R . .
C13B C 0.7207(3) 0.3338(3) 0.79273(17) 0.0699(9) Uani 1 1 d . . .
H13D H 0.7510 0.4020 0.8193 0.105 Uiso 1 1 calc R . .
H13E H 0.6551 0.3241 0.7549 0.105 Uiso 1 1 calc R . .
H13F H 0.7830 0.3304 0.7773 0.105 Uiso 1 1 calc R . .
C14B C 0.6278(3) 0.1411(2) 0.79274(15) 0.0602(8) Uani 1 1 d . . .
H14D H 0.6883 0.1360 0.7762 0.090 Uiso 1 1 calc R . .
H14E H 0.5616 0.1325 0.7556 0.090 Uiso 1 1 calc R . .
H14F H 0.6009 0.0862 0.8197 0.090 Uiso 1 1 calc R . .
C15B C 0.8612(2) 0.3241(2) 1.08360(13) 0.0505(7) Uani 1 1 d . . .
H15B H 0.7857 0.3263 1.0806 0.061 Uiso 1 1 calc R . .
C16B C 0.9609(3) 0.4316(3) 1.11634(16) 0.0739(10) Uani 1 1 d . . .
H16D H 1.0362 0.4305 1.1222 0.111 Uiso 1 1 calc R . .
H16E H 0.9539 0.4495 1.1593 0.111 Uiso 1 1 calc R . .
H16F H 0.9565 0.4839 1.0886 0.111 Uiso 1 1 calc R . .
C17B C 0.8684(3) 0.2428(3) 1.12710(17) 0.0781(11) Uani 1 1 d . . .
H17D H 0.8063 0.1734 1.1054 0.117 Uiso 1 1 calc R . .
H17E H 0.8585 0.2594 1.1694 0.117 Uiso 1 1 calc R . .
H17F H 0.9449 0.2437 1.1343 0.117 Uiso 1 1 calc R . .
C18B C 0.28790(18) 0.13871(17) 0.91518(10) 0.0277(5) Uani 1 1 d . . .
C19B C 0.2440(2) 0.08648(19) 0.84989(11) 0.0324(5) Uani 1 1 d . . .
C20B C 0.1257(2) 0.0164(2) 0.82660(12) 0.0464(7) Uani 1 1 d . . .
H20B H 0.0946 -0.0181 0.7825 0.056 Uiso 1 1 calc R . .
C21B C 0.0522(2) -0.0045(3) 0.86578(13) 0.0576(8) Uani 1 1 d . . .
H21B H -0.0289 -0.0510 0.8484 0.069 Uiso 1 1 calc R . .
C22B C 0.0977(2) 0.0427(2) 0.93041(13) 0.0529(8) Uani 1 1 d . . .
H22B H 0.0474 0.0270 0.9577 0.063 Uiso 1 1 calc R . .
C23B C 0.2157(2) 0.1128(2) 0.95658(11) 0.0370(6) Uani 1 1 d . . .
C24B C 0.3252(2) 0.10544(19) 0.80700(11) 0.0354(5) Uani 1 1 d . . .
H24B H 0.4035 0.1187 0.8366 0.042 Uiso 1 1 calc R . .
C25B C 0.2852(2) 0.0106(2) 0.75540(13) 0.0466(7) Uani 1 1 d . . .
H25D H 0.2694 -0.0518 0.7767 0.070 Uiso 1 1 calc R . .
H25E H 0.3469 0.0224 0.7345 0.070 Uiso 1 1 calc R . .
H25F H 0.2136 0.0006 0.7221 0.070 Uiso 1 1 calc R . .
C26B C 0.3432(3) 0.2017(2) 0.77422(13) 0.0514(7) Uani 1 1 d . . .
H26D H 0.2670 0.1950 0.7486 0.077 Uiso 1 1 calc R . .
H26E H 0.3918 0.2082 0.7450 0.077 Uiso 1 1 calc R . .
H26F H 0.3823 0.2639 0.8079 0.077 Uiso 1 1 calc R . .
C27B C 0.2635(2) 0.1530(2) 1.03000(12) 0.0418(6) Uani 1 1 d . . .
H27B H 0.3486 0.2027 1.0397 0.050 Uiso 1 1 calc R . .
C28B C 0.2038(3) 0.2114(2) 1.05350(14) 0.0526(7) Uani 1 1 d . . .
H28D H 0.2111 0.2696 1.0289 0.079 Uiso 1 1 calc R . .
H28E H 0.2413 0.2386 1.1005 0.079 Uiso 1 1 calc R . .
H28F H 0.1207 0.1636 1.0462 0.079 Uiso 1 1 calc R . .
C29B C 0.2536(3) 0.0627(3) 1.06820(13) 0.0544(8) Uani 1 1 d . . .
H29D H 0.1708 0.0160 1.0629 0.082 Uiso 1 1 calc R . .
H29E H 0.2947 0.0902 1.1149 0.082 Uiso 1 1 calc R . .
H29F H 0.2890 0.0237 1.0514 0.082 Uiso 1 1 calc R . .
C30B C 0.5239(2) 0.0100(2) 1.08160(12) 0.0397(6) Uani 1 1 d . . .
C31B C 0.5505(2) 0.08762(19) 1.11882(11) 0.0373(6) Uani 1 1 d . . .
C32B C 0.5796(2) 0.18990(19) 1.15350(12) 0.0409(6) Uani 1 1 d . . .
H32C H 0.5212 0.1837 1.1766 0.049 Uiso 1 1 calc R . .
H32D H 0.6583 0.2200 1.1859 0.049 Uiso 1 1 calc R . .
C33B C 0.6043(3) 0.3575(2) 1.12670(15) 0.0633(9) Uani 1 1 d . . .
H33D H 0.5498 0.3558 1.1510 0.095 Uiso 1 1 calc R . .
H33E H 0.5968 0.3954 1.0896 0.095 Uiso 1 1 calc R . .
H33F H 0.6847 0.3928 1.1559 0.095 Uiso 1 1 calc R . .
C1S C 0.9803(3) 0.2698(3) 0.72663(15) 0.112(4) Uani 0.50 1 d PGD A 1
C2S C 0.9181(4) 0.1622(3) 0.72259(18) 0.133(3) Uani 1 1 d GD A 1
C3S C 0.8145(4) 0.1062(3) 0.6724(2) 0.099(3) Uani 0.50 1 d PGD A 1
C4S C 0.7732(3) 0.1577(4) 0.62623(18) 0.214(5) Uani 1 1 d GD A 1
C5S C 0.8354(4) 0.2653(4) 0.63027(18) 0.078(2) Uani 0.50 1 d PGD A 1
C6S C 0.9390(4) 0.3214(3) 0.6805(2) 0.119(2) Uani 1 1 d GD A 1
C7S C 1.0829(3) 0.3308(4) 0.7764(2) 0.127(2) Uani 1 1 d GD A 1
C8S C 0.8777(3) 0.2138(3) 0.67749(14) 0.133(6) Uani 0.50 1 d PGD A 1
C9S C 1.0408(4) 0.2294(5) 0.77932(17) 0.079(2) Uani 0.50 1 d PGD A 1
C10S C 1.0288(4) 0.3687(3) 0.7272(2) 0.179(8) Uani 0.50 1 d PGD A 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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 Ca1 N1 83.06(6) . . ?
N2 Ca1 C30 101.46(7) . 2_666 ?
N1 Ca1 C30 110.69(8) . 2_666 ?
N2 Ca1 O1 90.07(6) . . ?
N1 Ca1 O1 89.65(6) . . ?
C30 Ca1 O1 157.53(7) 2_666 . ?
N2 Ca1 C30 146.18(8) . . ?
N1 Ca1 C30 127.84(8) . . ?
C30 Ca1 C30 81.61(9) 2_666 . ?
O1 Ca1 C30 78.21(7) . . ?
N2 Ca1 C31 132.81(7) . . ?
N1 Ca1 C31 118.58(7) . . ?
C30 Ca1 C31 107.48(8) 2_666 . ?
O1 Ca1 C31 52.14(7) . . ?
C30 Ca1 C31 26.10(8) . . ?
N2B Ca1B N1B 80.22(6) . . ?
N2B Ca1B O1B 93.32(6) . . ?
N1B Ca1B O1B 90.15(6) . . ?
N2B Ca1B C30B 100.41(7) . 2_657 ?
N1B Ca1B C30B 109.11(7) . 2_657 ?
O1B Ca1B C30B 157.89(7) . 2_657 ?
N2B Ca1B C30B 136.48(7) . . ?
N1B Ca1B C30B 141.18(8) . . ?
O1B Ca1B C30B 77.69(7) . . ?
C30B Ca1B C30B 80.43(8) 2_657 . ?
N2B Ca1B C31B 128.39(7) . . ?
N1B Ca1B C31B 128.30(7) . . ?
O1B Ca1B C31B 51.98(6) . . ?
C30B Ca1B C31B 106.16(8) 2_657 . ?
C30B Ca1B C31B 25.73(7) . . ?
C33 O1 C32 113.2(2) . . ?
C33 O1 Ca1 139.94(17) . . ?
C32 O1 Ca1 106.59(13) . . ?
C33B O1B C32B 113.37(19) . . ?
C33B O1B Ca1B 138.14(16) . . ?
C32B O1B Ca1B 108.42(13) . . ?
C1 N1 C6 119.32(18) . . ?
C1 N1 Ca1 122.83(14) . . ?
C6 N1 Ca1 117.76(13) . . ?
C3 N2 C18 119.79(18) . . ?
C3 N2 Ca1 122.15(14) . . ?
C18 N2 Ca1 117.59(13) . . ?
C1B N1B C6B 120.50(18) . . ?
C1B N1B Ca1B 123.84(14) . . ?
C6B N1B Ca1B 115.45(13) . . ?
C3B N2B C18B 119.45(18) . . ?
C3B N2B Ca1B 123.34(14) . . ?
C18B N2B Ca1B 116.04(13) . . ?
N1 C1 C2 124.9(2) . . ?
N1 C1 C4 120.3(2) . . ?
C2 C1 C4 114.8(2) . . ?
C3 C2 C1 131.7(2) . . ?
N2 C3 C2 124.9(2) . . ?
N2 C3 C5 119.6(2) . . ?
C2 C3 C5 115.6(2) . . ?
C7 C6 C11 120.2(2) . . ?
C7 C6 N1 119.97(19) . . ?
C11 C6 N1 119.7(2) . . ?
C8 C7 C6 118.7(2) . . ?
C8 C7 C12 118.3(2) . . ?
C6 C7 C12 123.0(2) . . ?
C9 C8 C7 121.6(2) . . ?
C10 C9 C8 119.3(2) . . ?
C9 C10 C11 121.8(2) . . ?
C10 C11 C6 118.3(2) . . ?
C10 C11 C15 119.3(2) . . ?
C6 C11 C15 122.3(2) . . ?
C7 C12 C13 110.5(2) . . ?
C7 C12 C14 111.7(2) . . ?
C13 C12 C14 109.9(2) . . ?
C16 C15 C11 110.9(3) . . ?
C16 C15 C17 111.2(3) . . ?
C11 C15 C17 112.4(3) . . ?
C23 C18 C19 120.1(2) . . ?
C23 C18 N2 119.9(2) . . ?
C19 C18 N2 119.7(2) . . ?
C20 C19 C18 118.7(2) . . ?
C20 C19 C24 119.2(2) . . ?
C18 C19 C24 122.1(2) . . ?
C21 C20 C19 121.5(3) . . ?
C22 C21 C20 119.5(3) . . ?
C21 C22 C23 121.5(3) . . ?
C22 C23 C18 118.7(2) . . ?
C22 C23 C27 119.1(2) . . ?
C18 C23 C27 122.2(2) . . ?
C19 C24 C25 110.4(2) . . ?
C19 C24 C26 112.2(3) . . ?
C25 C24 C26 109.8(2) . . ?
C23 C27 C28 112.0(2) . . ?
C23 C27 C29 111.9(2) . . ?
C28 C27 C29 109.8(2) . . ?
C31 C30 Ca1 172.1(2) . 2_666 ?
C31 C30 Ca1 79.46(16) . . ?
Ca1 C30 Ca1 98.39(9) 2_666 . ?
C30 C31 C32 170.4(3) . . ?
C30 C31 Ca1 74.44(16) . . ?
C32 C31 Ca1 96.02(15) . . ?
O1 C32 C31 105.19(19) . . ?
N1B C1B C2B 124.3(2) . . ?
N1B C1B C4B 120.5(2) . . ?
C2B C1B C4B 115.2(2) . . ?
C3B C2B C1B 130.1(2) . . ?
N2B C3B C2B 124.6(2) . . ?
N2B C3B C5B 120.3(2) . . ?
C2B C3B C5B 115.1(2) . . ?
C11B C6B C7B 120.4(2) . . ?
C11B C6B N1B 120.6(2) . . ?
C7B C6B N1B 118.7(2) . . ?
C8B C7B C6B 118.5(2) . . ?
C8B C7B C12B 119.5(2) . . ?
C6B C7B C12B 122.0(2) . . ?
C9B C8B C7B 121.4(2) . . ?
C8B C9B C10B 119.6(2) . . ?
C9B C10B C11B 121.5(3) . . ?
C10B C11B C6B 118.7(2) . . ?
C10B C11B C15B 119.2(2) . . ?
C6B C11B C15B 122.1(2) . . ?
C7B C12B C14B 111.4(2) . . ?
C7B C12B C13B 111.9(2) . . ?
C14B C12B C13B 109.9(2) . . ?
C11B C15B C16B 111.8(2) . . ?
C11B C15B C17B 112.3(3) . . ?
C16B C15B C17B 109.3(3) . . ?
C23B C18B C19B 120.2(2) . . ?
C23B C18B N2B 120.79(19) . . ?
C19B C18B N2B 118.79(19) . . ?
C20B C19B C18B 118.2(2) . . ?
C20B C19B C24B 121.2(2) . . ?
C18B C19B C24B 120.6(2) . . ?
C21B C20B C19B 121.8(2) . . ?
C22B C21B C20B 119.3(2) . . ?
C21B C22B C23B 121.4(2) . . ?
C22B C23B C18B 118.8(2) . . ?
C22B C23B C27B 118.9(2) . . ?
C18B C23B C27B 122.2(2) . . ?
C26B C24B C19B 112.4(2) . . ?
C26B C24B C25B 110.1(2) . . ?
C19B C24B C25B 112.9(2) . . ?
C23B C27B C29B 109.9(2) . . ?
C23B C27B C28B 113.4(2) . . ?
C29B C27B C28B 110.1(2) . . ?
C31B C30B Ca1B 178.4(2) . 2_657 ?
C31B C30B Ca1B 79.25(16) . . ?
Ca1B C30B Ca1B 99.57(8) 2_657 . ?
C30B C31B C32B 170.0(2) . . ?
C30B C31B Ca1B 75.02(15) . . ?
C32B C31B Ca1B 95.01(14) . . ?
O1B C32B C31B 104.54(18) . . ?
C10S C1S C8S 115.5 . . ?
C10S C1S C7S 62.0 . . ?
C8S C1S C7S 177.1 . . ?
C10S C1S C2S 174.7 . . ?
C8S C1S C2S 59.5 . . ?
C7S C1S C2S 122.9 . . ?
C10S C1S C6S 55.1 . . ?
C8S C1S C6S 60.5 . . ?
C7S C1S C6S 117.1 . . ?
C2S C1S C6S 120.0 . . ?
C10S C1S C9S 116.7 . . ?
C8S C1S C9S 127.8 . . ?
C7S C1S C9S 54.7 . . ?
C2S C1S C9S 68.3 . . ?
C6S C1S C9S 171.6 . . ?
C8S C2S C3S 60.4 . . ?
C8S C2S C1S 59.6 . . ?
C3S C2S C1S 120.0 . . ?
C8S C2S C9S 118.4 . . ?
C3S C2S C9S 178.1 . . ?
C1S C2S C9S 58.8 . . ?
C8S C3S C2S 59.1 . . ?
C8S C3S C4S 60.9 . . ?
C2S C3S C4S 120.0 . . ?
C3S C4S C5S 120.0 . . ?
C3S C4S C8S 59.5 . . ?
C5S C4S C8S 60.5 . . ?
C6S C5S C4S 120.0 . . ?
C6S C5S C8S 59.6 . . ?
C4S C5S C8S 60.4 . . ?
C10S C6S C5S 177.1 . . ?
C10S C6S C1S 57.9 . . ?
C5S C6S C1S 120.0 . . ?
C10S C6S C8S 117.0 . . ?
C5S C6S C8S 60.9 . . ?
C1S C6S C8S 59.1 . . ?
C9S C7S C10S 121.6 . . ?
C9S C7S C1S 66.5 . . ?
C10S C7S C1S 55.1 . . ?
C2S C8S C1S 60.9 . . ?
C2S C8S C3S 60.5 . . ?
C1S C8S C3S 121.4 . . ?
C2S C8S C6S 121.3 . . ?
C1S C8S C6S 60.4 . . ?
C3S C8S C6S 178.1 . . ?
C2S C8S C4S 120.1 . . ?
C1S C8S C4S 178.9 . . ?
C3S C8S C4S 59.6 . . ?
C6S C8S C4S 118.6 . . ?
C2S C8S C5S 179.0 . . ?
C1S C8S C5S 119.9 . . ?
C3S C8S C5S 118.7 . . ?
C6S C8S C5S 59.5 . . ?
C4S C8S C5S 59.1 . . ?
C7S C9S C1S 58.8 . . ?
C7S C9S C2S 111.6 . . ?
C1S C9S C2S 52.9 . . ?
C6S C10S C1S 67.0 . . ?
C6S C10S C7S 129.9 . . ?
C1S C10S C7S 62.9 . . ?
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 N2 2.3320(18) . ?
Ca1 N1 2.3425(19) . ?
Ca1 C30 2.498(3) 2_666 ?
Ca1 O1 2.5068(16) . ?
Ca1 C30 2.666(2) . ?
Ca1 C31 2.721(2) . ?
Ca1B N2B 2.3387(18) . ?
Ca1B N1B 2.3428(18) . ?
Ca1B O1B 2.4694(16) . ?
Ca1B C30B 2.490(3) 2_657 ?
Ca1B C30B 2.696(2) . ?
Ca1B C31B 2.742(2) . ?
O1 C33 1.428(3) . ?
O1 C32 1.434(3) . ?
O1B C33B 1.429(3) . ?
O1B C32B 1.433(3) . ?
N1 C1 1.322(3) . ?
N1 C6 1.444(3) . ?
N2 C3 1.327(3) . ?
N2 C18 1.433(3) . ?
N1B C1B 1.324(3) . ?
N1B C6B 1.435(3) . ?
N2B C3B 1.322(3) . ?
N2B C18B 1.433(3) . ?
C1 C2 1.416(3) . ?
C1 C4 1.515(3) . ?
C2 C3 1.409(3) . ?
C3 C5 1.514(3) . ?
C6 C7 1.400(3) . ?
C6 C11 1.409(3) . ?
C7 C8 1.392(3) . ?
C7 C12 1.518(3) . ?
C8 C9 1.375(4) . ?
C9 C10 1.369(4) . ?
C10 C11 1.394(3) . ?
C11 C15 1.518(4) . ?
C12 C13 1.531(4) . ?
C12 C14 1.540(4) . ?
C15 C16 1.514(5) . ?
C15 C17 1.536(5) . ?
C18 C23 1.404(3) . ?
C18 C19 1.408(3) . ?
C19 C20 1.392(4) . ?
C19 C24 1.517(4) . ?
C20 C21 1.379(4) . ?
C21 C22 1.371(4) . ?
C22 C23 1.397(3) . ?
C23 C27 1.515(3) . ?
C24 C25 1.529(4) . ?
C24 C26 1.530(4) . ?
C27 C28 1.525(4) . ?
C27 C29 1.526(4) . ?
C30 C31 1.218(4) . ?
C30 Ca1 2.498(3) 2_666 ?
C31 C32 1.468(4) . ?
C1B C2B 1.409(3) . ?
C1B C4B 1.519(3) . ?
C2B C3B 1.409(3) . ?
C3B C5B 1.520(3) . ?
C6B C11B 1.405(3) . ?
C6B C7B 1.406(3) . ?
C7B C8B 1.394(3) . ?
C7B C12B 1.519(4) . ?
C8B C9B 1.377(4) . ?
C9B C10B 1.377(4) . ?
C10B C11B 1.389(3) . ?
C11B C15B 1.515(4) . ?
C12B C14B 1.523(4) . ?
C12B C13B 1.528(4) . ?
C15B C16B 1.526(4) . ?
C15B C17B 1.530(5) . ?
C18B C23B 1.400(3) . ?
C18B C19B 1.412(3) . ?
C19B C20B 1.390(3) . ?
C19B C24B 1.521(3) . ?
C20B C21B 1.378(4) . ?
C21B C22B 1.377(4) . ?
C22B C23B 1.391(3) . ?
C23B C27B 1.522(3) . ?
C24B C26B 1.519(4) . ?
C24B C25B 1.532(3) . ?
C27B C29B 1.525(4) . ?
C27B C28B 1.527(4) . ?
C30B C31B 1.212(3) . ?
C30B Ca1B 2.490(3) 2_657 ?
C31B C32B 1.471(3) . ?
C1S C10S 1.2801 . ?
C1S C8S 1.3721 . ?
C1S C7S 1.3898 . ?
C1S C2S 1.3900 . ?
C1S C6S 1.3900 . ?
C1S C9S 1.4907 . ?
C2S C8S 1.3710 . ?
C2S C3S 1.3900 . ?
C2S C9S 1.6195 . ?
C3S C8S 1.3891 . ?
C3S C4S 1.3900 . ?
C4S C5S 1.3900 . ?
C4S C8S 1.4080 . ?
C5S C6S 1.3900 . ?
C5S C8S 1.4091 . ?
C6S C10S 1.2385 . ?
C6S C8S 1.3913 . ?
C7S C9S 1.3259 . ?
C7S C10S 1.3784 . ?
