#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:04:53 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178767 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/21/4102132.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_4102132
loop_
_publ_author_name
'Cameron A. Lippert'
'Stephen A. Arnstein'
'C. David Sherrill'
'Jake D. Soper'
_publ_contact_author_address
;School of Chemistry and Biochemistry
Georgia Institute of Technology
Atlanta, GA  30332-0400
;
_publ_contact_author_email       jake.soper@chemistry.gatech.edu
_publ_contact_author_name        'Jake D. Soper'
_publ_contact_author_phone       404-894-4022
_publ_section_title
;
 Redox-Active Ligands Facilitate Bimetallic O2 Homolysis at
 Five-Coordinate Oxorhenium(V) Centers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3879
_journal_page_last               3892
_journal_paper_doi               10.1021/ja910500a
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C46.25 H67 N3 O3.25 Re'
_chemical_formula_weight         903.23
_chemical_name_common            (Et3NH)[ReV(O)(apPh)2]0.25MeOH
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 114.484(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6961(17)
_cell_length_b                   23.198(3)
_cell_length_c                   15.4092(19)
_cell_measurement_reflns_used    8761
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.28
_cell_volume                     4455.6(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            64625
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.768
_exptl_absorpt_correction_T_max  0.8515
_exptl_absorpt_correction_T_min  0.5685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10,Sheldrick 2003'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1866
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.988
_refine_diff_density_min         -2.288
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         11138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0364P)²+14.1003P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0951
_reflns_number_gt                9431
_reflns_number_total             11138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910500a_si_002.cif
_cod_data_source_block           '[ReV(O)(apPh)2]-'
_cod_original_cell_volume        4455.6(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4102132
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
C1 C 0.7725(3) 0.14393(16) 0.3474(3) 0.0161(8) Uani 1 1 d . . .
C2 C 0.8417(3) 0.19104(16) 0.3638(3) 0.0170(8) Uani 1 1 d . . .
C3 C 0.9454(3) 0.18316(17) 0.3711(3) 0.0187(8) Uani 1 1 d . . .
H3 H 0.9922 0.2152 0.3822 0.022 Uiso 1 1 calc R . .
C4 C 0.9804(3) 0.12773(18) 0.3618(3) 0.0207(8) Uani 1 1 d . . .
C5 C 0.9100(3) 0.08181(17) 0.3467(3) 0.0203(8) Uani 1 1 d . . .
H5 H 0.9344 0.0443 0.3409 0.024 Uiso 1 1 calc R . .
C6 C 0.8048(3) 0.08789(17) 0.3396(3) 0.0181(8) Uani 1 1 d . . .
C7 C 0.8597(3) 0.29259(17) 0.4094(3) 0.0176(8) Uani 1 1 d . . .
C8 C 0.8351(4) 0.3444(2) 0.3597(3) 0.0305(10) Uani 1 1 d . . .
H8 H 0.7766 0.3462 0.2987 0.037 Uiso 1 1 calc R . .
C9 C 0.8945(4) 0.3933(2) 0.3981(4) 0.0347(11) Uani 1 1 d . . .
H9 H 0.8765 0.4284 0.3634 0.042 Uiso 1 1 calc R . .
C10 C 0.9802(4) 0.39160(19) 0.4867(4) 0.0314(10) Uani 1 1 d . . .
H10 H 1.0214 0.4253 0.5126 0.038 Uiso 1 1 calc R . .
C11 C 1.0052(3) 0.34068(19) 0.5370(3) 0.0263(9) Uani 1 1 d . . .
H11 H 1.0630 0.3394 0.5984 0.032 Uiso 1 1 calc R . .
C12 C 0.9464(3) 0.29124(18) 0.4986(3) 0.0220(8) Uani 1 1 d . . .
H12 H 0.9652 0.2561 0.5332 0.026 Uiso 1 1 calc R . .
C13 C 0.5858(3) 0.31399(17) 0.4591(3) 0.0188(8) Uani 1 1 d . . .
C14 C 0.5766(3) 0.36455(17) 0.5040(3) 0.0201(8) Uani 1 1 d . . .
C15 C 0.4894(3) 0.36725(19) 0.5291(3) 0.0247(9) Uani 1 1 d . . .
H15 H 0.4801 0.4014 0.5590 0.030 Uiso 1 1 calc R . .
C16 C 0.4160(3) 0.32293(19) 0.5130(3) 0.0251(9) Uani 1 1 d . . .
C17 C 0.4325(3) 0.27201(18) 0.4733(3) 0.0231(9) Uani 1 1 d . . .
H17 H 0.3855 0.2403 0.4645 0.028 Uiso 1 1 calc R . .
C18 C 0.5169(3) 0.26722(16) 0.4463(3) 0.0181(8) Uani 1 1 d . . .
C19 C 0.4978(3) 0.16489(17) 0.4055(3) 0.0202(8) Uani 1 1 d . . .
C20 C 0.4554(3) 0.12998(18) 0.3244(3) 0.0246(9) Uani 1 1 d . . .
H20 H 0.4525 0.1437 0.2653 0.029 Uiso 1 1 calc R . .
C21 C 0.4174(3) 0.07521(19) 0.3302(4) 0.0324(11) Uani 1 1 d . . .
H21 H 0.3882 0.0517 0.2748 0.039 Uiso 1 1 calc R . .
C22 C 0.4221(4) 0.0548(2) 0.4164(4) 0.0364(12) Uani 1 1 d . . .
H22 H 0.3965 0.0172 0.4203 0.044 Uiso 1 1 calc R . .
C23 C 0.4637(4) 0.0890(2) 0.4964(4) 0.0350(11) Uani 1 1 d . . .
H23 H 0.4662 0.0751 0.5553 0.042 Uiso 1 1 calc R . .
C24 C 0.5022(3) 0.1440(2) 0.4916(3) 0.0260(9) Uani 1 1 d . . .
H24 H 0.5315 0.1672 0.5473 0.031 Uiso 1 1 calc R . .
C25 C 0.7302(3) 0.03640(17) 0.3253(3) 0.0207(8) Uani 1 1 d . . .
C26 C 0.6298(3) 0.04394(19) 0.2319(3) 0.0263(9) Uani 1 1 d . . .
H26A H 0.5943 0.0803 0.2338 0.039 Uiso 1 1 calc R . .
H26B H 0.5804 0.0118 0.2240 0.039 Uiso 1 1 calc R . .
H26C H 0.6505 0.0446 0.1782 0.039 Uiso 1 1 calc R . .
C27 C 0.6974(3) 0.03157(18) 0.4087(3) 0.0260(9) Uani 1 1 d . . .
H27A H 0.7615 0.0261 0.4682 0.039 Uiso 1 1 calc R . .
H27B H 0.6492 -0.0014 0.3984 0.039 Uiso 1 1 calc R . .
H27C H 0.6605 0.0669 0.4130 0.039 Uiso 1 1 calc R . .
C28 C 0.7839(4) -0.02053(18) 0.3192(4) 0.0286(10) Uani 1 1 d . . .
H28A H 0.8010 -0.0198 0.2635 0.043 Uiso 1 1 calc R . .
H28B H 0.7349 -0.0526 0.3132 0.043 Uiso 1 1 calc R . .
H28C H 0.8500 -0.0256 0.3771 0.043 Uiso 1 1 calc R . .
C29 C 1.0959(3) 0.11949(19) 0.3714(3) 0.0259(9) Uani 1 1 d . . .
C30 C 1.1185(4) 0.1589(2) 0.3015(4) 0.0324(10) Uani 1 1 d . . .
H30A H 1.1936 0.1547 0.3115 0.049 Uiso 1 1 calc R . .
H30B H 1.1048 0.1991 0.3128 0.049 Uiso 1 1 calc R . .
H30C H 1.0715 0.1481 0.2359 0.049 Uiso 1 1 calc R . .
C31 C 1.1738(3) 0.1349(2) 0.4733(4) 0.0375(12) Uani 1 1 d . . .
H31A H 1.1616 0.1092 0.5183 0.056 Uiso 1 1 calc R . .
H31B H 1.1620 0.1749 0.4869 0.056 Uiso 1 1 calc R . .
H31C H 1.2477 0.1304 0.4799 0.056 Uiso 1 1 calc R . .
C32 C 1.1167(4) 0.0575(2) 0.3502(4) 0.0385(12) Uani 1 1 d . . .
H32A H 1.1054 0.0314 0.3952 0.058 Uiso 1 1 calc R . .
H32B H 1.1908 0.0539 0.3569 0.058 Uiso 1 1 calc R . .
H32C H 1.0672 0.0474 0.2850 0.058 Uiso 1 1 calc R . .
C33 C 0.6557(3) 0.41436(18) 0.5209(3) 0.0229(9) Uani 1 1 d . . .
C34 C 0.6418(4) 0.46146(19) 0.5847(3) 0.0302(10) Uani 1 1 d . . .
H34A H 0.5710 0.4793 0.5522 0.045 Uiso 1 1 calc R . .
H34B H 0.6976 0.4908 0.5978 0.045 Uiso 1 1 calc R . .
H34C H 0.6479 0.4443 0.6449 0.045 Uiso 1 1 calc R . .
C35 C 0.6404(4) 0.4410(2) 0.4254(3) 0.0329(11) Uani 1 1 d . . .
H35A H 0.6498 0.4112 0.3844 0.049 Uiso 1 1 calc R . .
H35B H 0.6934 0.4716 0.4362 0.049 Uiso 1 1 calc R . .
H35C H 0.5680 0.4572 0.3943 0.049 Uiso 1 1 calc R . .
C36 C 0.7710(3) 0.3919(2) 0.5731(3) 0.0295(10) Uani 1 1 d . . .
H36A H 0.7793 0.3737 0.6331 0.044 Uiso 1 1 calc R . .
H36B H 0.8214 0.4242 0.5865 0.044 Uiso 1 1 calc R . .
H36C H 0.7858 0.3636 0.5329 0.044 Uiso 1 1 calc R . .
C37 C 0.3166(4) 0.3284(2) 0.5348(3) 0.0310(10) Uani 1 1 d . . .
C38 C 0.2159(4) 0.3206(3) 0.4410(4) 0.0426(13) Uani 1 1 d . . .
H38A H 0.1517 0.3234 0.4538 0.064 Uiso 1 1 calc R . .
H38B H 0.2179 0.2827 0.4137 0.064 Uiso 1 1 calc R . .
H38C H 0.2139 0.3508 0.3958 0.064 Uiso 1 1 calc R . .
C39 C 0.3099(4) 0.3866(2) 0.5777(4) 0.0460(14) Uani 1 1 d . . .
H39A H 0.3734 0.3920 0.6377 0.069 Uiso 1 1 calc R . .
H39B H 0.2452 0.3879 0.5901 0.069 Uiso 1 1 calc R . .
H39C H 0.3067 0.4173 0.5330 0.069 Uiso 1 1 calc R . .
C40 C 0.3195(4) 0.2814(3) 0.6062(4) 0.0429(12) Uani 1 1 d . . .
H40A H 0.3808 0.2882 0.6673 0.064 Uiso 1 1 calc R . .
H40B H 0.3267 0.2435 0.5814 0.064 Uiso 1 1 calc R . .
H40C H 0.2530 0.2827 0.6155 0.064 Uiso 1 1 calc R . .
C1S C 0.3761(4) 0.3559(2) 0.0863(3) 0.0287(10) Uani 1 1 d . . .
H1S1 H 0.3134 0.3820 0.0590 0.034 Uiso 1 1 calc R . .
H1S2 H 0.3718 0.3283 0.0359 0.034 Uiso 1 1 calc R . .
C2S C 0.4766(4) 0.3910(2) 0.1139(4) 0.0445(13) Uani 1 1 d . . .
H2S1 H 0.4774 0.4216 0.1579 0.067 Uiso 1 1 calc R . .
H2S2 H 0.4789 0.4082 0.0566 0.067 Uiso 1 1 calc R . .
H2S3 H 0.5393 0.3660 0.1451 0.067 Uiso 1 1 calc R . .
C3S C 0.3750(4) 0.3606(2) 0.2484(3) 0.0336(11) Uani 1 1 d . . .
H3S1 H 0.4440 0.3818 0.2735 0.040 Uiso 1 1 calc R . .
H3S2 H 0.3742 0.3357 0.3002 0.040 Uiso 1 1 calc R . .
C4S C 0.2845(5) 0.4036(2) 0.2218(4) 0.0523(15) Uani 1 1 d . . .
H4S1 H 0.2887 0.4308 0.1749 0.078 Uiso 1 1 calc R . .
H4S2 H 0.2903 0.4247 0.2789 0.078 Uiso 1 1 calc R . .
H4S3 H 0.2157 0.3832 0.1944 0.078 Uiso 1 1 calc R . .
C5S C 0.2739(3) 0.2833(2) 0.1284(3) 0.0277(9) Uani 1 1 d . . .
H5S1 H 0.2089 0.3064 0.0919 0.033 Uiso 1 1 calc R . .
H5S2 H 0.2840 0.2560 0.0835 0.033 Uiso 1 1 calc R . .
C6S C 0.2553(4) 0.2496(2) 0.2030(4) 0.0389(12) Uani 1 1 d . . .
H6S1 H 0.3214 0.2294 0.2435 0.058 Uiso 1 1 calc R . .
H6S2 H 0.1979 0.2215 0.1722 0.058 Uiso 1 1 calc R . .
H6S3 H 0.2346 0.2760 0.2422 0.058 Uiso 1 1 calc R . .
C7S C 0.5469(15) 0.1883(8) 0.6993(14) 0.034(4) Uiso 0.25 1 d P . .
H7S1 H 0.5008 0.2116 0.6445 0.051 Uiso 0.25 1 calc PR . .
H7S2 H 0.5967 0.1658 0.6820 0.051 Uiso 0.25 1 calc PR . .
H7S3 H 0.5877 0.2138 0.7529 0.051 Uiso 0.25 1 calc PR . .
H1 H 0.420(4) 0.3031(19) 0.188(3) 0.019(12) Uiso 1 1 d . . .
N1 N 0.7931(3) 0.24362(14) 0.3708(2) 0.0178(7) Uani 1 1 d . . .
N2 N 0.5391(2) 0.22034(14) 0.3986(2) 0.0171(6) Uani 1 1 d . . .
N1S N 0.3694(3) 0.32330(16) 0.1671(2) 0.0221(7) Uani 1 1 d . . .
O1 O 0.5621(2) 0.26020(12) 0.22228(19) 0.0221(6) Uani 1 1 d . . .
O2 O 0.6734(2) 0.15687(11) 0.34450(19) 0.0179(6) Uani 1 1 d . . .
O3 O 0.6602(2) 0.30659(11) 0.4221(2) 0.0190(6) Uani 1 1 d . . .
O1S O 0.4840(17) 0.1513(9) 0.7253(16) 0.080(6) Uiso 0.25 1 d P . .
H1S H 0.4336 0.1700 0.7295 0.120 Uiso 0.25 1 calc PR . .
Re1 Re 0.637393(11) 0.239346(6) 0.337751(10) 0.01526(4) 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'
Re Re -1.0185 7.2310 '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
O2 C1 C6 123.1(3) . . ?
O2 C1 C2 115.0(3) . . ?
C6 C1 C2 121.9(4) . . ?
C3 C2 C1 120.3(4) . . ?
C3 C2 N1 127.2(3) . . ?
C1 C2 N1 112.4(3) . . ?
C2 C3 C4 119.7(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 118.5(4) . . ?
C5 C4 C29 122.3(4) . . ?
C3 C4 C29 119.1(4) . . ?
C4 C5 C6 123.6(4) . . ?
C4 C5 H5 118.2 . . ?
C6 C5 H5 118.2 . . ?
C1 C6 C5 116.0(4) . . ?
C1 C6 C25 121.6(3) . . ?
C5 C6 C25 122.4(3) . . ?
C8 C7 C12 118.3(4) . . ?
C8 C7 N1 119.6(4) . . ?
C12 C7 N1 122.0(4) . . ?
C9 C8 C7 120.7(4) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 120.6(4) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 119.4(4) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 120.4(4) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 120.6(4) . . ?
C11 C12 H12 119.7 . . ?
C7 C12 H12 119.7 . . ?
O3 C13 C14 123.2(4) . . ?
O3 C13 C18 114.8(3) . . ?
C14 C13 C18 122.0(4) . . ?
C13 C14 C15 115.9(4) . . ?
C13 C14 C33 121.1(4) . . ?
C15 C14 C33 122.9(4) . . ?
C16 C15 C14 123.7(4) . . ?
C16 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
C15 C16 C17 118.1(4) . . ?
C15 C16 C37 122.8(4) . . ?
C17 C16 C37 119.0(4) . . ?
C18 C17 C16 120.5(4) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C13 119.6(4) . . ?
C17 C18 N2 127.1(4) . . ?
C13 C18 N2 113.2(3) . . ?
C24 C19 C20 119.2(4) . . ?
C24 C19 N2 121.6(4) . . ?
C20 C19 N2 119.1(4) . . ?
C21 C20 C19 120.1(4) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C22 C21 C20 120.2(5) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C23 C22 C21 120.0(4) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.4(5) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C19 C24 C23 120.2(4) . . ?
C19 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C6 C25 C27 110.3(3) . . ?
C6 C25 C28 111.9(3) . . ?
C27 C25 C28 107.6(3) . . ?
C6 C25 C26 109.4(3) . . ?
C27 C25 C26 109.6(3) . . ?
C28 C25 C26 107.9(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C32 C29 C31 109.0(4) . . ?
C32 C29 C30 107.5(4) . . ?
C31 C29 C30 108.8(4) . . ?
C32 C29 C4 111.8(4) . . ?
C31 C29 C4 108.7(4) . . ?
C30 C29 C4 110.8(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C35 C33 C14 109.6(3) . . ?
C35 C33 C34 109.0(4) . . ?
C14 C33 C34 112.3(4) . . ?
C35 C33 C36 110.1(4) . . ?
C14 C33 C36 109.6(3) . . ?
C34 C33 C36 106.2(3) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C39 C37 C16 112.7(4) . . ?
C39 C37 C40 107.7(4) . . ?
C16 C37 C40 109.6(4) . . ?
C39 C37 C38 108.6(4) . . ?
C16 C37 C38 108.4(4) . . ?
C40 C37 C38 109.7(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N1S C1S C2S 113.9(4) . . ?
N1S C1S H1S1 108.8 . . ?
C2S C1S H1S1 108.8 . . ?
N1S C1S H1S2 108.8 . . ?
C2S C1S H1S2 108.8 . . ?
H1S1 C1S H1S2 107.7 . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
N1S C3S C4S 113.8(4) . . ?
N1S C3S H3S1 108.8 . . ?
C4S C3S H3S1 108.8 . . ?
N1S C3S H3S2 108.8 . . ?
C4S C3S H3S2 108.8 . . ?
H3S1 C3S H3S2 107.7 . . ?
C3S C4S H4S1 109.5 . . ?
C3S C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
C3S C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?
C6S C5S N1S 114.3(4) . . ?
C6S C5S H5S1 108.7 . . ?
N1S C5S H5S1 108.7 . . ?
C6S C5S H5S2 108.7 . . ?
N1S C5S H5S2 108.7 . . ?
H5S1 C5S H5S2 107.6 . . ?
C5S C6S H6S1 109.5 . . ?
C5S C6S H6S2 109.5 . . ?
H6S1 C6S H6S2 109.5 . . ?
C5S C6S H6S3 109.5 . . ?
H6S1 C6S H6S3 109.5 . . ?
H6S2 C6S H6S3 109.5 . . ?
O1S C7S H7S1 109.5 . . ?
O1S C7S H7S2 109.4 . . ?
H7S1 C7S H7S2 109.5 . . ?
O1S C7S H7S3 109.5 . . ?
H7S1 C7S H7S3 109.5 . . ?
H7S2 C7S H7S3 109.5 . . ?
C2 N1 C7 118.7(3) . . ?
C2 N1 Re1 115.3(2) . . ?
C7 N1 Re1 125.6(3) . . ?
C18 N2 C19 118.5(3) . . ?
C18 N2 Re1 114.1(3) . . ?
C19 N2 Re1 127.1(3) . . ?
C1S N1S C3S 113.9(4) . . ?
C1S N1S C5S 108.9(3) . . ?
C3S N1S C5S 114.9(4) . . ?
C1S N1S H1 107(3) . . ?
C3S N1S H1 106(3) . . ?
C5S N1S H1 105(3) . . ?
C1 O2 Re1 115.9(2) . . ?
C13 O3 Re1 115.6(2) . . ?
C7S O1S H1S 109.4 . . ?
O1 Re1 O2 111.03(12) . . ?
O1 Re1 O3 108.88(13) . . ?
O2 Re1 O3 140.09(11) . . ?
O1 Re1 N1 111.92(14) . . ?
O2 Re1 N1 79.35(12) . . ?
O3 Re1 N1 86.06(12) . . ?
O1 Re1 N2 108.60(13) . . ?
O2 Re1 N2 87.91(12) . . ?
O3 Re1 N2 79.48(12) . . ?
N1 Re1 N2 139.45(13) . . ?
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
C1 O2 1.371(4) . ?
C1 C6 1.394(5) . ?
C1 C2 1.400(5) . ?
C2 C3 1.389(5) . ?
C2 N1 1.415(5) . ?
C3 C4 1.400(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(6) . ?
C4 C29 1.539(6) . ?
C5 C6 1.407(5) . ?
C5 H5 0.9500 . ?
C6 C25 1.527(5) . ?
C7 C8 1.390(6) . ?
C7 C12 1.395(5) . ?
C7 N1 1.423(5) . ?
C8 C9 1.377(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.376(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 O3 1.370(5) . ?
C13 C14 1.393(5) . ?
C13 C18 1.397(5) . ?
C14 C15 1.401(6) . ?
C14 C33 1.531(6) . ?
C15 C16 1.386(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.391(6) . ?
C16 C37 1.536(6) . ?
C17 C18 1.386(6) . ?
C17 H17 0.9500 . ?
C18 N2 1.414(5) . ?
C19 C24 1.390(6) . ?
C19 C20 1.397(6) . ?
C19 N2 1.427(5) . ?
C20 C21 1.389(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.375(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.393(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C27 1.531(6) . ?
C25 C28 1.533(6) . ?
C25 C26 1.533(6) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C32 1.527(6) . ?
C29 C31 1.531(6) . ?
C29 C30 1.538(6) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C35 1.528(6) . ?
C33 C34 1.534(6) . ?
C33 C36 1.535(6) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C39 1.524(7) . ?
C37 C40 1.537(7) . ?
C37 C38 1.540(7) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C1S N1S 1.492(5) . ?
C1S C2S 1.501(7) . ?
C1S H1S1 0.9900 . ?
C1S H1S2 0.9900 . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
C3S N1S 1.498(6) . ?
C3S C4S 1.509(7) . ?
C3S H3S1 0.9900 . ?
C3S H3S2 0.9900 . ?
C4S H4S1 0.9800 . ?
C4S H4S2 0.9800 . ?
C4S H4S3 0.9800 . ?
C5S C6S 1.497(7) . ?
C5S N1S 1.510(5) . ?
C5S H5S1 0.9900 . ?
C5S H5S2 0.9900 . ?
C6S H6S1 0.9800 . ?
C6S H6S2 0.9800 . ?
C6S H6S3 0.9800 . ?
C7S O1S 1.39(3) . ?
C7S H7S1 0.9800 . ?
C7S H7S2 0.9800 . ?
C7S H7S3 0.9800 . ?
N1 Re1 1.980(3) . ?
N2 Re1 1.983(3) . ?
N1S H1 0.78(4) . ?
O1 Re1 1.715(3) . ?
O2 Re1 1.968(3) . ?
O3 Re1 1.970(3) . ?
O1S H1S 0.8400 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1S H1 O1 0.78(4) 2.05(5) 2.823(4) 167(5) .
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
O2 C1 C2 C3 178.1(3) . . . . ?
C6 C1 C2 C3 1.2(6) . . . . ?
O2 C1 C2 N1 -2.1(5) . . . . ?
C6 C1 C2 N1 -179.0(3) . . . . ?
C1 C2 C3 C4 0.0(6) . . . . ?
N1 C2 C3 C4 -179.7(4) . . . . ?
C2 C3 C4 C5 -0.8(6) . . . . ?
C2 C3 C4 C29 -179.1(4) . . . . ?
C3 C4 C5 C6 0.4(6) . . . . ?
C29 C4 C5 C6 178.7(4) . . . . ?
O2 C1 C6 C5 -178.2(3) . . . . ?
C2 C1 C6 C5 -1.6(6) . . . . ?
O2 C1 C6 C25 1.1(6) . . . . ?
C2 C1 C6 C25 177.8(4) . . . . ?
C4 C5 C6 C1 0.8(6) . . . . ?
C4 C5 C6 C25 -178.6(4) . . . . ?
C12 C7 C8 C9 -0.4(7) . . . . ?
N1 C7 C8 C9 176.2(4) . . . . ?
C7 C8 C9 C10 0.2(8) . . . . ?
C8 C9 C10 C11 -0.6(8) . . . . ?
C9 C10 C11 C12 1.2(7) . . . . ?
C10 C11 C12 C7 -1.4(7) . . . . ?
C8 C7 C12 C11 1.0(6) . . . . ?
N1 C7 C12 C11 -175.6(4) . . . . ?
O3 C13 C14 C15 173.7(4) . . . . ?
C18 C13 C14 C15 -4.5(6) . . . . ?
O3 C13 C14 C33 -4.3(6) . . . . ?
C18 C13 C14 C33 177.5(4) . . . . ?
C13 C14 C15 C16 1.0(6) . . . . ?
C33 C14 C15 C16 179.0(4) . . . . ?
C14 C15 C16 C17 2.8(7) . . . . ?
C14 C15 C16 C37 -175.6(4) . . . . ?
C15 C16 C17 C18 -3.2(6) . . . . ?
C37 C16 C17 C18 175.2(4) . . . . ?
C16 C17 C18 C13 -0.1(6) . . . . ?
C16 C17 C18 N2 -174.7(4) . . . . ?
O3 C13 C18 C17 -174.2(3) . . . . ?
C14 C13 C18 C17 4.1(6) . . . . ?
O3 C13 C18 N2 1.1(5) . . . . ?
C14 C13 C18 N2 179.5(3) . . . . ?
C24 C19 C20 C21 0.5(6) . . . . ?
N2 C19 C20 C21 178.3(4) . . . . ?
C19 C20 C21 C22 -0.4(6) . . . . ?
C20 C21 C22 C23 0.5(7) . . . . ?
C21 C22 C23 C24 -0.6(7) . . . . ?
C20 C19 C24 C23 -0.6(6) . . . . ?
N2 C19 C24 C23 -178.3(4) . . . . ?
C22 C23 C24 C19 0.7(7) . . . . ?
C1 C6 C25 C27 -59.9(5) . . . . ?
C5 C6 C25 C27 119.4(4) . . . . ?
C1 C6 C25 C28 -179.7(4) . . . . ?
C5 C6 C25 C28 -0.4(5) . . . . ?
C1 C6 C25 C26 60.8(5) . . . . ?
C5 C6 C25 C26 -120.0(4) . . . . ?
C5 C4 C29 C32 7.0(6) . . . . ?
C3 C4 C29 C32 -174.8(4) . . . . ?
C5 C4 C29 C31 -113.4(5) . . . . ?
C3 C4 C29 C31 64.8(5) . . . . ?
C5 C4 C29 C30 127.0(4) . . . . ?
C3 C4 C29 C30 -54.8(5) . . . . ?
C13 C14 C33 C35 67.7(5) . . . . ?
C15 C14 C33 C35 -110.2(4) . . . . ?
C13 C14 C33 C34 -171.0(4) . . . . ?
C15 C14 C33 C34 11.1(6) . . . . ?
C13 C14 C33 C36 -53.2(5) . . . . ?
C15 C14 C33 C36 128.9(4) . . . . ?
C15 C16 C37 C39 -1.4(7) . . . . ?
C17 C16 C37 C39 -179.8(4) . . . . ?
C15 C16 C37 C40 -121.4(5) . . . . ?
C17 C16 C37 C40 60.2(5) . . . . ?
C15 C16 C37 C38 118.8(5) . . . . ?
C17 C16 C37 C38 -59.6(6) . . . . ?
C3 C2 N1 C7 -15.0(6) . . . . ?
C1 C2 N1 C7 165.3(3) . . . . ?
C3 C2 N1 Re1 171.3(3) . . . . ?
C1 C2 N1 Re1 -8.4(4) . . . . ?
C8 C7 N1 C2 129.1(4) . . . . ?
C12 C7 N1 C2 -54.4(5) . . . . ?
C8 C7 N1 Re1 -57.9(5) . . . . ?
C12 C7 N1 Re1 118.6(4) . . . . ?
C17 C18 N2 C19 -23.3(6) . . . . ?
C13 C18 N2 C19 161.7(3) . . . . ?
C17 C18 N2 Re1 161.9(3) . . . . ?
C13 C18 N2 Re1 -13.1(4) . . . . ?
C24 C19 N2 C18 -43.3(5) . . . . ?
C20 C19 N2 C18 139.0(4) . . . . ?
C24 C19 N2 Re1 130.7(3) . . . . ?
C20 C19 N2 Re1 -47.0(5) . . . . ?
C2S C1S N1S C3S 58.5(5) . . . . ?
C2S C1S N1S C5S -171.8(4) . . . . ?
C4S C3S N1S C1S 61.6(5) . . . . ?
C4S C3S N1S C5S -65.0(5) . . . . ?
C6S C5S N1S C1S -177.6(4) . . . . ?
C6S C5S N1S C3S -48.5(5) . . . . ?
C6 C1 O2 Re1 -171.2(3) . . . . ?
C2 C1 O2 Re1 11.9(4) . . . . ?
C14 C13 O3 Re1 -166.8(3) . . . . ?
C18 C13 O3 Re1 11.5(4) . . . . ?
C1 O2 Re1 O1 96.8(3) . . . . ?
C1 O2 Re1 O3 -83.2(3) . . . . ?
C1 O2 Re1 N1 -12.7(2) . . . . ?
C1 O2 Re1 N2 -154.0(3) . . . . ?
C13 O3 Re1 O1 91.7(3) . . . . ?
C13 O3 Re1 O2 -88.2(3) . . . . ?
C13 O3 Re1 N1 -156.4(3) . . . . ?
C13 O3 Re1 N2 -14.5(3) . . . . ?
C2 N1 Re1 O1 -97.1(3) . . . . ?
C7 N1 Re1 O1 89.7(3) . . . . ?
C2 N1 Re1 O2 11.4(3) . . . . ?
C7 N1 Re1 O2 -161.8(3) . . . . ?
C2 N1 Re1 O3 154.1(3) . . . . ?
C7 N1 Re1 O3 -19.1(3) . . . . ?
C2 N1 Re1 N2 85.3(3) . . . . ?
C7 N1 Re1 N2 -87.9(4) . . . . ?
C18 N2 Re1 O1 -91.7(3) . . . . ?
C19 N2 Re1 O1 94.0(3) . . . . ?
C18 N2 Re1 O2 156.8(3) . . . . ?
C19 N2 Re1 O2 -17.5(3) . . . . ?
C18 N2 Re1 O3 14.8(2) . . . . ?
C19 N2 Re1 O3 -159.4(3) . . . . ?
C18 N2 Re1 N1 85.9(3) . . . . ?
C19 N2 Re1 N1 -88.4(3) . . . . ?
