#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:34:11 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179067 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/29/4302945.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_4302945
loop_
_publ_author_name
'Patrick Achord'
'Etsuko Fujita'
'James T. Muckerman'
'Brian Scott'
'George C. Fortman'
'Manuel Temprado'
'Xiaochen Cai'
'Burjor Captain'
'Derek Isrow'
'John J. Weir'
'James Eric McDonough'
'Carl D. Hoff'
_publ_section_title
;
Experimental and Computational Studies of Binding of Dinitrogen, Nitriles,
Azides, Diazoalkanes, Pyridine, and Pyrazines to M(PR3)2(CO)3 (M = Mo, W; R
= Me,iPr).
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7891
_journal_page_last               7904
_journal_paper_doi               10.1021/ic900764e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C32 H57 N O3 P2 W'
_chemical_formula_weight         749.58
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.337(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.191(6)
_cell_length_b                   13.287(4)
_cell_length_c                   27.577(8)
_cell_measurement_temperature    141(2)
_cell_volume                     6937(4)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.10 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART 1k CCD'
_diffrn_measurement_method       'φ 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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31280
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.453
_exptl_absorpt_correction_T_max  0.7240
_exptl_absorpt_correction_T_min  0.4448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2001)'
_exptl_crystal_colour            yelow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.555
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.717
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         12671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.717
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0240P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                10420
_reflns_number_total             12671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900764e_si_002_3.cif
_cod_data_source_block           WkAdNC
_cod_original_cell_volume        6937(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4302945
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'
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
W1 W 0.762666(11) 0.797314(17) 0.430975(8) 0.02603(7) Uani 1 1 d . . .
W2 W 0.585206(10) 0.713125(17) 0.729095(8) 0.02357(7) Uani 1 1 d . . .
P1 P 0.76604(8) 0.60849(12) 0.43332(7) 0.0350(4) Uani 1 1 d . . .
P2 P 0.75551(8) 0.98435(11) 0.41801(6) 0.0299(3) Uani 1 1 d . . .
P3 P 0.63212(7) 0.71442(11) 0.65598(5) 0.0282(3) Uani 1 1 d . . .
P4 P 0.55240(7) 0.70867(11) 0.80887(5) 0.0238(3) Uani 1 1 d . . .
O11 O 0.9043(2) 0.7875(4) 0.4065(2) 0.0635(14) Uani 1 1 d . . .
O13 O 0.8594(3) 0.8400(4) 0.54597(18) 0.0644(14) Uani 1 1 d . . .
O12 O 0.6401(2) 0.7782(4) 0.47753(17) 0.0496(12) Uani 1 1 d . . .
O4 O 0.5701(2) 0.9510(4) 0.72005(19) 0.0563(13) Uani 1 1 d . . .
O5 O 0.4266(2) 0.7198(4) 0.65447(17) 0.0578(13) Uani 1 1 d . . .
O6 O 0.5659(3) 0.4771(4) 0.71818(19) 0.0610(14) Uani 1 1 d . . .
N1 N 0.6496(3) 0.7840(4) 0.31235(19) 0.0391(12) Uani 1 1 d . . .
N2 N 0.7477(2) 0.7111(4) 0.81230(18) 0.0326(11) Uani 1 1 d . . .
C1 C 0.6899(3) 0.5504(5) 0.4478(3) 0.0463(17) Uani 1 1 d . . .
H1 H 0.6862 0.5887 0.4771 0.056 Uiso 1 1 calc R . .
C2 C 0.6943(4) 0.4401(5) 0.4644(4) 0.076(3) Uani 1 1 d . . .
H2A H 0.6560 0.4250 0.4763 0.114 Uiso 1 1 calc R . .
H2B H 0.7384 0.4284 0.4918 0.114 Uiso 1 1 calc R . .
H2C H 0.6912 0.3977 0.4355 0.114 Uiso 1 1 calc R . .
C3 C 0.6197(3) 0.5685(6) 0.4033(3) 0.068(2) Uani 1 1 d . . .
H3A H 0.6174 0.5260 0.3746 0.101 Uiso 1 1 calc R . .
H3B H 0.6168 0.6377 0.3928 0.101 Uiso 1 1 calc R . .
H3C H 0.5811 0.5531 0.4148 0.101 Uiso 1 1 calc R . .
C4 C 0.7621(6) 0.5435(6) 0.3714(3) 0.084(3) Uani 1 1 d . . .
H4 H 0.7117 0.5457 0.3506 0.100 Uiso 1 1 calc R . .
C5 C 0.7942(5) 0.5950(6) 0.3392(3) 0.079(3) Uani 1 1 d . . .
H5A H 0.8447 0.5902 0.3545 0.119 Uiso 1 1 calc R . .
H5B H 0.7804 0.6645 0.3360 0.119 Uiso 1 1 calc R . .
H5C H 0.7789 0.5645 0.3055 0.119 Uiso 1 1 calc R . .
C6 C 0.7781(7) 0.4291(6) 0.3764(4) 0.108(4) Uani 1 1 d . . .
C7 C 0.8425(3) 0.5504(5) 0.4850(3) 0.0520(19) Uani 1 1 d . . .
H7 H 0.8378 0.4772 0.4807 0.062 Uiso 1 1 calc R . .
C8 C 0.8398(4) 0.5759(6) 0.5386(3) 0.069(2) Uani 1 1 d . . .
H8A H 0.8784 0.5436 0.5648 0.103 Uiso 1 1 calc R . .
H8B H 0.7960 0.5527 0.5409 0.103 Uiso 1 1 calc R . .
H8C H 0.8434 0.6475 0.5437 0.103 Uiso 1 1 calc R . .
C9 C 0.9133(4) 0.5797(7) 0.4814(4) 0.112(4) Uani 1 1 d . . .
H9A H 0.9201 0.6510 0.4864 0.168 Uiso 1 1 calc R . .
H9B H 0.9142 0.5619 0.4478 0.168 Uiso 1 1 calc R . .
H9C H 0.9504 0.5447 0.5075 0.168 Uiso 1 1 calc R . .
C11 C 0.8506(3) 0.7932(4) 0.4130(2) 0.0362(14) Uani 1 1 d . . .
C13 C 0.8245(3) 0.8207(5) 0.5034(2) 0.0384(15) Uani 1 1 d . . .
C12 C 0.6824(3) 0.7879(4) 0.4585(2) 0.0336(13) Uani 1 1 d . . .
C14 C 0.7425(3) 1.0264(4) 0.3506(2) 0.0373(14) Uani 1 1 d . . .
H14 H 0.6955 1.0014 0.3299 0.045 Uiso 1 1 calc R . .
C15 C 0.7388(4) 1.1403(5) 0.3407(3) 0.0510(18) Uani 1 1 d . . .
H15A H 0.7849 1.1692 0.3564 0.077 Uiso 1 1 calc R . .
H15B H 0.7068 1.1705 0.3553 0.077 Uiso 1 1 calc R . .
H15C H 0.7224 1.1526 0.3041 0.077 Uiso 1 1 calc R . .
C16 C 0.7922(4) 0.9782(5) 0.3266(3) 0.0524(18) Uani 1 1 d . . .
H16A H 0.7781 0.9971 0.2908 0.079 Uiso 1 1 calc R . .
H16B H 0.7901 0.9063 0.3292 0.079 Uiso 1 1 calc R . .
H16C H 0.8396 1.0007 0.3445 0.079 Uiso 1 1 calc R . .
C17 C 0.6791(3) 1.0468(5) 0.4284(3) 0.0423(16) Uani 1 1 d . . .
H17 H 0.6813 1.1186 0.4209 0.051 Uiso 1 1 calc R . .
C18 C 0.6835(4) 1.0375(6) 0.4846(3) 0.068(2) Uani 1 1 d . . .
H18A H 0.6457 1.0752 0.4896 0.102 Uiso 1 1 calc R . .
H18B H 0.7280 1.0634 0.5070 0.102 Uiso 1 1 calc R . .
H18C H 0.6794 0.9680 0.4927 0.102 Uiso 1 1 calc R . .
C19 C 0.6089(3) 1.0059(5) 0.3913(3) 0.056(2) Uani 1 1 d . . .
H19A H 0.6098 0.9337 0.3922 0.083 Uiso 1 1 calc R . .
H19B H 0.6019 1.0287 0.3569 0.083 Uiso 1 1 calc R . .
H19C H 0.5710 1.0298 0.4017 0.083 Uiso 1 1 calc R . .
C20 C 0.8311(3) 1.0574(5) 0.4635(2) 0.0446(16) Uani 1 1 d . . .
H20 H 0.8367 1.0308 0.4979 0.054 Uiso 1 1 calc R . .
C21 C 0.8224(4) 1.1714(5) 0.4681(3) 0.071(2) Uani 1 1 d . . .
H21A H 0.8611 1.1970 0.4967 0.107 Uiso 1 1 calc R . .
H21B H 0.7788 1.1847 0.4737 0.107 Uiso 1 1 calc R . .
H21C H 0.8216 1.2036 0.4368 0.107 Uiso 1 1 calc R . .
C22 C 0.9020(3) 1.0344(6) 0.4563(3) 0.071(2) Uani 1 1 d . . .
H22A H 0.9011 1.0606 0.4236 0.107 Uiso 1 1 calc R . .
H22B H 0.9093 0.9629 0.4571 0.107 Uiso 1 1 calc R . .
H22C H 0.9398 1.0653 0.4837 0.107 Uiso 1 1 calc R . .
C24 C 0.5503(4) 0.6899(5) 0.2548(3) 0.0481(17) Uani 1 1 d . . .
H24A H 0.5270 0.6921 0.2802 0.058 Uiso 1 1 calc R . .
H24B H 0.5786 0.6291 0.2605 0.058 Uiso 1 1 calc R . .
C25 C 0.4943(4) 0.6894(5) 0.1993(3) 0.0554(19) Uani 1 1 d . . .
H25 H 0.4635 0.6306 0.1952 0.067 Uiso 1 1 calc R . .
C26 C 0.4503(4) 0.7845(6) 0.1906(3) 0.064(2) Uani 1 1 d . . .
H26A H 0.4149 0.7837 0.1562 0.077 Uiso 1 1 calc R . .
H26B H 0.4263 0.7879 0.2155 0.077 Uiso 1 1 calc R . .
C27 C 0.4976(3) 0.8755(5) 0.1966(3) 0.0540(19) Uani 1 1 d . . .
H27 H 0.4685 0.9365 0.1907 0.065 Uiso 1 1 calc R . .
C28 C 0.5526(3) 0.8783(5) 0.2524(3) 0.0490(17) Uani 1 1 d . . .
H28A H 0.5824 0.9374 0.2568 0.059 Uiso 1 1 calc R . .
H28B H 0.5288 0.8814 0.2774 0.059 Uiso 1 1 calc R . .
C29 C 0.6350(3) 0.7782(6) 0.2211(2) 0.0510(18) Uani 1 1 d . . .
H29A H 0.6641 0.7183 0.2267 0.061 Uiso 1 1 calc R . .
H29B H 0.6653 0.8366 0.2251 0.061 Uiso 1 1 calc R . .
C30 C 0.5791(4) 0.7766(7) 0.1659(3) 0.062(2) Uani 1 1 d . . .
H30 H 0.6026 0.7730 0.1402 0.074 Uiso 1 1 calc R . .
C31 C 0.5311(4) 0.6845(6) 0.1607(3) 0.066(2) Uani 1 1 d . . .
H31A H 0.4963 0.6822 0.1260 0.079 Uiso 1 1 calc R . .
H31B H 0.5591 0.6235 0.1661 0.079 Uiso 1 1 calc R . .
C32 C 0.5350(4) 0.8722(6) 0.1580(3) 0.063(2) Uani 1 1 d . . .
H32A H 0.5653 0.9307 0.1624 0.076 Uiso 1 1 calc R . .
H32B H 0.5006 0.8735 0.1232 0.076 Uiso 1 1 calc R . .
C33 C 0.5777(3) 0.8641(5) 0.7244(3) 0.0426(16) Uani 1 1 d . . .
C34 C 0.4849(3) 0.7172(5) 0.6822(2) 0.0349(14) Uani 1 1 d . . .
C35 C 0.5763(3) 0.5628(4) 0.7239(2) 0.0297(13) Uani 1 1 d . . .
C36 C 0.5641(3) 0.7177(5) 0.5900(2) 0.0381(15) Uani 1 1 d . . .
H36 H 0.5890 0.7184 0.5651 0.046 Uiso 1 1 calc R . .
C37 C 0.5171(3) 0.6237(5) 0.5790(2) 0.0468(17) Uani 1 1 d . . .
H37A H 0.4975 0.6155 0.6059 0.070 Uiso 1 1 calc R . .
H37B H 0.5448 0.5656 0.5780 0.070 Uiso 1 1 calc R . .
H37C H 0.4795 0.6312 0.5464 0.070 Uiso 1 1 calc R . .
C38 C 0.5192(3) 0.8153(5) 0.5816(2) 0.0463(17) Uani 1 1 d . . .
H38A H 0.4794 0.8097 0.5502 0.069 Uiso 1 1 calc R . .
H38B H 0.5476 0.8719 0.5794 0.069 Uiso 1 1 calc R . .
H38C H 0.5030 0.8245 0.6102 0.069 Uiso 1 1 calc R . .
C39 C 0.6834(3) 0.8322(5) 0.6527(2) 0.0428(16) Uani 1 1 d . . .
C40 C 0.7452(4) 0.8514(6) 0.7016(3) 0.060(2) Uani 1 1 d . . .
H40A H 0.7805 0.8006 0.7056 0.090 Uiso 1 1 calc R . .
H40B H 0.7295 0.8495 0.7307 0.090 Uiso 1 1 calc R . .
H40C H 0.7649 0.9164 0.6997 0.090 Uiso 1 1 calc R . .
C41 C 0.7066(4) 0.8439(6) 0.6064(3) 0.074(3) Uani 1 1 d . . .
H41A H 0.7231 0.9114 0.6054 0.110 Uiso 1 1 calc R . .
H41B H 0.6673 0.8306 0.5753 0.110 Uiso 1 1 calc R . .
H41C H 0.7440 0.7972 0.6091 0.110 Uiso 1 1 calc R . .
C42 C 0.6808(3) 0.5966(5) 0.6504(2) 0.0429(16) Uani 1 1 d . . .
C43 C 0.7010(4) 0.5861(6) 0.6024(3) 0.075(3) Uani 1 1 d . . .
H43A H 0.7373 0.6341 0.6038 0.112 Uiso 1 1 calc R . .
H43B H 0.6603 0.5984 0.5721 0.112 Uiso 1 1 calc R . .
H43C H 0.7183 0.5193 0.6009 0.112 Uiso 1 1 calc R . .
C44 C 0.7452(4) 0.5777(6) 0.6979(3) 0.067(2) Uani 1 1 d . . .
H44A H 0.7641 0.5124 0.6954 0.101 Uiso 1 1 calc R . .
H44B H 0.7320 0.5805 0.7281 0.101 Uiso 1 1 calc R . .
H44C H 0.7802 0.6281 0.7003 0.101 Uiso 1 1 calc R . .
C45 C 0.5635(3) 0.5815(4) 0.8402(2) 0.0300(13) Uani 1 1 d . . .
H45 H 0.5335 0.5359 0.8137 0.036 Uiso 1 1 calc R . .
C46 C 0.6383(3) 0.5403(4) 0.8542(2) 0.0386(15) Uani 1 1 d . . .
H46A H 0.6700 0.5799 0.8816 0.058 Uiso 1 1 calc R . .
H46B H 0.6526 0.5433 0.8245 0.058 Uiso 1 1 calc R . .
H46C H 0.6394 0.4717 0.8654 0.058 Uiso 1 1 calc R . .
C47 C 0.5396(3) 0.5702(4) 0.8867(2) 0.0416(16) Uani 1 1 d . . .
H47A H 0.5415 0.5006 0.8964 0.062 Uiso 1 1 calc R . .
H47B H 0.4921 0.5944 0.8779 0.062 Uiso 1 1 calc R . .
H47C H 0.5702 0.6086 0.9152 0.062 Uiso 1 1 calc R . .
C48 C 0.4586(3) 0.7377(4) 0.7997(2) 0.0356(14) Uani 1 1 d . . .
H48 H 0.4545 0.7408 0.8340 0.043 Uiso 1 1 calc R . .
C49 C 0.6907(3) 0.7878(4) 0.3544(2) 0.0306(13) Uani 1 1 d . . .
C50 C 0.5977(3) 0.7824(4) 0.2607(2) 0.0328(13) Uani 1 1 d . . .
C51 C 0.6042(3) 0.7895(4) 0.8654(2) 0.0357(14) Uani 1 1 d . . .
H51 H 0.6431 0.7470 0.8868 0.043 Uiso 1 1 calc R . .
C52 C 0.6392(3) 0.8805(4) 0.8512(2) 0.0403(15) Uani 1 1 d . . .
H52A H 0.6035 0.9267 0.8313 0.060 Uiso 1 1 calc R . .
H52B H 0.6672 0.8592 0.8312 0.060 Uiso 1 1 calc R . .
H52C H 0.6689 0.9131 0.8822 0.060 Uiso 1 1 calc R . .
C53 C 0.5649(3) 0.8245(5) 0.9015(2) 0.0466(17) Uani 1 1 d . . .
H53A H 0.5979 0.8550 0.9319 0.070 Uiso 1 1 calc R . .
H53B H 0.5431 0.7676 0.9113 0.070 Uiso 1 1 calc R . .
H53C H 0.5293 0.8727 0.8838 0.070 Uiso 1 1 calc R . .
C54 C 0.6909(3) 0.7104(4) 0.7817(2) 0.0257(12) Uani 1 1 d . . .
C55 C 0.8200(3) 0.7139(4) 0.8480(2) 0.0287(12) Uani 1 1 d . . .
C56 C 0.8196(3) 0.7187(5) 0.9030(2) 0.0414(15) Uani 1 1 d . . .
H56A H 0.7956 0.6603 0.9100 0.050 Uiso 1 1 calc R . .
H56B H 0.7947 0.7785 0.9073 0.050 Uiso 1 1 calc R . .
C57 C 0.8969(3) 0.7216(5) 0.9411(2) 0.0477(17) Uani 1 1 d . . .
H57 H 0.8969 0.7247 0.9766 0.057 Uiso 1 1 calc R . .
C58 C 0.9337(4) 0.8130(5) 0.9306(3) 0.0562(19) Uani 1 1 d . . .
H58A H 0.9819 0.8152 0.9546 0.067 Uiso 1 1 calc R . .
H58B H 0.9097 0.8734 0.9354 0.067 Uiso 1 1 calc R . .
C59 C 0.9334(4) 0.8090(6) 0.8757(3) 0.063(2) Uani 1 1 d . . .
H59 H 0.9578 0.8684 0.8691 0.075 Uiso 1 1 calc R . .
C60 C 0.8564(3) 0.8077(5) 0.8375(3) 0.0510(18) Uani 1 1 d . . .
H60A H 0.8317 0.8675 0.8422 0.061 Uiso 1 1 calc R . .
H60B H 0.8558 0.8069 0.8022 0.061 Uiso 1 1 calc R . .
C61 C 0.8575(3) 0.6192(5) 0.8416(3) 0.0509(18) Uani 1 1 d . . .
H61A H 0.8574 0.6148 0.8064 0.061 Uiso 1 1 calc R . .
H61B H 0.8333 0.5606 0.8481 0.061 Uiso 1 1 calc R . .
C62 C 0.9346(3) 0.6213(6) 0.8800(3) 0.060(2) Uani 1 1 d . . .
H62 H 0.9592 0.5600 0.8760 0.072 Uiso 1 1 calc R . .
C63 C 0.9339(3) 0.6273(5) 0.9344(3) 0.0529(18) Uani 1 1 d . . .
H63A H 0.9099 0.5689 0.9414 0.063 Uiso 1 1 calc R . .
H63B H 0.9820 0.6272 0.9587 0.063 Uiso 1 1 calc R . .
C64 C 0.9714(3) 0.7134(7) 0.8681(3) 0.071(3) Uani 1 1 d . . .
H64A H 0.9705 0.7101 0.8327 0.085 Uiso 1 1 calc R . .
H64B H 1.0203 0.7148 0.8910 0.085 Uiso 1 1 calc R . .
C48A C 0.4076(3) 0.6567(5) 0.7689(3) 0.0485(17) Uani 1 1 d . . .
H48A H 0.3598 0.6787 0.7619 0.073 Uiso 1 1 calc R . .
H48B H 0.4157 0.5955 0.7885 0.073 Uiso 1 1 calc R . .
H48C H 0.4151 0.6451 0.7368 0.073 Uiso 1 1 calc R . .
C48B C 0.4382(3) 0.8409(5) 0.7746(3) 0.0497(18) Uani 1 1 d . . .
H48D H 0.4378 0.8387 0.7397 0.075 Uiso 1 1 calc R . .
H48E H 0.4719 0.8901 0.7939 0.075 Uiso 1 1 calc R . .
H48F H 0.3920 0.8588 0.7744 0.075 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'
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'
W W -0.8490 6.8722 '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
C13 W1 C11 87.2(2) . . ?
C13 W1 C12 86.4(2) . . ?
C11 W1 C12 171.1(2) . . ?
C13 W1 C49 173.4(2) . . ?
C11 W1 C49 96.4(2) . . ?
C12 W1 C49 90.5(2) . . ?
C13 W1 P2 88.44(18) . . ?
C11 W1 P2 90.23(17) . . ?
C12 W1 P2 95.81(17) . . ?
C49 W1 P2 86.03(16) . . ?
C13 W1 P1 97.43(18) . . ?
C11 W1 P1 87.73(17) . . ?
C12 W1 P1 86.92(17) . . ?
C49 W1 P1 88.24(16) . . ?
P2 W1 P1 173.67(5) . . ?
C34 W2 C35 86.3(2) . . ?
C34 W2 C33 83.9(2) . . ?
C35 W2 C33 170.1(2) . . ?
C34 W2 C54 177.62(19) . . ?
C35 W2 C54 94.3(2) . . ?
C33 W2 C54 95.5(2) . . ?
C34 W2 P3 93.50(15) . . ?
C35 W2 P3 89.94(14) . . ?
C33 W2 P3 88.99(18) . . ?
C54 W2 P3 88.80(13) . . ?
C34 W2 P4 92.92(15) . . ?
C35 W2 P4 89.69(14) . . ?
C33 W2 P4 92.47(18) . . ?
C54 W2 P4 84.78(13) . . ?
P3 W2 P4 173.53(5) . . ?
C7 P1 C4 105.3(4) . . ?
C7 P1 C1 100.9(3) . . ?
C4 P1 C1 102.9(4) . . ?
C7 P1 W1 116.2(3) . . ?
C4 P1 W1 116.2(3) . . ?
C1 P1 W1 113.5(2) . . ?
C17 P2 C14 100.5(3) . . ?
C17 P2 C20 101.0(3) . . ?
C14 P2 C20 108.2(3) . . ?
C17 P2 W1 115.5(2) . . ?
C14 P2 W1 114.79(19) . . ?
C20 P2 W1 115.1(2) . . ?
C36 P3 C42 99.7(3) . . ?
C36 P3 C39 99.4(3) . . ?
C42 P3 C39 111.9(3) . . ?
C36 P3 W2 115.49(18) . . ?
C42 P3 W2 114.5(2) . . ?
C39 P3 W2 114.1(2) . . ?
C48 P4 C45 101.7(2) . . ?
C48 P4 C51 104.0(3) . . ?
C45 P4 C51 101.0(3) . . ?
C48 P4 W2 116.2(2) . . ?
C45 P4 W2 113.50(17) . . ?
C51 P4 W2 118.16(18) . . ?
C49 N1 C50 178.1(6) . . ?
C54 N2 C55 176.5(5) . . ?
C2 C1 C3 109.3(6) . . ?
C2 C1 P1 119.3(5) . . ?
C3 C1 P1 111.2(5) . . ?
C5 C4 C6 113.4(7) . . ?
C5 C4 P1 117.0(6) . . ?
C6 C4 P1 115.2(6) . . ?
C9 C7 C8 110.8(7) . . ?
C9 C7 P1 113.1(5) . . ?
C8 C7 P1 110.3(5) . . ?
O11 C11 W1 174.5(5) . . ?
O13 C13 W1 176.2(6) . . ?
O12 C12 W1 174.5(5) . . ?
C16 C14 C15 109.5(5) . . ?
C16 C14 P2 114.9(4) . . ?
C15 C14 P2 117.0(4) . . ?
C18 C17 C19 111.2(6) . . ?
C18 C17 P2 111.3(5) . . ?
C19 C17 P2 111.3(4) . . ?
C21 C20 C22 110.1(6) . . ?
C21 C20 P2 118.4(5) . . ?
C22 C20 P2 112.8(5) . . ?
C50 C24 C25 108.8(5) . . ?
C31 C25 C26 109.4(6) . . ?
C31 C25 C24 109.2(6) . . ?
C26 C25 C24 109.7(6) . . ?
C27 C26 C25 109.7(6) . . ?
C32 C27 C26 110.6(6) . . ?
C32 C27 C28 109.8(6) . . ?
C26 C27 C28 109.5(6) . . ?
C50 C28 C27 108.1(5) . . ?
C50 C29 C30 109.4(5) . . ?
C32 C30 C31 109.4(6) . . ?
C32 C30 C29 108.6(6) . . ?
C31 C30 C29 108.9(6) . . ?
C25 C31 C30 110.6(6) . . ?
C27 C32 C30 109.6(6) . . ?
O4 C33 W2 176.7(6) . . ?
O5 C34 W2 179.3(5) . . ?
O6 C35 W2 174.7(6) . . ?
C37 C36 C38 111.1(5) . . ?
C37 C36 P3 111.7(4) . . ?
C38 C36 P3 111.0(4) . . ?
C40 C39 C41 109.5(5) . . ?
C40 C39 P3 113.2(4) . . ?
C41 C39 P3 117.3(5) . . ?
C44 C42 C43 109.2(5) . . ?
C44 C42 P3 112.5(4) . . ?
C43 C42 P3 117.0(5) . . ?
C46 C45 C47 109.0(5) . . ?
C46 C45 P4 113.0(4) . . ?
C47 C45 P4 116.9(4) . . ?
C48B C48 C48A 110.9(5) . . ?
C48B C48 P4 110.4(4) . . ?
C48A C48 P4 112.8(4) . . ?
N1 C49 W1 178.2(5) . . ?
N1 C50 C29 109.7(5) . . ?
N1 C50 C24 109.2(5) . . ?
C29 C50 C24 109.9(5) . . ?
N1 C50 C28 108.9(5) . . ?
C29 C50 C28 109.6(5) . . ?
C24 C50 C28 109.5(5) . . ?
C52 C51 C53 108.4(5) . . ?
C52 C51 P4 114.6(4) . . ?
C53 C51 P4 116.3(4) . . ?
N2 C54 W2 176.7(4) . . ?
N2 C55 C61 109.1(5) . . ?
N2 C55 C56 109.0(4) . . ?
C61 C55 C56 109.2(5) . . ?
N2 C55 C60 109.3(5) . . ?
C61 C55 C60 111.4(5) . . ?
C56 C55 C60 108.8(5) . . ?
C55 C56 C57 109.0(5) . . ?
C63 C57 C58 110.4(6) . . ?
C63 C57 C56 108.8(6) . . ?
C58 C57 C56 109.7(5) . . ?
C57 C58 C59 109.5(6) . . ?
C58 C59 C64 109.7(6) . . ?
C58 C59 C60 109.6(6) . . ?
C64 C59 C60 109.2(6) . . ?
C55 C60 C59 108.5(5) . . ?
C55 C61 C62 109.3(5) . . ?
C63 C62 C64 110.2(6) . . ?
C63 C62 C61 109.2(5) . . ?
C64 C62 C61 108.4(6) . . ?
C57 C63 C62 110.1(5) . . ?
C62 C64 C59 109.3(5) . . ?
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
W1 C13 1.977(6) . ?
W1 C11 2.004(5) . ?
W1 C12 2.018(6) . ?
W1 C49 2.111(6) . ?
W1 P2 2.5079(17) . ?
W1 P1 2.5102(17) . ?
W2 C34 1.988(6) . ?
W2 C35 2.006(6) . ?
W2 C33 2.013(7) . ?
W2 C54 2.124(6) . ?
W2 P3 2.5081(14) . ?
W2 P4 2.5090(14) . ?
P1 C7 1.865(6) . ?
P1 C4 1.890(7) . ?
P1 C1 1.883(6) . ?
P2 C17 1.859(6) . ?
P2 C14 1.869(6) . ?
P2 C20 1.875(6) . ?
P3 C36 1.860(6) . ?
P3 C42 1.883(6) . ?
P3 C39 1.895(6) . ?
P4 C48 1.862(5) . ?
P4 C45 1.875(5) . ?
P4 C51 1.882(6) . ?
O11 C11 1.162(6) . ?
O13 C13 1.169(7) . ?
O12 C12 1.154(6) . ?
O4 C33 1.166(8) . ?
O5 C34 1.162(7) . ?
O6 C35 1.159(7) . ?
N1 C49 1.169(7) . ?
N1 C50 1.445(7) . ?
N2 C54 1.162(7) . ?
N2 C55 1.450(7) . ?
C1 C2 1.529(9) . ?
C1 C3 1.536(9) . ?
C4 C5 1.441(10) . ?
C4 C6 1.549(11) . ?
C7 C9 1.519(9) . ?
C7 C8 1.538(10) . ?
C14 C16 1.524(8) . ?
C14 C15 1.536(8) . ?
C17 C18 1.528(9) . ?
C17 C19 1.530(9) . ?
C20 C21 1.535(9) . ?
C20 C22 1.543(9) . ?
C24 C50 1.530(8) . ?
C24 C25 1.555(9) . ?
C25 C31 1.497(10) . ?
C25 C26 1.515(9) . ?
C26 C27 1.513(9) . ?
C27 C32 1.505(9) . ?
C27 C28 1.554(9) . ?
C28 C50 1.537(8) . ?
C29 C50 1.528(8) . ?
C29 C30 1.548(9) . ?
C30 C32 1.524(10) . ?
C30 C31 1.537(11) . ?
C36 C37 1.534(8) . ?
C36 C38 1.553(8) . ?
C39 C40 1.507(8) . ?
C39 C41 1.514(8) . ?
C42 C44 1.511(9) . ?
C42 C43 1.521(8) . ?
C45 C46 1.524(7) . ?
C45 C47 1.529(7) . ?
C48 C48B 1.527(8) . ?
C48 C48A 1.527(8) . ?
C51 C52 1.517(8) . ?
C51 C53 1.546(7) . ?
C55 C61 1.511(8) . ?
C55 C56 1.522(8) . ?
C55 C60 1.525(8) . ?
C56 C57 1.549(8) . ?
C57 C63 1.504(9) . ?
C57 C58 1.504(9) . ?
C58 C59 1.512(10) . ?
C59 C64 1.536(11) . ?
C59 C60 1.547(8) . ?
C61 C62 1.548(9) . ?
C62 C63 1.506(9) . ?
C62 C64 1.526(10) . ?
