#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:05:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179740 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/36/7003600.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_7003600
loop_
_publ_author_name
'Barrett, Anthony G. M.'
'Crimmin, Mark R.'
'Hill, Michael S.'
'Hitchcock, Peter B.'
'Procopiou, Panayiotis A.'
_publ_section_title
;
 Insertion reactions of β-diketiminate-stabilised calcium amides with
 1,3-dialkylcarbodiimides
;
_journal_issue                   33
_journal_name_full               'Dalton Transactions'
_journal_page_first              4474
_journal_page_last               4481
_journal_paper_doi               10.1039/b717383k
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C58 H89 Ca N5 O'
_chemical_formula_sum            'C58 H89 Ca N5 O'
_chemical_formula_weight         912.42
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-10-23T10:44:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 113.849(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1755(3)
_cell_length_b                   11.3831(2)
_cell_length_c                   21.1589(3)
_cell_measurement_reflns_used    49901
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     5545.87(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and 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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.448604E-1
_diffrn_orient_matrix_UB_12      -0.71763E-2
_diffrn_orient_matrix_UB_13      -0.42004E-2
_diffrn_orient_matrix_UB_21      0.25207E-1
_diffrn_orient_matrix_UB_22      -0.36246E-2
_diffrn_orient_matrix_UB_23      0.432017E-1
_diffrn_orient_matrix_UB_31      -0.47244E-2
_diffrn_orient_matrix_UB_32      -0.874809E-1
_diffrn_orient_matrix_UB_33      -0.14454E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.029
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            70644
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  0.9589
_exptl_absorpt_correction_T_min  0.9101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         10880
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0611P)²+3.6166P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                8688
_reflns_number_total             10880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717383k.txt
_cod_data_source_block           (6)-oct1406
_cod_original_cell_volume        5545.87(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7003600
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Ca Ca 0.227651(14) 0.51007(3) 0.250433(17) 0.02398(10) Uani 1 1 d . A .
O O 0.19627(6) 0.68710(12) 0.28788(8) 0.0432(4) Uani 1 1 d . . .
N1 N 0.17551(6) 0.54347(14) 0.12915(8) 0.0291(3) Uani 1 1 d . . .
N2 N 0.13682(6) 0.42347(14) 0.23478(8) 0.0297(3) Uani 1 1 d . . .
N3 N 0.40533(6) 0.42080(14) 0.33364(8) 0.0286(3) Uani 1 1 d . . .
H3X H 0.4254(10) 0.484(2) 0.3394(11) 0.039(6) Uiso 1 1 d . . .
N4 N 0.32734(6) 0.54742(13) 0.32213(8) 0.0308(3) Uani 1 1 d . . .
N5 N 0.30389(6) 0.36471(13) 0.27712(8) 0.0296(3) Uani 1 1 d . . .
C1 C 0.15241(8) 0.44441(18) 0.09702(9) 0.0329(4) Uani 1 1 d . . .
C2 C 0.13291(9) 0.35093(19) 0.12582(10) 0.0384(5) Uani 1 1 d . . .
H2 H 0.1275 0.2791 0.1011 0.046 Uiso 1 1 calc R . .
C3 C 0.11999(8) 0.34460(18) 0.18459(10) 0.0347(4) Uani 1 1 d . . .
C4 C 0.14566(10) 0.4226(2) 0.02326(11) 0.0519(6) Uani 1 1 d . . .
H4A H 0.1794 0.3788 0.0238 0.078 Uiso 1 1 calc R . .
H4B H 0.143 0.498 -0.0002 0.078 Uiso 1 1 calc R . .
H4C H 0.1103 0.377 -0.0014 0.078 Uiso 1 1 calc R . .
C5 C 0.08408(11) 0.2392(2) 0.18752(13) 0.0542(6) Uani 1 1 d . . .
H5A H 0.043 0.2616 0.1701 0.081 Uiso 1 1 calc R . .
H5B H 0.0971 0.2123 0.2354 0.081 Uiso 1 1 calc R . .
H5C H 0.0889 0.1758 0.159 0.081 Uiso 1 1 calc R . .
C6 C 0.18398(8) 0.63945(17) 0.09032(9) 0.0308(4) Uani 1 1 d . . .
C7 C 0.14041(9) 0.7260(2) 0.06427(11) 0.0443(5) Uani 1 1 d . . .
C8 C 0.14959(11) 0.8216(2) 0.02872(12) 0.0541(6) Uani 1 1 d . . .
H8 H 0.1201 0.8794 0.0103 0.065 Uiso 1 1 calc R . .
C9 C 0.20051(11) 0.8338(2) 0.01970(12) 0.0521(6) Uani 1 1 d . . .
H9 H 0.206 0.8995 -0.0047 0.063 Uiso 1 1 calc R . .
C10 C 0.24315(10) 0.75075(19) 0.04620(11) 0.0424(5) Uani 1 1 d . . .
H10 H 0.2783 0.7601 0.0402 0.051 Uiso 1 1 calc R . .
C11 C 0.23627(8) 0.65276(17) 0.08167(9) 0.0312(4) Uani 1 1 d . . .
C12 C 0.08413(11) 0.7168(3) 0.07469(16) 0.0690(8) Uani 1 1 d . . .
H12 H 0.093 0.6726 0.1186 0.083 Uiso 1 1 calc R . .
C13 C 0.06079(16) 0.8383(3) 0.0830(2) 0.1068(15) Uani 1 1 d . . .
H13A H 0.0452 0.8787 0.0383 0.16 Uiso 1 1 calc R . .
H13B H 0.0924 0.885 0.1165 0.16 Uiso 1 1 calc R . .
H13C H 0.0299 0.8285 0.0996 0.16 Uiso 1 1 calc R . .
C14 C 0.03875(13) 0.6478(5) 0.0174(2) 0.1208(16) Uani 1 1 d . . .
H14A H 0.0314 0.6851 -0.0271 0.181 Uiso 1 1 calc R . .
H14B H 0.0027 0.6461 0.0247 0.181 Uiso 1 1 calc R . .
H14C H 0.0526 0.5673 0.0174 0.181 Uiso 1 1 calc R . .
C15 C 0.28523(8) 0.56424(19) 0.10981(11) 0.0367(5) Uani 1 1 d . . .
H15 H 0.273 0.5017 0.1344 0.044 Uiso 1 1 calc R . .
C16 C 0.29793(11) 0.5053(2) 0.05247(14) 0.0571(6) Uani 1 1 d . . .
H16A H 0.3111 0.5645 0.0284 0.086 Uiso 1 1 calc R . .
H16B H 0.2625 0.4676 0.0196 0.086 Uiso 1 1 calc R . .
H16C H 0.3283 0.4459 0.0727 0.086 Uiso 1 1 calc R . .
C17 C 0.34032(10) 0.6204(3) 0.16175(13) 0.0592(7) Uani 1 1 d . . .
H17A H 0.3319 0.6593 0.198 0.089 Uiso 1 1 calc R . .
H17B H 0.3547 0.6785 0.1383 0.089 Uiso 1 1 calc R . .
H17C H 0.3699 0.5597 0.1825 0.089 Uiso 1 1 calc R . .
C18 C 0.11195(8) 0.42437(17) 0.28479(10) 0.0311(4) Uani 1 1 d . . .
C19 C 0.05750(8) 0.47780(19) 0.26895(11) 0.0386(5) Uani 1 1 d . . .
C20 C 0.03746(9) 0.4891(2) 0.32121(12) 0.0446(5) Uani 1 1 d . . .
H20 H 0.0009 0.5253 0.311 0.053 Uiso 1 1 calc R . .
C21 C 0.06922(9) 0.4491(2) 0.38706(12) 0.0445(5) Uani 1 1 d . . .
H21 H 0.0549 0.4584 0.422 0.053 Uiso 1 1 calc R . .
C22 C 0.12211(9) 0.3952(2) 0.40217(11) 0.0403(5) Uani 1 1 d . . .
H22 H 0.1438 0.3669 0.4476 0.048 Uiso 1 1 calc R . .
C23 C 0.14419(8) 0.38160(17) 0.35171(10) 0.0342(4) Uani 1 1 d . . .
C24 C 0.02040(9) 0.5246(2) 0.19720(13) 0.0523(6) Uani 1 1 d . . .
H24 H 0.0403 0.5053 0.166 0.063 Uiso 1 1 calc R . .
C25 C 0.01343(14) 0.6577(3) 0.19773(18) 0.0804(9) Uani 1 1 d . . .
H25A H 0.0517 0.6951 0.2131 0.121 Uiso 1 1 calc R . .
H25B H -0.0047 0.6786 0.2294 0.121 Uiso 1 1 calc R . .
H25C H -0.0111 0.6848 0.151 0.121 Uiso 1 1 calc R . .
C26 C -0.03964(12) 0.4659(4) 0.16794(17) 0.0914(11) Uani 1 1 d . . .
H26A H -0.0615 0.4923 0.1203 0.137 Uiso 1 1 calc R . .
H26B H -0.0608 0.4874 0.1963 0.137 Uiso 1 1 calc R . .
H26C H -0.035 0.3803 0.1685 0.137 Uiso 1 1 calc R . .
C27 C 0.20204(9) 0.32091(19) 0.37066(11) 0.0402(5) Uani 1 1 d . . .
H27 H 0.2118 0.3252 0.3293 0.048 Uiso 1 1 calc R . .
C28 C 0.25012(11) 0.3831(3) 0.42925(19) 0.0818(10) Uani 1 1 d . . .
H28A H 0.2876 0.3476 0.4363 0.123 Uiso 1 1 calc R . .
H28B H 0.2435 0.3755 0.4717 0.123 Uiso 1 1 calc R . .
H28C H 0.2504 0.4664 0.4178 0.123 Uiso 1 1 calc R . .
C29 C 0.19906(14) 0.1922(2) 0.38671(17) 0.0717(8) Uani 1 1 d . . .
H29A H 0.1909 0.1846 0.4281 0.108 Uiso 1 1 calc R . .
H29B H 0.2363 0.1545 0.3949 0.108 Uiso 1 1 calc R . .
H29C H 0.1681 0.1542 0.3475 0.108 Uiso 1 1 calc R . .
C30 C 0.43780(7) 0.31429(15) 0.35362(9) 0.0268(4) Uani 1 1 d . . .
C31 C 0.43525(7) 0.24539(16) 0.40768(9) 0.0287(4) Uani 1 1 d . . .
C32 C 0.46557(8) 0.13975(17) 0.42298(10) 0.0339(4) Uani 1 1 d . . .
H32 H 0.463 0.0903 0.4578 0.041 Uiso 1 1 calc R . .
C33 C 0.49937(8) 0.10522(17) 0.38858(10) 0.0368(5) Uani 1 1 d . . .
H33 H 0.5191 0.032 0.3992 0.044 Uiso 1 1 calc R . .
C34 C 0.50437(8) 0.17737(18) 0.33877(10) 0.0355(4) Uani 1 1 d . . .
H34 H 0.5291 0.1547 0.3168 0.043 Uiso 1 1 calc R . .
C35 C 0.47389(8) 0.28262(17) 0.32021(9) 0.0306(4) Uani 1 1 d . . .
C36 C 0.40318(8) 0.28848(18) 0.45069(10) 0.0357(4) Uani 1 1 d . . .
H36 H 0.3673 0.3301 0.419 0.043 Uiso 1 1 calc R . .
C37 C 0.38458(11) 0.1899(2) 0.48631(14) 0.0564(6) Uani 1 1 d . . .
H37A H 0.3617 0.2229 0.5101 0.085 Uiso 1 1 calc R . .
H37B H 0.4191 0.1508 0.52 0.085 Uiso 1 1 calc R . .
H37C H 0.361 0.1328 0.4517 0.085 Uiso 1 1 calc R . .
C38 C 0.44068(11) 0.3772(2) 0.50476(12) 0.0533(6) Uani 1 1 d . . .
H38A H 0.4521 0.4409 0.4817 0.08 Uiso 1 1 calc R . .
H38B H 0.4755 0.3378 0.5377 0.08 Uiso 1 1 calc R . .
H38C H 0.4184 0.4096 0.5294 0.08 Uiso 1 1 calc R . .
C39 C 0.48192(9) 0.36227(19) 0.26700(11) 0.0406(5) Uani 1 1 d . . .
H39 H 0.4485 0.4182 0.2496 0.049 Uiso 1 1 calc R . .
C40 C 0.48282(18) 0.2945(3) 0.20522(16) 0.0870(10) Uani 1 1 d . . .
H40A H 0.4479 0.2455 0.1854 0.13 Uiso 1 1 calc R . .
H40B H 0.5174 0.2445 0.2203 0.13 Uiso 1 1 calc R . .
H40C H 0.4837 0.3501 0.1703 0.13 Uiso 1 1 calc R . .
C41 C 0.53703(13) 0.4334(3) 0.30067(18) 0.0836(10) Uani 1 1 d . . .
H41A H 0.5705 0.3802 0.319 0.125 Uiso 1 1 calc R . .
H41B H 0.5349 0.4801 0.3385 0.125 Uiso 1 1 calc R . .
H41C H 0.5414 0.4858 0.2664 0.125 Uiso 1 1 calc R . .
C42 C 0.19586(14) 0.7962(2) 0.25439(16) 0.0657(7) Uani 1 1 d . . .
H42A H 0.1689 0.792 0.2051 0.079 Uiso 1 1 calc R . .
H42B H 0.2352 0.8144 0.2572 0.079 Uiso 1 1 calc R . .
C43 C 0.1767(2) 0.8880(3) 0.2900(2) 0.0957(12) Uani 1 1 d . . .
H43A H 0.1354 0.9083 0.263 0.115 Uiso 1 1 calc R . .
H43B H 0.2005 0.9599 0.2965 0.115 Uiso 1 1 calc R . .
C44 C 0.18493(13) 0.8361(2) 0.35788(15) 0.0683(8) Uani 1 1 d . . .
H44A H 0.1552 0.8654 0.3735 0.082 Uiso 1 1 calc R . .
H44B H 0.224 0.8544 0.3936 0.082 Uiso 1 1 calc R . .
C45 C 0.17812(11) 0.7070(2) 0.34338(13) 0.0533(6) Uani 1 1 d . . .
H45A H 0.2027 0.6617 0.3849 0.064 Uiso 1 1 calc R . .
H45B H 0.1371 0.683 0.3295 0.064 Uiso 1 1 calc R . .
C46 C 0.34526(7) 0.44163(15) 0.31132(9) 0.0257(4) Uani 1 1 d . A .
C47 C 0.36620(8) 0.62956(16) 0.37265(10) 0.0323(4) Uani 1 1 d . . .
H47 H 0.4056 0.5928 0.3939 0.039 Uiso 1 1 calc R . .
C48 C 0.37146(12) 0.7435(2) 0.33885(12) 0.0568(7) Uani 1 1 d . . .
H48A H 0.332 0.7745 0.3115 0.068 Uiso 1 1 calc R . .
H48B H 0.3901 0.7273 0.3065 0.068 Uiso 1 1 calc R . .
C49 C 0.40678(13) 0.8373(2) 0.39070(13) 0.0622(7) Uani 1 1 d . . .
H49A H 0.4479 0.8123 0.413 0.075 Uiso 1 1 calc R . .
H49B H 0.4052 0.9119 0.366 0.075 Uiso 1 1 calc R . .
C50 C 0.38342(10) 0.8571(2) 0.44553(14) 0.0560(7) Uani 1 1 d . . .
H50A H 0.4081 0.9151 0.4797 0.067 Uiso 1 1 calc R . .
H50B H 0.3435 0.8891 0.4239 0.067 Uiso 1 1 calc R . .
C51 C 0.38283(10) 0.7433(2) 0.48164(12) 0.0494(6) Uani 1 1 d . . .
H51A H 0.3671 0.7571 0.517 0.059 Uiso 1 1 calc R . .
H51B H 0.423 0.7134 0.5054 0.059 Uiso 1 1 calc R . .
C52 C 0.34556(9) 0.6519(2) 0.42964(11) 0.0439(5) Uani 1 1 d . . .
H52A H 0.3466 0.5773 0.4541 0.053 Uiso 1 1 calc R . .
H52B H 0.3048 0.6794 0.4089 0.053 Uiso 1 1 calc R . .
C53 C 0.31556(8) 0.25432(17) 0.25016(9) 0.0308(4) Uiso 0.62 1 d PD A 1
H53 H 0.3535 0.2221 0.2836 0.037 Uiso 0.62 1 calc PR A 1
C54 C 0.26650(16) 0.1658(3) 0.2428(2) 0.0450(8) Uiso 0.62 1 d PD A 1
H54A H 0.2662 0.1517 0.2888 0.054 Uiso 0.62 1 calc PR A 1
H54B H 0.2286 0.2002 0.2127 0.054 Uiso 0.62 1 calc PR A 1
C55 C 0.27452(19) 0.0475(4) 0.2119(2) 0.0568(10) Uiso 0.62 1 d PD A 1
H55A H 0.3091 0.0066 0.2455 0.068 Uiso 0.62 1 calc PR A 1
H55B H 0.2402 -0.003 0.203 0.068 Uiso 0.62 1 calc PR A 1
C56 C 0.28190(18) 0.0661(4) 0.1455(2) 0.0548(10) Uiso 0.62 1 d PD A 1
H56A H 0.291 -0.0101 0.1298 0.066 Uiso 0.62 1 calc PR A 1
H56B H 0.2447 0.0945 0.1098 0.066 Uiso 0.62 1 calc PR A 1
C57 C 0.32879(19) 0.1522(4) 0.1522(2) 0.0541(10) Uiso 0.62 1 d PD A 1
H57A H 0.3295 0.1656 0.1063 0.065 Uiso 0.62 1 calc PR A 1
H57B H 0.3669 0.1199 0.1833 0.065 Uiso 0.62 1 calc PR A 1
C58 C 0.31801(16) 0.2687(3) 0.18121(17) 0.0395(7) Uiso 0.62 1 d PD A 1
H58A H 0.3495 0.3245 0.1855 0.047 Uiso 0.62 1 calc PR A 1
H58B H 0.2809 0.3027 0.1484 0.047 Uiso 0.62 1 calc PR A 1
C53A C 0.31556(8) 0.25432(17) 0.25016(9) 0.0308(4) Uiso 0.38 1 d PD A 2
H53A H 0.3583 0.2491 0.2631 0.037 Uiso 0.38 1 calc PR A 2
C54A C 0.2985(3) 0.1540(5) 0.2803(3) 0.0403(12) Uiso 0.38 1 d PD A 2
H54C H 0.2565 0.1598 0.2697 0.048 Uiso 0.38 1 calc PR A 2
H54D H 0.3199 0.1566 0.3312 0.048 Uiso 0.38 1 calc PR A 2
C55A C 0.3103(3) 0.0371(6) 0.2538(3) 0.0548(16) Uiso 0.38 1 d PD A 2
H55C H 0.3526 0.0284 0.2669 0.066 Uiso 0.38 1 calc PR A 2
H55D H 0.2975 -0.0277 0.2755 0.066 Uiso 0.38 1 calc PR A 2
C56A C 0.2795(3) 0.0293(7) 0.1780(4) 0.0619(18) Uiso 0.38 1 d PD A 2
H56C H 0.2371 0.0299 0.1654 0.074 Uiso 0.38 1 calc PR A 2
H56D H 0.2894 -0.046 0.162 0.074 Uiso 0.38 1 calc PR A 2
C57A C 0.2950(4) 0.1302(7) 0.1414(4) 0.068(2) Uiso 0.38 1 d PD A 2
H57C H 0.2709 0.1259 0.0911 0.082 Uiso 0.38 1 calc PR A 2
H57D H 0.3363 0.1241 0.1487 0.082 Uiso 0.38 1 calc PR A 2
C58A C 0.2844(3) 0.2484(6) 0.1701(3) 0.0507(15) Uiso 0.38 1 d PD A 2
H58C H 0.2422 0.2596 0.156 0.061 Uiso 0.38 1 calc PR A 2
H58D H 0.2987 0.3132 0.1498 0.061 Uiso 0.38 1 calc PR A 2
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 0 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ca N4 149.71(6) . . ?
N2 Ca N1 80.65(5) . . ?
N4 Ca N1 129.25(5) . . ?
N2 Ca O 88.17(5) . . ?
N4 Ca O 92.43(5) . . ?
N1 Ca O 96.26(5) . . ?
N2 Ca N5 112.00(5) . . ?
N4 Ca N5 56.16(5) . . ?
N1 Ca N5 113.45(5) . . ?
O Ca N5 145.91(5) . . ?
C42 O C45 109.09(18) . . ?
C42 O Ca 120.09(14) . . ?
C45 O Ca 130.79(14) . . ?
C1 N1 C6 119.42(15) . . ?
C1 N1 Ca 110.61(12) . . ?
C6 N1 Ca 126.24(11) . . ?
C3 N2 C18 120.31(15) . . ?
C3 N2 Ca 111.69(11) . . ?
C18 N2 Ca 125.14(11) . . ?
C46 N3 C30 130.56(15) . . ?
C46 N3 H3X 113.4(15) . . ?
C30 N3 H3X 115.8(15) . . ?
C46 N4 C47 121.98(14) . . ?
C46 N4 Ca 94.11(10) . . ?
C47 N4 Ca 143.20(11) . . ?
C46 N5 C53 122.90(15) . . ?
C46 N5 Ca 92.85(11) . . ?
C53 N5 Ca 139.79(11) . . ?
N1 C1 C2 125.34(17) . . ?
N1 C1 C4 120.64(18) . . ?
C2 C1 C4 114.01(18) . . ?
C3 C2 C1 131.72(19) . . ?
C3 C2 H2 114.1 . . ?
C1 C2 H2 114.1 . . ?
N2 C3 C2 124.10(17) . . ?
N2 C3 C5 120.41(17) . . ?
C2 C3 C5 115.48(18) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 119.60(18) . . ?
C11 C6 N1 121.32(16) . . ?
C7 C6 N1 118.95(17) . . ?
C8 C7 C6 118.94(19) . . ?
C8 C7 C12 119.9(2) . . ?
C6 C7 C12 121.2(2) . . ?
C9 C8 C7 121.4(2) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C10 C9 C8 119.5(2) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 121.7(2) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C10 C11 C6 118.83(18) . . ?
C10 C11 C15 119.04(17) . . ?
C6 C11 C15 122.13(17) . . ?
C14 C12 C7 111.5(3) . . ?
C14 C12 C13 111.1(3) . . ?
C7 C12 C13 112.0(3) . . ?
C14 C12 H12 107.3 . . ?
C7 C12 H12 107.3 . . ?
C13 C12 H12 107.3 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 111.35(19) . . ?
C11 C15 C16 112.21(18) . . ?
C17 C15 C16 109.64(18) . . ?
C11 C15 H15 107.8 . . ?
C17 C15 H15 107.8 . . ?
C16 C15 H15 107.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 119.94(17) . . ?
C23 C18 N2 119.72(16) . . ?
C19 C18 N2 120.08(17) . . ?
C20 C19 C18 118.65(19) . . ?
C20 C19 C24 119.10(19) . . ?
C18 C19 C24 122.24(18) . . ?
C21 C20 C19 121.7(2) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C20 C21 C22 119.55(19) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C21 C22 C23 121.1(2) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C22 C23 C18 119.07(18) . . ?
C22 C23 C27 119.07(18) . . ?
C18 C23 C27 121.87(17) . . ?
C19 C24 C25 111.5(2) . . ?
C19 C24 C26 110.9(2) . . ?
C25 C24 C26 109.7(3) . . ?
C19 C24 H24 108.2 . . ?
C25 C24 H24 108.2 . . ?
C26 C24 H24 108.2 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C29 C27 C23 111.85(19) . . ?
C29 C27 C28 111.4(2) . . ?
C23 C27 C28 111.67(19) . . ?
C29 C27 H27 107.2 . . ?
C23 C27 H27 107.2 . . ?
C28 C27 H27 107.2 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C35 C30 C31 121.09(16) . . ?
C35 C30 N3 118.58(16) . . ?
C31 C30 N3 120.29(16) . . ?
C32 C31 C30 117.98(17) . . ?
C32 C31 C36 120.91(17) . . ?
C30 C31 C36 121.02(16) . . ?
C33 C32 C31 121.36(18) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C34 C33 C32 119.88(18) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 121.16(18) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 H34 119.4 . . ?
C34 C35 C30 118.30(17) . . ?
C34 C35 C39 119.93(17) . . ?
C30 C35 C39 121.73(17) . . ?
C31 C36 C37 113.64(18) . . ?
C31 C36 C38 110.09(16) . . ?
C37 C36 C38 109.60(19) . . ?
C31 C36 H36 107.8 . . ?
C37 C36 H36 107.8 . . ?
C38 C36 H36 107.8 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C41 C39 C35 109.96(19) . . ?
C41 C39 C40 110.2(2) . . ?
C35 C39 C40 112.7(2) . . ?
C41 C39 H39 107.9 . . ?
C35 C39 H39 107.9 . . ?
C40 C39 H39 107.9 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O C42 C43 107.5(2) . . ?
O C42 H42A 110.2 . . ?
C43 C42 H42A 110.2 . . ?
O C42 H42B 110.2 . . ?
C43 C42 H42B 110.2 . . ?
H42A C42 H42B 108.5 . . ?
C42 C43 C44 105.3(2) . . ?
C42 C43 H43A 110.7 . . ?
C44 C43 H43A 110.7 . . ?
C42 C43 H43B 110.7 . . ?
C44 C43 H43B 110.7 . . ?
H43A C43 H43B 108.8 . . ?
C43 C44 C45 103.4(2) . . ?
C43 C44 H44A 111.1 . . ?
C45 C44 H44A 111.1 . . ?
C43 C44 H44B 111.1 . . ?
C45 C44 H44B 111.1 . . ?
H44A C44 H44B 109 . . ?
O C45 C44 105.9(2) . . ?
O C45 H45A 110.6 . . ?
C44 C45 H45A 110.6 . . ?
O C45 H45B 110.6 . . ?
C44 C45 H45B 110.6 . . ?
H45A C45 H45B 108.7 . . ?
N5 C46 N4 116.22(15) . . ?
N5 C46 N3 124.75(16) . . ?
N4 C46 N3 118.97(15) . . ?
N5 C46 Ca 59.07(9) . . ?
N4 C46 Ca 57.65(9) . . ?
N3 C46 Ca 170.19(12) . . ?
N4 C47 C48 111.34(16) . . ?
N4 C47 C52 110.28(15) . . ?
C48 C47 C52 110.87(18) . . ?
N4 C47 H47 108.1 . . ?
C48 C47 H47 108.1 . . ?
C52 C47 H47 108.1 . . ?
C47 C48 C49 113.31(19) . . ?
C47 C48 H48A 108.9 . . ?
C49 C48 H48A 108.9 . . ?
C47 C48 H48B 108.9 . . ?
C49 C48 H48B 108.9 . . ?
H48A C48 H48B 107.7 . . ?
C50 C49 C48 111.1(2) . . ?
C50 C49 H49A 109.4 . . ?
C48 C49 H49A 109.4 . . ?
C50 C49 H49B 109.4 . . ?
C48 C49 H49B 109.4 . . ?
H49A C49 H49B 108 . . ?
C51 C50 C49 110.31(19) . . ?
C51 C50 H50A 109.6 . . ?
C49 C50 H50A 109.6 . . ?
C51 C50 H50B 109.6 . . ?
C49 C50 H50B 109.6 . . ?
H50A C50 H50B 108.1 . . ?
C50 C51 C52 110.42(19) . . ?
C50 C51 H51A 109.6 . . ?
C52 C51 H51A 109.6 . . ?
C50 C51 H51B 109.6 . . ?
C52 C51 H51B 109.6 . . ?
H51A C51 H51B 108.1 . . ?
C47 C52 C51 112.25(17) . . ?
C47 C52 H52A 109.2 . . ?
C51 C52 H52A 109.2 . . ?
C47 C52 H52B 109.2 . . ?
C51 C52 H52B 109.2 . . ?
H52A C52 H52B 107.9 . . ?
N5 C53 C58 112.44(19) . . ?
N5 C53 C54 108.70(18) . . ?
C58 C53 C54 108.6(2) . . ?
N5 C53 H53 109 . . ?
C58 C53 H53 109 . . ?
C54 C53 H53 109 . . ?
C55 C54 C53 111.9(3) . . ?
C55 C54 H54A 109.2 . . ?
C53 C54 H54A 109.2 . . ?
C55 C54 H54B 109.2 . . ?
C53 C54 H54B 109.2 . . ?
H54A C54 H54B 107.9 . . ?
C56 C55 C54 111.0(4) . . ?
C56 C55 H55A 109.4 . . ?
C54 C55 H55A 109.4 . . ?
C56 C55 H55B 109.4 . . ?
C54 C55 H55B 109.4 . . ?
H55A C55 H55B 108 . . ?
C57 C56 C55 113.3(3) . . ?
C57 C56 H56A 108.9 . . ?
C55 C56 H56A 108.9 . . ?
C57 C56 H56B 108.9 . . ?
C55 C56 H56B 108.9 . . ?
H56A C56 H56B 107.7 . . ?
C56 C57 C58 110.1(4) . . ?
C56 C57 H57A 109.6 . . ?
C58 C57 H57A 109.6 . . ?
C56 C57 H57B 109.6 . . ?
C58 C57 H57B 109.6 . . ?
H57A C57 H57B 108.2 . . ?
C53 C58 C57 112.4(3) . . ?
C53 C58 H58A 109.1 . . ?
C57 C58 H58A 109.1 . . ?
C53 C58 H58B 109.1 . . ?
C57 C58 H58B 109.1 . . ?
H58A C58 H58B 107.9 . . ?
C55A C54A H54C 109 . . ?
C55A C54A H54D 109 . . ?
H54C C54A H54D 107.8 . . ?
C56A C55A C54A 111.0(6) . . ?
C56A C55A H55C 109.4 . . ?
C54A C55A H55C 109.4 . . ?
C56A C55A H55D 109.4 . . ?
C54A C55A H55D 109.4 . . ?
H55C C55A H55D 108 . . ?
C55A C56A C57A 112.2(6) . . ?
C55A C56A H56C 109.2 . . ?
C57A C56A H56C 109.2 . . ?
C55A C56A H56D 109.2 . . ?
C57A C56A H56D 109.2 . . ?
H56C C56A H56D 107.9 . . ?
C56A C57A C58A 109.8(6) . . ?
C56A C57A H57C 109.7 . . ?
C58A C57A H57C 109.7 . . ?
C56A C57A H57D 109.7 . . ?
C58A C57A H57D 109.7 . . ?
H57C C57A H57D 108.2 . . ?
C57A C58A H58C 109.2 . . ?
C57A C58A H58D 109.2 . . ?
H58C C58A H58D 107.9 . . ?
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
Ca N2 2.3870(15) . ?
Ca N4 2.3879(15) . ?
Ca N1 2.3936(15) . ?
Ca O 2.4123(14) . ?
Ca N5 2.4215(15) . ?
O C42 1.428(3) . ?
O C45 1.440(3) . ?
N1 C1 1.324(3) . ?
N1 C6 1.434(2) . ?
N2 C3 1.323(2) . ?
N2 C18 1.431(2) . ?
N3 C46 1.410(2) . ?
N3 C30 1.427(2) . ?
N3 H3X 0.86(2) . ?
N4 C46 1.338(2) . ?
N4 C47 1.459(2) . ?
N5 C46 1.329(2) . ?
N5 C53 1.458(2) . ?
C1 C2 1.409(3) . ?
C1 C4 1.520(3) . ?
C2 C3 1.409(3) . ?
C2 H2 0.95 . ?
C3 C5 1.518(3) . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C11 1.409(3) . ?
C6 C7 1.410(3) . ?
C7 C8 1.394(3) . ?
C7 C12 1.523(3) . ?
C8 C9 1.377(3) . ?
C8 H8 0.95 . ?
C9 C10 1.369(3) . ?
C9 H9 0.95 . ?
C10 C11 1.394(3) . ?
C10 H10 0.95 . ?
C11 C15 1.515(3) . ?
C12 C14 1.507(5) . ?
C12 C13 1.540(4) . ?
C12 H12 1 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 C17 1.519(3) . ?
C15 C16 1.529(3) . ?
C15 H15 1 . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 C23 1.404(3) . ?
C18 C19 1.411(3) . ?
C19 C20 1.394(3) . ?
C19 C24 1.521(3) . ?
C20 C21 1.374(3) . ?
C20 H20 0.95 . ?
C21 C22 1.381(3) . ?
C21 H21 0.95 . ?
C22 C23 1.397(3) . ?
C22 H22 0.95 . ?
C23 C27 1.512(3) . ?
C24 C25 1.526(4) . ?
C24 C26 1.536(4) . ?
C24 H24 1 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 C29 1.512(3) . ?
C27 C28 1.513(4) . ?
C27 H27 1 . ?
C28 H28A 0.98 . ?
C28 H28B 0.98 . ?
C28 H28C 0.98 . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
C30 C35 1.405(3) . ?
C30 C31 1.410(3) . ?
C31 C32 1.391(3) . ?
C31 C36 1.521(3) . ?
C32 C33 1.382(3) . ?
C32 H32 0.95 . ?
C33 C34 1.381(3) . ?
C33 H33 0.95 . ?
C34 C35 1.391(3) . ?
C34 H34 0.95 . ?
C35 C39 1.522(3) . ?
C36 C37 1.527(3) . ?
C36 C38 1.532(3) . ?
C36 H36 1 . ?
C37 H37A 0.98 . ?
C37 H37B 0.98 . ?
C37 H37C 0.98 . ?
C38 H38A 0.98 . ?
C38 H38B 0.98 . ?
C38 H38C 0.98 . ?
C39 C41 1.513(4) . ?
C39 C40 1.526(3) . ?
C39 H39 1 . ?
C40 H40A 0.98 . ?
C40 H40B 0.98 . ?
C40 H40C 0.98 . ?
C41 H41A 0.98 . ?
C41 H41B 0.98 . ?
C41 H41C 0.98 . ?
C42 C43 1.478(4) . ?
C42 H42A 0.99 . ?
C42 H42B 0.99 . ?
C43 C44 1.489(4) . ?
C43 H43A 0.99 . ?
C43 H43B 0.99 . ?
C44 C45 1.497(4) . ?
C44 H44A 0.99 . ?
C44 H44B 0.99 . ?
C45 H45A 0.99 . ?
C45 H45B 0.99 . ?
C47 C48 1.512(3) . ?
C47 C52 1.515(3) . ?
C47 H47 1 . ?
C48 C49 1.532(3) . ?
C48 H48A 0.99 . ?
C48 H48B 0.99 . ?
C49 C50 1.514(4) . ?
C49 H49A 0.99 . ?
C49 H49B 0.99 . ?
C50 C51 1.507(4) . ?
C50 H50A 0.99 . ?
C50 H50B 0.99 . ?
C51 C52 1.529(3) . ?
C51 H51A 0.99 . ?
C51 H51B 0.99 . ?
C52 H52A 0.99 . ?
C52 H52B 0.99 . ?
C53 C58 1.494(4) . ?
C53 C54 1.552(4) . ?
C53 H53 1 . ?
C54 C55 1.545(5) . ?
C54 H54A 0.99 . ?
C54 H54B 0.99 . ?
C55 C56 1.504(6) . ?
C55 H55A 0.99 . ?
C55 H55B 0.99 . ?
C56 C57 1.496(6) . ?
C56 H56A 0.99 . ?
C56 H56B 0.99 . ?
C57 C58 1.532(5) . ?
C57 H57A 0.99 . ?
C57 H57B 0.99 . ?
C58 H58A 0.99 . ?
C58 H58B 0.99 . ?
C54A C55A 1.519(8) . ?
C54A H54C 0.99 . ?
C54A H54D 0.99 . ?
C55A C56A 1.475(10) . ?
C55A H55C 0.99 . ?
C55A H55D 0.99 . ?
C56A C57A 1.521(10) . ?
C56A H56C 0.99 . ?
C56A H56D 0.99 . ?
C57A C58A 1.542(9) . ?
C57A H57C 0.99 . ?
C57A H57D 0.99 . ?
C58A H58C 0.99 . ?
C58A H58D 0.99 . ?
