#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:10:55 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178598 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/09/4070917.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_4070917
loop_
_publ_author_name
'Crimmin, Mark R.'
'Barrett, Anthony G. M.'
'Hill, Michael S.'
'Hitchcock, Peter B.'
'Procopiou, Panayiotis A.'
_publ_section_title
;
 Heavier Group 2 Element Catalyzed Hydrophosphination of Carbodiimides
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              497
_journal_paper_doi               10.1021/om7011198
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C52 H73 Ca N4 O P, 0.5(C6 H14)'
_chemical_formula_sum            'C55 H80 Ca N4 O P'
_chemical_formula_weight         884.28
_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             2006-11-02T10:41:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 103.202(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2577(2)
_cell_length_b                   14.4217(3)
_cell_length_c                   28.4727(4)
_cell_measurement_reflns_used    39264
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     5300.06(16)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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      -0.163336E-1
_diffrn_orient_matrix_UB_12      -0.478155E-1
_diffrn_orient_matrix_UB_13      -0.260705E-1
_diffrn_orient_matrix_UB_21      0.715353E-1
_diffrn_orient_matrix_UB_22      0.63959E-2
_diffrn_orient_matrix_UB_23      -0.5485E-2
_diffrn_orient_matrix_UB_31      0.248664E-1
_diffrn_orient_matrix_UB_32      -0.498076E-1
_diffrn_orient_matrix_UB_33      0.243235E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0417
_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       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            52237
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.4
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_correction_T_min  0.9047
_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    1.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         10351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0449
_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)+(0.0535P)²+2.4378P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                7802
_reflns_number_total             10351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7011198-file001.cif
_cod_data_source_block           nov206
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4070917
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 0.71225(3) 0.77907(2) 0.160297(12) 0.02473(10) Uani 1 1 d . B .
P P 0.62269(4) 0.69749(4) -0.005273(17) 0.03779(14) Uani 1 1 d . . .
O O 0.71760(11) 0.66536(10) 0.22155(5) 0.0410(3) Uani 1 1 d . . .
N1 N 0.86659(11) 0.85705(10) 0.20071(5) 0.0269(3) Uani 1 1 d . . .
N2 N 0.64118(11) 0.89060(10) 0.20488(5) 0.0275(3) Uani 1 1 d . . .
N3 N 0.66161(13) 0.82202(10) 0.07703(5) 0.0329(4) Uani 1 1 d . . .
N4 N 0.65961(12) 0.66886(10) 0.09417(5) 0.0307(3) Uani 1 1 d . . .
C1 C 0.85675(13) 0.94643(13) 0.18940(6) 0.0289(4) Uani 1 1 d . B .
C2 C 0.76306(14) 0.99621(13) 0.18191(6) 0.0291(4) Uani 1 1 d . . .
H2 H 0.764 1.0541 0.1661 0.035 Uiso 1 1 calc R B .
C3 C 0.66820(13) 0.97501(12) 0.19382(6) 0.0269(4) Uani 1 1 d . B .
C4 C 0.94982(15) 1.00265(15) 0.18315(8) 0.0416(5) Uani 1 1 d . . .
H4A H 1.0135 0.974 0.2018 0.062 Uiso 1 1 calc R B .
H4B H 0.9443 1.066 0.1947 0.062 Uiso 1 1 calc R . .
H4C H 0.9517 1.0042 0.1489 0.062 Uiso 1 1 calc R . .
C5 C 0.59467(15) 1.05613(13) 0.19266(7) 0.0343(4) Uani 1 1 d . . .
H5A H 0.5387 1.0523 0.1635 0.051 Uiso 1 1 calc R B .
H5B H 0.6326 1.1144 0.1924 0.051 Uiso 1 1 calc R . .
H5C H 0.5653 1.0541 0.2213 0.051 Uiso 1 1 calc R . .
C6 C 0.96748(13) 0.81639(13) 0.21560(6) 0.0292(4) Uani 1 1 d . B .
C7 C 1.01337(14) 0.80971(14) 0.26555(7) 0.0344(4) Uani 1 1 d . . .
C8 C 1.10759(15) 0.76293(16) 0.27958(8) 0.0434(5) Uani 1 1 d . B .
H8 H 1.1396 0.7585 0.3129 0.052 Uiso 1 1 calc R . .
C9 C 1.15537(16) 0.72315(16) 0.24656(8) 0.0466(5) Uani 1 1 d . . .
H9 H 1.2192 0.6912 0.2571 0.056 Uiso 1 1 calc R B .
C10 C 1.11016(15) 0.72995(15) 0.19815(8) 0.0427(5) Uani 1 1 d . B .
H10 H 1.1432 0.702 0.1754 0.051 Uiso 1 1 calc R . .
C11 C 1.01685(14) 0.77701(14) 0.18173(7) 0.0345(4) Uani 1 1 d . . .
C12 C 0.96088(16) 0.85077(16) 0.30287(7) 0.0426(5) Uani 1 1 d . B .
H12 H 0.8846 0.8417 0.2907 0.051 Uiso 1 1 calc R . .
C13 C 0.9922(2) 0.8020(2) 0.35193(8) 0.0664(7) Uani 1 1 d . . .
H13A H 0.9863 0.7347 0.3472 0.1 Uiso 1 1 calc R B .
H13B H 0.9463 0.8221 0.3725 0.1 Uiso 1 1 calc R . .
H13C H 1.0639 0.818 0.3674 0.1 Uiso 1 1 calc R . .
C14 C 0.9797(2) 0.95433(19) 0.30950(9) 0.0648(7) Uani 1 1 d . . .
H14A H 1.0544 0.9665 0.3175 0.097 Uiso 1 1 calc R B .
H14B H 0.9494 0.9767 0.3357 0.097 Uiso 1 1 calc R . .
H14C H 0.9475 0.9867 0.2796 0.097 Uiso 1 1 calc R . .
C15 C 0.96965(16) 0.77996(16) 0.12795(7) 0.0429(5) Uani 1 1 d . B .
H15 H 0.9064 0.8199 0.1227 0.051 Uiso 1 1 calc R . .
C16 C 1.0436(2) 0.8225(2) 0.09959(9) 0.0696(8) Uani 1 1 d . . .
H16A H 1.0669 0.8834 0.1132 0.104 Uiso 1 1 calc R B .
H16B H 1.0074 0.8297 0.0657 0.104 Uiso 1 1 calc R . .
H16C H 1.1036 0.7818 0.1018 0.104 Uiso 1 1 calc R . .
C17 C 0.9357(2) 0.6831(2) 0.10956(9) 0.0694(8) Uani 1 1 d . . .
H17A H 0.9966 0.6431 0.1131 0.104 Uiso 1 1 calc R B .
H17B H 0.8997 0.6865 0.0755 0.104 Uiso 1 1 calc R . .
H17C H 0.8887 0.6575 0.1283 0.104 Uiso 1 1 calc R . .
C18 C 0.55545(14) 0.88068(12) 0.22727(6) 0.0283(4) Uani 1 1 d . B .
C19 C 0.57173(15) 0.89482(13) 0.27757(7) 0.0332(4) Uani 1 1 d . . .
C20 C 0.48829(16) 0.88326(14) 0.29915(7) 0.0405(5) Uani 1 1 d . B .
H20 H 0.4978 0.8941 0.3328 0.049 Uiso 1 1 calc R . .
C21 C 0.39230(17) 0.85643(16) 0.27285(8) 0.0473(5) Uani 1 1 d . . .
H21 H 0.3362 0.8495 0.2882 0.057 Uiso 1 1 calc R B .
C22 C 0.37784(16) 0.83963(15) 0.22396(8) 0.0423(5) Uani 1 1 d . B .
H22 H 0.312 0.8194 0.2061 0.051 Uiso 1 1 calc R . .
C23 C 0.45847(14) 0.85190(13) 0.20040(7) 0.0329(4) Uani 1 1 d . . .
C24 C 0.67735(16) 0.92102(15) 0.30837(7) 0.0408(5) Uani 1 1 d . B .
H24 H 0.7297 0.9118 0.2885 0.049 Uiso 1 1 calc R . .
C25 C 0.7087(2) 0.8610(2) 0.35299(10) 0.0778(9) Uani 1 1 d . . .
H25A H 0.6605 0.8712 0.374 0.117 Uiso 1 1 calc R B .
H25B H 0.7791 0.8775 0.3704 0.117 Uiso 1 1 calc R . .
H25C H 0.7068 0.7956 0.3435 0.117 Uiso 1 1 calc R . .
C26 C 0.6821(2) 1.02196(19) 0.32413(10) 0.0679(7) Uani 1 1 d . . .
H26A H 0.6657 1.062 0.2956 0.102 Uiso 1 1 calc R B .
H26B H 0.752 1.0362 0.343 0.102 Uiso 1 1 calc R . .
H26C H 0.6319 1.0327 0.344 0.102 Uiso 1 1 calc R . .
C27 C 0.43702(14) 0.83458(14) 0.14625(7) 0.0345(4) Uani 1 1 d . B .
H27 H 0.5033 0.8441 0.1357 0.041 Uiso 1 1 calc R . .
C28 C 0.35755(17) 0.90312(16) 0.11858(8) 0.0463(5) Uani 1 1 d . . .
H28A H 0.2924 0.8965 0.129 0.069 Uiso 1 1 calc R B .
H28B H 0.3454 0.8904 0.0839 0.069 Uiso 1 1 calc R . .
H28C H 0.3838 0.9665 0.125 0.069 Uiso 1 1 calc R . .
C29 C 0.40113(19) 0.73499(16) 0.13362(9) 0.0517(6) Uani 1 1 d . . .
H29A H 0.4542 0.6917 0.1504 0.078 Uiso 1 1 calc R B .
H29B H 0.39 0.7257 0.0987 0.078 Uiso 1 1 calc R . .
H29C H 0.3362 0.7238 0.1436 0.078 Uiso 1 1 calc R . .
C30 C 0.49532(17) 0.74706(14) -0.03088(7) 0.0379(5) Uani 1 1 d . . .
C31 C 0.42755(17) 0.77251(14) -0.00232(7) 0.0410(5) Uani 1 1 d . . .
H31 H 0.4519 0.7751 0.0317 0.049 Uiso 1 1 calc R . .
C32 C 0.32516(18) 0.79406(16) -0.02280(8) 0.0494(6) Uani 1 1 d . . .
H32 H 0.2798 0.8109 -0.0028 0.059 Uiso 1 1 calc R . .
C33 C 0.28854(19) 0.79116(16) -0.07253(8) 0.0518(6) Uani 1 1 d . . .
H33 H 0.2183 0.806 -0.0866 0.062 Uiso 1 1 calc R . .
C34 C 0.35471(19) 0.76664(16) -0.10115(8) 0.0512(6) Uani 1 1 d . . .
H34 H 0.3301 0.7652 -0.1352 0.061 Uiso 1 1 calc R . .
C35 C 0.45655(19) 0.74403(15) -0.08098(7) 0.0461(5) Uani 1 1 d . . .
H35 H 0.5009 0.7262 -0.1013 0.055 Uiso 1 1 calc R . .
C36 C 0.71566(17) 0.76216(14) -0.03139(7) 0.0393(5) Uani 1 1 d . . .
C37 C 0.69769(18) 0.84097(15) -0.06066(7) 0.0429(5) Uani 1 1 d . . .
H37 H 0.6302 0.8671 -0.0691 0.051 Uiso 1 1 calc R . .
C38 C 0.77753(19) 0.88131(17) -0.07738(8) 0.0507(6) Uani 1 1 d . . .
H38 H 0.7643 0.9352 -0.097 0.061 Uiso 1 1 calc R . .
C39 C 0.8762(2) 0.84434(19) -0.06586(8) 0.0573(6) Uani 1 1 d . . .
H39 H 0.9308 0.8732 -0.077 0.069 Uiso 1 1 calc R . .
C40 C 0.8948(2) 0.76519(18) -0.03804(8) 0.0561(6) Uani 1 1 d . . .
H40 H 0.9623 0.739 -0.0301 0.067 Uiso 1 1 calc R . .
C41 C 0.81494(18) 0.72392(16) -0.02169(7) 0.0476(6) Uani 1 1 d . . .
H41 H 0.8281 0.6683 -0.0034 0.057 Uiso 1 1 calc R . .
C42 C 0.65010(14) 0.73538(13) 0.06104(6) 0.0303(4) Uani 1 1 d . B .
C43 C 0.65029(15) 0.90285(13) 0.04540(6) 0.0324(4) Uani 1 1 d . B .
H43 H 0.6196 0.8825 0.0116 0.039 Uiso 1 1 calc R . .
C44 C 0.75577(16) 0.94717(14) 0.04713(7) 0.0408(5) Uani 1 1 d . . .
H44A H 0.7858 0.9688 0.08 0.061 Uiso 1 1 calc R B .
H44B H 0.7472 0.9999 0.0248 0.061 Uiso 1 1 calc R . .
H44C H 0.802 0.9013 0.0377 0.061 Uiso 1 1 calc R . .
C45 C 0.57756(16) 0.97269(13) 0.06049(7) 0.0356(4) Uani 1 1 d . . .
H45A H 0.5087 0.945 0.0567 0.053 Uiso 1 1 calc R B .
H45B H 0.5727 1.0281 0.0402 0.053 Uiso 1 1 calc R . .
H45C H 0.6045 0.9899 0.0943 0.053 Uiso 1 1 calc R . .
C46 C 0.64585(15) 0.57030(12) 0.08148(7) 0.0332(4) Uani 1 1 d . B .
H46 H 0.6733 0.5587 0.0521 0.04 Uiso 1 1 calc R . .
C47 C 0.7075(2) 0.51202(15) 0.12272(8) 0.0548(6) Uani 1 1 d . . .
H47A H 0.781 0.5287 0.1286 0.082 Uiso 1 1 calc R B .
H47B H 0.699 0.4462 0.1142 0.082 Uiso 1 1 calc R . .
H47C H 0.6822 0.5236 0.1519 0.082 Uiso 1 1 calc R . .
C48 C 0.53240(17) 0.54231(15) 0.07078(9) 0.0534(6) Uani 1 1 d . . .
H48A H 0.5046 0.5532 0.0994 0.08 Uiso 1 1 calc R B .
H48B H 0.526 0.4764 0.0623 0.08 Uiso 1 1 calc R . .
H48C H 0.4934 0.5793 0.0438 0.08 Uiso 1 1 calc R . .
C49 C 0.62976(16) 0.63436(17) 0.23928(9) 0.0503(6) Uani 1 1 d . B .
H49A H 0.5907 0.5863 0.2177 0.06 Uiso 1 1 calc R A 1
H49B H 0.5826 0.6868 0.241 0.06 Uiso 1 1 calc R A 1
C50 C 0.67269(18) 0.5954(2) 0.28856(9) 0.0623(7) Uani 0.512(10) 1 d P B 1
H50A H 0.6521 0.5296 0.29 0.075 Uiso 0.512(10) 1 calc PR B 1
H50B H 0.6465 0.6307 0.3131 0.075 Uiso 0.512(10) 1 calc PR B 1
C51 C 0.7895(3) 0.6035(5) 0.29768(19) 0.0484(16) Uiso 0.512(10) 1 d P B 1
H51A H 0.8152 0.656 0.3196 0.058 Uiso 0.512(10) 1 calc PR B 1
H51B H 0.8237 0.5457 0.3119 0.058 Uiso 0.512(10) 1 calc PR B 1
C52 C 0.80841(17) 0.62001(19) 0.24906(8) 0.0560(6) Uani 0.512(10) 1 d P B 1
H52A H 0.8702 0.6597 0.2512 0.067 Uiso 0.512(10) 1 calc PR B 1
H52B H 0.82 0.5605 0.2337 0.067 Uiso 0.512(10) 1 calc PR B 1
C50A C 0.67269(18) 0.5954(2) 0.28856(9) 0.0623(7) Uani 0.488(10) 1 d P B 2
H50C H 0.6286 0.5448 0.2962 0.075 Uiso 0.488(10) 1 calc PR B 2
H50D H 0.6805 0.6439 0.3137 0.075 Uiso 0.488(10) 1 calc PR B 2
C51A C 0.7791(4) 0.5585(5) 0.28333(19) 0.0440(16) Uiso 0.488(10) 1 d P B 2
H51C H 0.8303 0.5606 0.3146 0.053 Uiso 0.488(10) 1 calc PR B 2
H51D H 0.7733 0.4939 0.2712 0.053 Uiso 0.488(10) 1 calc PR B 2
C52A C 0.80841(17) 0.62001(19) 0.24906(8) 0.0560(6) Uani 0.488(10) 1 d P B 2
H52C H 0.8581 0.6668 0.2662 0.067 Uiso 0.488(10) 1 calc PR B 2
H52D H 0.8424 0.5845 0.2272 0.067 Uiso 0.488(10) 1 calc PR B 2
C1S C 0.94950(19) 0.48398(19) -0.01558(9) 0.0611(7) Uani 1 1 d . . 2
H1S1 H 0.9634 0.4312 -0.0355 0.073 Uiso 1 1 calc R . 2
H1S2 H 0.9201 0.5349 -0.0378 0.073 Uiso 1 1 calc R . 2
C2S C 0.8690(2) 0.45410(19) 0.01153(11) 0.0673(7) Uani 1 1 d . C 2
H2S1 H 0.8958 0.4 0.032 0.081 Uiso 1 1 calc R C 2
H2S2 H 0.8581 0.5052 0.0331 0.081 Uiso 1 1 calc R C 2
C3S C 0.7661(2) 0.4287(2) -0.02110(13) 0.0915(10) Uani 1 1 d . C 2
H3S1 H 0.7175 0.4104 -0.0015 0.137 Uiso 1 1 calc R C 2
H3S2 H 0.7757 0.3769 -0.0419 0.137 Uiso 1 1 calc R C 2
H3S3 H 0.7382 0.4822 -0.0411 0.137 Uiso 1 1 calc R C 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
N2 Ca O 91.38(5) .
N2 Ca N1 79.88(5) .
O Ca N1 95.31(5) .
N2 Ca N3 107.37(5) .
O Ca N3 149.07(5) .
N1 Ca N3 111.78(5) .
N2 Ca N4 140.84(5) .
O Ca N4 94.13(5) .
N1 Ca N4 137.82(5) .
N3 Ca N4 55.83(5) .
C30 P C36 106.57(9) .
C30 P C42 103.39(9) .
C36 P C42 105.09(9) .
C52 O C49 108.16(15) .
C52 O Ca 126.43(12) .
C49 O Ca 125.31(12) .
C1 N1 C6 120.16(15) .
C1 N1 Ca 108.33(11) .
C6 N1 Ca 126.09(11) .
C3 N2 C18 118.82(15) .
C3 N2 Ca 109.46(11) .
C18 N2 Ca 128.53(11) .
C42 N3 C43 123.56(15) .
C42 N3 Ca 94.62(11) .
C43 N3 Ca 141.62(11) .
C42 N4 C46 122.50(15) .
C42 N4 Ca 92.38(11) .
C46 N4 Ca 144.89(11) .
N1 C1 C2 124.48(16) .
N1 C1 C4 120.57(16) .
C2 C1 C4 114.94(17) .
C1 C2 C3 131.14(17) .
C1 C2 H2 114.4 .
C3 C2 H2 114.4 .
N2 C3 C2 124.08(16) .
N2 C3 C5 120.35(16) .
C2 C3 C5 115.57(16) .
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 120.10(17) .
C11 C6 N1 120.85(16) .
C7 C6 N1 118.85(16) .
C8 C7 C6 118.13(18) .
C8 C7 C12 120.79(17) .
C6 C7 C12 121.07(17) .
C9 C8 C7 121.91(19) .
C9 C8 H8 119 .
C7 C8 H8 119 .
C8 C9 C10 119.52(19) .
C8 C9 H9 120.2 .
C10 C9 H9 120.2 .
C9 C10 C11 121.4(2) .
C9 C10 H10 119.3 .
C11 C10 H10 119.3 .
C10 C11 C6 118.94(18) .
C10 C11 C15 118.81(18) .
C6 C11 C15 122.19(17) .
C7 C12 C14 112.47(18) .
C7 C12 C13 112.75(19) .
C14 C12 C13 109.6(2) .
C7 C12 H12 107.2 .
C14 C12 H12 107.2 .
C13 C12 H12 107.2 .
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 110.06(19) .
C11 C15 C16 112.15(18) .
C17 C15 C16 111.1(2) .
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 120.32(16) .
C23 C18 N2 120.63(16) .
C19 C18 N2 118.93(16) .
C20 C19 C18 118.49(18) .
C20 C19 C24 119.66(17) .
C18 C19 C24 121.85(16) .
C21 C20 C19 121.49(19) .
C21 C20 H20 119.3 .
C19 C20 H20 119.3 .
C20 C21 C22 119.70(19) .
C20 C21 H21 120.2 .
C22 C21 H21 120.2 .
C21 C22 C23 121.06(19) .
C21 C22 H22 119.5 .
C23 C22 H22 119.5 .
C22 C23 C18 118.88(18) .
C22 C23 C27 118.61(17) .
C18 C23 C27 122.51(16) .
C25 C24 C26 108.3(2) .
C25 C24 C19 112.47(19) .
C26 C24 C19 112.28(18) .
C25 C24 H24 107.9 .
C26 C24 H24 107.9 .
C19 C24 H24 107.9 .
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 .
C23 C27 C28 111.32(16) .
C23 C27 C29 111.60(17) .
C28 C27 C29 110.23(17) .
C23 C27 H27 107.8 .
C28 C27 H27 107.8 .
C29 C27 H27 107.8 .
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 .
C31 C30 C35 117.8(2) .
C31 C30 P 122.12(15) .
C35 C30 P 119.00(17) .
C32 C31 C30 120.98(19) .
C32 C31 H31 119.5 .
C30 C31 H31 119.5 .
C31 C32 C33 120.2(2) .
C31 C32 H32 119.9 .
C33 C32 H32 119.9 .
C34 C33 C32 119.4(2) .
C34 C33 H33 120.3 .
C32 C33 H33 120.3 .
C33 C34 C35 120.7(2) .
C33 C34 H34 119.6 .
C35 C34 H34 119.6 .
C34 C35 C30 120.8(2) .
C34 C35 H35 119.6 .
C30 C35 H35 119.6 .
C41 C36 C37 117.7(2) .
C41 C36 P 114.19(16) .
C37 C36 P 128.09(17) .
C38 C37 C36 120.5(2) .
C38 C37 H37 119.8 .
C36 C37 H37 119.8 .
C39 C38 C37 120.9(2) .
C39 C38 H38 119.6 .
C37 C38 H38 119.6 .
C40 C39 C38 119.4(2) .
C40 C39 H39 120.3 .
C38 C39 H39 120.3 .
C39 C40 C41 119.9(2) .
C39 C40 H40 120 .
C41 C40 H40 120 .
C40 C41 C36 121.5(2) .
C40 C41 H41 119.3 .
C36 C41 H41 119.3 .
N3 C42 N4 116.79(16) .
N3 C42 P 125.95(14) .
N4 C42 P 117.26(13) .
N3 C43 C45 109.68(15) .
N3 C43 C44 110.47(16) .
C45 C43 C44 110.37(16) .
N3 C43 H43 108.8 .
C45 C43 H43 108.8 .
C44 C43 H43 108.8 .
C43 C44 H44A 109.5 .
C43 C44 H44B 109.5 .
H44A C44 H44B 109.5 .
C43 C44 H44C 109.5 .
H44A C44 H44C 109.5 .
H44B C44 H44C 109.5 .
C43 C45 H45A 109.5 .
C43 C45 H45B 109.5 .
H45A C45 H45B 109.5 .
C43 C45 H45C 109.5 .
H45A C45 H45C 109.5 .
H45B C45 H45C 109.5 .
N4 C46 C48 111.61(16) .
N4 C46 C47 109.29(15) .
C48 C46 C47 109.91(18) .
N4 C46 H46 108.7 .
C48 C46 H46 108.7 .
C47 C46 H46 108.7 .
C46 C47 H47A 109.5 .
C46 C47 H47B 109.5 .
H47A C47 H47B 109.5 .
C46 C47 H47C 109.5 .
H47A C47 H47C 109.5 .
H47B C47 H47C 109.5 .
C46 C48 H48A 109.5 .
C46 C48 H48B 109.5 .
H48A C48 H48B 109.5 .
C46 C48 H48C 109.5 .
H48A C48 H48C 109.5 .
H48B C48 H48C 109.5 .
O C49 C50 106.24(17) .
O C49 H49A 110.5 .
C50 C49 H49A 110.5 .
O C49 H49B 110.5 .
C50 C49 H49B 110.5 .
H49A C49 H49B 108.7 .
C49 C50 C51 106.6(2) .
C49 C50 H50A 110.4 .
C51 C50 H50A 110.4 .
C49 C50 H50B 110.4 .
C51 C50 H50B 110.4 .
H50A C50 H50B 108.6 .
C52 C51 C50 103.7(3) .
C52 C51 H51A 111 .
C50 C51 H51A 111 .
C52 C51 H51B 111 .
C50 C51 H51B 111 .
H51A C51 H51B 109 .
O C52 C51 106.4(2) .
O C52 H52A 110.4 .
C51 C52 H52A 110.4 .
O C52 H52B 110.4 .
C51 C52 H52B 110.4 .
H52A C52 H52B 108.6 .
H51C C51A H51D 108.9 .
C1S C1S C2S 115.1(3) 3_765
C1S C1S H1S1 108.5 3_765
C2S C1S H1S1 108.5 .
C1S C1S H1S2 108.5 3_765
C2S C1S H1S2 108.5 .
H1S1 C1S H1S2 107.5 .
C3S C2S C1S 113.5(3) .
C3S C2S H2S1 108.9 .
C1S C2S H2S1 108.9 .
C3S C2S H2S2 108.9 .
C1S C2S H2S2 108.9 .
H2S1 C2S H2S2 107.7 .
C2S C3S H3S1 109.5 .
C2S C3S H3S2 109.5 .
H3S1 C3S H3S2 109.5 .
C2S C3S H3S3 109.5 .
H3S1 C3S H3S3 109.5 .
H3S2 C3S H3S3 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca N2 2.3733(15) .
Ca O 2.3832(13) .
Ca N1 2.3876(14) .
Ca N3 2.3934(15) .
Ca N4 2.4410(15) .
P C30 1.825(2) .
P C36 1.833(2) .
P C42 1.9188(18) .
O C52 1.435(3) .
O C49 1.442(2) .
N1 C1 1.328(2) .
N1 C6 1.433(2) .
N2 C3 1.327(2) .
N2 C18 1.432(2) .
N3 C42 1.327(2) .
N3 C43 1.460(2) .
N4 C42 1.331(2) .
N4 C46 1.468(2) .
C1 C2 1.408(3) .
C1 C4 1.520(2) .
C2 C3 1.409(2) .
C2 H2 0.95 .
C3 C5 1.518(2) .
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 1.403(3) .
C6 C7 1.417(3) .
C7 C8 1.395(3) .
C7 C12 1.517(3) .
C8 C9 1.373(3) .
C8 H8 0.95 .
C9 C10 1.375(3) .
C9 H9 0.95 .
C10 C11 1.395(3) .
C10 H10 0.95 .
C11 C15 1.517(3) .
C12 C14 1.519(3) .
C12 C13 1.534(3) .
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 1.523(3) .
C15 C16 1.533(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 1.401(3) .
C18 C19 1.414(3) .
C19 C20 1.393(3) .
C19 C24 1.520(3) .
C20 C21 1.376(3) .
C20 H20 0.95 .
C21 C22 1.383(3) .
C21 H21 0.95 .
C22 C23 1.397(3) .
C22 H22 0.95 .
C23 C27 1.523(3) .
C24 C25 1.515(3) .
C24 C26 1.520(3) .
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 C28 1.526(3) .
C27 C29 1.530(3) .
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 C31 1.392(3) .
C30 C35 1.402(3) .
C31 C32 1.385(3) .
C31 H31 0.95 .
C32 C33 1.388(3) .
C32 H32 0.95 .
C33 C34 1.373(3) .
C33 H33 0.95 .
C34 C35 1.380(3) .
C34 H34 0.95 .
C35 H35 0.95 .
C36 C41 1.395(3) .
C36 C37 1.397(3) .
C37 C38 1.384(3) .
C37 H37 0.95 .
C38 C39 1.380(3) .
C38 H38 0.95 .
C39 C40 1.379(3) .
C39 H39 0.95 .
C40 C41 1.384(3) .
C40 H40 0.95 .
C41 H41 0.95 .
C43 C45 1.523(3) .
C43 C44 1.528(3) .
C43 H43 1 .
C44 H44A 0.98 .
C44 H44B 0.98 .
C44 H44C 0.98 .
C45 H45A 0.98 .
C45 H45B 0.98 .
C45 H45C 0.98 .
C46 C48 1.520(3) .
C46 C47 1.521(3) .
C46 H46 1 .
C47 H47A 0.98 .
C47 H47B 0.98 .
C47 H47C 0.98 .
C48 H48A 0.98 .
C48 H48B 0.98 .
C48 H48C 0.98 .
C49 C50 1.498(3) .
C49 H49A 0.99 .
C49 H49B 0.99 .
C50 C51 1.515(5) .
C50 H50A 0.99 .
C50 H50B 0.99 .
C51 C52 1.481(5) .
C51 H51A 0.99 .
C51 H51B 0.99 .
C52 H52A 0.99 .
C52 H52B 0.99 .
C51A H51C 0.99 .
C51A H51D 0.99 .
C1S C1S 1.500(5) 3_765
C1S C2S 1.516(4) .
C1S H1S1 0.99 .
C1S H1S2 0.99 .
C2S C3S 1.510(4) .
C2S H2S1 0.99 .
C2S H2S2 0.99 .
C3S H3S1 0.98 .
C3S H3S2 0.98 .
C3S H3S3 0.98 .
