#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/09/4310928.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4310928
loop_
_publ_author_name
'Paul Sood'
'Mohan Koutha'
'Maomian Fan'
'Yaroslav Klichko'
'Hongming Zhang'
'Michael Lattman'
_publ_section_title
;
 Phosphorus-Based p-tert-Butylcalix[5]arene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2975
_journal_page_last               2980
_journal_paper_doi               10.1021/ic035359d
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C62 H74 Cl2 O5 P2'
_chemical_formula_weight         1032.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.288(7)
_cell_angle_beta                 102.074(8)
_cell_angle_gamma                96.007(8)
_cell_formula_units_Z            2
_cell_length_a                   14.353(1)
_cell_length_b                   14.612(1)
_cell_length_c                   14.916(1)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      15.00
_cell_measurement_theta_min      10.29
_cell_volume                     2952.3(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_sigmaI/netI    0.091
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10718
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        8.49
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.210
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.403
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         10269
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.151
_refine_ls_R_factor_gt           0.087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1452P)²+0.9571P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.228
_refine_ls_wR_factor_ref         0.260
_reflns_number_gt                5965
_reflns_number_total             10269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035359dsi20031124_025643_3.cif
_cod_data_source_block           3(mhclxpcl)
_cod_original_cell_volume        2952.3(3)
_cod_original_formula_sum        '[C55 H66 Cl2 O5 P2] . [C7 H8]'
_cod_database_code               4310928
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.25005(9) 0.45320(9) 0.53854(9) 0.0321(3) Uani 1 1 d . . .
P2 P 0.29400(11) 0.23936(11) 0.64669(11) 0.0464(4) Uani 1 1 d . . .
Cl1 Cl 0.26732(10) 0.59837(9) 0.56828(11) 0.0522(4) Uani 1 1 d . . .
Cl2 Cl 0.33034(15) 0.11974(13) 0.56873(13) 0.0770(6) Uani 1 1 d . . .
O1 O 0.0596(3) 0.2388(2) 0.6444(2) 0.0383(8) Uani 1 1 d . . .
H1 H 0.0517 0.2313 0.5871 0.046 Uiso 1 1 calc R . .
O2 O 0.1456(2) 0.4366(2) 0.4616(2) 0.0325(8) Uani 1 1 d . . .
O3 O 0.3263(2) 0.4450(2) 0.4709(2) 0.0328(8) Uani 1 1 d . . .
O4 O 0.3957(2) 0.3073(2) 0.6842(2) 0.0361(8) Uani 1 1 d . . .
O5 O 0.2838(2) 0.1948(2) 0.7368(2) 0.0385(8) Uani 1 1 d . . .
C11 C 0.0849(3) 0.3340(3) 0.6879(3) 0.0307(11) Uani 1 1 d . . .
C12 C 0.1333(3) 0.3587(3) 0.7831(3) 0.0328(11) Uani 1 1 d . . .
C13 C 0.1549(4) 0.4531(4) 0.8288(4) 0.0395(12) Uani 1 1 d . . .
H13 H 0.1879 0.4693 0.8920 0.047 Uiso 1 1 calc R . .
C14 C 0.1306(4) 0.5254(4) 0.7862(4) 0.0415(13) Uani 1 1 d . A .
C15 C 0.0814(4) 0.4974(4) 0.6909(4) 0.0374(12) Uani 1 1 d . . .
H15 H 0.0644 0.5442 0.6598 0.045 Uiso 1 1 calc R . .
C16 C 0.0569(3) 0.4039(3) 0.6409(3) 0.0282(10) Uani 1 1 d . . .
C17 C 0.1495(5) 0.6295(4) 0.8418(4) 0.0550(16) Uani 1 1 d . . .
C18 C 0.0535(9) 0.6562(9) 0.8595(14) 0.111(5) Uani 0.83(3) 1 d PU A 1
H18A H 0.0639 0.7200 0.8973 0.166 Uiso 0.83(3) 1 calc PR A 1
H18B H 0.0271 0.6137 0.8922 0.166 Uiso 0.83(3) 1 calc PR A 1
H18C H 0.0092 0.6516 0.8002 0.166 Uiso 0.83(3) 1 calc PR A 1
C19 C 0.1889(17) 0.6941(7) 0.7858(8) 0.104(6) Uani 0.83(3) 1 d PU A 1
H19A H 0.1405 0.6925 0.7301 0.156 Uiso 0.83(3) 1 calc PR A 1
H19B H 0.2449 0.6727 0.7681 0.156 Uiso 0.83(3) 1 calc PR A 1
H19C H 0.2061 0.7579 0.8242 0.156 Uiso 0.83(3) 1 calc PR A 1
C20 C 0.2227(11) 0.6466(6) 0.9350(9) 0.081(4) Uani 0.83(3) 1 d PU A 1
H20A H 0.2820 0.6271 0.9240 0.122 Uiso 0.83(3) 1 calc PR A 1
H20B H 0.1985 0.6106 0.9744 0.122 Uiso 0.83(3) 1 calc PR A 1
H20C H 0.2341 0.7128 0.9659 0.122 Uiso 0.83(3) 1 calc PR A 1
C181 C 0.075(4) 0.639(4) 0.908(4) 0.070(13) Uiso 0.17(3) 1 d PU A 2
H18D H 0.0642 0.7041 0.9227 0.105 Uiso 0.17(3) 1 calc PR A 2
H18E H 0.1008 0.6212 0.9648 0.105 Uiso 0.17(3) 1 calc PR A 2
H18F H 0.0150 0.5992 0.8750 0.105 Uiso 0.17(3) 1 calc PR A 2
C191 C 0.133(5) 0.694(5) 0.787(5) 0.075(15) Uiso 0.17(3) 1 d PU A 2
H19D H 0.1494 0.7569 0.8267 0.113 Uiso 0.17(3) 1 calc PR A 2
H19E H 0.0662 0.6825 0.7546 0.113 Uiso 0.17(3) 1 calc PR A 2
H19F H 0.1722 0.6864 0.7419 0.113 Uiso 0.17(3) 1 calc PR A 2
C201 C 0.254(4) 0.653(4) 0.894(5) 0.078(14) Uiso 0.17(3) 1 d PU A 2
H20D H 0.2932 0.6644 0.8513 0.117 Uiso 0.17(3) 1 calc PR A 2
H20E H 0.2729 0.6017 0.9203 0.117 Uiso 0.17(3) 1 calc PR A 2
H20F H 0.2632 0.7095 0.9441 0.117 Uiso 0.17(3) 1 calc PR A 2
C21 C 0.0981(3) 0.3421(3) 0.4272(3) 0.0301(10) Uani 1 1 d . . .
C22 C 0.0229(3) 0.3128(3) 0.4651(3) 0.0320(11) Uani 1 1 d . . .
C23 C -0.0260(4) 0.2204(3) 0.4266(3) 0.0375(12) Uani 1 1 d . . .
H23 H -0.0776 0.1999 0.4498 0.045 Uiso 1 1 calc R . .
C24 C -0.0002(4) 0.1575(4) 0.3544(4) 0.0422(13) Uani 1 1 d . B .
C25 C 0.0734(4) 0.1910(4) 0.3178(3) 0.0387(12) Uani 1 1 d . . .
H25 H 0.0905 0.1507 0.2687 0.046 Uiso 1 1 calc R . .
C26 C 0.1230(3) 0.2834(3) 0.3519(3) 0.0306(10) Uani 1 1 d . . .
C27 C -0.0527(5) 0.0546(4) 0.3158(4) 0.0630(19) Uani 1 1 d . . .
C28 C -0.1129(12) 0.0236(8) 0.3769(9) 0.097(5) Uani 0.659(11) 1 d PU B 3
H28A H -0.1350 -0.0435 0.3550 0.145 Uiso 0.659(11) 1 calc PR B 3
H28B H -0.1675 0.0566 0.3744 0.145 Uiso 0.659(11) 1 calc PR B 3
H28C H -0.0753 0.0375 0.4408 0.145 Uiso 0.659(11) 1 calc PR B 3
C29 C 0.0346(10) -0.0098(7) 0.3331(11) 0.102(5) Uani 0.659(11) 1 d PU B 3
H29A H 0.0644 0.0035 0.3993 0.153 Uiso 0.659(11) 1 calc PR B 3
H29B H 0.0819 0.0056 0.2995 0.153 Uiso 0.659(11) 1 calc PR B 3
H29C H 0.0081 -0.0759 0.3104 0.153 Uiso 0.659(11) 1 calc PR B 3
C30 C -0.0950(11) 0.0326(8) 0.2187(8) 0.088(5) Uani 0.659(11) 1 d PU B 3
H30A H -0.1314 -0.0301 0.1997 0.132 Uiso 0.659(11) 1 calc PR B 3
H30B H -0.0455 0.0356 0.1845 0.132 Uiso 0.659(11) 1 calc PR B 3
H30C H -0.1371 0.0774 0.2052 0.132 Uiso 0.659(11) 1 calc PR B 3
C281 C -0.043(2) 0.0073(17) 0.3860(17) 0.075(7) Uiso 0.341(11) 1 d PU B 4
H28D H -0.0739 -0.0574 0.3605 0.113 Uiso 0.341(11) 1 calc PR B 4
H28E H -0.0732 0.0371 0.4341 0.113 Uiso 0.341(11) 1 calc PR B 4
H28F H 0.0240 0.0089 0.4130 0.113 Uiso 0.341(11) 1 calc PR B 4
C291 C -0.036(2) 0.0017(18) 0.2236(18) 0.077(7) Uiso 0.341(11) 1 d PU B 4
H29D H 0.0318 0.0059 0.2277 0.115 Uiso 0.341(11) 1 calc PR B 4
H29E H -0.0654 0.0292 0.1737 0.115 Uiso 0.341(11) 1 calc PR B 4
H29F H -0.0645 -0.0636 0.2105 0.115 Uiso 0.341(11) 1 calc PR B 4
C301 C -0.1776(16) 0.0632(16) 0.2855(16) 0.075(7) Uiso 0.341(11) 1 d P B 4
H30A H -0.2146 0.0007 0.2631 0.113 Uiso 0.341(11) 1 calc PR B 4
H30B H -0.1895 0.0971 0.2368 0.113 Uiso 0.341(11) 1 calc PR B 4
H30C H -0.1962 0.0963 0.3402 0.113 Uiso 0.341(11) 1 calc PR B 4
C31 C 0.3543(3) 0.3556(3) 0.4395(3) 0.0285(10) Uani 1 1 d . . .
C32 C 0.3008(3) 0.2952(3) 0.3577(3) 0.0328(11) Uani 1 1 d . . .
C33 C 0.3345(4) 0.2123(4) 0.3217(3) 0.0378(12) Uani 1 1 d . . .
H33 H 0.2988 0.1712 0.2656 0.045 Uiso 1 1 calc R . .
C34 C 0.4206(4) 0.1899(4) 0.3683(4) 0.0414(13) Uani 1 1 d . C .
C35 C 0.4714(4) 0.2526(3) 0.4521(3) 0.0368(12) Uani 1 1 d . . .
H35 H 0.5288 0.2382 0.4843 0.044 Uiso 1 1 calc R . .
C36 C 0.4398(3) 0.3365(3) 0.4903(3) 0.0301(10) Uani 1 1 d . . .
C37 C 0.4577(5) 0.0975(4) 0.3302(4) 0.0582(17) Uani 1 1 d . . .
C38 C 0.5461(15) 0.0835(12) 0.3958(12) 0.099(7) Uani 0.532(14) 1 d PU C 5
H38A H 0.5354 0.0910 0.4581 0.149 Uiso 0.532(14) 1 calc PR C 5
H38B H 0.5994 0.1296 0.3970 0.149 Uiso 0.532(14) 1 calc PR C 5
H38C H 0.5603 0.0210 0.3743 0.149 Uiso 0.532(14) 1 calc PR C 5
C39 C 0.4716(18) 0.0895(15) 0.2339(13) 0.092(6) Uani 0.532(14) 1 d PU C 5
H39A H 0.5131 0.1448 0.2324 0.138 Uiso 0.532(14) 1 calc PR C 5
H39B H 0.4103 0.0842 0.1907 0.138 Uiso 0.532(14) 1 calc PR C 5
H39C H 0.5003 0.0341 0.2157 0.138 Uiso 0.532(14) 1 calc PR C 5
C40 C 0.3765(17) 0.0109(10) 0.3246(15) 0.111(7) Uani 0.532(14) 1 d PU C 5
H40A H 0.4004 -0.0479 0.3084 0.166 Uiso 0.532(14) 1 calc PR C 5
H40B H 0.3199 0.0114 0.2773 0.166 Uiso 0.532(14) 1 calc PR C 5
H40C H 0.3605 0.0173 0.3848 0.166 Uiso 0.532(14) 1 calc PR C 5
C381 C 0.4549(19) 0.0341(13) 0.3927(14) 0.085(6) Uani 0.468(14) 1 d PU C 6
H38D H 0.4756 -0.0240 0.3665 0.127 Uiso 0.468(14) 1 calc PR C 6
H38E H 0.3902 0.0207 0.3996 0.127 Uiso 0.468(14) 1 calc PR C 6
H38F H 0.4970 0.0636 0.4535 0.127 Uiso 0.468(14) 1 calc PR C 6
C391 C 0.5669(14) 0.1285(14) 0.3217(17) 0.104(7) Uani 0.468(14) 1 d PU C 6
H39D H 0.6062 0.1608 0.3829 0.156 Uiso 0.468(14) 1 calc PR C 6
H39E H 0.5661 0.1700 0.2796 0.156 Uiso 0.468(14) 1 calc PR C 6
H39F H 0.5928 0.0730 0.2974 0.156 Uiso 0.468(14) 1 calc PR C 6
C401 C 0.4024(18) 0.0500(15) 0.2291(14) 0.091(8) Uani 0.468(14) 1 d PU C 6
H40D H 0.4372 0.0032 0.2015 0.137 Uiso 0.468(14) 1 calc PR C 6
H40E H 0.3957 0.0968 0.1927 0.137 Uiso 0.468(14) 1 calc PR C 6
H40F H 0.3397 0.0200 0.2293 0.137 Uiso 0.468(14) 1 calc PR C 6
C41 C 0.4936(3) 0.2992(3) 0.6989(3) 0.0284(10) Uani 1 1 d . . .
C42 C 0.5463(3) 0.3486(3) 0.6506(3) 0.0314(11) Uani 1 1 d . . .
C43 C 0.6442(3) 0.3445(4) 0.6645(4) 0.0391(12) Uani 1 1 d . . .
H43 H 0.6800 0.3763 0.6322 0.047 Uiso 1 1 calc R . .
C44 C 0.6906(4) 0.2942(4) 0.7253(4) 0.0429(13) Uani 1 1 d . . .
C45 C 0.6357(4) 0.2489(4) 0.7733(4) 0.0435(13) Uani 1 1 d . . .
H45 H 0.6662 0.2165 0.8154 0.052 Uiso 1 1 calc R . .
C46 C 0.5366(4) 0.2491(3) 0.7619(3) 0.0344(11) Uani 1 1 d . . .
C47 C 0.7990(4) 0.2889(5) 0.7336(5) 0.0614(18) Uani 1 1 d . . .
C48 C 0.8555(5) 0.3864(6) 0.7565(6) 0.084(2) Uani 1 1 d . . .
H48A H 0.8406 0.4249 0.8108 0.126 Uiso 1 1 calc R . .
H48B H 0.8390 0.4142 0.7036 0.126 Uiso 1 1 calc R . .
H48C H 0.9232 0.3826 0.7697 0.126 Uiso 1 1 calc R . .
C49 C 0.8087(5) 0.2311(5) 0.6366(5) 0.072(2) Uani 1 1 d . . .
H49A H 0.8734 0.2175 0.6420 0.108 Uiso 1 1 calc R . .
H49B H 0.7944 0.2673 0.5901 0.108 Uiso 1 1 calc R . .
H49C H 0.7643 0.1727 0.6177 0.108 Uiso 1 1 calc R . .
C50 C 0.8380(5) 0.2352(7) 0.8062(6) 0.092(3) Uani 1 1 d . . .
H50A H 0.9034 0.2276 0.8048 0.138 Uiso 1 1 calc R . .
H50B H 0.7991 0.1740 0.7918 0.138 Uiso 1 1 calc R . .
H50C H 0.8363 0.2700 0.8680 0.138 Uiso 1 1 calc R . .
C51 C 0.3235(3) 0.2468(3) 0.8304(3) 0.0298(10) Uani 1 1 d . . .
C52 C 0.4197(3) 0.2489(3) 0.8711(3) 0.0303(11) Uani 1 1 d . . .
C53 C 0.4557(4) 0.2977(3) 0.9638(3) 0.0347(11) Uani 1 1 d . . .
H53 H 0.5207 0.3000 0.9913 0.042 Uiso 1 1 calc R . .
C54 C 0.3981(4) 0.3440(3) 1.0186(4) 0.0370(12) Uani 1 1 d . . .
C55 C 0.3023(4) 0.3379(3) 0.9745(3) 0.0337(11) Uani 1 1 d . . .
H55 H 0.2623 0.3676 1.0091 0.040 Uiso 1 1 calc R . .
C56 C 0.2624(3) 0.2901(3) 0.8815(3) 0.0312(11) Uani 1 1 d . . .
C57 C 0.4418(4) 0.3940(4) 1.1220(4) 0.0502(15) Uani 1 1 d . . .
C58 C 0.4872(7) 0.3220(6) 1.1753(5) 0.096(3) Uani 1 1 d . . .
H58A H 0.5383 0.2998 1.1483 0.145 Uiso 1 1 calc R . .
H58B H 0.4386 0.2692 1.1694 0.145 Uiso 1 1 calc R . .
H58C H 0.5127 0.3528 1.2409 0.145 Uiso 1 1 calc R . .
C59 C 0.5189(6) 0.4756(5) 1.1308(5) 0.078(2) Uani 1 1 d . . .
H59A H 0.4908 0.5222 1.1020 0.117 Uiso 1 1 calc R . .
H59B H 0.5672 0.4531 1.0996 0.117 Uiso 1 1 calc R . .
H59C H 0.5480 0.5036 1.1964 0.117 Uiso 1 1 calc R . .
C60 C 0.3654(6) 0.4295(7) 1.1730(5) 0.097(3) Uani 1 1 d . . .
H60A H 0.3939 0.4517 1.2395 0.146 Uiso 1 1 calc R . .
H60B H 0.3134 0.3786 1.1626 0.146 Uiso 1 1 calc R . .
H60C H 0.3412 0.4805 1.1489 0.146 Uiso 1 1 calc R . .
C61 C -0.0085(3) 0.3778(3) 0.5423(3) 0.0340(11) Uani 1 1 d . . .
H61A H -0.0709 0.3484 0.5462 0.041 Uiso 1 1 calc R . .
H61B H -0.0178 0.4361 0.5230 0.041 Uiso 1 1 calc R . .
C62 C 0.2039(4) 0.3163(4) 0.3090(3) 0.0359(11) Uani 1 1 d . . .
H62A H 0.2080 0.3840 0.3143 0.043 Uiso 1 1 calc R . .
H62B H 0.1891 0.2848 0.2424 0.043 Uiso 1 1 calc R . .
C63 C 0.4982(3) 0.4015(3) 0.5831(3) 0.0334(11) Uani 1 1 d . . .
H63A H 0.5470 0.4448 0.5703 0.040 Uiso 1 1 calc R . .
H63B H 0.4559 0.4391 0.6125 0.040 Uiso 1 1 calc R . .
C64 C 0.4827(4) 0.1941(4) 0.8158(4) 0.0390(12) Uani 1 1 d . . .
H64A H 0.5294 0.1714 0.8595 0.047 Uiso 1 1 calc R . .
H64B H 0.4422 0.1390 0.7712 0.047 Uiso 1 1 calc R . .
C65 C 0.1558(3) 0.2829(4) 0.8358(4) 0.0383(12) Uani 1 1 d . . .
H65A H 0.1338 0.2212 0.7922 0.046 Uiso 1 1 calc R . .
H65B H 0.1199 0.2871 0.8845 0.046 Uiso 1 1 calc R . .
C71 C 0.2783(7) 0.0052(7) -0.0027(6) 0.096(3) Uani 1 1 d . . .
C72 C 0.2638(8) 0.0958(6) 0.0020(6) 0.090(3) Uani 1 1 d . . .
H72 H 0.3050 0.1370 -0.0172 0.108 Uiso 1 1 calc R . .
C73 C 0.1871(9) 0.1263(7) 0.0357(6) 0.105(3) Uani 1 1 d . . .
H73 H 0.1773 0.1886 0.0387 0.127 Uiso 1 1 calc R . .
C74 C 0.1273(8) 0.0701(9) 0.0636(6) 0.105(3) Uani 1 1 d . . .
H74 H 0.0757 0.0919 0.0857 0.126 Uiso 1 1 calc R . .
C75 C 0.1438(10) -0.0236(9) 0.0591(7) 0.124(4) Uani 1 1 d . . .
H75 H 0.1023 -0.0640 0.0790 0.149 Uiso 1 1 calc R . .
C76 C 0.2188(9) -0.0576(7) 0.0264(7) 0.104(3) Uani 1 1 d . . .
H76 H 0.2293 -0.1198 0.0238 0.125 Uiso 1 1 calc R . .
C77 C 0.3596(8) -0.0314(10) -0.0409(9) 0.163(6) Uani 1 1 d . . .
H77A H 0.3404 -0.0495 -0.1087 0.245 Uiso 1 1 calc R . .
H77B H 0.3753 -0.0854 -0.0173 0.245 Uiso 1 1 calc R . .
H77C H 0.4150 0.0174 -0.0212 0.245 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 P1 O2 102.45(17) . . y
O3 P1 Cl1 94.35(13) . . y
O2 P1 Cl1 95.39(13) . . y
O4 P2 O5 103.10(19) . . y
O4 P2 Cl2 101.63(15) . . y
O5 P2 Cl2 95.69(15) . . y
C21 O2 P1 116.2(3) . . ?
C31 O3 P1 119.0(3) . . ?
C41 O4 P2 138.2(3) . . ?
C51 O5 P2 121.6(3) . . ?
O1 C11 C12 117.5(4) . . ?
O1 C11 C16 121.6(4) . . ?
C12 C11 C16 120.7(4) . . ?
C13 C12 C11 118.3(4) . . ?
C13 C12 C65 120.9(5) . . ?
C11 C12 C65 120.6(4) . . ?
C12 C13 C14 123.8(5) . . ?
C13 C14 C15 116.0(5) . . ?
C13 C14 C17 122.1(5) . . ?
C15 C14 C17 121.8(5) . . ?
C16 C15 C14 123.2(5) . . ?
C15 C16 C11 117.9(4) . . ?
C15 C16 C61 120.4(4) . . ?
C11 C16 C61 121.3(4) . . ?
C191 C17 C201 107(3) . . ?
C191 C17 C20 126(3) . . ?
C201 C17 C20 33(2) . . ?
C191 C17 C19 32(2) . . ?
C201 C17 C19 79(2) . . ?
C20 C17 C19 106.8(8) . . ?
C191 C17 C18 79(2) . . ?
C201 C17 C18 137(2) . . ?
C20 C17 C18 109.6(8) . . ?
C19 C17 C18 109.3(9) . . ?
C191 C17 C14 115(3) . . ?
C201 C17 C14 108(2) . . ?
C20 C17 C14 112.5(5) . . ?
C19 C17 C14 110.9(6) . . ?
C18 C17 C14 107.8(6) . . ?
C191 C17 C181 106(3) . . ?
C201 C17 C181 115(3) . . ?
C20 C17 C181 83(2) . . ?
C19 C17 C181 133(2) . . ?
C18 C17 C181 30(2) . . ?
C14 C17 C181 107(2) . . ?
C22 C21 C26 122.1(4) . . ?
C22 C21 O2 118.5(4) . . ?
C26 C21 O2 119.2(4) . . ?
C21 C22 C23 117.3(4) . . ?
C21 C22 C61 122.4(4) . . ?
C23 C22 C61 120.2(4) . . ?
C22 C23 C24 122.5(5) . . ?
C25 C24 C23 117.7(5) . . ?
C25 C24 C27 120.8(5) . . ?
C23 C24 C27 121.5(5) . . ?
C24 C25 C26 122.1(5) . . ?
C25 C26 C21 118.1(4) . . ?
C25 C26 C62 119.8(4) . . ?
C21 C26 C62 122.1(4) . . ?
C281 C27 C30 136.4(12) . . ?
C281 C27 C28 42.5(11) . . ?
C30 C27 C28 116.6(9) . . ?
C281 C27 C291 115.7(15) . . ?
C30 C27 C291 39.8(10) . . ?
C28 C27 C291 130.2(11) . . ?
C281 C27 C24 110.4(12) . . ?
C30 C27 C24 113.1(6) . . ?
C28 C27 C24 113.5(6) . . ?
C291 C27 C24 116.3(11) . . ?
C281 C27 C29 59.1(12) . . ?
C30 C27 C29 107.9(10) . . ?
C28 C27 C29 100.1(9) . . ?
C291 C27 C29 68.6(12) . . ?
C24 C27 C29 103.7(6) . . ?
C281 C27 C301 104.9(14) . . ?
C30 C27 C301 64.9(10) . . ?
C28 C27 C301 63.0(10) . . ?
C291 C27 C301 102.5(13) . . ?
C24 C27 C301 105.5(8) . . ?
C29 C27 C301 150.3(9) . . ?
C32 C31 C36 122.7(4) . . ?
C32 C31 O3 119.2(4) . . ?
C36 C31 O3 117.9(4) . . ?
C31 C32 C33 119.0(5) . . ?
C31 C32 C62 120.4(4) . . ?
C33 C32 C62 120.6(4) . . ?
C34 C33 C32 121.1(5) . . ?
C35 C34 C33 117.7(5) . . ?
C35 C34 C37 120.6(5) . . ?
C33 C34 C37 121.6(5) . . ?
C34 C35 C36 122.7(5) . . ?
C31 C36 C35 116.8(4) . . ?
C31 C36 C63 123.1(4) . . ?
C35 C36 C63 120.1(4) . . ?
C381 C37 C39 135.7(11) . . ?
C381 C37 C38 57.4(11) . . ?
C39 C37 C38 111.5(12) . . ?
C381 C37 C401 112.0(14) . . ?
C39 C37 C401 42.0(10) . . ?
C38 C37 C401 135.5(9) . . ?
C381 C37 C34 110.7(8) . . ?
C39 C37 C34 112.6(8) . . ?
C38 C37 C34 112.6(7) . . ?
C401 C37 C34 111.4(8) . . ?
C381 C37 C40 50.3(11) . . ?
C39 C37 C40 106.9(12) . . ?
C38 C37 C40 105.4(12) . . ?
C401 C37 C40 67.4(12) . . ?
C34 C37 C40 107.3(7) . . ?
C381 C37 C391 111.6(14) . . ?
C39 C37 C391 63.6(12) . . ?
C38 C37 C391 55.9(11) . . ?
C401 C37 C391 104.4(13) . . ?
C34 C37 C391 106.5(8) . . ?
C40 C37 C391 145.8(9) . . ?
C46 C41 C42 122.3(4) . . ?
C46 C41 O4 121.9(4) . . ?
C42 C41 O4 115.8(4) . . ?
C43 C42 C41 117.9(5) . . ?
C43 C42 C63 120.9(4) . . ?
C41 C42 C63 121.1(4) . . ?
C42 C43 C44 122.3(5) . . ?
C45 C44 C43 117.4(5) . . ?
C45 C44 C47 123.2(5) . . ?
C43 C44 C47 119.3(5) . . ?
C44 C45 C46 123.4(5) . . ?
C41 C46 C45 116.7(4) . . ?
C41 C46 C64 124.4(4) . . ?
C45 C46 C64 118.9(5) . . ?
C48 C47 C50 110.8(6) . . ?
C48 C47 C44 110.4(5) . . ?
C50 C47 C44 111.8(5) . . ?
C48 C47 C49 110.0(6) . . ?
C50 C47 C49 106.6(6) . . ?
C44 C47 C49 107.1(5) . . ?
C52 C51 C56 121.8(4) . . ?
C52 C51 O5 119.7(4) . . ?
C56 C51 O5 118.4(4) . . ?
C53 C52 C51 118.4(4) . . ?
C53 C52 C64 121.0(5) . . ?
C51 C52 C64 120.5(4) . . ?
C52 C53 C54 122.5(5) . . ?
C55 C54 C53 116.3(5) . . ?
C55 C54 C57 123.8(5) . . ?
C53 C54 C57 119.8(5) . . ?
C54 C55 C56 123.6(5) . . ?
C55 C56 C51 117.4(4) . . ?
C55 C56 C65 122.1(4) . . ?
C51 C56 C65 120.5(4) . . ?
C59 C57 C54 110.9(5) . . ?
C59 C57 C60 109.5(6) . . ?
C54 C57 C60 112.1(5) . . ?
C59 C57 C58 108.9(6) . . ?
C54 C57 C58 109.5(5) . . ?
C60 C57 C58 105.8(6) . . ?
C22 C61 C16 118.2(4) . . ?
C26 C62 C32 111.8(4) . . ?
C42 C63 C36 112.8(4) . . ?
C46 C64 C52 115.6(4) . . ?
C12 C65 C56 113.9(4) . . ?
C72 C71 C76 121.8(11) . . ?
C72 C71 C77 120.8(11) . . ?
C76 C71 C77 117.4(11) . . ?
C71 C72 C73 119.1(9) . . ?
C74 C73 C72 122.2(11) . . ?
C73 C74 C75 118.0(11) . . ?
C76 C75 C74 122.2(10) . . ?
C75 C76 C71 116.6(10) . . ?
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
P1 O3 1.633(3) . y
P1 O2 1.645(3) . y
P1 Cl1 2.0498(18) . y
P2 O4 1.597(3) . y
P2 O5 1.640(4) . y
P2 Cl2 2.064(2) . y
O1 C11 1.379(6) . ?
O2 C21 1.411(5) . ?
O3 C31 1.419(5) . ?
O4 C41 1.398(5) . ?
O5 C51 1.406(6) . ?
C11 C12 1.395(7) . ?
C11 C16 1.403(6) . ?
C12 C13 1.372(7) . ?
C12 C65 1.513(7) . ?
C13 C14 1.383(7) . ?
C14 C15 1.399(7) . ?
C14 C17 1.535(7) . ?
C15 C16 1.380(7) . ?
C16 C61 1.515(6) . ?
C17 C191 1.38(7) . ?
C17 C201 1.51(6) . ?
C17 C20 1.513(10) . ?
C17 C19 1.526(14) . ?
C17 C18 1.531(13) . ?
C17 C181 1.59(5) . ?
C21 C22 1.389(7) . ?
C21 C26 1.395(6) . ?
C22 C23 1.395(7) . ?
C22 C61 1.508(7) . ?
C23 C24 1.400(7) . ?
C24 C25 1.378(7) . ?
C24 C27 1.541(7) . ?
C25 C26 1.394(7) . ?
C26 C62 1.521(7) . ?
C27 C281 1.36(2) . ?
C27 C30 1.401(12) . ?
C27 C28 1.486(12) . ?
C27 C291 1.51(3) . ?
C27 C29 1.654(14) . ?
C27 C301 1.78(2) . ?
C31 C32 1.365(7) . ?
C31 C36 1.390(6) . ?
C32 C33 1.395(7) . ?
C32 C62 1.523(7) . ?
C33 C34 1.393(7) . ?
C34 C35 1.387(7) . ?
C34 C37 1.542(7) . ?
C35 C36 1.400(6) . ?
C36 C63 1.520(7) . ?
C37 C381 1.452(17) . ?
C37 C39 1.473(17) . ?
C37 C38 1.493(16) . ?
C37 C401 1.52(2) . ?
C37 C40 1.60(2) . ?
C37 C391 1.62(2) . ?
C41 C46 1.394(7) . ?
C41 C42 1.395(6) . ?
C42 C43 1.385(7) . ?
C42 C63 1.497(7) . ?
C43 C44 1.392(7) . ?
C44 C45 1.378(7) . ?
C44 C47 1.545(7) . ?
C45 C46 1.397(7) . ?
C46 C64 1.515(7) . ?
C47 C48 1.496(10) . ?
C47 C50 1.518(10) . ?
C47 C49 1.555(9) . ?
C51 C52 1.382(7) . ?
C51 C56 1.393(6) . ?
C52 C53 1.375(7) . ?
C52 C64 1.524(6) . ?
C53 C54 1.407(7) . ?
C54 C55 1.379(7) . ?
C54 C57 1.525(7) . ?
C55 C56 1.382(7) . ?
C56 C65 1.521(7) . ?
C57 C59 1.504(8) . ?
C57 C60 1.532(9) . ?
C57 C58 1.563(9) . ?
C71 C72 1.350(12) . ?
C71 C76 1.386(13) . ?
C71 C77 1.501(14) . ?
C72 C73 1.379(13) . ?
C73 C74 1.315(13) . ?
C74 C75 1.404(15) . ?
C75 C76 1.368(15) . ?
