# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global #============================================================================== # SUBMISSION DETAILS # ================== _publ_contact_author_name 'Professor W. Levason' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email wxl@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3792' _publ_contact_letter ; 9th Jan 2006 Dear Sirs, This file contains supplementary crystallographic data in CIF format for four compounds as part of a manuscript submitted to New J. Chem. Yours faihfully William Levason ; _journal_coden_Cambridge 440 _publ_requested_journal 'New J. Chem.' _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Synthesis, spectroscopic studies and structural systematics of phosphine oxide complexes with Group II (beryllium-barium) metal nitrates ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # Note order: Family_name, first name(s) or initials (or mixture). loop_ _publ_author_name _publ_author_address 'Davis Martin F.' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Levason, William' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Ratnani, Raju' ; Department of Pure and Applied Chemistry M.D.S. University Ajmer 305009 India ; 'Reid, Gillian' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Webster, Michael' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; #============================================================================ # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique (to this file) identifier. #============================================================================ # 05mfd037 data_05mfd037 _database_code_depnum_ccdc_archive 'CCDC 298677' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2005-12-16 _chemical_name_systematic ; Bis(nitrato-O)bis(triphenylphosphine oxide-O)beryllium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Be N2 O8 P2' _chemical_formula_sum 'C36 H30 Be N2 O8 P2' _chemical_formula_structural 'Be (N O3)2 (C18 H15 O P)2' _chemical_formula_weight 689.57 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.272(3) _cell_length_b 9.579(2) _cell_length_c 34.807(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.868(10) _cell_angle_gamma 90.00 _cell_volume 3424.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 6617 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8406 # shelxl 0.9821 _exptl_absorpt_correction_T_max 1.0000 # 0.9856 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31143 _diffrn_reflns_av_R_equivalents 0.1131 _diffrn_reflns_av_sigmaI/netI 0.1437 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5996 _reflns_number_gt 2538 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+1.1698P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5996 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2107 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1523 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Be1 Be 0.2557(5) 0.2172(6) 0.87023(16) 0.0488(15) Uani 1 1 d . . . N1 N 0.2069(4) 0.3465(5) 0.93351(14) 0.0659(11) Uani 1 1 d . . . N2 N 0.0946(5) 0.2509(4) 0.81352(13) 0.0688(11) Uani 1 1 d . . . O1 O 0.1820(3) 0.3334(3) 0.89701(10) 0.0662(9) Uani 1 1 d . . . O2 O 0.2741(3) 0.2572(4) 0.94920(9) 0.0870(11) Uani 1 1 d . . . O3 O 0.1607(4) 0.4464(4) 0.94996(10) 0.0984(13) Uani 1 1 d . . . O4 O 0.2148(3) 0.2560(3) 0.82553(8) 0.0648(8) Uani 1 1 d . . . O5 O 0.0701(4) 0.2862(4) 0.78083(11) 0.1009(13) Uani 1 1 d . . . O6 O 0.0109(3) 0.2120(4) 0.83574(11) 0.0987(12) Uani 1 1 d . . . O7 O 0.2267(3) 0.0592(3) 0.87858(8) 0.0661(9) Uani 1 1 d . . . O8 O 0.4092(2) 0.2505(3) 0.87226(7) 0.0623(8) Uani 1 1 d . . . P1 P 0.19909(11) -0.08640(13) 0.89112(3) 0.0588(4) Uani 1 1 d . . . P2 P 0.54850(11) 0.24222(12) 0.86064(3) 0.0522(3) Uani 1 1 d . . . C1 C 0.0731(4) -0.0893(5) 0.92552(12) 0.0517(11) Uani 1 1 d . . . C2 C -0.0117(4) 0.0223(5) 0.92778(12) 0.0599(12) Uani 1 1 d . . . H2 H -0.0014 0.0991 0.9118 0.072 Uiso 1 1 calc R . . C3 C -0.1120(5) 0.0197(6) 0.95391(15) 0.0721(14) Uani 1 1 d . . . H3 H -0.1683 0.0954 0.9555 0.087 Uiso 1 1 calc R . . C4 C -0.1290(4) -0.0924(7) 0.97720(14) 0.0735(14) Uani 1 1 d . . . H4 H -0.1971 -0.0931 0.9945 0.088 Uiso 1 1 calc R . . C5 C -0.0455(5) -0.2058(5) 0.97529(13) 0.0726(14) Uani 1 1 d . . . H5 H -0.0575 -0.2828 0.9911 0.087 Uiso 1 1 calc R . . C6 C 0.0560(4) -0.2032(5) 0.94956(13) 0.0682(13) Uani 1 1 d . . . H6 H 0.1132 -0.2784 0.9484 0.082 Uiso 1 1 calc R . . C7 C 0.1503(4) -0.1920(5) 0.85107(13) 0.0636(13) Uani 1 1 d . . . C8 C 0.0825(6) -0.3141(6) 0.85607(17) 0.108(2) Uani 1 1 d . . . H8 H 0.0596 -0.3416 0.8807 0.129 Uiso 1 1 calc R . . C9 C 0.0479(7) -0.3966(7) 0.8249(2) 0.124(2) Uani 1 1 d . . . H9 H 0.0004 -0.4780 0.8287 0.149 Uiso 1 1 calc R . . C10 C 0.0828(8) -0.3593(8) 0.7891(2) 0.119(2) Uani 1 1 d . . . H10 H 0.0594 -0.4152 0.7682 0.143 Uiso 1 1 calc R . . C11 C 0.1519(6) -0.2407(8) 0.78339(17) 0.1044(19) Uani 1 1 d . . . H11 H 0.1778 -0.2166 0.7588 0.125 Uiso 1 1 calc R . . C12 C 0.1842(5) -0.1547(6) 0.81449(17) 0.0875(16) Uani 1 1 d . . . H12 H 0.2288 -0.0717 0.8104 0.105 Uiso 1 1 calc R . . C13 C 0.3401(4) -0.1622(5) 0.91309(13) 0.0605(13) Uani 1 1 d . . . C14 C 0.3789(6) -0.2951(6) 0.90649(16) 0.1025(19) Uani 1 1 d . . . H14 H 0.3321 -0.3511 0.8894 0.123 Uiso 1 1 calc R . . C15 C 0.4885(8) -0.3478(8) 0.9253(2) 0.134(3) Uani 1 1 d . . . H15 H 0.5161 -0.4384 0.9202 0.161 Uiso 1 1 calc R . . C16 C 0.5558(6) -0.2679(9) 0.9510(2) 0.124(2) Uani 1 1 d . . . H16 H 0.6288 -0.3041 0.9635 0.149 Uiso 1 1 calc R . . C17 C 0.5171(6) -0.1367(8) 0.95825(19) 0.118(2) Uani 1 1 d . . . H17 H 0.5628 -0.0818 0.9759 0.142 Uiso 1 1 calc R . . C18 C 0.4086(5) -0.0842(6) 0.93926(17) 0.0886(16) Uani 1 1 d . . . H18 H 0.3816 0.0065 0.9444 0.106 Uiso 1 1 calc R . . C19 C 0.5975(4) 0.0690(5) 0.85013(12) 0.0535(11) Uani 1 1 d . . . C20 C 0.5260(5) -0.0062(6) 0.82422(15) 0.0795(15) Uani 1 1 d . . . H20 H 0.4540 0.0354 0.8124 0.095 Uiso 1 1 calc R . . C21 C 0.5568(6) -0.1420(7) 0.81492(16) 0.0937(17) Uani 1 1 d . . . H21 H 0.5065 -0.1908 0.7970 0.112 Uiso 1 1 calc R . . C22 C 0.6599(7) -0.2030(6) 0.83197(19) 0.105(2) Uani 1 1 d . . . H22 H 0.6807 -0.2952 0.8263 0.126 Uiso 1 1 calc R . . C23 C 0.7333(7) -0.1299(8) 0.8573(2) 0.157(3) Uani 1 1 d . . . H23 H 0.8059 -0.1713 0.8688 0.188 Uiso 1 1 calc R . . C24 C 0.7013(6) 0.0063(6) 0.86636(18) 0.123(2) Uani 1 1 d . . . H24 H 0.7527 0.0554 0.8840 0.148 Uiso 1 1 calc R . . C25 C 0.6498(4) 0.3065(4) 0.89863(12) 0.0502(11) Uani 1 1 d . . . C26 C 0.6062(4) 0.3008(4) 0.93615(14) 0.0654(13) Uani 1 1 d . . . H26 H 0.5258 0.2606 0.9412 0.079 Uiso 1 1 calc R . . C27 C 0.6810(6) 0.3542(5) 0.96626(13) 0.0753(14) Uani 1 1 d . . . H27 H 0.6506 0.3497 0.9913 0.090 Uiso 1 1 calc R . . C28 C 0.7979(6) 0.4129(5) 0.95927(18) 0.0822(15) Uani 1 1 d . . . H28 H 0.8470 0.4503 0.9794 0.099 Uiso 1 1 calc R . . C29 C 0.8445(5) 0.4174(6) 0.92263(19) 0.0888(16) Uani 1 1 d . . . H29 H 0.9262 0.4553 0.9180 0.107 Uiso 1 1 calc R . . C30 C 0.7701(5) 0.3656(5) 0.89266(14) 0.0743(14) Uani 1 1 d . . . H30 H 0.8017 0.3707 0.8678 0.089 Uiso 1 1 calc R . . C31 C 0.5748(5) 0.3430(5) 0.81865(12) 0.0575(12) Uani 1 1 d . . . C32 C 0.6861(5) 0.3283(5) 0.79745(15) 0.0839(16) Uani 1 1 d . . . H32 H 0.7491 0.2638 0.8049 0.101 Uiso 1 1 calc R . . C33 C 0.7044(7) 0.4095(8) 0.76503(19) 0.108(2) Uani 1 1 d . . . H33 H 0.7805 0.4011 0.7511 0.130 Uiso 1 1 calc R . . C34 C 0.6099(9) 0.5021(8) 0.75357(18) 0.113(2) Uani 1 1 d . . . H34 H 0.6217 0.5550 0.7315 0.136 Uiso 1 1 calc R . . C35 C 0.4993(7) 0.5178(5) 0.77400(19) 0.0953(18) Uani 1 1 d . . . H35 H 0.4354 0.5805 0.7659 0.114 Uiso 1 1 calc R . . C36 C 0.4829(5) 0.4397(5) 0.80690(14) 0.0676(13) Uani 1 1 d . . . H36 H 0.4086 0.4525 0.8214 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Be1 0.049(4) 0.046(4) 0.051(4) 0.003(3) 0.003(3) 0.003(3) N1 0.060(3) 0.074(4) 0.064(3) 0.002(3) 0.007(2) -0.004(2) N2 0.080(4) 0.062(3) 0.064(3) -0.008(3) -0.006(3) 0.004(3) O1 0.069(2) 0.069(2) 0.061(2) -0.0024(18) -0.0006(17) 0.0176(16) O2 0.091(3) 0.109(3) 0.061(2) 0.014(2) 0.0069(19) 0.018(2) O3 0.112(3) 0.088(3) 0.095(3) -0.039(2) 0.012(2) 0.011(2) O4 0.056(2) 0.074(2) 0.063(2) 0.0098(16) -0.0074(16) -0.0013(17) O5 0.136(3) 0.107(3) 0.059(2) -0.003(2) -0.037(2) 0.009(2) O6 0.064(2) 0.134(3) 0.098(3) 0.004(2) -0.003(2) -0.001(2) O7 0.071(2) 0.042(2) 0.085(2) 0.0134(16) 0.0075(16) -0.0050(15) O8 0.0440(18) 0.081(2) 0.0617(19) 0.0032(16) 0.0043(14) -0.0052(15) P1 0.0610(8) 0.0483(8) 0.0672(9) 0.0040(7) 0.0065(6) 0.0051(7) P2 0.0492(7) 0.0554(8) 0.0520(7) 0.0019(6) 0.0012(5) -0.0015(6) C1 0.059(3) 0.039(3) 0.057(3) 0.001(2) 0.002(2) -0.001(2) C2 0.057(3) 0.061(3) 0.061(3) -0.001(2) 0.002(3) 0.000(3) C3 0.058(3) 0.082(4) 0.076(4) -0.004(3) -0.002(3) 0.013(3) C4 0.056(3) 0.101(4) 0.064(4) -0.004(3) 0.007(3) -0.005(3) C5 0.082(4) 0.069(4) 0.067(3) 0.007(3) 0.004(3) -0.009(3) C6 0.069(3) 0.061(3) 0.075(3) 0.002(3) 0.011(3) 0.006(3) C7 0.076(3) 0.054(3) 0.060(4) 0.002(3) 0.006(3) 0.005(3) C8 0.166(6) 0.077(4) 0.082(4) -0.020(4) 0.027(4) -0.026(4) C9 0.183(7) 0.085(5) 0.105(6) -0.036(5) 0.020(5) -0.029(4) C10 0.174(7) 0.093(6) 0.091(6) -0.023(5) -0.009(5) 0.008(5) C11 0.136(5) 0.112(6) 0.065(4) -0.001(4) -0.004(4) 0.012(5) C12 0.107(5) 0.088(4) 0.067(4) 0.013(4) 0.000(3) 0.006(3) C13 0.061(3) 0.050(3) 0.071(4) 0.009(3) 0.012(3) 0.014(3) C14 0.109(5) 0.089(5) 0.109(5) -0.008(4) -0.018(4) 0.048(4) C15 0.157(7) 0.092(6) 0.153(7) -0.016(5) -0.013(5) 0.070(5) C16 0.096(5) 0.126(7) 0.151(7) 0.007(5) -0.007(5) 0.038(5) C17 0.076(5) 0.114(6) 0.164(6) -0.006(5) -0.029(4) 0.013(4) C18 0.062(4) 0.075(4) 0.128(5) 0.000(4) -0.018(3) 0.013(3) C19 0.059(3) 0.058(3) 0.043(3) -0.002(2) -0.005(2) -0.006(3) C20 0.074(4) 0.073(4) 0.091(4) -0.022(3) -0.010(3) 0.011(3) C21 0.097(5) 0.085(5) 0.098(5) -0.034(4) -0.003(4) -0.012(4) C22 0.138(6) 0.065(4) 0.112(5) -0.018(4) -0.017(4) 0.017(4) C23 0.185(7) 0.104(6) 0.177(7) -0.056(5) -0.107(6) 0.070(5) C24 0.137(5) 0.077(5) 0.152(6) -0.043(4) -0.090(5) 0.042(4) C25 0.049(3) 0.049(3) 0.053(3) -0.002(2) 0.004(2) -0.002(2) C26 0.064(3) 0.062(3) 0.070(4) 0.001(3) -0.006(3) -0.002(2) C27 0.088(4) 0.088(4) 0.049(3) -0.008(3) -0.011(3) 0.001(3) C28 0.093(5) 0.065(4) 0.088(5) -0.012(3) -0.033(3) -0.004(3) C29 0.070(4) 0.097(4) 0.100(5) -0.001(4) -0.013(4) -0.026(3) C30 0.062(4) 0.091(4) 0.070(4) -0.005(3) 0.001(3) -0.015(3) C31 0.060(3) 0.058(3) 0.054(3) 0.002(2) 0.002(3) 0.000(3) C32 0.093(4) 0.093(4) 0.066(4) 0.009(3) 0.016(3) -0.002(3) C33 0.125(6) 0.123(6) 0.077(5) 0.005(4) 0.036(4) -0.015(5) C34 0.163(8) 0.107(6) 0.069(5) 0.026(4) -0.002(5) -0.048(5) C35 0.128(6) 0.070(4) 0.087(5) 0.024(4) -0.031(4) -0.018(4) C36 0.077(4) 0.057(3) 0.068(4) 0.004(3) -0.003(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Be1 O7 1.571(6) . ? Be1 O8 1.609(6) . ? Be1 O1 1.644(6) . ? Be1 O4 1.648(6) . ? N1 O3 1.215(4) . ? N1 O2 1.223(4) . ? N1 O1 1.298(4) . ? N2 O5 1.210(4) . ? N2 O6 1.224(4) . ? N2 O4 1.298(4) . ? O7 P1 1.490(3) . ? O8 P2 1.495(3) . ? P1 C1 1.777(4) . ? P1 C13 1.782(5) . ? P1 C7 1.788(5) . ? P2 C19 1.774(5) . ? P2 C31 1.776(4) . ? P2 C25 1.780(4) . ? C1 C2 1.381(5) . ? C1 C6 1.388(5) . ? C2 C3 1.385(6) . ? C2 H2 0.9300 . ? C3 C4 1.358(6) . ? C3 H3 0.9300 . ? C4 C5 1.386(6) . ? C4 H4 0.9300 . ? C5 C6 1.385(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.372(6) . ? C7 C8 1.373(6) . ? C8 C9 1.383(7) . ? C8 H8 0.9300 . ? C9 C10 1.353(7) . ? C9 H9 0.9300 . ? C10 C11 1.355(7) . ? C10 H10 0.9300 . ? C11 C12 1.396(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.355(6) . ? C13 C18 1.365(6) . ? C14 C15 1.388(8) . ? C14 H14 0.9300 . ? C15 C16 1.358(8) . ? C15 H15 0.9300 . ? C16 C17 1.344(7) . ? C16 H16 0.9300 . ? C17 C18 1.382(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.341(6) . ? C19 C20 1.361(6) . ? C20 C21 1.378(6) . ? C20 H20 0.9300 . ? C21 C22 1.341(7) . ? C21 H21 0.9300 . ? C22 C23 1.349(7) . ? C22 H22 0.9300 . ? C23 C24 1.383(7) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.378(5) . ? C25 C26 1.388(5) . ? C26 C27 1.388(6) . ? C26 H26 0.9300 . ? C27 C28 1.351(6) . ? C27 H27 0.9300 . ? C28 C29 1.369(6) . ? C28 H28 0.9300 . ? C29 C30 1.377(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.377(6) . ? C31 C36 1.380(6) . ? C32 C33 1.385(7) . ? C32 H32 0.9300 . ? C33 C34 1.370(8) . ? C33 H33 0.9300 . ? C34 C35 1.357(8) . ? C34 H34 0.9300 . ? C35 C36 1.380(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? 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 O7 Be1 O8 111.8(4) . . ? O7 Be1 O1 117.2(3) . . ? O8 Be1 O1 107.5(4) . . ? O7 Be1 O4 110.2(4) . . ? O8 Be1 O4 103.4(3) . . ? O1 Be1 O4 105.7(3) . . ? O3 N1 O2 124.2(5) . . ? O3 N1 O1 117.7(5) . . ? O2 N1 O1 118.1(5) . . ? O5 N2 O6 122.8(5) . . ? O5 N2 O4 118.4(4) . . ? O6 N2 O4 118.8(4) . . ? N1 O1 Be1 122.3(4) . . ? N2 O4 Be1 121.5(3) . . ? P1 O7 Be1 173.6(3) . . ? P2 O8 Be1 156.8(3) . . ? O7 P1 C1 110.83(19) . . ? O7 P1 C13 110.5(2) . . ? C1 P1 C13 107.5(2) . . ? O7 P1 C7 110.7(2) . . ? C1 P1 C7 108.6(2) . . ? C13 P1 C7 108.7(2) . . ? O8 P2 C19 112.39(19) . . ? O8 P2 C31 110.6(2) . . ? C19 P2 C31 107.0(2) . . ? O8 P2 C25 109.38(18) . . ? C19 P2 C25 108.2(2) . . ? C31 P2 C25 109.2(2) . . ? C2 C1 C6 119.2(4) . . ? C2 C1 P1 119.5(4) . . ? C6 C1 P1 121.2(4) . . ? C1 C2 C3 120.0(4) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.7(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.3(5) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C1 120.5(4) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C12 C7 C8 118.4(5) . . ? C12 C7 P1 120.3(4) . . ? C8 C7 P1 121.3(4) . . ? C7 C8 C9 120.8(5) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 120.2(6) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.2(6) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 120.0(6) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 120.4(5) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C18 118.5(5) . . ? C14 C13 P1 123.3(5) . . ? C18 C13 P1 118.0(4) . . ? C13 C14 C15 120.0(6) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.4(6) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 120.2(7) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.3(7) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C13 C18 C17 121.6(5) . . ? C13 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C24 C19 C20 117.4(5) . . ? C24 C19 P2 123.9(4) . . ? C20 C19 P2 118.7(4) . . ? C19 C20 C21 122.1(5) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C22 C21 C20 119.4(5) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 119.6(6) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C22 C23 C24 120.4(6) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 121.1(5) . . ? C19 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C30 C25 C26 117.4(4) . . ? C30 C25 P2 123.1(4) . . ? C26 C25 P2 119.5(3) . . ? C25 C26 C27 120.9(4) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C28 C27 C26 120.0(5) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.3(5) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C30 119.8(5) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C25 C30 C29 121.5(5) . . ? C25 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C32 C31 C36 118.6(4) . . ? C32 C31 P2 121.6(4) . . ? C36 C31 P2 119.8(4) . . ? C31 C32 C33 120.2(5) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 119.7(6) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 120.9(6) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 119.2(6) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C35 C36 C31 121.2(5) . . ? C35 C36 H36 119.4 . . ? C31 C36 H36 119.4 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.182 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.045 #===END OF CIF ============================================================== # 05mfd025 data_05mfd025 _database_code_depnum_ccdc_archive 'CCDC 298678' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2005-11-11 _chemical_name_systematic ; Bis(nitrato-O,O')bis(triphenylphosphine oxide-O)magnesium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Mg N2 O8 P2' _chemical_formula_sum 'C36 H30 Mg N2 O8 P2' _chemical_formula_weight 704.87 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' Mg Mg 0.0486 0.0363 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 # Superceded ** _symmetry_space_group_name_Hall '-C 2yc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.343(3) _cell_length_b 13.705(2) _cell_length_c 17.202(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.971(4) _cell_angle_gamma 90.00 _cell_volume 3590.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3717 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8189 # 0.9274 _exptl_absorpt_correction_T_max 1.0000 # 0.9811 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14502 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.67 _reflns_number_total 4116 _reflns_number_gt 2838 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+3.4035P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4116 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Mg1 Mg 0.0000 0.21512(7) 0.2500 0.0327(3) Uani 1 2 d S . . N1 N -0.04037(13) 0.11542(15) 0.36365(12) 0.0414(5) Uani 1 1 d . . . O2 O 0.01675(11) 0.18344(12) 0.36951(9) 0.0434(4) Uani 1 1 d . . . O3 O -0.07777(11) 0.09942(12) 0.29501(10) 0.0448(4) Uani 1 1 d . . . O4 O -0.05672(13) 0.06916(15) 0.42045(12) 0.0643(6) Uani 1 1 d . . . P1 P 0.17346(4) 0.37310(4) 0.27559(3) 0.03143(16) Uani 1 1 d . . . O1 O 0.09691(11) 0.30659(12) 0.25405(9) 0.0441(4) Uani 1 1 d . . . C1 C 0.22869(17) 0.39467(15) 0.19055(13) 0.0393(6) Uani 1 1 d . . . C2 C 0.1827(2) 0.3726(2) 0.11782(15) 0.0598(8) Uani 1 1 d . . . H2 H 0.1237 0.3504 0.1144 0.072 Uiso 1 1 calc R . . C3 C 0.2229(3) 0.3830(3) 0.05071(17) 0.0854(12) Uani 1 1 d . . . H3 H 0.1919 0.3666 0.0012 0.102 Uiso 1 1 calc R . . C4 C 0.3074(3) 0.4169(2) 0.0555(2) 0.0860(13) Uani 1 1 d . . . H4 H 0.3342 0.4251 0.0089 0.103 Uiso 1 1 calc R . . C5 C 0.3542(3) 0.43936(19) 0.1269(2) 0.0749(11) Uani 1 1 d . . . H5 H 0.4129 0.4624 0.1296 0.090 Uiso 1 1 calc R . . C6 C 0.3142(2) 0.42786(17) 0.19538(16) 0.0530(7) Uani 1 1 d . . . H6 H 0.3457 0.4428 0.2449 0.064 Uiso 1 1 calc R . . C7 C 0.25025(14) 0.32026(15) 0.35094(11) 0.0313(5) Uani 1 1 d . . . C8 C 0.24597(15) 0.22010(16) 0.36511(13) 0.0358(5) Uani 1 1 d . . . H8 H 0.2029 0.1811 0.3353 0.043 Uiso 1 1 calc R . . C9 C 0.30489(16) 0.17797(18) 0.42277(14) 0.0424(6) Uani 1 1 d . . . H9 H 0.3020 0.1100 0.4329 0.051 Uiso 1 1 calc R . . C10 C 0.36779(17) 0.23456(19) 0.46561(14) 0.0453(6) Uani 1 1 d . . . H10 H 0.4080 0.2052 0.5051 0.054 Uiso 1 1 calc R . . C11 C 0.37293(17) 0.33348(19) 0.45156(14) 0.0456(6) Uani 1 1 d . . . H11 H 0.4169 0.3717 0.4809 0.055 Uiso 1 1 calc R . . C12 C 0.31406(16) 0.37662(17) 0.39486(13) 0.0395(5) Uani 1 1 d . . . H12 H 0.3170 0.4448 0.3857 0.047 Uiso 1 1 calc R . . C13 C 0.13613(15) 0.48775(16) 0.31009(12) 0.0341(5) Uani 1 1 d . . . C14 C 0.17814(18) 0.57577(17) 0.30173(16) 0.0475(6) Uani 1 1 d . . . H14 H 0.2312 0.5773 0.2784 0.057 Uiso 1 1 calc R . . C15 C 0.1433(2) 0.66181(19) 0.32719(17) 0.0595(8) Uani 1 1 d . . . H15 H 0.1725 0.7220 0.3213 0.071 Uiso 1 1 calc R . . C16 C 0.0666(2) 0.6600(2) 0.36092(18) 0.0598(8) Uani 1 1 d . . . H16 H 0.0424 0.7191 0.3776 0.072 Uiso 1 1 calc R . . C17 C 0.02480(19) 0.5726(2) 0.37060(19) 0.0634(8) Uani 1 1 d . . . H17 H -0.0282 0.5716 0.3940 0.076 Uiso 1 1 calc R . . C18 C 0.05978(17) 0.4864(2) 0.34635(16) 0.0502(6) Uani 1 1 d . . . H18 H 0.0317 0.4262 0.3544 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0346(6) 0.0260(5) 0.0344(5) 0.000 -0.0086(4) 0.000 N1 0.0370(11) 0.0408(11) 0.0460(12) 0.0042(9) 0.0031(9) -0.0016(9) O2 0.0412(9) 0.0471(10) 0.0388(9) 0.0059(7) -0.0073(7) -0.0134(8) O3 0.0451(10) 0.0386(9) 0.0483(10) -0.0035(7) -0.0037(8) -0.0082(8) O4 0.0622(13) 0.0745(14) 0.0581(12) 0.0205(10) 0.0146(10) -0.0171(11) P1 0.0374(3) 0.0278(3) 0.0286(3) -0.0003(2) 0.0021(2) -0.0046(2) O1 0.0468(10) 0.0366(9) 0.0467(10) 0.0017(7) -0.0036(8) -0.0107(8) C1 0.0623(16) 0.0263(11) 0.0313(11) 0.0018(9) 0.0134(11) 0.0026(11) C2 0.075(2) 0.0675(19) 0.0354(13) 0.0009(12) 0.0008(13) 0.0249(16) C3 0.134(4) 0.091(3) 0.0339(15) 0.0097(16) 0.0192(19) 0.037(3) C4 0.159(4) 0.0529(19) 0.058(2) 0.0158(15) 0.064(2) 0.025(2) C5 0.113(3) 0.0366(15) 0.089(2) -0.0045(15) 0.067(2) -0.0137(17) C6 0.0761(19) 0.0342(13) 0.0542(15) -0.0106(11) 0.0305(14) -0.0156(13) C7 0.0366(12) 0.0318(11) 0.0262(10) -0.0009(9) 0.0063(9) -0.0001(9) C8 0.0368(12) 0.0339(12) 0.0381(12) -0.0016(9) 0.0103(10) 0.0009(10) C9 0.0454(14) 0.0373(13) 0.0461(14) 0.0059(11) 0.0129(11) 0.0074(11) C10 0.0467(15) 0.0556(16) 0.0334(12) 0.0034(11) 0.0045(11) 0.0152(12) C11 0.0478(15) 0.0485(15) 0.0385(13) -0.0071(11) -0.0026(11) 0.0019(12) C12 0.0465(14) 0.0341(12) 0.0365(12) -0.0026(10) -0.0007(10) 0.0002(10) C13 0.0359(12) 0.0325(11) 0.0333(11) -0.0006(9) 0.0014(9) -0.0021(9) C14 0.0560(16) 0.0347(13) 0.0561(15) -0.0014(11) 0.0248(13) -0.0020(12) C15 0.079(2) 0.0333(14) 0.0711(19) -0.0017(13) 0.0289(16) -0.0022(14) C16 0.0618(18) 0.0473(16) 0.0721(19) -0.0116(14) 0.0159(15) 0.0121(14) C17 0.0455(16) 0.0620(19) 0.086(2) -0.0194(16) 0.0223(15) -0.0009(14) C18 0.0428(14) 0.0449(14) 0.0651(17) -0.0081(13) 0.0155(13) -0.0082(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Mg1 O1 1.9397(17) . ? Mg1 O1 1.9397(17) 2 ? Mg1 O2 2.0863(16) 2 ? Mg1 O2 2.0863(16) . ? Mg1 O3 2.1822(18) 2 ? Mg1 O3 2.1822(18) . ? Mg1 N1 2.523(2) 2 ? Mg1 N1 2.523(2) . ? N1 O4 1.216(3) . ? N1 O3 1.268(2) . ? N1 O2 1.275(2) . ? P1 O1 1.4972(16) . ? P1 C7 1.795(2) . ? P1 C13 1.798(2) . ? P1 C1 1.802(2) . ? C1 C6 1.381(4) . ? C1 C2 1.393(4) . ? C2 C3 1.380(4) . ? C2 H2 0.9500 . ? C3 C4 1.371(6) . ? C3 H3 0.9500 . ? C4 C5 1.380(5) . ? C4 H4 0.9500 . ? C5 C6 1.402(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.395(3) . ? C7 C8 1.397(3) . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.380(4) . ? C9 H9 0.9500 . ? C10 C11 1.381(4) . ? C10 H10 0.9500 . ? C11 C12 1.379(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.383(3) . ? C13 C18 1.392(3) . ? C14 C15 1.387(4) . ? C14 H14 0.9500 . ? C15 C16 1.374(4) . ? C15 H15 0.9500 . ? C16 C17 1.379(4) . ? C16 H16 0.9500 . ? C17 C18 1.383(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? 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 O1 Mg1 O1 99.47(11) . 2 ? O1 Mg1 O2 99.91(7) . 2 ? O1 Mg1 O2 95.56(6) 2 2 ? O1 Mg1 O2 95.56(6) . . ? O1 Mg1 O2 99.91(7) 2 . ? O2 Mg1 O2 155.98(11) 2 . ? O1 Mg1 O3 91.87(7) . 2 ? O1 Mg1 O3 155.05(6) 2 2 ? O2 Mg1 O3 60.42(6) 2 2 ? O2 Mg1 O3 101.02(7) . 2 ? O1 Mg1 O3 155.05(6) . . ? O1 Mg1 O3 91.87(7) 2 . ? O2 Mg1 O3 101.02(7) 2 . ? O2 Mg1 O3 60.42(6) . . ? O3 Mg1 O3 86.79(10) 2 . ? O1 Mg1 N1 96.82(7) . 2 ? O1 Mg1 N1 125.55(7) 2 2 ? O2 Mg1 N1 30.26(6) 2 2 ? O2 Mg1 N1 129.67(8) . 2 ? O3 Mg1 N1 30.16(6) 2 2 ? O3 Mg1 N1 94.45(7) . 2 ? O1 Mg1 N1 125.55(7) . . ? O1 Mg1 N1 96.82(7) 2 . ? O2 Mg1 N1 129.67(8) 2 . ? O2 Mg1 N1 30.26(6) . . ? O3 Mg1 N1 94.45(7) 2 . ? O3 Mg1 N1 30.16(6) . . ? N1 Mg1 N1 114.43(10) 2 . ? O4 N1 O3 122.9(2) . . ? O4 N1 O2 121.6(2) . . ? O3 N1 O2 115.42(18) . . ? O4 N1 Mg1 177.14(18) . . ? O3 N1 Mg1 59.87(11) . . ? O2 N1 Mg1 55.55(10) . . ? N1 O2 Mg1 94.18(12) . . ? N1 O3 Mg1 89.97(12) . . ? O1 P1 C7 111.07(10) . . ? O1 P1 C13 110.00(10) . . ? C7 P1 C13 108.77(10) . . ? O1 P1 C1 109.33(11) . . ? C7 P1 C1 108.68(11) . . ? C13 P1 C1 108.95(10) . . ? P1 O1 Mg1 167.75(11) . . ? C6 C1 C2 120.0(2) . . ? C6 C1 P1 122.82(19) . . ? C2 C1 P1 117.2(2) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 119.3(3) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C1 C6 C5 119.7(3) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C12 C7 C8 119.6(2) . . ? C12 C7 P1 121.58(17) . . ? C8 C7 P1 118.80(17) . . ? C9 C8 C7 119.6(2) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 120.1(2) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.6(2) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 119.9(2) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C7 120.1(2) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 C18 119.1(2) . . ? C14 C13 P1 123.83(18) . . ? C18 C13 P1 117.10(18) . . ? C13 C14 C15 120.4(2) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.1(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.2(2) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.367 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.049 #===END OF CIF ============================================================== # 04rju008 data_04rju008 _database_code_depnum_ccdc_archive 'CCDC 298679' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2005-11-01 _chemical_name_systematic ; Bis(nitrato-O,O')bis(1,2-bis(diphenylphosphinoyl)benzene)Calcium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H48 Ca N2 O10 P4' _chemical_formula_sum 'C60 H48 Ca N2 O10 P4' _chemical_formula_structural 'Ca (N O3)2 (C30 H24 O2 P2)2' _chemical_formula_weight 1120.96 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' _symmetry_Int_Tables_number 13 # Superceded ** _symmetry_space_group_name_Hall '-P 2yac' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 21.771(4) _cell_length_b 10.6990(10) _cell_length_c 24.074(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.394(5) _cell_angle_gamma 90.00 _cell_volume 5431.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 52871 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 0.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9322 _exptl_absorpt_correction_T_max 0.9824 _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 60223 _diffrn_reflns_av_R_equivalents 0.0983 _diffrn_reflns_av_sigmaI/netI 0.0965 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12261 _reflns_number_gt 6807 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12261 _refine_ls_number_parameters 695 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1278 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.7500 0.22526(7) 0.2500 0.0287(2) Uani 1 2 d S . . P1 P 0.82937(3) -0.02640(7) 0.34565(3) 0.03150(19) Uani 1 1 d . . . P2 P 0.84485(3) 0.28640(7) 0.39473(3) 0.02945(18) Uani 1 1 d . . . O1 O 0.81636(8) 0.07215(16) 0.30076(8) 0.0322(5) Uani 1 1 d . . . O2 O 0.79814(9) 0.31875(17) 0.34034(8) 0.0337(5) Uani 1 1 d . . . O3 O 0.68129(9) 0.17441(18) 0.32032(9) 0.0407(5) Uani 1 1 d . . . O4 O 0.66673(9) 0.35338(18) 0.27772(9) 0.0370(5) Uani 1 1 d . . . O5 O 0.63284(12) 0.3232(2) 0.35382(10) 0.0537(6) Uani 1 1 d . . . N1 N 0.65969(11) 0.2842(2) 0.31814(11) 0.0360(6) Uani 1 1 d . . . C1 C 0.81994(13) 0.0275(3) 0.41504(13) 0.0322(7) Uani 1 1 d . . . C2 C 0.80573(14) -0.0648(3) 0.45036(14) 0.0406(8) Uani 1 1 d . . . H2 H 0.8018 -0.1489 0.4373 0.049 Uiso 1 1 calc R . . C3 C 0.79712(15) -0.0378(3) 0.50376(15) 0.0442(8) Uani 1 1 d . . . H3 H 0.7878 -0.1029 0.5272 0.053 Uiso 1 1 calc R . . C4 C 0.80206(14) 0.0836(3) 0.52318(14) 0.0411(8) Uani 1 1 d . . . H4 H 0.7961 0.1028 0.5600 0.049 Uiso 1 1 calc R . . C5 C 0.81571(14) 0.1772(3) 0.48857(13) 0.0362(7) Uani 1 1 d . . . H5 H 0.8186 0.2609 0.5022 0.043 Uiso 1 1 calc R . . C6 C 0.82537(13) 0.1536(3) 0.43461(13) 0.0316(7) Uani 1 1 d . . . C7 C 0.90931(13) -0.0839(3) 0.35596(13) 0.0349(7) Uani 1 1 d . . . C8 C 0.94113(14) -0.0544(3) 0.31481(14) 0.0395(8) Uani 1 1 d . . . H8 H 0.9205 -0.0059 0.2825 0.047 Uiso 1 1 calc R . . C9 C 1.00327(15) -0.0948(3) 0.32012(15) 0.0467(8) Uani 1 1 d . . . H9 H 1.0246 -0.0742 0.2914 0.056 Uiso 1 1 calc R . . C10 C 1.03360(17) -0.1641(3) 0.36656(17) 0.0561(10) Uani 1 1 d . . . H10 H 1.0760 -0.1911 0.3703 0.067 Uiso 1 1 calc R . . C11 C 1.00251(18) -0.1944(4) 0.40778(17) 0.0617(11) Uani 1 1 d . . . H11 H 1.0238 -0.2423 0.4400 0.074 Uiso 1 1 calc R . . C12 C 0.94018(16) -0.1559(3) 0.40315(15) 0.0511(9) Uani 1 1 d . . . H12 H 0.9190 -0.1784 0.4317 0.061 Uiso 1 1 calc R . . C13 C 0.77611(14) -0.1573(3) 0.32928(13) 0.0353(7) Uani 1 1 d . . . C14 C 0.79642(15) -0.2800(3) 0.32694(13) 0.0405(8) Uani 1 1 d . . . H14 H 0.8403 -0.2975 0.3321 0.049 Uiso 1 1 calc R . . C15 C 0.75291(17) -0.3763(3) 0.31710(15) 0.0489(9) Uani 1 1 d . . . H15 H 0.7669 -0.4599 0.3152 0.059 Uiso 1 1 calc R . . C16 C 0.68958(17) -0.3516(3) 0.30998(15) 0.0502(9) Uani 1 1 d . . . H16 H 0.6601 -0.4187 0.3047 0.060 Uiso 1 1 calc R . . C17 C 0.66832(16) -0.2297(3) 0.31052(16) 0.0488(9) Uani 1 1 d . . . H17 H 0.6243 -0.2129 0.3042 0.059 Uiso 1 1 calc R . . C18 C 0.71160(15) -0.1324(3) 0.32034(15) 0.0439(8) Uani 1 1 d . . . H18 H 0.6973 -0.0486 0.3210 0.053 Uiso 1 1 calc R . . C19 C 0.92273(13) 0.2593(3) 0.38509(13) 0.0344(7) Uani 1 1 d . . . C20 C 0.93887(16) 0.3202(3) 0.33934(14) 0.0481(9) Uani 1 1 d . . . H20 H 0.9089 0.3733 0.3150 0.058 Uiso 1 1 calc R . . C21 C 0.99781(19) 0.3039(4) 0.32937(18) 0.0627(11) Uani 1 1 d . . . H21 H 1.0087 0.3469 0.2986 0.075 Uiso 1 1 calc R . . C22 C 1.04022(19) 0.2270(4) 0.3631(2) 0.0648(12) Uani 1 1 d . . . H22 H 1.0804 0.2149 0.3552 0.078 Uiso 1 1 calc R . . C23 C 1.02633(15) 0.1652(3) 0.40905(18) 0.0555(10) Uani 1 1 d . . . H23 H 1.0569 0.1117 0.4325 0.067 Uiso 1 1 calc R . . C24 C 0.96675(14) 0.1822(3) 0.42069(14) 0.0406(8) Uani 1 1 d . . . H24 H 0.9568 0.1415 0.4524 0.049 Uiso 1 1 calc R . . C25 C 0.85153(13) 0.4171(3) 0.44334(12) 0.0317(7) Uani 1 1 d . . . C26 C 0.90770(14) 0.4506(3) 0.48247(13) 0.0372(7) Uani 1 1 d . . . H26 H 0.9455 0.4054 0.4833 0.045 Uiso 1 1 calc R . . C27 C 0.90912(15) 0.5486(3) 0.52005(14) 0.0434(8) Uani 1 1 d . . . H27 H 0.9475 0.5693 0.5472 0.052 Uiso 1 1 calc R . . C28 C 0.85471(16) 0.6165(3) 0.51810(14) 0.0457(8) Uani 1 1 d . . . H28 H 0.8556 0.6836 0.5441 0.055 Uiso 1 1 calc R . . C29 C 0.79920(15) 0.5869(3) 0.47848(15) 0.0450(8) Uani 1 1 d . . . H29 H 0.7622 0.6356 0.4764 0.054 Uiso 1 1 calc R . . C30 C 0.79702(14) 0.4866(3) 0.44174(14) 0.0393(8) Uani 1 1 d . . . H30 H 0.7582 0.4652 0.4153 0.047 Uiso 1 1 calc R . . Ca2 Ca 0.7500 0.02836(7) 0.7500 0.0306(2) Uani 1 2 d S . . P3 P 0.66252(3) 0.28376(7) 0.66171(3) 0.02987(18) Uani 1 1 d . . . P4 P 0.63119(3) -0.02983(7) 0.61607(3) 0.03184(19) Uani 1 1 d . . . O6 O 0.68067(9) 0.18157(17) 0.70445(8) 0.0328(5) Uani 1 1 d . . . O7 O 0.68874(9) -0.06180(18) 0.66194(9) 0.0371(5) Uani 1 1 d . . . O8 O 0.80983(10) 0.0664(2) 0.67233(10) 0.0492(6) Uani 1 1 d . . . O9 O 0.82236(9) -0.1114(2) 0.71562(10) 0.0442(5) Uani 1 1 d . . . O10 O 0.82899(15) -0.1014(3) 0.62793(12) 0.0804(9) Uani 1 1 d . . . N2 N 0.82141(13) -0.0483(3) 0.67174(13) 0.0478(7) Uani 1 1 d . . . C31 C 0.63838(12) 0.1029(3) 0.56985(12) 0.0311(7) Uani 1 1 d . . . C32 C 0.63181(13) 0.0775(3) 0.51192(13) 0.0357(7) Uani 1 1 d . . . H32 H 0.6237 -0.0061 0.4990 0.043 Uiso 1 1 calc R . . C33 C 0.63658(14) 0.1689(3) 0.47227(13) 0.0372(7) Uani 1 1 d . . . H33 H 0.6311 0.1482 0.4330 0.045 Uiso 1 1 calc R . . C34 C 0.64939(13) 0.2904(3) 0.49091(13) 0.0373(7) Uani 1 1 d . . . H34 H 0.6530 0.3541 0.4644 0.045 Uiso 1 1 calc R . . C35 C 0.65692(13) 0.3187(3) 0.54756(13) 0.0349(7) Uani 1 1 d . . . H35 H 0.6662 0.4026 0.5597 0.042 Uiso 1 1 calc R . . C36 C 0.65149(12) 0.2289(3) 0.58854(13) 0.0309(7) Uani 1 1 d . . . C37 C 0.72137(13) 0.4047(3) 0.66845(13) 0.0341(7) Uani 1 1 d . . . C38 C 0.78147(15) 0.3697(3) 0.66310(16) 0.0487(9) Uani 1 1 d . . . H38 H 0.7904 0.2845 0.6573 0.058 Uiso 1 1 calc R . . C39 C 0.82782(16) 0.4595(3) 0.66632(17) 0.0571(10) Uani 1 1 d . . . H39 H 0.8687 0.4358 0.6627 0.069 Uiso 1 1 calc R . . C40 C 0.81508(16) 0.5835(3) 0.67483(15) 0.0514(9) Uani 1 1 d . . . H40 H 0.8470 0.6449 0.6764 0.062 Uiso 1 1 calc R . . C41 C 0.75720(16) 0.6181(3) 0.68094(14) 0.0486(9) Uani 1 1 d . . . H41 H 0.7488 0.7034 0.6871 0.058 Uiso 1 1 calc R . . C42 C 0.71016(15) 0.5293(3) 0.67822(13) 0.0417(8) Uani 1 1 d . . . H42 H 0.6699 0.5540 0.6831 0.050 Uiso 1 1 calc R . . C43 C 0.59008(13) 0.3563(3) 0.66826(13) 0.0321(7) Uani 1 1 d . . . C44 C 0.55982(14) 0.4534(3) 0.63248(14) 0.0383(7) Uani 1 1 d . . . H44 H 0.5761 0.4807 0.6014 0.046 Uiso 1 1 calc R . . C45 C 0.50615(15) 0.5093(3) 0.64250(15) 0.0445(8) Uani 1 1 d . . . H45 H 0.4861 0.5755 0.6184 0.053 Uiso 1 1 calc R . . C46 C 0.48185(15) 0.4699(3) 0.68686(16) 0.0485(9) Uani 1 1 d . . . H46 H 0.4452 0.5091 0.6936 0.058 Uiso 1 1 calc R . . C47 C 0.51069(15) 0.3730(3) 0.72186(16) 0.0479(8) Uani 1 1 d . . . H47 H 0.4934 0.3450 0.7522 0.058 Uiso 1 1 calc R . . C48 C 0.56477(14) 0.3167(3) 0.71282(14) 0.0399(8) Uani 1 1 d . . . H48 H 0.5846 0.2507 0.7372 0.048 Uiso 1 1 calc R . . C49 C 0.61091(13) -0.1627(3) 0.56853(13) 0.0337(7) Uani 1 1 d . . . C50 C 0.65982(14) -0.2376(3) 0.55959(14) 0.0413(8) Uani 1 1 d . . . H50 H 0.7026 -0.2181 0.5781 0.050 Uiso 1 1 calc R . . C51 C 0.64630(16) -0.3405(3) 0.52381(15) 0.0470(8) Uani 1 1 d . . . H51 H 0.6799 -0.3909 0.5177 0.056 Uiso 1 1 calc R . . C52 C 0.58460(17) -0.3706(3) 0.49704(15) 0.0500(9) Uani 1 1 d . . . H52 H 0.5759 -0.4406 0.4720 0.060 Uiso 1 1 calc R . . C53 C 0.53531(16) -0.2994(3) 0.50638(14) 0.0467(9) Uani 1 1 d . . . H53 H 0.4927 -0.3217 0.4887 0.056 Uiso 1 1 calc R . . C54 C 0.54828(14) -0.1947(3) 0.54181(13) 0.0396(8) Uani 1 1 d . . . H54 H 0.5144 -0.1448 0.5478 0.048 Uiso 1 1 calc R . . C55 C 0.56015(13) -0.0054(3) 0.63967(13) 0.0338(7) Uani 1 1 d . . . C56 C 0.54851(15) -0.0886(3) 0.68053(14) 0.0411(8) Uani 1 1 d . . . H56 H 0.5806 -0.1446 0.6999 0.049 Uiso 1 1 calc R . . C57 C 0.48939(15) -0.0883(3) 0.69233(15) 0.0480(8) Uani 1 1 d . . . H57 H 0.4810 -0.1447 0.7200 0.058 Uiso 1 1 calc R . . C58 C 0.44282(15) -0.0076(3) 0.66457(14) 0.0455(8) Uani 1 1 d . . . H58 H 0.4022 -0.0099 0.6724 0.055 Uiso 1 1 calc R . . C59 C 0.45498(14) 0.0770(3) 0.62530(14) 0.0402(8) Uani 1 1 d . . . H59 H 0.4231 0.1347 0.6071 0.048 Uiso 1 1 calc R . . C60 C 0.51296(13) 0.0779(3) 0.61259(13) 0.0351(7) Uani 1 1 d . . . H60 H 0.5210 0.1355 0.5852 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0286(4) 0.0211(4) 0.0315(5) 0.000 -0.0019(3) 0.000 P1 0.0338(4) 0.0227(4) 0.0343(5) 0.0023(3) 0.0014(3) 0.0029(3) P2 0.0295(4) 0.0252(4) 0.0298(4) -0.0004(3) 0.0001(3) -0.0019(3) O1 0.0330(10) 0.0231(10) 0.0358(12) 0.0034(8) -0.0004(9) 0.0028(8) O2 0.0350(11) 0.0246(10) 0.0348(12) -0.0001(8) -0.0041(9) -0.0025(8) O3 0.0415(12) 0.0235(11) 0.0563(15) 0.0035(9) 0.0107(10) 0.0002(8) O4 0.0443(12) 0.0319(12) 0.0311(12) 0.0038(9) 0.0023(10) 0.0068(9) O5 0.0689(16) 0.0513(15) 0.0482(15) 0.0046(11) 0.0284(13) 0.0185(12) N1 0.0365(14) 0.0316(15) 0.0377(16) 0.0010(12) 0.0048(12) 0.0009(11) C1 0.0291(15) 0.0259(15) 0.0388(18) 0.0024(13) 0.0029(13) 0.0023(11) C2 0.0462(19) 0.0301(17) 0.044(2) 0.0014(14) 0.0086(16) -0.0002(13) C3 0.052(2) 0.0341(19) 0.048(2) 0.0076(15) 0.0150(16) -0.0036(14) C4 0.0431(18) 0.0420(19) 0.0390(19) 0.0012(15) 0.0115(15) 0.0016(14) C5 0.0372(17) 0.0309(16) 0.040(2) 0.0002(13) 0.0088(14) 0.0000(12) C6 0.0266(15) 0.0267(15) 0.0373(19) 0.0029(12) 0.0001(13) 0.0029(11) C7 0.0363(16) 0.0304(16) 0.0319(18) -0.0028(13) -0.0033(14) 0.0051(12) C8 0.0360(17) 0.0385(18) 0.0382(19) -0.0067(14) -0.0015(15) 0.0042(13) C9 0.0402(18) 0.048(2) 0.048(2) -0.0129(16) 0.0049(16) 0.0055(14) C10 0.044(2) 0.062(2) 0.058(3) -0.0096(19) 0.0041(19) 0.0200(17) C11 0.054(2) 0.065(3) 0.055(3) 0.0053(19) -0.009(2) 0.0298(18) C12 0.055(2) 0.051(2) 0.044(2) 0.0056(16) 0.0048(17) 0.0177(16) C13 0.0392(17) 0.0276(16) 0.0353(18) 0.0039(12) 0.0020(14) -0.0003(12) C14 0.0494(19) 0.0264(16) 0.042(2) -0.0007(13) 0.0051(15) 0.0030(13) C15 0.062(2) 0.0270(18) 0.053(2) -0.0018(14) 0.0048(17) 0.0049(15) C16 0.061(2) 0.0260(18) 0.059(2) 0.0012(15) 0.0073(18) -0.0102(14) C17 0.0459(19) 0.0348(19) 0.067(2) -0.0011(16) 0.0160(17) -0.0050(14) C18 0.0442(19) 0.0250(16) 0.060(2) 0.0002(14) 0.0077(16) -0.0006(13) C19 0.0304(15) 0.0381(17) 0.0309(18) -0.0107(13) 0.0006(13) -0.0063(12) C20 0.045(2) 0.062(2) 0.038(2) -0.0094(16) 0.0114(16) -0.0198(16) C21 0.056(2) 0.083(3) 0.052(2) -0.019(2) 0.021(2) -0.027(2) C22 0.052(2) 0.071(3) 0.081(3) -0.041(2) 0.035(2) -0.024(2) C23 0.0337(18) 0.042(2) 0.084(3) -0.0283(19) 0.0017(19) -0.0029(14) C24 0.0341(17) 0.0321(17) 0.050(2) -0.0133(14) 0.0007(15) -0.0034(12) C25 0.0403(17) 0.0239(15) 0.0275(17) 0.0024(12) 0.0024(13) -0.0023(12) C26 0.0386(17) 0.0309(17) 0.0373(19) -0.0031(13) 0.0004(14) 0.0003(12) C27 0.0450(19) 0.0345(18) 0.046(2) -0.0043(14) 0.0015(16) -0.0045(14) C28 0.061(2) 0.0332(18) 0.044(2) -0.0086(14) 0.0142(17) -0.0017(15) C29 0.0431(19) 0.0351(18) 0.057(2) -0.0021(15) 0.0135(17) 0.0059(14) C30 0.0377(17) 0.0341(17) 0.044(2) -0.0009(14) 0.0057(15) -0.0016(13) Ca2 0.0250(4) 0.0270(4) 0.0348(5) 0.000 -0.0018(4) 0.000 P3 0.0282(4) 0.0260(4) 0.0322(4) 0.0020(3) 0.0015(3) -0.0002(3) P4 0.0274(4) 0.0298(4) 0.0345(5) 0.0003(3) 0.0004(3) -0.0017(3) O6 0.0347(11) 0.0252(10) 0.0359(12) 0.0040(8) 0.0036(9) 0.0025(8) O7 0.0329(11) 0.0333(11) 0.0398(13) -0.0015(9) -0.0011(9) -0.0018(8) O8 0.0535(14) 0.0360(14) 0.0609(16) 0.0007(11) 0.0194(12) 0.0012(10) O9 0.0400(12) 0.0436(13) 0.0423(14) -0.0012(11) -0.0023(10) 0.0059(9) O10 0.123(2) 0.0734(19) 0.0504(17) -0.0001(15) 0.0329(17) 0.0450(17) N2 0.0524(17) 0.0430(18) 0.046(2) 0.0044(15) 0.0078(14) 0.0116(12) C31 0.0224(14) 0.0359(16) 0.0320(18) 0.0043(13) 0.0010(12) -0.0023(11) C32 0.0340(16) 0.0329(17) 0.038(2) 0.0000(13) 0.0047(14) -0.0033(12) C33 0.0409(17) 0.0410(18) 0.0308(18) -0.0011(14) 0.0110(14) -0.0004(13) C34 0.0371(17) 0.0387(18) 0.037(2) 0.0068(14) 0.0111(14) -0.0012(13) C35 0.0363(17) 0.0294(16) 0.038(2) 0.0018(13) 0.0079(14) -0.0009(12) C36 0.0250(14) 0.0294(16) 0.0366(18) 0.0014(13) 0.0044(12) 0.0004(11) C37 0.0340(16) 0.0323(17) 0.0324(18) 0.0028(13) 0.0011(13) -0.0031(12) C38 0.0398(19) 0.0328(18) 0.073(3) 0.0081(16) 0.0124(17) -0.0005(13) C39 0.0357(18) 0.057(2) 0.080(3) 0.0148(19) 0.0152(18) -0.0054(15) C40 0.046(2) 0.044(2) 0.059(2) 0.0130(17) 0.0035(17) -0.0144(15) C41 0.054(2) 0.0338(18) 0.050(2) -0.0039(15) -0.0008(17) -0.0119(15) C42 0.0443(18) 0.0350(18) 0.040(2) -0.0013(14) 0.0005(15) -0.0021(13) C43 0.0280(15) 0.0263(15) 0.0371(18) -0.0021(12) -0.0010(13) 0.0006(11) C44 0.0382(17) 0.0361(18) 0.0358(18) -0.0008(13) 0.0002(14) 0.0044(13) C45 0.0399(18) 0.0374(18) 0.049(2) -0.0026(15) -0.0029(16) 0.0099(13) C46 0.0352(17) 0.046(2) 0.064(2) -0.0068(17) 0.0109(17) 0.0080(14) C47 0.046(2) 0.046(2) 0.056(2) -0.0001(16) 0.0215(17) 0.0043(15) C48 0.0405(18) 0.0330(17) 0.047(2) 0.0055(14) 0.0123(15) 0.0039(13) C49 0.0318(16) 0.0334(16) 0.0334(18) 0.0015(13) 0.0036(13) -0.0026(12) C50 0.0358(17) 0.0351(18) 0.052(2) 0.0057(15) 0.0100(15) -0.0010(13) C51 0.053(2) 0.0352(19) 0.055(2) 0.0007(15) 0.0190(17) 0.0029(14) C52 0.065(2) 0.0336(19) 0.046(2) -0.0033(15) 0.0048(18) -0.0033(16) C53 0.049(2) 0.0346(18) 0.048(2) 0.0019(15) -0.0044(16) -0.0054(14) C54 0.0394(17) 0.0340(17) 0.0396(19) 0.0014(14) -0.0013(14) -0.0009(13) C55 0.0291(16) 0.0353(17) 0.0331(18) -0.0033(13) 0.0005(13) -0.0054(12) C56 0.0390(18) 0.0455(19) 0.0363(19) 0.0013(15) 0.0045(14) -0.0012(14) C57 0.047(2) 0.050(2) 0.049(2) 0.0042(16) 0.0180(17) -0.0065(15) C58 0.0385(18) 0.053(2) 0.046(2) -0.0097(16) 0.0137(16) -0.0070(15) C59 0.0329(17) 0.0457(19) 0.041(2) -0.0034(15) 0.0070(14) -0.0018(13) C60 0.0316(16) 0.0326(16) 0.0383(18) 0.0026(13) 0.0034(14) -0.0017(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O1 2.3208(18) 2_655 ? Ca1 O1 2.3208(18) . ? Ca1 O2 2.3866(19) . ? Ca1 O2 2.3866(19) 2_655 ? Ca1 O4 2.493(2) 2_655 ? Ca1 O4 2.493(2) . ? Ca1 O3 2.580(2) 2_655 ? Ca1 O3 2.580(2) . ? Ca1 N1 2.925(3) 2_655 ? Ca1 N1 2.925(3) . ? P1 O1 1.486(2) . ? P1 C13 1.798(3) . ? P1 C7 1.804(3) . ? P1 C1 1.827(3) . ? P2 O2 1.4853(19) . ? P2 C19 1.791(3) . ? P2 C25 1.806(3) . ? P2 C6 1.823(3) . ? O3 N1 1.262(3) . ? O4 N1 1.262(3) . ? O5 N1 1.226(3) . ? C1 C2 1.387(4) . ? C1 C6 1.424(4) . ? C2 C3 1.375(5) . ? C2 H2 0.9500 . ? C3 C4 1.375(4) . ? C3 H3 0.9500 . ? C4 C5 1.382(4) . ? C4 H4 0.9500 . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C7 C8 1.379(4) . ? C7 C12 1.398(4) . ? C8 C9 1.396(4) . ? C8 H8 0.9500 . ? C9 C10 1.367(5) . ? C9 H9 0.9500 . ? C10 C11 1.372(6) . ? C10 H10 0.9500 . ? C11 C12 1.396(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.391(4) . ? C13 C18 1.393(4) . ? C14 C15 1.380(4) . ? C14 H14 0.9500 . ? C15 C16 1.372(5) . ? C15 H15 0.9500 . ? C16 C17 1.386(5) . ? C16 H16 0.9500 . ? C17 C18 1.384(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.388(4) . ? C19 C20 1.398(5) . ? C20 C21 1.374(5) . ? C20 H20 0.9500 . ? C21 C22 1.348(6) . ? C21 H21 0.9500 . ? C22 C23 1.385(6) . ? C22 H22 0.9500 . ? C23 C24 1.405(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.392(4) . ? C25 C30 1.393(4) . ? C26 C27 1.380(4) . ? C26 H26 0.9500 . ? C27 C28 1.380(5) . ? C27 H27 0.9500 . ? C28 C29 1.378(4) . ? C28 H28 0.9500 . ? C29 C30 1.383(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? Ca2 O6 2.3119(19) 2_656 ? Ca2 O6 2.3119(19) . ? Ca2 O7 2.4079(19) . ? Ca2 O7 2.4079(19) 2_656 ? Ca2 O9 2.460(2) . ? Ca2 O9 2.460(2) 2_656 ? Ca2 O8 2.563(2) . ? Ca2 O8 2.563(2) 2_656 ? Ca2 N2 2.845(3) . ? Ca2 N2 2.845(3) 2_656 ? P3 O6 1.486(2) . ? P3 C43 1.799(3) . ? P3 C37 1.800(3) . ? P3 C36 1.815(3) . ? P4 O7 1.489(2) . ? P4 C55 1.795(3) . ? P4 C49 1.810(3) . ? P4 C31 1.835(3) . ? O8 N2 1.254(3) . ? O9 N2 1.250(3) . ? O10 N2 1.245(4) . ? C31 C32 1.393(4) . ? C31 C36 1.427(4) . ? C32 C33 1.388(4) . ? C32 H32 0.9500 . ? C33 C34 1.381(4) . ? C33 H33 0.9500 . ? C34 C35 1.366(4) . ? C34 H34 0.9500 . ? C35 C36 1.403(4) . ? C35 H35 0.9500 . ? C37 C42 1.385(4) . ? C37 C38 1.398(4) . ? C38 C39 1.381(5) . ? C38 H38 0.9500 . ? C39 C40 1.381(5) . ? C39 H39 0.9500 . ? C40 C41 1.356(5) . ? C40 H40 0.9500 . ? C41 C42 1.386(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.388(4) . ? C43 C44 1.405(4) . ? C44 C45 1.386(4) . ? C44 H44 0.9500 . ? C45 C46 1.371(5) . ? C45 H45 0.9500 . ? C46 C47 1.384(5) . ? C46 H46 0.9500 . ? C47 C48 1.387(4) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.392(4) . ? C49 C54 1.398(4) . ? C50 C51 1.384(5) . ? C50 H50 0.9500 . ? C51 C52 1.376(5) . ? C51 H51 0.9500 . ? C52 C53 1.379(5) . ? C52 H52 0.9500 . ? C53 C54 1.394(4) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.393(4) . ? C55 C56 1.396(4) . ? C56 C57 1.385(5) . ? C56 H56 0.9500 . ? C57 C58 1.373(5) . ? C57 H57 0.9500 . ? C58 C59 1.381(5) . ? C58 H58 0.9500 . ? C59 C60 1.371(4) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? 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 O1 Ca1 O1 90.21(9) 2_655 . ? O1 Ca1 O2 148.27(7) 2_655 . ? O1 Ca1 O2 75.00(6) . . ? O1 Ca1 O2 75.00(6) 2_655 2_655 ? O1 Ca1 O2 148.27(7) . 2_655 ? O2 Ca1 O2 130.44(9) . 2_655 ? O1 Ca1 O4 130.26(7) 2_655 2_655 ? O1 Ca1 O4 97.48(7) . 2_655 ? O2 Ca1 O4 80.19(7) . 2_655 ? O2 Ca1 O4 73.11(7) 2_655 2_655 ? O1 Ca1 O4 97.48(7) 2_655 . ? O1 Ca1 O4 130.26(7) . . ? O2 Ca1 O4 73.11(6) . . ? O2 Ca1 O4 80.19(7) 2_655 . ? O4 Ca1 O4 113.28(10) 2_655 . ? O1 Ca1 O3 83.82(7) 2_655 2_655 ? O1 Ca1 O3 79.05(7) . 2_655 ? O2 Ca1 O3 119.43(7) . 2_655 ? O2 Ca1 O3 71.67(7) 2_655 2_655 ? O4 Ca1 O3 50.31(6) 2_655 2_655 ? O4 Ca1 O3 150.52(7) . 2_655 ? O1 Ca1 O3 79.05(7) 2_655 . ? O1 Ca1 O3 83.82(7) . . ? O2 Ca1 O3 71.67(7) . . ? O2 Ca1 O3 119.43(7) 2_655 . ? O4 Ca1 O3 150.52(7) 2_655 . ? O4 Ca1 O3 50.31(6) . . ? O3 Ca1 O3 155.66(9) 2_655 . ? O1 Ca1 N1 105.91(7) 2_655 2_655 ? O1 Ca1 N1 91.73(7) . 2_655 ? O2 Ca1 N1 102.50(7) . 2_655 ? O2 Ca1 N1 66.60(7) 2_655 2_655 ? O4 Ca1 N1 25.35(6) 2_655 2_655 ? O4 Ca1 N1 131.80(7) . 2_655 ? O3 Ca1 N1 25.52(6) 2_655 2_655 ? O3 Ca1 N1 173.40(6) . 2_655 ? O1 Ca1 N1 91.73(7) 2_655 . ? O1 Ca1 N1 105.91(7) . . ? O2 Ca1 N1 66.60(7) . . ? O2 Ca1 N1 102.50(7) 2_655 . ? O4 Ca1 N1 131.80(7) 2_655 . ? O4 Ca1 N1 25.35(6) . . ? O3 Ca1 N1 173.40(6) 2_655 . ? O3 Ca1 N1 25.52(6) . . ? N1 Ca1 N1 155.10(10) 2_655 . ? O1 P1 C13 113.41(12) . . ? O1 P1 C7 110.20(13) . . ? C13 P1 C7 108.18(14) . . ? O1 P1 C1 113.38(12) . . ? C13 P1 C1 103.48(14) . . ? C7 P1 C1 107.80(13) . . ? O2 P2 C19 112.72(13) . . ? O2 P2 C25 108.54(12) . . ? C19 P2 C25 106.43(13) . . ? O2 P2 C6 116.61(12) . . ? C19 P2 C6 107.08(14) . . ? C25 P2 C6 104.72(14) . . ? P1 O1 Ca1 149.88(13) . . ? P2 O2 Ca1 139.02(11) . . ? N1 O3 Ca1 92.71(17) . . ? N1 O4 Ca1 96.88(16) . . ? O5 N1 O3 121.7(3) . . ? O5 N1 O4 120.7(2) . . ? O3 N1 O4 117.6(3) . . ? O5 N1 Ca1 166.0(2) . . ? O3 N1 Ca1 61.77(15) . . ? O4 N1 Ca1 57.77(14) . . ? C2 C1 C6 119.0(3) . . ? C2 C1 P1 115.4(2) . . ? C6 C1 P1 125.6(2) . . ? C3 C2 C1 121.8(3) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 119.9(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 119.3(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 122.5(3) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 117.5(3) . . ? C5 C6 P2 117.3(2) . . ? C1 C6 P2 125.1(2) . . ? C8 C7 C12 118.9(3) . . ? C8 C7 P1 117.5(2) . . ? C12 C7 P1 123.5(3) . . ? C7 C8 C9 120.8(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 120.2(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.7(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 121.2(3) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 119.3(4) . . ? C11 C12 H12 120.4 . . ? C7 C12 H12 120.4 . . ? C14 C13 C18 119.5(3) . . ? C14 C13 P1 123.3(2) . . ? C18 C13 P1 117.1(2) . . ? C15 C14 C13 120.0(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.5(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 119.7(3) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C13 120.0(3) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C24 C19 C20 119.6(3) . . ? C24 C19 P2 123.1(3) . . ? C20 C19 P2 117.3(2) . . ? C21 C20 C19 120.5(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 120.1(4) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 121.3(4) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C24 119.5(4) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C19 C24 C23 118.9(3) . . ? C19 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C26 C25 C30 118.7(3) . . ? C26 C25 P2 123.6(2) . . ? C30 C25 P2 117.7(2) . . ? C27 C26 C25 120.8(3) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 119.9(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.4(3) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C25 120.2(3) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? O6 Ca2 O6 89.69(10) 2_656 . ? O6 Ca2 O7 148.77(7) 2_656 . ? O6 Ca2 O7 73.32(7) . . ? O6 Ca2 O7 73.32(7) 2_656 2_656 ? O6 Ca2 O7 148.77(7) . 2_656 ? O7 Ca2 O7 132.77(10) . 2_656 ? O6 Ca2 O9 101.15(7) 2_656 . ? O6 Ca2 O9 131.97(7) . . ? O7 Ca2 O9 73.81(7) . . ? O7 Ca2 O9 77.98(7) 2_656 . ? O6 Ca2 O9 131.97(7) 2_656 2_656 ? O6 Ca2 O9 101.15(7) . 2_656 ? O7 Ca2 O9 77.98(7) . 2_656 ? O7 Ca2 O9 73.81(7) 2_656 2_656 ? O9 Ca2 O9 105.13(11) . 2_656 ? O6 Ca2 O8 80.97(7) 2_656 . ? O6 Ca2 O8 86.08(7) . . ? O7 Ca2 O8 72.07(7) . . ? O7 Ca2 O8 115.80(7) 2_656 . ? O9 Ca2 O8 50.73(7) . . ? O9 Ca2 O8 145.70(8) 2_656 . ? O6 Ca2 O8 86.08(7) 2_656 2_656 ? O6 Ca2 O8 80.97(7) . 2_656 ? O7 Ca2 O8 115.80(7) . 2_656 ? O7 Ca2 O8 72.07(7) 2_656 2_656 ? O9 Ca2 O8 145.70(8) . 2_656 ? O9 Ca2 O8 50.73(7) 2_656 2_656 ? O8 Ca2 O8 161.71(10) . 2_656 ? O6 Ca2 N2 96.81(8) 2_656 . ? O6 Ca2 N2 106.86(8) . . ? O7 Ca2 N2 64.90(8) . . ? O7 Ca2 N2 101.15(8) 2_656 . ? O9 Ca2 N2 25.97(7) . . ? O9 Ca2 N2 123.27(9) 2_656 . ? O8 Ca2 N2 26.15(7) . . ? O8 Ca2 N2 171.60(8) 2_656 . ? O6 Ca2 N2 106.86(8) 2_656 2_656 ? O6 Ca2 N2 96.81(8) . 2_656 ? O7 Ca2 N2 101.15(8) . 2_656 ? O7 Ca2 N2 64.90(8) 2_656 2_656 ? O9 Ca2 N2 123.27(9) . 2_656 ? O9 Ca2 N2 25.97(7) 2_656 2_656 ? O8 Ca2 N2 171.60(9) . 2_656 ? O8 Ca2 N2 26.15(7) 2_656 2_656 ? N2 Ca2 N2 146.49(12) . 2_656 ? O6 P3 C43 110.15(13) . . ? O6 P3 C37 113.94(12) . . ? C43 P3 C37 107.57(13) . . ? O6 P3 C36 112.49(12) . . ? C43 P3 C36 108.48(13) . . ? C37 P3 C36 103.85(14) . . ? O7 P4 C55 115.54(13) . . ? O7 P4 C49 108.45(12) . . ? C55 P4 C49 102.75(13) . . ? O7 P4 C31 116.39(12) . . ? C55 P4 C31 106.83(13) . . ? C49 P4 C31 105.59(14) . . ? P3 O6 Ca2 151.64(12) . . ? P4 O7 Ca2 137.77(12) . . ? N2 O8 Ca2 89.59(19) . . ? N2 O9 Ca2 94.51(18) . . ? O10 N2 O9 119.5(3) . . ? O10 N2 O8 121.7(3) . . ? O9 N2 O8 118.7(3) . . ? O10 N2 Ca2 154.4(2) . . ? O9 N2 Ca2 59.53(16) . . ? O8 N2 Ca2 64.27(17) . . ? C32 C31 C36 117.6(3) . . ? C32 C31 P4 117.0(2) . . ? C36 C31 P4 125.5(2) . . ? C33 C32 C31 123.0(3) . . ? C33 C32 H32 118.5 . . ? C31 C32 H32 118.5 . . ? C34 C33 C32 118.9(3) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C35 C34 C33 119.8(3) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 122.7(3) . . ? C34 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C35 C36 C31 118.1(3) . . ? C35 C36 P3 116.6(2) . . ? C31 C36 P3 125.4(2) . . ? C42 C37 C38 118.8(3) . . ? C42 C37 P3 123.7(2) . . ? C38 C37 P3 117.4(2) . . ? C39 C38 C37 119.8(3) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C38 C39 C40 120.4(3) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 120.3(3) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 120.2(3) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C37 C42 C41 120.5(3) . . ? C37 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C48 C43 C44 118.9(3) . . ? C48 C43 P3 117.5(2) . . ? C44 C43 P3 123.6(2) . . ? C45 C44 C43 120.0(3) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 120.5(3) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 120.0(3) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C48 120.3(3) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C47 C48 C43 120.3(3) . . ? C47 C48 H48 119.9 . . ? C43 C48 H48 119.9 . . ? C50 C49 C54 119.0(3) . . ? C50 C49 P4 118.3(2) . . ? C54 C49 P4 122.7(2) . . ? C51 C50 C49 120.1(3) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C52 C51 C50 120.6(3) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C51 C52 C53 120.2(3) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C52 C53 C54 119.7(3) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C53 C54 C49 120.3(3) . . ? C53 C54 H54 119.9 . . ? C49 C54 H54 119.9 . . ? C60 C55 C56 119.7(3) . . ? C60 C55 P4 122.6(2) . . ? C56 C55 P4 116.9(2) . . ? C57 C56 C55 118.9(3) . . ? C57 C56 H56 120.5 . . ? C55 C56 H56 120.5 . . ? C58 C57 C56 120.9(3) . . ? C58 C57 H57 119.6 . . ? C56 C57 H57 119.6 . . ? C57 C58 C59 120.1(3) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C60 C59 C58 120.1(3) . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C55 120.3(3) . . ? C59 C60 H60 119.9 . . ? C55 C60 H60 119.9 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # N1 Ca1 O1 P1 -179.7(2) 2_655 . . . ? # N1 Ca1 O1 P1 18.0(2) . . . . ? # N1 Ca1 O2 P2 -87.57(19) 2_655 . . . ? # N1 Ca1 O2 P2 116.0(2) . . . . ? # N1 Ca1 O3 N1 102.3(7) 2_655 . . . ? # N1 Ca1 O4 N1 -162.65(10) 2_655 . . . ? # Ca1 O3 N1 O5 -164.3(2) . . . . ? # Ca1 O3 N1 O4 15.6(2) . . . . ? # Ca1 O4 N1 O5 163.6(2) . . . . ? # Ca1 O4 N1 O3 -16.3(2) . . . . ? # O1 Ca1 N1 O5 167.9(8) 2_655 . . . ? # O1 Ca1 N1 O5 77.2(8) . . . . ? # O2 Ca1 N1 O5 11.8(8) . . . . ? # O2 Ca1 N1 O5 -117.1(8) 2_655 . . . ? # O4 Ca1 N1 O5 -38.7(8) 2_655 . . . ? # O4 Ca1 N1 O5 -88.2(8) . . . . ? # O3 Ca1 N1 O5 -144.6(7) 2_655 . . . ? # O3 Ca1 N1 O5 108.2(8) . . . . ? # N1 Ca1 N1 O5 -56.3(8) 2_655 . . . ? # O1 Ca1 N1 O3 59.70(15) 2_655 . . . ? # O1 Ca1 N1 O3 -31.01(16) . . . . ? # O2 Ca1 N1 O3 -96.38(15) . . . . ? # O2 Ca1 N1 O3 134.72(14) 2_655 . . . ? # O4 Ca1 N1 O3 -146.88(13) 2_655 . . . ? # O4 Ca1 N1 O3 163.6(2) . . . . ? # O3 Ca1 N1 O3 107.2(7) 2_655 . . . ? # N1 Ca1 N1 O3 -164.53(15) 2_655 . . . ? # O1 Ca1 N1 O4 -103.90(15) 2_655 . . . ? # O1 Ca1 N1 O4 165.39(14) . . . . ? # O2 Ca1 N1 O4 100.02(16) . . . . ? # O2 Ca1 N1 O4 -28.89(16) 2_655 . . . ? # O4 Ca1 N1 O4 49.5(2) 2_655 . . . ? # O3 Ca1 N1 O4 -56.4(7) 2_655 . . . ? # O3 Ca1 N1 O4 -163.6(2) . . . . ? # N1 Ca1 N1 O4 31.87(14) 2_655 . . . ? # N2 Ca2 O6 P3 -26.5(3) . . . . ? # N2 Ca2 O6 P3 177.4(2) 2_656 . . . ? # N2 Ca2 O7 P4 -129.5(2) . . . . ? # N2 Ca2 O7 P4 82.73(19) 2_656 . . . ? # N2 Ca2 O8 N2 -32.6(7) 2_656 . . . ? # N2 Ca2 O9 N2 158.50(13) 2_656 . . . ? # Ca2 O9 N2 O10 -150.4(3) . . . . ? # Ca2 O9 N2 O8 26.3(3) . . . . ? # Ca2 O8 N2 O10 151.6(3) . . . . ? # Ca2 O8 N2 O9 -25.1(3) . . . . ? # O6 Ca2 N2 O10 -163.2(5) 2_656 . . . ? # O6 Ca2 N2 O10 -71.5(5) . . . . ? # O7 Ca2 N2 O10 -9.7(5) . . . . ? # O7 Ca2 N2 O10 122.5(5) 2_656 . . . ? # O9 Ca2 N2 O10 95.3(6) . . . . ? # O9 Ca2 N2 O10 44.7(5) 2_656 . . . ? # O8 Ca2 N2 O10 -110.2(6) . . . . ? # O8 Ca2 N2 O10 87.0(7) 2_656 . . . ? # N2 Ca2 N2 O10 61.6(5) 2_656 . . . ? # O6 Ca2 N2 O9 101.50(17) 2_656 . . . ? # O6 Ca2 N2 O9 -166.75(16) . . . . ? # O7 Ca2 N2 O9 -105.00(18) . . . . ? # O7 Ca2 N2 O9 27.22(18) 2_656 . . . ? # O9 Ca2 N2 O9 -50.6(2) 2_656 . . . ? # O8 Ca2 N2 O9 154.5(3) . . . . ? # O8 Ca2 N2 O9 -8.2(6) 2_656 . . . ? # N2 Ca2 N2 O9 -33.72(15) 2_656 . . . ? # O6 Ca2 N2 O8 -52.98(17) 2_656 . . . ? # O6 Ca2 N2 O8 38.77(18) . . . . ? # O7 Ca2 N2 O8 100.53(17) . . . . ? # O7 Ca2 N2 O8 -127.25(16) 2_656 . . . ? # O9 Ca2 N2 O8 -154.5(3) . . . . ? # O9 Ca2 N2 O8 154.91(15) 2_656 . . . ? # O8 Ca2 N2 O8 -162.7(4) 2_656 . . . ? # N2 Ca2 N2 O8 171.81(17) 2_656 . . . ? C13 P1 O1 Ca1 65.3(3) . . . . ? C7 P1 O1 Ca1 -173.3(2) . . . . ? C1 P1 O1 Ca1 -52.4(3) . . . . ? O1 Ca1 O1 P1 -73.8(2) 2_655 . . . ? O2 Ca1 O1 P1 77.8(2) . . . . ? O2 Ca1 O1 P1 -134.7(2) 2_655 . . . ? O4 Ca1 O1 P1 155.5(2) 2_655 . . . ? O4 Ca1 O1 P1 26.2(3) . . . . ? O3 Ca1 O1 P1 -157.5(2) 2_655 . . . ? O3 Ca1 O1 P1 5.2(2) . . . . ? C19 P2 O2 Ca1 64.3(2) . . . . ? C25 P2 O2 Ca1 -178.03(17) . . . . ? C6 P2 O2 Ca1 -60.1(2) . . . . ? O1 Ca1 O2 P2 65.6(2) 2_655 . . . ? O1 Ca1 O2 P2 0.87(18) . . . . ? O2 Ca1 O2 P2 -157.3(2) 2_655 . . . ? O4 Ca1 O2 P2 -99.68(19) 2_655 . . . ? O4 Ca1 O2 P2 142.2(2) . . . . ? O3 Ca1 O2 P2 -67.0(2) 2_655 . . . ? O3 Ca1 O2 P2 89.22(19) . . . . ? O1 Ca1 O3 N1 -118.48(15) 2_655 . . . ? O1 Ca1 O3 N1 150.11(15) . . . . ? O2 Ca1 O3 N1 73.91(15) . . . . ? O2 Ca1 O3 N1 -52.80(16) 2_655 . . . ? O4 Ca1 O3 N1 55.8(2) 2_655 . . . ? O4 Ca1 O3 N1 -9.04(13) . . . . ? O3 Ca1 O3 N1 -164.55(15) 2_655 . . . ? O1 Ca1 O4 N1 78.12(15) 2_655 . . . ? O1 Ca1 O4 N1 -18.53(18) . . . . ? O2 Ca1 O4 N1 -70.82(15) . . . . ? O2 Ca1 O4 N1 151.41(16) 2_655 . . . ? O4 Ca1 O4 N1 -141.89(16) 2_655 . . . ? O3 Ca1 O4 N1 168.78(15) 2_655 . . . ? O3 Ca1 O4 N1 9.09(14) . . . . ? O1 P1 C1 C2 154.7(2) . . . . ? C13 P1 C1 C2 31.4(2) . . . . ? C7 P1 C1 C2 -83.1(2) . . . . ? O1 P1 C1 C6 -24.7(3) . . . . ? C13 P1 C1 C6 -148.0(2) . . . . ? C7 P1 C1 C6 97.6(3) . . . . ? C6 C1 C2 C3 -0.4(4) . . . . ? P1 C1 C2 C3 -179.8(2) . . . . ? C1 C2 C3 C4 0.5(5) . . . . ? C2 C3 C4 C5 0.0(5) . . . . ? C3 C4 C5 C6 -0.6(4) . . . . ? C4 C5 C6 C1 0.8(4) . . . . ? C4 C5 C6 P2 -178.6(2) . . . . ? C2 C1 C6 C5 -0.3(4) . . . . ? P1 C1 C6 C5 179.1(2) . . . . ? C2 C1 C6 P2 179.0(2) . . . . ? P1 C1 C6 P2 -1.6(4) . . . . ? O2 P2 C6 C5 -115.8(2) . . . . ? C19 P2 C6 C5 116.9(2) . . . . ? C25 P2 C6 C5 4.1(2) . . . . ? O2 P2 C6 C1 64.8(3) . . . . ? C19 P2 C6 C1 -62.5(3) . . . . ? C25 P2 C6 C1 -175.2(2) . . . . ? O1 P1 C7 C8 -14.5(3) . . . . ? C13 P1 C7 C8 110.0(2) . . . . ? C1 P1 C7 C8 -138.7(2) . . . . ? O1 P1 C7 C12 165.4(3) . . . . ? C13 P1 C7 C12 -70.1(3) . . . . ? C1 P1 C7 C12 41.2(3) . . . . ? C12 C7 C8 C9 -0.3(5) . . . . ? P1 C7 C8 C9 179.5(2) . . . . ? C7 C8 C9 C10 -0.3(5) . . . . ? C8 C9 C10 C11 0.4(5) . . . . ? C9 C10 C11 C12 0.2(6) . . . . ? C10 C11 C12 C7 -0.8(6) . . . . ? C8 C7 C12 C11 0.9(5) . . . . ? P1 C7 C12 C11 -179.0(3) . . . . ? O1 P1 C13 C14 123.8(3) . . . . ? C7 P1 C13 C14 1.3(3) . . . . ? C1 P1 C13 C14 -112.9(3) . . . . ? O1 P1 C13 C18 -58.1(3) . . . . ? C7 P1 C13 C18 179.3(3) . . . . ? C1 P1 C13 C18 65.2(3) . . . . ? C18 C13 C14 C15 -1.5(5) . . . . ? P1 C13 C14 C15 176.6(3) . . . . ? C13 C14 C15 C16 -0.5(5) . . . . ? C14 C15 C16 C17 2.3(6) . . . . ? C15 C16 C17 C18 -2.3(6) . . . . ? C16 C17 C18 C13 0.4(5) . . . . ? C14 C13 C18 C17 1.5(5) . . . . ? P1 C13 C18 C17 -176.7(3) . . . . ? O2 P2 C19 C24 -153.0(2) . . . . ? C25 P2 C19 C24 88.1(3) . . . . ? C6 P2 C19 C24 -23.5(3) . . . . ? O2 P2 C19 C20 27.2(3) . . . . ? C25 P2 C19 C20 -91.6(2) . . . . ? C6 P2 C19 C20 156.8(2) . . . . ? C24 C19 C20 C21 0.2(5) . . . . ? P2 C19 C20 C21 180.0(3) . . . . ? C19 C20 C21 C22 1.2(5) . . . . ? C20 C21 C22 C23 -1.5(6) . . . . ? C21 C22 C23 C24 0.4(5) . . . . ? C20 C19 C24 C23 -1.3(4) . . . . ? P2 C19 C24 C23 178.9(2) . . . . ? C22 C23 C24 C19 1.0(4) . . . . ? O2 P2 C25 C26 -145.9(2) . . . . ? C19 P2 C25 C26 -24.4(3) . . . . ? C6 P2 C25 C26 88.8(3) . . . . ? O2 P2 C25 C30 34.9(3) . . . . ? C19 P2 C25 C30 156.5(2) . . . . ? C6 P2 C25 C30 -90.3(3) . . . . ? C30 C25 C26 C27 1.7(5) . . . . ? P2 C25 C26 C27 -177.4(2) . . . . ? C25 C26 C27 C28 -1.5(5) . . . . ? C26 C27 C28 C29 -0.4(5) . . . . ? C27 C28 C29 C30 2.2(5) . . . . ? C28 C29 C30 C25 -2.0(5) . . . . ? C26 C25 C30 C29 0.0(5) . . . . ? P2 C25 C30 C29 179.2(2) . . . . ? C43 P3 O6 Ca2 -174.8(2) . . . . ? C37 P3 O6 Ca2 -53.8(3) . . . . ? C36 P3 O6 Ca2 64.0(3) . . . . ? O6 Ca2 O6 P3 70.5(2) 2_656 . . . ? O7 Ca2 O6 P3 -82.9(3) . . . . ? O7 Ca2 O6 P3 126.3(2) 2_656 . . . ? O9 Ca2 O6 P3 -34.3(3) . . . . ? O9 Ca2 O6 P3 -156.6(2) 2_656 . . . ? O8 Ca2 O6 P3 -10.5(2) . . . . ? O8 Ca2 O6 P3 156.6(3) 2_656 . . . ? C55 P4 O7 Ca2 -57.7(2) . . . . ? C49 P4 O7 Ca2 -172.36(17) . . . . ? C31 P4 O7 Ca2 68.8(2) . . . . ? O6 Ca2 O7 P4 -70.8(2) 2_656 . . . ? O6 Ca2 O7 P4 -11.12(17) . . . . ? O7 Ca2 O7 P4 148.7(2) 2_656 . . . ? O9 Ca2 O7 P4 -155.6(2) . . . . ? O9 Ca2 O7 P4 94.55(19) 2_656 . . . ? O8 Ca2 O7 P4 -102.38(19) . . . . ? O8 Ca2 O7 P4 59.8(2) 2_656 . . . ? O6 Ca2 O8 N2 126.61(17) 2_656 . . . ? O6 Ca2 O8 N2 -143.08(17) . . . . ? O7 Ca2 O8 N2 -69.35(17) . . . . ? O7 Ca2 O8 N2 60.16(18) 2_656 . . . ? O9 Ca2 O8 N2 14.10(15) . . . . ? O9 Ca2 O8 N2 -39.0(2) 2_656 . . . ? O8 Ca2 O8 N2 172.05(17) 2_656 . . . ? O6 Ca2 O9 N2 -82.62(17) 2_656 . . . ? O6 Ca2 O9 N2 17.2(2) . . . . ? O7 Ca2 O9 N2 65.62(17) . . . . ? O7 Ca2 O9 N2 -152.68(18) 2_656 . . . ? O9 Ca2 O9 N2 137.98(18) 2_656 . . . ? O8 Ca2 O9 N2 -14.20(16) . . . . ? O8 Ca2 O9 N2 177.87(17) 2_656 . . . ? O7 P4 C31 C32 116.3(2) . . . . ? C55 P4 C31 C32 -112.9(2) . . . . ? C49 P4 C31 C32 -4.0(3) . . . . ? O7 P4 C31 C36 -62.2(3) . . . . ? C55 P4 C31 C36 68.6(3) . . . . ? C49 P4 C31 C36 177.4(2) . . . . ? C36 C31 C32 C33 -0.9(4) . . . . ? P4 C31 C32 C33 -179.6(2) . . . . ? C31 C32 C33 C34 1.0(4) . . . . ? C32 C33 C34 C35 -0.2(4) . . . . ? C33 C34 C35 C36 -0.7(4) . . . . ? C34 C35 C36 C31 0.8(4) . . . . ? C34 C35 C36 P3 -179.6(2) . . . . ? C32 C31 C36 C35 0.0(4) . . . . ? P4 C31 C36 C35 178.5(2) . . . . ? C32 C31 C36 P3 -179.5(2) . . . . ? P4 C31 C36 P3 -1.0(4) . . . . ? O6 P3 C36 C35 -157.8(2) . . . . ? C43 P3 C36 C35 80.1(2) . . . . ? C37 P3 C36 C35 -34.2(2) . . . . ? O6 P3 C36 C31 21.6(3) . . . . ? C43 P3 C36 C31 -100.5(2) . . . . ? C37 P3 C36 C31 145.3(2) . . . . ? O6 P3 C37 C42 -121.1(3) . . . . ? C43 P3 C37 C42 1.3(3) . . . . ? C36 P3 C37 C42 116.2(3) . . . . ? O6 P3 C37 C38 59.3(3) . . . . ? C43 P3 C37 C38 -178.3(2) . . . . ? C36 P3 C37 C38 -63.4(3) . . . . ? C42 C37 C38 C39 -1.4(5) . . . . ? P3 C37 C38 C39 178.2(3) . . . . ? C37 C38 C39 C40 0.0(6) . . . . ? C38 C39 C40 C41 1.0(6) . . . . ? C39 C40 C41 C42 -0.5(5) . . . . ? C38 C37 C42 C41 1.9(5) . . . . ? P3 C37 C42 C41 -177.7(2) . . . . ? C40 C41 C42 C37 -0.9(5) . . . . ? O6 P3 C43 C48 4.9(3) . . . . ? C37 P3 C43 C48 -119.8(2) . . . . ? C36 P3 C43 C48 128.4(2) . . . . ? O6 P3 C43 C44 -177.9(2) . . . . ? C37 P3 C43 C44 57.3(3) . . . . ? C36 P3 C43 C44 -54.4(3) . . . . ? C48 C43 C44 C45 1.0(4) . . . . ? P3 C43 C44 C45 -176.2(2) . . . . ? C43 C44 C45 C46 -0.6(5) . . . . ? C44 C45 C46 C47 -0.4(5) . . . . ? C45 C46 C47 C48 1.0(5) . . . . ? C46 C47 C48 C43 -0.6(5) . . . . ? C44 C43 C48 C47 -0.4(4) . . . . ? P3 C43 C48 C47 176.9(2) . . . . ? O7 P4 C49 C50 -32.7(3) . . . . ? C55 P4 C49 C50 -155.5(2) . . . . ? C31 P4 C49 C50 92.7(3) . . . . ? O7 P4 C49 C54 145.6(2) . . . . ? C55 P4 C49 C54 22.8(3) . . . . ? C31 P4 C49 C54 -89.0(3) . . . . ? C54 C49 C50 C51 1.3(5) . . . . ? P4 C49 C50 C51 179.6(2) . . . . ? C49 C50 C51 C52 -0.5(5) . . . . ? C50 C51 C52 C53 -1.1(5) . . . . ? C51 C52 C53 C54 1.8(5) . . . . ? C52 C53 C54 C49 -0.9(5) . . . . ? C50 C49 C54 C53 -0.6(5) . . . . ? P4 C49 C54 C53 -178.8(2) . . . . ? O7 P4 C55 C60 148.5(2) . . . . ? C49 P4 C55 C60 -93.6(3) . . . . ? C31 P4 C55 C60 17.2(3) . . . . ? O7 P4 C55 C56 -42.1(3) . . . . ? C49 P4 C55 C56 75.8(2) . . . . ? C31 P4 C55 C56 -173.3(2) . . . . ? C60 C55 C56 C57 1.5(5) . . . . ? P4 C55 C56 C57 -168.3(2) . . . . ? C55 C56 C57 C58 -0.2(5) . . . . ? C56 C57 C58 C59 -1.6(5) . . . . ? C57 C58 C59 C60 2.1(5) . . . . ? C58 C59 C60 C55 -0.8(5) . . . . ? C56 C55 C60 C59 -1.0(4) . . . . ? P4 C55 C60 C59 168.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.342 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.065 #===END OF CIF ============================================================== # 04rju010 data_04rju010 _database_code_depnum_ccdc_archive 'CCDC 298680' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2005-10-23 _chemical_name_systematic ; Bis(nitrato-O,O')bis(bis(diphenylphosphinoyl)methane)calcium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H44 Ca N2 O10 P4' _chemical_formula_sum 'C50 H44 Ca N2 O10 P4' _chemical_formula_weight 996.83 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_Int_Tables_number 29 # Superceded ** _symmetry_space_group_name_Hall 'P 2c -2ac' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 20.4255(16) _cell_length_b 11.3207(10) _cell_length_c 22.2120(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5136.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 14383 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 21.49 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 0.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8968 _exptl_absorpt_correction_T_max 1.0042 _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15486 _diffrn_reflns_av_R_equivalents 0.1198 _diffrn_reflns_av_sigmaI/netI 0.1139 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 21.55 _reflns_number_total 5673 _reflns_number_gt 4196 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(11) _chemical_absolute_configuration ad _refine_ls_number_reflns 5673 _refine_ls_number_parameters 604 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_ref 0.2361 _refine_ls_wR_factor_gt 0.2133 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.28711(10) 0.4360(2) 0.15903(10) 0.0365(6) Uani 1 1 d . . . P1 P 0.42644(13) 0.5778(3) 0.09347(13) 0.0339(7) Uani 1 1 d . . . P2 P 0.41432(15) 0.3199(3) 0.05918(14) 0.0402(8) Uani 1 1 d . . . P3 P 0.39559(14) 0.2653(3) 0.25117(14) 0.0445(8) Uani 1 1 d . . . P4 P 0.27576(14) 0.1298(3) 0.20300(14) 0.0435(8) Uani 1 1 d . . . O1 O 0.3574(3) 0.5701(6) 0.1143(3) 0.0358(18) Uani 1 1 d . . . O2 O 0.3515(3) 0.3092(6) 0.0919(4) 0.0442(19) Uani 1 1 d . . . O3 O 0.3737(3) 0.3767(7) 0.2224(4) 0.048(2) Uani 1 1 d . . . O4 O 0.2487(4) 0.2477(6) 0.1877(4) 0.0443(19) Uani 1 1 d . . . N1 N 0.1750(5) 0.5028(11) 0.0802(6) 0.059(3) Uani 1 1 d . . . N2 N 0.2512(6) 0.5685(13) 0.2689(5) 0.060(3) Uani 1 1 d . . . O5 O 0.2069(7) 0.4098(12) 0.0753(6) 0.121(5) Uani 1 1 d . . . O6 O 0.1937(7) 0.5606(13) 0.1227(6) 0.124(6) Uani 1 1 d . . . O7 O 0.1280(4) 0.5295(10) 0.0495(5) 0.082(3) Uani 1 1 d . . . O8 O 0.2878(4) 0.6164(9) 0.2286(4) 0.066(3) Uani 1 1 d . . . O9 O 0.2273(4) 0.4723(10) 0.2566(4) 0.063(2) Uani 1 1 d . . . O10 O 0.2404(6) 0.6134(11) 0.3162(5) 0.099(4) Uani 1 1 d . . . C1 C 0.4755(6) 0.6598(9) 0.1447(5) 0.037(3) Uani 1 1 d . . . C2 C 0.4435(7) 0.7233(12) 0.1885(6) 0.060(4) Uani 1 1 d . . . H2 H 0.3970 0.7217 0.1898 0.072 Uiso 1 1 calc R . . C3 C 0.4775(8) 0.7903(13) 0.2315(7) 0.073(4) Uani 1 1 d . . . H3 H 0.4548 0.8311 0.2625 0.088 Uiso 1 1 calc R . . C4 C 0.5460(8) 0.7951(13) 0.2272(7) 0.075(5) Uani 1 1 d . . . H4 H 0.5700 0.8423 0.2547 0.090 Uiso 1 1 calc R . . C5 C 0.5788(6) 0.7324(13) 0.1836(8) 0.073(5) Uani 1 1 d . . . H5 H 0.6252 0.7366 0.1817 0.088 Uiso 1 1 calc R . . C6 C 0.5451(6) 0.6629(11) 0.1422(6) 0.054(4) Uani 1 1 d . . . H6 H 0.5682 0.6183 0.1129 0.065 Uiso 1 1 calc R . . C7 C 0.4292(6) 0.6421(9) 0.0180(5) 0.038(3) Uani 1 1 d . . . C8 C 0.4857(7) 0.6705(12) -0.0095(6) 0.058(4) Uani 1 1 d . . . H8 H 0.5261 0.6584 0.0108 0.069 Uiso 1 1 calc R . . C9 C 0.4852(7) 0.7167(12) -0.0665(6) 0.068(4) Uani 1 1 d . . . H9 H 0.5251 0.7388 -0.0854 0.082 Uiso 1 1 calc R . . C10 C 0.4255(8) 0.7312(13) -0.0969(6) 0.064(4) Uani 1 1 d . . . H10 H 0.4243 0.7617 -0.1367 0.077 Uiso 1 1 calc R . . C11 C 0.3711(7) 0.7011(13) -0.0687(7) 0.066(4) Uani 1 1 d . . . H11 H 0.3306 0.7104 -0.0891 0.080 Uiso 1 1 calc R . . C12 C 0.3705(5) 0.6558(10) -0.0096(5) 0.039(3) Uani 1 1 d . . . H12 H 0.3307 0.6358 0.0101 0.046 Uiso 1 1 calc R . . C13 C 0.4658(5) 0.4343(8) 0.0891(5) 0.031(2) Uani 1 1 d . . . H13A H 0.5053 0.4412 0.0635 0.037 Uiso 1 1 calc R . . H13B H 0.4802 0.4110 0.1299 0.037 Uiso 1 1 calc R . . C14 C 0.4619(7) 0.1870(11) 0.0634(6) 0.051(3) Uani 1 1 d . . . C15 C 0.5260(9) 0.1792(14) 0.0790(6) 0.076(5) Uani 1 1 d . . . H15 H 0.5489 0.2499 0.0884 0.091 Uiso 1 1 calc R . . C16 C 0.5584(11) 0.0764(17) 0.0818(8) 0.102(6) Uani 1 1 d . . . H16 H 0.6032 0.0771 0.0931 0.122 Uiso 1 1 calc R . . C17 C 0.5311(15) -0.0230(18) 0.0697(10) 0.113(7) Uani 1 1 d . . . H17 H 0.5564 -0.0932 0.0681 0.136 Uiso 1 1 calc R . . C18 C 0.4630(17) -0.0268(16) 0.0589(9) 0.123(8) Uani 1 1 d . . . H18 H 0.4401 -0.0995 0.0556 0.147 Uiso 1 1 calc R . . C19 C 0.4309(9) 0.0825(15) 0.0532(8) 0.086(5) Uani 1 1 d . . . H19 H 0.3861 0.0834 0.0419 0.103 Uiso 1 1 calc R . . C20 C 0.4037(6) 0.3526(9) -0.0189(6) 0.044(3) Uani 1 1 d . . . C21 C 0.3401(7) 0.3667(12) -0.0420(6) 0.057(4) Uani 1 1 d . . . H21 H 0.3032 0.3554 -0.0165 0.068 Uiso 1 1 calc R . . C22 C 0.3311(8) 0.3968(15) -0.1011(7) 0.076(5) Uani 1 1 d . . . H22 H 0.2883 0.4062 -0.1170 0.092 Uiso 1 1 calc R . . C23 C 0.3859(9) 0.4133(12) -0.1375(6) 0.073(5) Uani 1 1 d . . . H23 H 0.3796 0.4375 -0.1780 0.088 Uiso 1 1 calc R . . C24 C 0.4471(9) 0.3965(15) -0.1174(6) 0.079(5) Uani 1 1 d . . . H24 H 0.4834 0.4049 -0.1438 0.095 Uiso 1 1 calc R . . C25 C 0.4566(7) 0.3668(14) -0.0579(6) 0.067(4) Uani 1 1 d . . . H25 H 0.4998 0.3559 -0.0432 0.080 Uiso 1 1 calc R . . C26 C 0.4811(5) 0.2530(9) 0.2457(5) 0.034(3) Uani 1 1 d . . . C27 C 0.5190(6) 0.3583(12) 0.2408(5) 0.051(3) Uani 1 1 d . . . H27 H 0.4981 0.4331 0.2430 0.062 Uiso 1 1 calc R . . C28 C 0.5868(5) 0.3520(12) 0.2329(5) 0.044(3) Uani 1 1 d . . . H28 H 0.6111 0.4231 0.2286 0.053 Uiso 1 1 calc R . . C29 C 0.6190(6) 0.2464(12) 0.2311(6) 0.052(3) Uani 1 1 d . . . H29 H 0.6649 0.2435 0.2245 0.062 Uiso 1 1 calc R . . C30 C 0.5832(6) 0.1436(14) 0.2392(6) 0.061(4) Uani 1 1 d . . . H30 H 0.6052 0.0697 0.2408 0.073 Uiso 1 1 calc R . . C31 C 0.5171(7) 0.1477(12) 0.2449(6) 0.058(4) Uani 1 1 d . . . H31 H 0.4940 0.0752 0.2485 0.070 Uiso 1 1 calc R . . C32 C 0.3714(6) 0.2579(17) 0.3302(6) 0.069(5) Uani 1 1 d . . . C33 C 0.3547(8) 0.3620(19) 0.3577(7) 0.087(6) Uani 1 1 d . . . H33 H 0.3521 0.4330 0.3350 0.104 Uiso 1 1 calc R . . C34 C 0.3407(9) 0.363(2) 0.4231(11) 0.118(8) Uani 1 1 d . . . H34 H 0.3324 0.4317 0.4461 0.141 Uiso 1 1 calc R . . C35 C 0.3414(9) 0.247(3) 0.4466(9) 0.102(7) Uani 1 1 d . . . H35 H 0.3268 0.2411 0.4872 0.123 Uiso 1 1 calc R . . C36 C 0.3588(12) 0.144(3) 0.4221(8) 0.130(10) Uani 1 1 d . . . H36 H 0.3615 0.0730 0.4450 0.156 Uiso 1 1 calc R . . C37 C 0.3724(8) 0.1473(16) 0.3620(7) 0.085(5) Uani 1 1 d . . . H37 H 0.3826 0.0765 0.3411 0.102 Uiso 1 1 calc R . . C38 C 0.3630(5) 0.1317(11) 0.2139(6) 0.047(3) Uani 1 1 d . . . H38A H 0.3844 0.1236 0.1741 0.056 Uiso 1 1 calc R . . H38B H 0.3753 0.0619 0.2382 0.056 Uiso 1 1 calc R . . C39 C 0.2402(5) 0.0750(11) 0.2716(6) 0.045(3) Uani 1 1 d . . . C40 C 0.1990(6) 0.1496(12) 0.3043(6) 0.059(4) Uani 1 1 d . . . H40 H 0.1914 0.2276 0.2902 0.071 Uiso 1 1 calc R . . C41 C 0.1691(7) 0.1131(13) 0.3563(6) 0.060(4) Uani 1 1 d . . . H41 H 0.1406 0.1643 0.3777 0.071 Uiso 1 1 calc R . . C42 C 0.1816(7) -0.0017(14) 0.3773(6) 0.062(4) Uani 1 1 d . . . H42 H 0.1619 -0.0289 0.4135 0.075 Uiso 1 1 calc R . . C43 C 0.2211(7) -0.0719(14) 0.3461(7) 0.072(5) Uani 1 1 d . . . H43 H 0.2288 -0.1493 0.3610 0.087 Uiso 1 1 calc R . . C44 C 0.2526(7) -0.0379(13) 0.2917(7) 0.070(4) Uani 1 1 d . . . H44 H 0.2806 -0.0902 0.2704 0.084 Uiso 1 1 calc R . . C45 C 0.2646(5) 0.0266(10) 0.1427(5) 0.038(3) Uani 1 1 d . . . C46 C 0.2472(9) 0.0725(13) 0.0874(7) 0.081(5) Uani 1 1 d . . . H46 H 0.2373 0.1543 0.0841 0.097 Uiso 1 1 calc R . . C47 C 0.2438(10) 0.0011(17) 0.0358(9) 0.101(6) Uani 1 1 d . . . H47 H 0.2362 0.0328 -0.0031 0.122 Uiso 1 1 calc R . . C48 C 0.2529(10) -0.1256(16) 0.0462(10) 0.104(7) Uani 1 1 d . . . H48 H 0.2444 -0.1805 0.0148 0.125 Uiso 1 1 calc R . . C49 C 0.2723(9) -0.1626(14) 0.0985(9) 0.083(5) Uani 1 1 d . . . H49 H 0.2840 -0.2434 0.1029 0.100 Uiso 1 1 calc R . . C50 C 0.2767(8) -0.0900(13) 0.1472(7) 0.075(5) Uani 1 1 d . . . H50 H 0.2886 -0.1223 0.1851 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0399(12) 0.0401(14) 0.0295(13) 0.0054(11) 0.0013(11) 0.0000(11) P1 0.0387(16) 0.0357(17) 0.0274(16) 0.0041(14) 0.0012(13) -0.0010(13) P2 0.0548(18) 0.0335(17) 0.0322(16) -0.0007(14) 0.0043(15) -0.0023(15) P3 0.0465(17) 0.058(2) 0.0294(17) 0.0075(16) -0.0055(14) 0.0012(16) P4 0.0421(17) 0.045(2) 0.044(2) 0.0090(16) -0.0010(14) -0.0054(15) O1 0.043(4) 0.034(4) 0.030(4) 0.000(3) 0.004(3) -0.001(3) O2 0.045(4) 0.036(4) 0.052(5) 0.005(4) 0.007(4) -0.014(4) O3 0.036(4) 0.053(5) 0.055(5) -0.002(4) -0.012(4) -0.001(4) O4 0.047(4) 0.036(5) 0.050(5) 0.012(4) 0.001(4) -0.009(3) N1 0.044(7) 0.049(8) 0.085(11) 0.005(7) 0.004(7) 0.004(6) N2 0.073(8) 0.071(9) 0.034(7) 0.017(7) 0.015(6) 0.019(7) O5 0.142(11) 0.112(11) 0.109(11) -0.025(8) -0.091(9) 0.018(10) O6 0.164(13) 0.128(12) 0.081(9) -0.030(8) -0.049(9) 0.091(10) O7 0.041(5) 0.136(9) 0.068(7) 0.040(6) -0.013(5) 0.011(6) O8 0.060(5) 0.079(7) 0.058(6) -0.010(5) 0.020(5) -0.004(5) O9 0.076(6) 0.056(7) 0.057(6) 0.011(5) 0.019(5) 0.007(5) O10 0.138(10) 0.122(9) 0.038(6) -0.019(6) 0.032(7) 0.041(8) C1 0.052(7) 0.025(6) 0.035(7) 0.008(5) -0.007(6) 0.008(5) C2 0.076(9) 0.063(9) 0.042(8) -0.009(7) -0.005(7) 0.009(7) C3 0.069(10) 0.079(11) 0.071(11) -0.021(8) -0.007(8) 0.002(8) C4 0.085(12) 0.055(10) 0.084(12) -0.032(9) -0.001(9) 0.002(8) C5 0.039(7) 0.065(10) 0.116(13) -0.001(10) -0.026(8) -0.006(7) C6 0.038(7) 0.049(8) 0.076(10) -0.009(7) -0.004(6) 0.010(6) C7 0.058(8) 0.018(6) 0.039(7) 0.006(5) 0.002(6) 0.012(5) C8 0.054(8) 0.079(10) 0.040(8) 0.014(7) 0.010(7) 0.000(7) C9 0.076(11) 0.078(11) 0.051(10) 0.011(8) 0.033(8) -0.010(8) C10 0.076(11) 0.073(10) 0.043(8) 0.020(7) 0.016(8) 0.020(8) C11 0.066(9) 0.070(10) 0.063(10) 0.022(8) -0.005(8) 0.015(8) C12 0.035(6) 0.052(8) 0.029(7) 0.023(6) 0.001(5) 0.013(5) C13 0.042(6) 0.029(6) 0.021(6) 0.001(5) -0.002(5) 0.001(5) C14 0.072(9) 0.039(8) 0.043(8) -0.002(6) 0.002(7) 0.008(7) C15 0.117(13) 0.061(10) 0.050(10) -0.008(7) -0.025(8) 0.035(9) C16 0.145(16) 0.058(12) 0.103(15) -0.009(10) -0.035(12) 0.055(12) C17 0.18(2) 0.049(13) 0.106(17) 0.013(11) -0.016(15) 0.035(15) C18 0.24(3) 0.053(13) 0.074(13) -0.005(10) 0.037(17) -0.015(17) C19 0.120(14) 0.053(11) 0.085(12) 0.029(9) 0.023(10) 0.019(10) C20 0.059(8) 0.027(7) 0.046(8) 0.001(5) -0.004(7) -0.001(6) C21 0.074(9) 0.061(9) 0.035(8) 0.007(6) -0.011(7) -0.027(7) C22 0.082(10) 0.101(13) 0.046(10) 0.005(9) -0.022(8) -0.018(9) C23 0.141(15) 0.054(9) 0.025(8) 0.012(6) -0.026(10) -0.032(9) C24 0.105(13) 0.110(14) 0.023(8) 0.012(8) 0.003(8) -0.004(10) C25 0.052(8) 0.103(12) 0.045(9) 0.011(8) 0.002(7) 0.006(8) C26 0.044(6) 0.027(6) 0.032(6) 0.005(5) 0.000(5) -0.007(5) C27 0.061(8) 0.075(10) 0.019(6) 0.004(6) -0.007(6) 0.007(7) C28 0.042(7) 0.054(9) 0.037(7) -0.016(6) 0.000(5) -0.008(6) C29 0.041(7) 0.059(9) 0.055(8) 0.002(7) -0.012(6) -0.004(7) C30 0.048(9) 0.085(11) 0.050(9) -0.008(7) -0.016(6) 0.007(8) C31 0.063(9) 0.056(9) 0.056(9) 0.016(7) -0.011(7) -0.030(7) C32 0.030(7) 0.145(16) 0.032(8) 0.011(10) -0.011(6) 0.015(8) C33 0.081(11) 0.142(17) 0.037(9) -0.004(10) 0.009(7) 0.045(11) C34 0.095(13) 0.14(2) 0.122(19) -0.034(16) -0.001(12) 0.064(14) C35 0.087(12) 0.16(2) 0.058(12) -0.046(15) 0.022(10) -0.005(14) C36 0.17(2) 0.19(3) 0.033(11) 0.005(13) 0.013(12) -0.092(19) C37 0.110(13) 0.096(13) 0.049(11) 0.009(9) -0.005(9) -0.019(10) C38 0.042(6) 0.053(8) 0.046(7) 0.015(6) 0.006(6) -0.011(6) C39 0.024(6) 0.056(9) 0.055(8) 0.010(7) -0.006(5) 0.002(6) C40 0.057(8) 0.061(10) 0.060(10) 0.026(7) 0.005(7) -0.005(7) C41 0.075(9) 0.060(10) 0.044(8) 0.009(7) 0.003(7) 0.005(8) C42 0.066(9) 0.070(11) 0.051(9) -0.001(8) 0.005(7) -0.018(8) C43 0.088(10) 0.066(10) 0.063(10) 0.051(9) 0.020(9) -0.015(9) C44 0.080(10) 0.056(10) 0.075(11) 0.021(8) 0.013(8) 0.003(8) C45 0.052(7) 0.031(7) 0.031(7) 0.004(5) -0.007(5) -0.001(5) C46 0.124(13) 0.051(9) 0.066(11) 0.005(8) -0.045(10) 0.003(9) C47 0.135(15) 0.090(14) 0.079(13) -0.017(11) -0.042(11) 0.039(12) C48 0.142(16) 0.054(11) 0.115(18) -0.047(11) -0.037(13) 0.031(11) C49 0.118(13) 0.051(10) 0.080(13) 0.012(10) 0.015(11) 0.025(9) C50 0.129(13) 0.054(10) 0.044(10) 0.018(8) 0.016(8) 0.045(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O1 2.313(7) . ? Ca1 O3 2.358(8) . ? Ca1 O4 2.359(7) . ? Ca1 O2 2.453(8) . ? Ca1 O5 2.496(10) . ? Ca1 O6 2.505(11) . ? Ca1 O9 2.521(9) . ? Ca1 O8 2.560(10) . ? Ca1 N2 2.957(13) . ? Ca1 N1 2.980(13) . ? P1 O1 1.487(7) . ? P1 C1 1.778(12) . ? P1 C13 1.814(10) . ? P1 C7 1.828(11) . ? P2 O2 1.479(8) . ? P2 C20 1.787(13) . ? P2 C14 1.794(13) . ? P2 C13 1.795(10) . ? P3 O3 1.483(9) . ? P3 C26 1.757(11) . ? P3 C32 1.826(13) . ? P3 C38 1.850(13) . ? P4 O4 1.484(8) . ? P4 C45 1.793(11) . ? P4 C38 1.798(11) . ? P4 C39 1.798(13) . ? N1 O6 1.211(15) . ? N1 O7 1.215(14) . ? N1 O5 1.242(15) . ? N2 O10 1.189(15) . ? N2 O9 1.223(14) . ? N2 O8 1.287(14) . ? C1 C2 1.376(17) . ? C1 C6 1.424(16) . ? C2 C3 1.403(19) . ? C2 H2 0.9500 . ? C3 C4 1.40(2) . ? C3 H3 0.9500 . ? C4 C5 1.37(2) . ? C4 H4 0.9500 . ? C5 C6 1.391(19) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.344(16) . ? C7 C12 1.355(15) . ? C8 C9 1.372(19) . ? C8 H8 0.9500 . ? C9 C10 1.40(2) . ? C9 H9 0.9500 . ? C10 C11 1.321(19) . ? C10 H10 0.9500 . ? C11 C12 1.410(17) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.36(2) . ? C14 C19 1.36(2) . ? C15 C16 1.34(2) . ? C15 H15 0.9500 . ? C16 C17 1.28(3) . ? C16 H16 0.9500 . ? C17 C18 1.41(3) . ? C17 H17 0.9500 . ? C18 C19 1.41(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.393(18) . ? C20 C21 1.406(18) . ? C21 C22 1.369(19) . ? C21 H21 0.9500 . ? C22 C23 1.39(2) . ? C22 H22 0.9500 . ? C23 C24 1.34(2) . ? C23 H23 0.9500 . ? C24 C25 1.377(19) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.400(17) . ? C26 C27 1.425(16) . ? C27 C28 1.397(17) . ? C27 H27 0.9500 . ? C28 C29 1.365(17) . ? C28 H28 0.9500 . ? C29 C30 1.386(19) . ? C29 H29 0.9500 . ? C30 C31 1.357(18) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.37(2) . ? C32 C37 1.44(2) . ? C33 C34 1.48(3) . ? C33 H33 0.9500 . ? C34 C35 1.41(3) . ? C34 H34 0.9500 . ? C35 C36 1.33(3) . ? C35 H35 0.9500 . ? C36 C37 1.36(2) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C44 1.377(18) . ? C39 C40 1.398(18) . ? C40 C41 1.369(18) . ? C40 H40 0.9500 . ? C41 C42 1.403(19) . ? C41 H41 0.9500 . ? C42 C43 1.33(2) . ? C42 H42 0.9500 . ? C43 C44 1.42(2) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.347(18) . ? C45 C46 1.380(18) . ? C46 C47 1.40(2) . ? C46 H46 0.9500 . ? C47 C48 1.46(3) . ? C47 H47 0.9500 . ? C48 C49 1.30(2) . ? C48 H48 0.9500 . ? C49 C50 1.36(2) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? 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 O1 Ca1 O3 88.7(3) . . ? O1 Ca1 O4 156.2(3) . . ? O3 Ca1 O4 80.3(3) . . ? O1 Ca1 O2 77.9(2) . . ? O3 Ca1 O2 78.1(3) . . ? O4 Ca1 O2 79.3(3) . . ? O1 Ca1 O5 99.5(4) . . ? O3 Ca1 O5 154.6(4) . . ? O4 Ca1 O5 82.9(4) . . ? O2 Ca1 O5 80.2(4) . . ? O1 Ca1 O6 88.0(4) . . ? O3 Ca1 O6 157.4(4) . . ? O4 Ca1 O6 110.0(5) . . ? O2 Ca1 O6 122.8(4) . . ? O5 Ca1 O6 47.7(4) . . ? O1 Ca1 O9 124.3(3) . . ? O3 Ca1 O9 84.1(3) . . ? O4 Ca1 O9 75.8(3) . . ? O2 Ca1 O9 151.4(3) . . ? O5 Ca1 O9 110.0(5) . . ? O6 Ca1 O9 79.4(4) . . ? O1 Ca1 O8 74.5(3) . . ? O3 Ca1 O8 82.1(3) . . ? O4 Ca1 O8 124.0(3) . . ? O2 Ca1 O8 146.1(3) . . ? O5 Ca1 O8 123.2(4) . . ? O6 Ca1 O8 75.5(4) . . ? O9 Ca1 O8 49.8(3) . . ? O1 Ca1 N2 100.1(3) . . ? O3 Ca1 N2 80.7(3) . . ? O4 Ca1 N2 98.8(3) . . ? O2 Ca1 N2 158.7(3) . . ? O5 Ca1 N2 120.8(4) . . ? O6 Ca1 N2 78.0(4) . . ? O9 Ca1 N2 24.2(3) . . ? O8 Ca1 N2 25.7(3) . . ? O1 Ca1 N1 93.3(3) . . ? O3 Ca1 N1 177.9(3) . . ? O4 Ca1 N1 97.6(3) . . ? O2 Ca1 N1 101.7(3) . . ? O5 Ca1 N1 24.2(4) . . ? O6 Ca1 N1 23.5(3) . . ? O9 Ca1 N1 95.3(3) . . ? O8 Ca1 N1 99.0(4) . . ? N2 Ca1 N1 99.6(4) . . ? O1 P1 C1 111.5(5) . . ? O1 P1 C13 112.6(4) . . ? C1 P1 C13 104.6(5) . . ? O1 P1 C7 109.7(5) . . ? C1 P1 C7 111.2(5) . . ? C13 P1 C7 107.1(5) . . ? O2 P2 C20 112.9(5) . . ? O2 P2 C14 112.0(6) . . ? C20 P2 C14 106.9(6) . . ? O2 P2 C13 112.6(5) . . ? C20 P2 C13 106.3(5) . . ? C14 P2 C13 105.6(6) . . ? O3 P3 C26 109.7(5) . . ? O3 P3 C32 111.9(7) . . ? C26 P3 C32 109.4(5) . . ? O3 P3 C38 113.2(5) . . ? C26 P3 C38 105.2(5) . . ? C32 P3 C38 107.2(7) . . ? O4 P4 C45 111.6(5) . . ? O4 P4 C38 112.9(5) . . ? C45 P4 C38 103.5(6) . . ? O4 P4 C39 110.8(5) . . ? C45 P4 C39 110.9(5) . . ? C38 P4 C39 106.9(5) . . ? P1 O1 Ca1 139.5(4) . . ? P2 O2 Ca1 135.7(4) . . ? P3 O3 Ca1 136.5(5) . . ? P4 O4 Ca1 138.7(4) . . ? O6 N1 O7 123.5(13) . . ? O6 N1 O5 111.1(12) . . ? O7 N1 O5 125.2(14) . . ? O6 N1 Ca1 55.7(7) . . ? O7 N1 Ca1 178.0(9) . . ? O5 N1 Ca1 55.5(7) . . ? O10 N2 O9 120.3(13) . . ? O10 N2 O8 122.9(15) . . ? O9 N2 O8 116.8(12) . . ? O10 N2 Ca1 173.3(10) . . ? O9 N2 Ca1 57.5(6) . . ? O8 N2 Ca1 59.7(7) . . ? N1 O5 Ca1 100.3(9) . . ? N1 O6 Ca1 100.8(9) . . ? N2 O8 Ca1 94.6(8) . . ? N2 O9 Ca1 98.3(7) . . ? C2 C1 C6 119.3(11) . . ? C2 C1 P1 117.3(10) . . ? C6 C1 P1 123.5(9) . . ? C1 C2 C3 121.9(13) . . ? C1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C2 C3 C4 117.8(14) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? C5 C4 C3 121.0(14) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 121.0(13) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 118.9(12) . . ? C5 C6 H6 120.6 . . ? C1 C6 H6 120.6 . . ? C8 C7 C12 121.8(11) . . ? C8 C7 P1 122.5(9) . . ? C12 C7 P1 115.6(8) . . ? C7 C8 C9 120.3(13) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C10 119.7(12) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 118.2(13) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C10 C11 C12 123.0(13) . . ? C10 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C7 C12 C11 117.0(11) . . ? C7 C12 H12 121.5 . . ? C11 C12 H12 121.5 . . ? P2 C13 P1 114.0(5) . . ? P2 C13 H13A 108.8 . . ? P1 C13 H13A 108.8 . . ? P2 C13 H13B 108.8 . . ? P1 C13 H13B 108.8 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C19 115.8(14) . . ? C15 C14 P2 126.2(11) . . ? C19 C14 P2 117.9(11) . . ? C16 C15 C14 123.0(17) . . ? C16 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C17 C16 C15 122(2) . . ? C17 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C16 C17 C18 119(2) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 117(2) . . ? C19 C18 H18 121.7 . . ? C17 C18 H18 121.7 . . ? C14 C19 C18 122(2) . . ? C14 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C25 C20 C21 118.5(11) . . ? C25 C20 P2 122.2(10) . . ? C21 C20 P2 119.3(10) . . ? C22 C21 C20 120.1(13) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 118.8(14) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 122.5(13) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C23 C24 C25 118.9(14) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C24 C25 C20 121.1(13) . . ? C24 C25 H25 119.4 . . ? C20 C25 H25 119.4 . . ? C31 C26 C27 115.2(10) . . ? C31 C26 P3 126.2(8) . . ? C27 C26 P3 118.6(9) . . ? C28 C27 C26 120.3(12) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C27 121.7(12) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C28 C29 C30 118.5(12) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? C31 C30 C29 120.5(13) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C26 123.5(12) . . ? C30 C31 H31 118.2 . . ? C26 C31 H31 118.2 . . ? C33 C32 C37 122.2(14) . . ? C33 C32 P3 117.1(13) . . ? C37 C32 P3 120.6(14) . . ? C32 C33 C34 119.3(18) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C35 C34 C33 111.0(18) . . ? C35 C34 H34 124.5 . . ? C33 C34 H34 124.5 . . ? C36 C35 C34 131(2) . . ? C36 C35 H35 114.3 . . ? C34 C35 H35 114.3 . . ? C35 C36 C37 115(2) . . ? C35 C36 H36 122.3 . . ? C37 C36 H36 122.3 . . ? C36 C37 C32 120(2) . . ? C36 C37 H37 119.9 . . ? C32 C37 H37 119.9 . . ? P4 C38 P3 115.2(7) . . ? P4 C38 H38A 108.5 . . ? P3 C38 H38A 108.5 . . ? P4 C38 H38B 108.5 . . ? P3 C38 H38B 108.5 . . ? H38A C38 H38B 107.5 . . ? C44 C39 C40 120.2(12) . . ? C44 C39 P4 121.4(10) . . ? C40 C39 P4 118.4(9) . . ? C41 C40 C39 121.6(13) . . ? C41 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? C40 C41 C42 118.6(14) . . ? C40 C41 H41 120.7 . . ? C42 C41 H41 120.7 . . ? C43 C42 C41 119.4(13) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C42 C43 C44 123.8(14) . . ? C42 C43 H43 118.1 . . ? C44 C43 H43 118.1 . . ? C39 C44 C43 116.4(14) . . ? C39 C44 H44 121.8 . . ? C43 C44 H44 121.8 . . ? C50 C45 C46 118.9(12) . . ? C50 C45 P4 124.1(10) . . ? C46 C45 P4 116.9(9) . . ? C45 C46 C47 121.4(14) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C46 C47 C48 115.5(16) . . ? C46 C47 H47 122.3 . . ? C48 C47 H47 122.3 . . ? C49 C48 C47 119.8(16) . . ? C49 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C48 C49 C50 122.4(15) . . ? C48 C49 H49 118.8 . . ? C50 C49 H49 118.8 . . ? C45 C50 C49 121.4(14) . . ? C45 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 21.55 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.372 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.103 #===END OF CIF ==============================================================