#------------------------------------------------------------------------------
#$Date: 2021-10-06 18:32:35 +0300 (Wed, 06 Oct 2021) $
#$Revision: 269706 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/81/7708149.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_7708149
loop_
_publ_author_name
'Guschlbauer, Jannick'
'Vollgraff, Tobias'
'Xie, Xiulan'
'Fetoh, Ahmed'
'Sundermeyer, Jörg'
_publ_section_title
;
 Heavy silylchalcogenido lanthanates synthesis
 Ph₄P[Cp₃La-ESiMe₃] (E = S, Se, and Te)
 via fluoride-induced demethylation of dimethylcarbonate to
 Ph₄P[OCO₂Me] key intermediate.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13103
_journal_page_last               13111
_journal_paper_doi               10.1039/d1dt02000e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '2(C36 H30 N P2 1+), 2(C2 H3 O3 1-), C2 H3 N'
_chemical_formula_sum            'C78 H69 N3 O6 P4'
_chemical_formula_weight         1268.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-05-31 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.36(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.620(2)
_cell_length_b                   35.750(7)
_cell_length_c                   17.320(3)
_cell_measurement_reflns_used    9109
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.1306
_cell_measurement_theta_min      2.2439
_cell_volume                     6522(2)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service v3.0.26'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics
'DIAMOND 4 (H. Putz, K.Brandenburg, Crystal Impact GbR, Kreuzherrenstr. 102, 53227 Bonn, Germany)'
_computing_publication_material
'WinGX 2014.1 (L.J. Farrugia, J. Appl. Cryst. 2012, 45, 849-854)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 Quest (Bruker AXS Inc.)'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            175989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'I\mS Microfocus Source'
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.633
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.232
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         11537
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0347P)²+5.7788P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9648
_reflns_number_total             11537
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02000e2.cif
_cod_data_source_block           hq07_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7708147--7708155.cif.
;
_cod_original_cell_volume        6521(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7708149
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.898
_shelx_estimated_absorpt_t_max   0.961
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.36250(5) 0.77787(2) 0.69122(3) 0.01261(11) Uani 1 1 d . . . . .
P2 P 0.46856(5) 0.72232(2) 0.80530(3) 0.01268(11) Uani 1 1 d . . . . .
P3 P 0.44586(5) 0.52950(2) 0.29034(3) 0.01356(11) Uani 1 1 d . . . . .
P4 P 0.65752(4) 0.48474(2) 0.24317(3) 0.01165(11) Uani 1 1 d . . . . .
O1 O 0.84577(16) 0.62669(5) 0.33518(10) 0.0385(4) Uani 1 1 d . . . . .
O2 O 0.9257(2) 0.64334(5) 0.45738(13) 0.0750(8) Uani 1 1 d . U . . .
O3 O 0.9610(2) 0.58613(5) 0.41452(11) 0.0563(6) Uani 1 1 d . . . . .
O4 O 0.01729(16) 0.41757(4) 0.08132(10) 0.0342(4) Uani 1 1 d . . . . .
O5 O 0.11720(14) 0.37570(4) 0.01488(9) 0.0263(4) Uani 1 1 d . . . . .
O6 O 0.11244(14) 0.36702(4) 0.13995(8) 0.0245(3) Uani 1 1 d . . . . .
N1 N 0.40632(15) 0.76069(4) 0.77475(9) 0.0155(4) Uani 1 1 d . . . . .
N2 N 0.58613(15) 0.51561(4) 0.28675(9) 0.0163(4) Uani 1 1 d . . . . .
N3 N 0.9315(2) 0.75667(8) 0.21575(16) 0.0571(7) Uani 1 1 d . . . . .
C1 C 0.23701(18) 0.81062(5) 0.69996(11) 0.0145(4) Uani 1 1 d . . . . .
C2 C 0.23224(19) 0.82918(6) 0.77032(12) 0.0204(4) Uani 1 1 d . . . . .
H2 H 0.292797 0.823664 0.814101 0.025 Uiso 1 1 calc R U . . .
C3 C 0.1388(2) 0.85573(6) 0.77614(13) 0.0258(5) Uani 1 1 d . . . . .
H3 H 0.134576 0.868225 0.824145 0.031 Uiso 1 1 calc R U . . .
C4 C 0.0517(2) 0.86401(6) 0.71214(13) 0.0247(5) Uani 1 1 d . . . . .
H4 H -0.012494 0.882124 0.716528 0.030 Uiso 1 1 calc R U . . .
C5 C 0.05698(19) 0.84623(6) 0.64186(13) 0.0229(5) Uani 1 1 d . . . . .
H5 H -0.002272 0.852402 0.597864 0.027 Uiso 1 1 calc R U . . .
C6 C 0.14915(18) 0.81932(6) 0.63579(12) 0.0191(4) Uani 1 1 d . . . . .
H6 H 0.152366 0.806786 0.587718 0.023 Uiso 1 1 calc R U . . .
C7 C 0.48900(18) 0.80378(5) 0.65686(11) 0.0136(4) Uani 1 1 d . . . . .
C8 C 0.6008(2) 0.80958(6) 0.70607(13) 0.0239(5) Uani 1 1 d . . . . .
H8 H 0.611302 0.798969 0.756781 0.029 Uiso 1 1 calc R U . . .
C9 C 0.6977(2) 0.83090(7) 0.68139(14) 0.0305(5) Uani 1 1 d . . . . .
H9 H 0.773711 0.835317 0.715447 0.037 Uiso 1 1 calc R U . . .
C10 C 0.6827(2) 0.84558(6) 0.60718(13) 0.0253(5) Uani 1 1 d . . . . .
H10 H 0.750456 0.858948 0.589060 0.030 Uiso 1 1 calc R U . . .
C11 C 0.5699(2) 0.84098(6) 0.55916(13) 0.0236(5) Uani 1 1 d . . . . .
H11 H 0.559310 0.852073 0.508907 0.028 Uiso 1 1 calc R U . . .
C12 C 0.47250(19) 0.82044(6) 0.58330(12) 0.0197(4) Uani 1 1 d . . . . .
H12 H 0.394581 0.817626 0.550176 0.024 Uiso 1 1 calc R U . . .
C13 C 0.29948(18) 0.74473(5) 0.61785(11) 0.0162(4) Uani 1 1 d . . . . .
C14 C 0.1850(2) 0.72750(6) 0.62817(13) 0.0227(5) Uani 1 1 d . . . . .
H14 H 0.145105 0.732981 0.672921 0.027 Uiso 1 1 calc R U . . .
C15 C 0.1296(2) 0.70241(6) 0.57318(14) 0.0288(5) Uani 1 1 d . . . . .
H15 H 0.051632 0.690669 0.580323 0.035 Uiso 1 1 calc R U . . .
C16 C 0.1870(2) 0.69436(6) 0.50791(14) 0.0295(5) Uani 1 1 d . . . . .
H16 H 0.148376 0.677270 0.470060 0.035 Uiso 1 1 calc R U . . .
C17 C 0.3006(2) 0.71122(6) 0.49792(13) 0.0291(5) Uani 1 1 d . . . . .
H17 H 0.339890 0.705660 0.453006 0.035 Uiso 1 1 calc R U . . .
C18 C 0.3582(2) 0.73629(6) 0.55291(12) 0.0220(5) Uani 1 1 d . . . . .
H18 H 0.437012 0.747534 0.546041 0.026 Uiso 1 1 calc R U . . .
C19 C 0.59908(18) 0.73189(5) 0.87979(11) 0.0148(4) Uani 1 1 d . . . . .
C20 C 0.68791(19) 0.70453(6) 0.90552(12) 0.0191(4) Uani 1 1 d . . . . .
H20 H 0.684604 0.680787 0.880696 0.023 Uiso 1 1 calc R U . . .
C21 C 0.7811(2) 0.71182(6) 0.96722(13) 0.0246(5) Uani 1 1 d . . . . .
H21 H 0.841249 0.693018 0.984848 0.030 Uiso 1 1 calc R U . . .
C22 C 0.7868(2) 0.74641(7) 1.00320(13) 0.0290(5) Uani 1 1 d . . . . .
H22 H 0.849272 0.751136 1.046465 0.035 Uiso 1 1 calc R U . . .
C23 C 0.7016(2) 0.77411(6) 0.97617(13) 0.0285(5) Uani 1 1 d . . . . .
H23 H 0.707847 0.798191 0.999545 0.034 Uiso 1 1 calc R U . . .
C24 C 0.6072(2) 0.76691(6) 0.91522(12) 0.0204(4) Uani 1 1 d . . . . .
H24 H 0.547906 0.785904 0.897516 0.025 Uiso 1 1 calc R U . . .
C25 C 0.52926(19) 0.69280(5) 0.73464(11) 0.0167(4) Uani 1 1 d . . . . .
C26 C 0.4576(2) 0.66347(6) 0.69851(12) 0.0221(5) Uani 1 1 d . . . . .
H26 H 0.374590 0.658687 0.710989 0.027 Uiso 1 1 calc R U . . .
C27 C 0.5080(2) 0.64138(6) 0.64447(13) 0.0297(6) Uani 1 1 d . . . . .
H27 H 0.459327 0.621409 0.619846 0.036 Uiso 1 1 calc R U . . .
C28 C 0.6288(2) 0.64824(6) 0.62614(13) 0.0320(6) Uani 1 1 d . . . . .
H28 H 0.663654 0.632590 0.589964 0.038 Uiso 1 1 calc R U . . .
C29 C 0.6989(2) 0.67786(7) 0.66036(13) 0.0305(5) Uani 1 1 d . . . . .
H29 H 0.781084 0.682932 0.646705 0.037 Uiso 1 1 calc R U . . .
C30 C 0.6495(2) 0.69998(6) 0.71424(12) 0.0227(5) Uani 1 1 d . . . . .
H30 H 0.697939 0.720285 0.737663 0.027 Uiso 1 1 calc R U . . .
C31 C 0.35397(18) 0.69564(5) 0.85020(11) 0.0158(4) Uani 1 1 d . . . . .
C32 C 0.2404(2) 0.71198(6) 0.86386(13) 0.0261(5) Uani 1 1 d . . . . .
H32 H 0.220492 0.736690 0.846148 0.031 Uiso 1 1 calc R U . . .
C33 C 0.1562(2) 0.69234(8) 0.90325(15) 0.0370(6) Uani 1 1 d . . . . .
H33 H 0.078859 0.703687 0.912973 0.044 Uiso 1 1 calc R U . . .
C34 C 0.1842(2) 0.65633(7) 0.92842(13) 0.0325(6) Uani 1 1 d . . . . .
H34 H 0.126669 0.643024 0.955979 0.039 Uiso 1 1 calc R U . . .
C35 C 0.2958(2) 0.63959(6) 0.91364(12) 0.0269(5) Uani 1 1 d . . . . .
H35 H 0.313991 0.614605 0.930106 0.032 Uiso 1 1 calc R U . . .
C36 C 0.3811(2) 0.65901(5) 0.87504(11) 0.0205(5) Uani 1 1 d . . . . .
H36 H 0.458210 0.647490 0.865375 0.025 Uiso 1 1 calc R U . . .
C37 C 0.45875(19) 0.57084(5) 0.35016(11) 0.0157(4) Uani 1 1 d . . . . .
C38 C 0.56470(19) 0.59384(5) 0.35048(12) 0.0195(4) Uani 1 1 d . . . . .
H38 H 0.629466 0.587624 0.319611 0.023 Uiso 1 1 calc R U . . .
C39 C 0.5752(2) 0.62589(6) 0.39615(12) 0.0220(5) Uani 1 1 d . . . . .
H39 H 0.647271 0.641672 0.396623 0.026 Uiso 1 1 calc R U . . .
C40 C 0.4810(2) 0.63475(6) 0.44073(12) 0.0226(5) Uani 1 1 d . . . . .
H40 H 0.488756 0.656671 0.471985 0.027 Uiso 1 1 calc R U . . .
C41 C 0.3756(2) 0.61222(6) 0.44062(13) 0.0250(5) Uani 1 1 d . . . . .
H41 H 0.311323 0.618633 0.471671 0.030 Uiso 1 1 calc R U . . .
C42 C 0.3636(2) 0.58013(6) 0.39505(12) 0.0212(5) Uani 1 1 d . . . . .
H42 H 0.290903 0.564618 0.394534 0.025 Uiso 1 1 calc R U . . .
C43 C 0.36072(18) 0.54184(5) 0.19723(11) 0.0150(4) Uani 1 1 d . . . . .
C44 C 0.3542(2) 0.57915(6) 0.17295(12) 0.0206(5) Uani 1 1 d . . . . .
H44 H 0.390684 0.598240 0.206870 0.025 Uiso 1 1 calc R U . . .
C45 C 0.2947(2) 0.58836(6) 0.09958(12) 0.0231(5) Uani 1 1 d . . . . .
H45 H 0.290101 0.613780 0.083503 0.028 Uiso 1 1 calc R U . . .
C46 C 0.24198(19) 0.56076(6) 0.04951(12) 0.0210(5) Uani 1 1 d . . . . .
H46 H 0.200483 0.567240 -0.000574 0.025 Uiso 1 1 calc R U . . .
C47 C 0.24990(18) 0.52359(6) 0.07270(12) 0.0194(4) Uani 1 1 d . . . . .
H47 H 0.215154 0.504570 0.038028 0.023 Uiso 1 1 calc R U . . .
C48 C 0.30816(18) 0.51416(6) 0.14608(12) 0.0169(4) Uani 1 1 d . . . . .
H48 H 0.312476 0.488681 0.161798 0.020 Uiso 1 1 calc R U . . .
C49 C 0.35150(18) 0.49674(5) 0.33768(11) 0.0154(4) Uani 1 1 d . . . . .
C50 C 0.2214(2) 0.49249(6) 0.31748(13) 0.0227(5) Uani 1 1 d . . . . .
H50 H 0.178627 0.505993 0.274682 0.027 Uiso 1 1 calc R U . . .
C51 C 0.1540(2) 0.46844(6) 0.36002(14) 0.0294(5) Uani 1 1 d . . . . .
H51 H 0.065236 0.465295 0.345557 0.035 Uiso 1 1 calc R U . . .
C52 C 0.2145(2) 0.44902(6) 0.42318(14) 0.0287(5) Uani 1 1 d . . . . .
H52 H 0.167519 0.432921 0.452467 0.034 Uiso 1 1 calc R U . . .
C53 C 0.3442(2) 0.45319(6) 0.44345(13) 0.0266(5) Uani 1 1 d . . . . .
H53 H 0.386321 0.439808 0.486636 0.032 Uiso 1 1 calc R U . . .
C54 C 0.4127(2) 0.47674(6) 0.40109(12) 0.0207(5) Uani 1 1 d . . . . .
H54 H 0.501702 0.479360 0.415130 0.025 Uiso 1 1 calc R U . . .
C55 C 0.55610(17) 0.45643(5) 0.17569(11) 0.0145(4) Uani 1 1 d . . . . .
C56 C 0.55009(19) 0.46162(6) 0.09561(12) 0.0201(4) Uani 1 1 d . . . . .
H56 H 0.607255 0.478322 0.075361 0.024 Uiso 1 1 calc R U . . .
C57 C 0.4604(2) 0.44232(6) 0.04545(13) 0.0270(5) Uani 1 1 d . . . . .
H57 H 0.456211 0.445772 -0.009203 0.032 Uiso 1 1 calc R U . . .
C58 C 0.3771(2) 0.41813(6) 0.07492(14) 0.0292(5) Uani 1 1 d . . . . .
H58 H 0.314687 0.405380 0.040455 0.035 Uiso 1 1 calc R U . . .
C59 C 0.3841(2) 0.41230(6) 0.15460(14) 0.0255(5) Uani 1 1 d . . . . .
H59 H 0.327538 0.395250 0.174389 0.031 Uiso 1 1 calc R U . . .
C60 C 0.47326(18) 0.43127(5) 0.20521(13) 0.0186(4) Uani 1 1 d . . . . .
H60 H 0.478266 0.427248 0.259732 0.022 Uiso 1 1 calc R U . . .
C61 C 0.74058(17) 0.45343(5) 0.31308(11) 0.0150(4) Uani 1 1 d . . . . .
C62 C 0.77393(19) 0.41744(5) 0.29114(12) 0.0191(4) Uani 1 1 d . . . . .
H62 H 0.748934 0.408859 0.239540 0.023 Uiso 1 1 calc R U . . .
C63 C 0.8435(2) 0.39442(6) 0.34493(13) 0.0243(5) Uani 1 1 d . . . . .
H63 H 0.865723 0.369963 0.330064 0.029 Uiso 1 1 calc R U . . .
C64 C 0.8806(2) 0.40656(6) 0.41958(13) 0.0253(5) Uani 1 1 d . . . . .
H64 H 0.928718 0.390568 0.455961 0.030 Uiso 1 1 calc R U . . .
C65 C 0.8480(2) 0.44222(6) 0.44196(13) 0.0254(5) Uani 1 1 d . . . . .
H65 H 0.873752 0.450545 0.493655 0.030 Uiso 1 1 calc R U . . .
C66 C 0.77751(18) 0.46580(6) 0.38887(12) 0.0193(4) Uani 1 1 d . . . . .
H66 H 0.754818 0.490142 0.404234 0.023 Uiso 1 1 calc R U . . .
C67 C 0.76993(17) 0.50613(5) 0.18809(11) 0.0127(4) Uani 1 1 d . . . . .
C68 C 0.86755(18) 0.48495(5) 0.16285(12) 0.0166(4) Uani 1 1 d . . . . .
H68 H 0.879942 0.459726 0.179314 0.020 Uiso 1 1 calc R U . . .
C69 C 0.94614(19) 0.50075(6) 0.11389(12) 0.0210(5) Uani 1 1 d . . . . .
H69 H 1.012890 0.486425 0.097066 0.025 Uiso 1 1 calc R U . . .
C70 C 0.92740(19) 0.53749(6) 0.08939(12) 0.0214(5) Uani 1 1 d . . . . .
H70 H 0.980613 0.548215 0.055209 0.026 Uiso 1 1 calc R U . . .
C71 C 0.83159(19) 0.55846(6) 0.11460(12) 0.0213(5) Uani 1 1 d . . . . .
H71 H 0.819729 0.583684 0.098012 0.026 Uiso 1 1 calc R U . . .
C72 C 0.75263(19) 0.54313(5) 0.16376(12) 0.0178(4) Uani 1 1 d . . . . .
H72 H 0.686859 0.557765 0.180889 0.021 Uiso 1 1 calc R U . . .
C73 C 0.9061(2) 0.62197(7) 0.40092(16) 0.0378(6) Uani 1 1 d . . . . .
C74 C 0.9348(3) 0.55936(7) 0.35486(15) 0.0413(6) Uani 1 1 d . . . . .
H74A H 0.970438 0.535148 0.372954 0.062 Uiso 1 1 calc R U . . .
H74B H 0.973044 0.567343 0.308980 0.062 Uiso 1 1 calc R U . . .
H74C H 0.842717 0.556987 0.341173 0.062 Uiso 1 1 calc R U . . .
C75 C 0.07924(19) 0.38906(6) 0.07321(12) 0.0200(5) Uani 1 1 d . . . . .
C76 C 0.0660(2) 0.37936(9) 0.20901(14) 0.0423(7) Uani 1 1 d . . . . .
H76A H 0.087509 0.360887 0.250407 0.063 Uiso 1 1 calc R U . . .
H76B H -0.026394 0.382261 0.199115 0.063 Uiso 1 1 calc R U . . .
H76C H 0.104963 0.403438 0.225121 0.063 Uiso 1 1 calc R U . . .
C77 C 0.9350(3) 0.71656(7) 0.33935(15) 0.0389(6) Uani 1 1 d . . . . .
H77A H 0.909573 0.690889 0.324895 0.058 Uiso 1 1 calc R U . . .
H77B H 0.875521 0.727153 0.372280 0.058 Uiso 1 1 calc R U . . .
H77C H 1.020785 0.716430 0.368044 0.058 Uiso 1 1 calc R U . . .
C78 C 0.9339(2) 0.73889(7) 0.27002(15) 0.0311(5) Uani 1 1 d . . . . .
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'
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
N1 P1 C1 108.07(9) . . ?
N1 P1 C7 110.96(9) . . ?
C1 P1 C7 106.67(9) . . ?
N1 P1 C13 115.32(9) . . ?
C1 P1 C13 105.99(9) . . ?
C7 P1 C13 109.36(9) . . ?
N1 P2 C25 116.85(9) . . ?
N1 P2 C31 109.10(9) . . ?
C25 P2 C31 107.72(9) . . ?
N1 P2 C19 108.96(9) . . ?
C25 P2 C19 106.80(9) . . ?
C31 P2 C19 106.98(9) . . ?
N2 P3 C43 114.21(9) . . ?
N2 P3 C37 106.16(9) . . ?
C43 P3 C37 107.86(9) . . ?
N2 P3 C49 113.28(9) . . ?
C43 P3 C49 108.77(9) . . ?
C37 P3 C49 106.08(9) . . ?
N2 P4 C67 110.39(9) . . ?
N2 P4 C61 109.68(9) . . ?
C67 P4 C61 108.78(9) . . ?
N2 P4 C55 114.76(9) . . ?
C67 P4 C55 106.19(9) . . ?
C61 P4 C55 106.82(9) . . ?
C74 O3 C73 117.02(19) . . ?
C75 O6 C76 116.13(17) . . ?
P2 N1 P1 134.55(11) . . ?
P3 N2 P4 138.54(11) . . ?
C6 C1 C2 119.73(18) . . ?
C6 C1 P1 120.50(15) . . ?
C2 C1 P1 119.65(15) . . ?
C3 C2 C1 119.72(19) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C4 C3 C2 120.0(2) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.6(2) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 119.7(2) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C1 120.2(2) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
C8 C7 C12 119.65(18) . . ?
C8 C7 P1 119.48(15) . . ?
C12 C7 P1 120.70(15) . . ?
C7 C8 C9 120.1(2) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 119.6(2) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C11 C10 C9 120.3(2) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C12 C11 C10 120.6(2) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C7 119.54(19) . . ?
C11 C12 H12 120.2 . . ?
C7 C12 H12 120.2 . . ?
C18 C13 C14 119.82(19) . . ?
C18 C13 P1 123.36(16) . . ?
C14 C13 P1 116.81(16) . . ?
C15 C14 C13 119.9(2) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 C14 120.3(2) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C17 C16 C15 119.8(2) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 120.7(2) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C13 C18 C17 119.4(2) . . ?
C13 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C24 119.31(18) . . ?
C20 C19 P2 121.58(15) . . ?
C24 C19 P2 119.03(15) . . ?
C21 C20 C19 120.19(19) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C20 120.1(2) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C23 C22 C21 119.9(2) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.3(2) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C19 120.11(19) . . ?
C23 C24 H24 119.9 . . ?
C19 C24 H24 119.9 . . ?
C30 C25 C26 119.31(19) . . ?
C30 C25 P2 119.05(15) . . ?
C26 C25 P2 121.62(16) . . ?
C27 C26 C25 119.8(2) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C28 C27 C26 120.3(2) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 120.1(2) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C30 C29 C28 119.9(2) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 120.5(2) . . ?
C29 C30 H30 119.7 . . ?
C25 C30 H30 119.7 . . ?
C32 C31 C36 119.49(19) . . ?
C32 C31 P2 120.07(15) . . ?
C36 C31 P2 120.37(16) . . ?
C33 C32 C31 120.1(2) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C34 C33 C32 120.1(2) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 120.1(2) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C36 C35 C34 120.3(2) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C31 119.9(2) . . ?
C35 C36 H36 120.1 . . ?
C31 C36 H36 120.1 . . ?
C42 C37 C38 120.04(18) . . ?
C42 C37 P3 120.69(15) . . ?
C38 C37 P3 119.26(15) . . ?
C39 C38 C37 119.69(19) . . ?
C39 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
C40 C39 C38 119.9(2) . . ?
C40 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
C39 C40 C41 120.85(19) . . ?
C39 C40 H40 119.6 . . ?
C41 C40 H40 119.6 . . ?
C40 C41 C42 119.9(2) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C41 C42 C37 119.6(2) . . ?
C41 C42 H42 120.2 . . ?
C37 C42 H42 120.2 . . ?
C48 C43 C44 119.03(18) . . ?
C48 C43 P3 120.58(15) . . ?
C44 C43 P3 120.23(15) . . ?
C45 C44 C43 120.15(19) . . ?
C45 C44 H44 119.9 . . ?
C43 C44 H44 119.9 . . ?
C46 C45 C44 120.42(19) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C45 C46 C47 119.78(19) . . ?
C45 C46 H46 120.1 . . ?
C47 C46 H46 120.1 . . ?
C48 C47 C46 120.22(19) . . ?
C48 C47 H47 119.9 . . ?
C46 C47 H47 119.9 . . ?
C47 C48 C43 120.39(19) . . ?
C47 C48 H48 119.8 . . ?
C43 C48 H48 119.8 . . ?
C50 C49 C54 119.26(19) . . ?
C50 C49 P3 123.26(15) . . ?
C54 C49 P3 117.33(15) . . ?
C51 C50 C49 119.8(2) . . ?
C51 C50 H50 120.1 . . ?
C49 C50 H50 120.1 . . ?
C52 C51 C50 120.7(2) . . ?
C52 C51 H51 119.6 . . ?
C50 C51 H51 119.6 . . ?
C51 C52 C53 119.6(2) . . ?
C51 C52 H52 120.2 . . ?
C53 C52 H52 120.2 . . ?
C54 C53 C52 120.3(2) . . ?
C54 C53 H53 119.9 . . ?
C52 C53 H53 119.9 . . ?
C53 C54 C49 120.3(2) . . ?
C53 C54 H54 119.8 . . ?
C49 C54 H54 119.8 . . ?
C56 C55 C60 119.90(18) . . ?
C56 C55 P4 121.33(15) . . ?
C60 C55 P4 118.48(15) . . ?
C57 C56 C55 119.8(2) . . ?
C57 C56 H56 120.1 . . ?
C55 C56 H56 120.1 . . ?
C58 C57 C56 120.1(2) . . ?
C58 C57 H57 120.0 . . ?
C56 C57 H57 120.0 . . ?
C57 C58 C59 120.4(2) . . ?
C57 C58 H58 119.8 . . ?
C59 C58 H58 119.8 . . ?
C60 C59 C58 120.1(2) . . ?
C60 C59 H59 120.0 . . ?
C58 C59 H59 120.0 . . ?
C59 C60 C55 119.7(2) . . ?
C59 C60 H60 120.2 . . ?
C55 C60 H60 120.2 . . ?
C66 C61 C62 119.80(18) . . ?
C66 C61 P4 119.50(15) . . ?
C62 C61 P4 120.63(15) . . ?
C63 C62 C61 119.7(2) . . ?
C63 C62 H62 120.1 . . ?
C61 C62 H62 120.1 . . ?
C64 C63 C62 120.7(2) . . ?
C64 C63 H63 119.7 . . ?
C62 C63 H63 119.7 . . ?
C63 C64 C65 120.1(2) . . ?
C63 C64 H64 120.0 . . ?
C65 C64 H64 120.0 . . ?
C64 C65 C66 120.2(2) . . ?
C64 C65 H65 119.9 . . ?
C66 C65 H65 119.9 . . ?
C65 C66 C61 119.5(2) . . ?
C65 C66 H66 120.2 . . ?
C61 C66 H66 120.2 . . ?
C72 C67 C68 119.60(18) . . ?
C72 C67 P4 119.68(15) . . ?
C68 C67 P4 120.42(14) . . ?
C69 C68 C67 120.00(18) . . ?
C69 C68 H68 120.0 . . ?
C67 C68 H68 120.0 . . ?
C68 C69 C70 119.98(19) . . ?
C68 C69 H69 120.0 . . ?
C70 C69 H69 120.0 . . ?
C71 C70 C69 120.05(19) . . ?
C71 C70 H70 120.0 . . ?
C69 C70 H70 120.0 . . ?
C70 C71 C72 120.65(19) . . ?
C70 C71 H71 119.7 . . ?
C72 C71 H71 119.7 . . ?
C71 C72 C67 119.71(19) . . ?
C71 C72 H72 120.1 . . ?
C67 C72 H72 120.1 . . ?
O2 C73 O1 130.8(2) . . ?
O2 C73 O3 113.8(2) . . ?
O1 C73 O3 115.3(2) . . ?
O3 C74 H74A 109.5 . . ?
O3 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
O3 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
O4 C75 O5 130.6(2) . . ?
O4 C75 O6 116.86(19) . . ?
O5 C75 O6 112.52(18) . . ?
O6 C76 H76A 109.5 . . ?
O6 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
O6 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C78 C77 H77A 109.5 . . ?
C78 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C78 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
N3 C78 C77 179.1(3) . . ?
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 N1 1.5858(17) . ?
P1 C1 1.7947(19) . ?
P1 C7 1.7947(19) . ?
P1 C13 1.802(2) . ?
P2 N1 1.5838(16) . ?
P2 C25 1.797(2) . ?
P2 C31 1.799(2) . ?
P2 C19 1.801(2) . ?
P3 N2 1.5790(17) . ?
P3 C43 1.800(2) . ?
P3 C37 1.800(2) . ?
P3 C49 1.805(2) . ?
P4 N2 1.5840(17) . ?
P4 C67 1.7922(19) . ?
P4 C61 1.7953(19) . ?
P4 C55 1.797(2) . ?
O1 C73 1.245(3) . ?
O2 C73 1.237(3) . ?
O3 C74 1.410(3) . ?
O3 C73 1.415(3) . ?
O4 C75 1.231(3) . ?
O5 C75 1.231(3) . ?
O6 C75 1.406(2) . ?
O6 C76 1.421(3) . ?
N3 C78 1.132(3) . ?
C1 C6 1.392(3) . ?
C1 C2 1.394(3) . ?
C2 C3 1.386(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.386(3) . ?
C7 C12 1.397(3) . ?
C8 C9 1.391(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.379(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.387(3) . ?
C13 C14 1.395(3) . ?
C14 C15 1.384(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.379(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.392(3) . ?
C19 C24 1.392(3) . ?
C20 C21 1.385(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.383(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.383(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.392(3) . ?
C25 C26 1.396(3) . ?
C26 C27 1.383(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.382(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.384(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.377(3) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.387(3) . ?
C31 C36 1.397(3) . ?
C32 C33 1.384(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.380(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.380(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.391(3) . ?
C37 C38 1.393(3) . ?
C38 C39 1.389(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.376(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.379(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.389(3) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C48 1.396(3) . ?
C43 C44 1.398(3) . ?
C44 C45 1.384(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.384(3) . ?
C45 H45 0.9500 . ?
C46 C47 1.388(3) . ?
C46 H46 0.9500 . ?
C47 C48 1.382(3) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C50 1.390(3) . ?
C49 C54 1.399(3) . ?
C50 C51 1.389(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.383(3) . ?
C51 H51 0.9500 . ?
C52 C53 1.385(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.383(3) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C56 1.393(3) . ?
C55 C60 1.400(3) . ?
C56 C57 1.388(3) . ?
C56 H56 0.9500 . ?
C57 C58 1.380(3) . ?
C57 H57 0.9500 . ?
C58 C59 1.388(3) . ?
C58 H58 0.9500 . ?
C59 C60 1.383(3) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 C66 1.393(3) . ?
C61 C62 1.400(3) . ?
C62 C63 1.384(3) . ?
C62 H62 0.9500 . ?
C63 C64 1.373(3) . ?
C63 H63 0.9500 . ?
C64 C65 1.389(3) . ?
C64 H64 0.9500 . ?
C65 C66 1.393(3) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C67 C72 1.393(3) . ?
C67 C68 1.398(3) . ?
C68 C69 1.384(3) . ?
C68 H68 0.9500 . ?
C69 C70 1.387(3) . ?
C69 H69 0.9500 . ?
C70 C71 1.379(3) . ?
C70 H70 0.9500 . ?
C71 C72 1.383(3) . ?
C71 H71 0.9500 . ?
C72 H72 0.9500 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 C78 1.441(4) . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
