#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/41/2224199.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2224199
loop_
_publ_author_name
'Schutte, Marietjie'
'Visser, Hendrik G.'
'Brink, Alice'
_publ_section_title
'[N,N-Bis(diphenylphosphino)propylamine-κ²P,P]bromidotricarbonylrhenium(I)'
_journal_coeditor_code           FI2092
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1575
_journal_page_last               m1576
_journal_paper_doi               10.1107/S1600536809047242
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Re Br (C27 H27 N P2) (C O)3]'
_chemical_formula_moiety         'C30 H27 Br N O3 P2 Re'
_chemical_formula_sum            'C30 H27 Br N O3 P2 Re'
_chemical_formula_weight         777.58
_chemical_name_systematic
;
[N,N-Bis(diphenylphosphino)propylamine-
κ²P,P]bromidotricarbonylrhenium(I)
;
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.00
_cell_angle_beta                 96.735(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0120(2)
_cell_length_b                   17.1620(3)
_cell_length_c                   15.2090(2)
_cell_measurement_reflns_used    10593
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.1450
_cell_measurement_theta_min      2.2035
_cell_volume                     2854.48(8)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'DIAMOND (Brandenberg & Putz, 2004)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1829
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur 3 CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22483
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.801
_exptl_absorpt_correction_T_max  0.7602
_exptl_absorpt_correction_T_min  0.5946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2006)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.946
_refine_diff_density_min         -1.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         6863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0476P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                5197
_reflns_number_total             6863
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fi2092.cif
_cod_data_source_block           I
_cod_original_cell_volume        2854.48(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2224199
_cod_database_fobs_code          2224199
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re Re1 0.686711(18) 0.106550(11) 0.202197(12) 0.02066(7) Uani d . 1 . .
P P2 0.73189(12) 0.20128(8) 0.32094(8) 0.0239(3) Uani d . 1 A .
P P1 0.85557(12) 0.19498(7) 0.17874(8) 0.0242(3) Uani d . 1 A .
C C2 0.5544(5) 0.0550(3) 0.2545(3) 0.0285(12) Uani d . 1 A .
O O2 0.4813(4) 0.0257(2) 0.2910(3) 0.0411(10) Uani d . 1 . .
C C34 0.8309(8) 0.0726(4) 0.5839(4) 0.054(2) Uani d . 1 A .
H H34 0.849 0.0436 0.6371 0.064 Uiso calc R 1 . .
C C35 0.9232(8) 0.0939(3) 0.5363(5) 0.059(2) Uani d . 1 . .
H H35 1.0051 0.0798 0.5564 0.071 Uiso calc R 1 . .
O O1 0.6682(4) -0.0050(2) 0.0405(2) 0.0438(10) Uani d . 1 . .
C C1 0.6767(5) 0.0357(3) 0.1004(3) 0.0295(12) Uani d . 1 A .
C C32 0.6847(6) 0.1351(3) 0.4772(3) 0.0330(13) Uani d . 1 A .
H H32 0.6024 0.1488 0.4576 0.04 Uiso calc R 1 . .
C C44 0.4952(6) 0.4065(3) 0.3942(4) 0.0443(17) Uani d . 1 A .
H H44 0.4454 0.4483 0.4098 0.053 Uiso calc R 1 . .
C C46 0.5319(6) 0.3030(3) 0.2950(4) 0.0370(14) Uani d . 1 A .
H H46 0.5082 0.2743 0.2424 0.044 Uiso calc R 1 . .
C C31 0.7784(5) 0.1570(3) 0.4284(3) 0.0271(11) Uani d . 1 . .
C C11 1.0162(5) 0.1714(3) 0.1741(3) 0.0243(11) Uani d . 1 . .
C C26 0.7771(5) 0.3402(3) 0.1033(4) 0.0368(14) Uani d . 1 A .
H H26 0.7563 0.3547 0.1599 0.044 Uiso calc R 1 . .
C C22 0.8530(5) 0.2457(3) 0.0066(4) 0.0332(13) Uani d . 1 A .
H H22 0.8869 0.196 -0.003 0.04 Uiso calc R 1 . .
C C21 0.8280(5) 0.2662(3) 0.0915(3) 0.0273(12) Uani d . 1 . .
C C13 1.1832(5) 0.0804(4) 0.1978(4) 0.0382(14) Uani d . 1 . .
H H13 1.2126 0.0295 0.2129 0.046 Uiso calc R 1 A .
C C16 1.0980(5) 0.2284(3) 0.1530(3) 0.0257(11) Uani d . 1 A .
H H16 1.0689 0.2792 0.1373 0.031 Uiso calc R 1 . .
C C41 0.6376(5) 0.2829(3) 0.3499(3) 0.0281(12) Uani d . 1 . .
C C36 0.8976(6) 0.1362(3) 0.4586(4) 0.0413(15) Uani d . 1 A .
H H36 0.9623 0.151 0.4258 0.05 Uiso calc R 1 . .
C C15 1.2208(5) 0.2120(3) 0.1548(3) 0.0313(12) Uani d . 1 . .
H H15 1.2759 0.2514 0.1407 0.038 Uiso calc R 1 A .
C C14 1.2640(5) 0.1374(4) 0.1772(4) 0.0396(14) Uani d . 1 A .
H H14 1.3485 0.1258 0.1784 0.048 Uiso calc R 1 . .
N N1 0.8534(5) 0.2416(3) 0.2781(3) 0.0355(12) Uani d . 1 . .
C C45 0.4617(6) 0.3653(4) 0.3180(4) 0.0447(16) Uani d . 1 . .
H H45 0.3899 0.3795 0.2807 0.054 Uiso calc R 1 A .
C C24 0.7837(6) 0.3709(4) -0.0495(4) 0.0439(15) Uani d . 1 A .
H H24 0.771 0.407 -0.097 0.053 Uiso calc R 1 . .
C C12 1.0608(5) 0.0966(3) 0.1967(3) 0.0287(12) Uani d . 1 A .
H H12 1.0062 0.0571 0.2113 0.034 Uiso calc R 1 . .
C C25 0.7571(6) 0.3919(3) 0.0334(4) 0.0454(16) Uani d . 1 . .
H H25 0.7248 0.4421 0.0427 0.054 Uiso calc R 1 A .
C C23 0.8290(5) 0.2972(4) -0.0641(4) 0.0407(14) Uani d . 1 . .
H H23 0.8436 0.282 -0.122 0.049 Uiso calc R 1 A .
C C42 0.6723(5) 0.3252(3) 0.4263(4) 0.0322(13) Uani d . 1 A .
H H42 0.7448 0.3115 0.4632 0.039 Uiso calc R 1 . .
C C43 0.6020(6) 0.3875(3) 0.4492(4) 0.0408(15) Uani d . 1 . .
H H43 0.626 0.4168 0.5013 0.049 Uiso calc R 1 A .
C C33 0.7130(8) 0.0925(3) 0.5559(4) 0.0489(19) Uani d . 1 . .
H H33 0.6496 0.0776 0.5897 0.059 Uiso calc R 1 A .
Br Br2 0.8260(2) 0.00301(16) 0.29098(18) 0.0268(5) Uani d P 0.462(4) A 1
C C3A 0.5759(17) 0.1762(8) 0.1278(10) 0.027(2) Uani d P 0.462(4) A 1
O O3A 0.5100(18) 0.2120(12) 0.0826(14) 0.041(6) Uani d P 0.462(4) A 1
Br Br1 0.5387(2) 0.19542(14) 0.09865(15) 0.0254(5) Uani d P 0.538(4) . 2
C C3B 0.7961(12) 0.0397(7) 0.2678(8) 0.027(2) Uani d P 0.538(4) . 2
O O3B 0.8632(15) -0.0078(12) 0.3052(13) 0.055(6) Uani d P 0.538(4) . 2
C C4B 0.9665(16) 0.2791(10) 0.3419(10) 0.026(4) Uani d P 0.352(9) A 1
H H4B1 0.9494 0.278 0.4043 0.031 Uiso calc PR 0.352(9) A 1
H H4B2 1.0424 0.2494 0.337 0.031 Uiso calc PR 0.352(9) A 1
C C5B 0.9802(16) 0.3627(10) 0.3113(11) 0.0342(18) Uani d P 0.352(9) A 1
H H5B1 0.9909 0.3637 0.2476 0.041 Uiso calc PR 0.352(9) A 1
H H5B2 0.9061 0.3931 0.3198 0.041 Uiso calc PR 0.352(9) A 1
C C6B 1.090(4) 0.3979(17) 0.365(3) 0.035(7) Uani d P 0.352(9) A 1
H H6B1 1.1007 0.4517 0.3454 0.052 Uiso calc PR 0.352(9) A 1
H H6B2 1.1631 0.3675 0.356 0.052 Uiso calc PR 0.352(9) A 1
H H6B3 1.0783 0.3975 0.4276 0.052 Uiso calc PR 0.352(9) A 1
C C4A 0.9176(8) 0.3160(5) 0.2997(5) 0.025(2) Uani d P 0.648(9) A 2
H H4A1 0.8637 0.3516 0.3285 0.03 Uiso calc PR 0.648(9) A 2
H H4A2 0.9376 0.341 0.2445 0.03 Uiso calc PR 0.648(9) A 2
C C5A 1.0330(10) 0.3019(5) 0.3604(6) 0.0342(18) Uani d P 0.648(9) A 2
H H5A1 1.0798 0.2593 0.3362 0.041 Uiso calc PR 0.648(9) A 2
H H5A2 1.012 0.2852 0.419 0.041 Uiso calc PR 0.648(9) A 2
C C6A 1.112(2) 0.3747(10) 0.3713(18) 0.046(4) Uani d P 0.648(9) A 2
H H6A1 1.1864 0.3636 0.4113 0.069 Uiso calc PR 0.648(9) A 2
H H6A2 1.0663 0.4167 0.3961 0.069 Uiso calc PR 0.648(9) A 2
H H6A3 1.1344 0.3907 0.3134 0.069 Uiso calc PR 0.648(9) A 2
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 0 '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 0.006 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.231 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3B Re1 C2 . . 88.2(3) ?
C3B Re1 C1 . . 90.8(3) ?
C2 Re1 C1 . . 93.7(2) ?
C3B Re1 C3A . . 177.1(5) ?
C2 Re1 C3A . . 93.9(5) ?
C1 Re1 C3A . . 87.1(4) ?
C3B Re1 P2 . . 87.2(3) ?
C2 Re1 P2 . . 95.62(16) ?
C1 Re1 P2 . . 170.40(16) ?
C3A Re1 P2 . . 94.6(4) ?
C3B Re1 P1 . . 90.3(3) ?
C2 Re1 P1 . . 162.26(16) ?
C1 Re1 P1 . . 104.00(16) ?
C3A Re1 P1 . . 88.3(4) ?
P2 Re1 P1 . . 66.65(4) y
C3B Re1 Br2 . . 5.0(3) ?
C2 Re1 Br2 . . 84.41(16) ?
C1 Re1 Br2 . . 87.79(16) ?
C3A Re1 Br2 . . 174.5(4) ?
P2 Re1 Br2 . . 90.82(7) ?
P1 Re1 Br2 . . 94.96(7) ?
C3B Re1 Br1 . . 175.4(3) ?
C2 Re1 Br1 . . 93.86(16) ?
C1 Re1 Br1 . . 85.02(16) ?
C3A Re1 Br1 . . 2.1(4) ?
P2 Re1 Br1 . . 96.64(7) ?
P1 Re1 Br1 . . 88.92(7) ?
Br2 Re1 Br1 . . 172.48(9) ?
N1 P2 C31 . . 111.2(3) ?
N1 P2 C41 . . 106.0(2) ?
C31 P2 C41 . . 102.2(2) ?
N1 P2 Re1 . . 95.10(15) ?
C31 P2 Re1 . . 113.44(16) ?
C41 P2 Re1 . . 128.11(19) ?
C31 P2 P1 . . 126.09(18) ?
C41 P2 P1 . . 125.45(16) ?
Re1 P2 P1 . . 57.05(4) ?
N1 P1 C21 . . 108.3(2) ?
N1 P1 C11 . . 104.6(2) ?
C21 P1 C11 . . 101.6(2) ?
N1 P1 Re1 . . 94.08(16) ?
C21 P1 Re1 . . 117.41(18) ?
C11 P1 Re1 . . 128.48(17) ?
C21 P1 P2 . . 120.47(17) ?
C11 P1 P2 . . 128.68(17) ?
Re1 P1 P2 . . 56.30(4) ?
O2 C2 Re1 . . 175.1(5) ?
C33 C34 C35 . . 120.5(6) ?
C33 C34 H34 . . 119.7 ?
C35 C34 H34 . . 119.7 ?
C34 C35 C36 . . 120.2(7) ?
C34 C35 H35 . . 119.9 ?
C36 C35 H35 . . 119.9 ?
O1 C1 Re1 . . 178.4(5) ?
C31 C32 C33 . . 119.3(6) ?
C31 C32 H32 . . 120.3 ?
C33 C32 H32 . . 120.3 ?
C45 C44 C43 . . 120.6(6) ?
C45 C44 H44 . . 119.7 ?
C43 C44 H44 . . 119.7 ?
C45 C46 C41 . . 119.3(6) ?
C45 C46 H46 . . 120.3 ?
C41 C46 H46 . . 120.3 ?
C36 C31 C32 . . 119.1(5) ?
C36 C31 P2 . . 124.1(4) ?
C32 C31 P2 . . 116.3(4) ?
C16 C11 C12 . . 118.9(5) ?
C16 C11 P1 . . 120.6(4) ?
C12 C11 P1 . . 120.4(4) ?
C25 C26 C21 . . 120.7(5) ?
C25 C26 H26 . . 119.7 ?
C21 C26 H26 . . 119.7 ?
C23 C22 C21 . . 120.9(5) ?
C23 C22 H22 . . 119.5 ?
C21 C22 H22 . . 119.5 ?
C22 C21 C26 . . 118.1(5) ?
C22 C21 P1 . . 118.4(4) ?
C26 C21 P1 . . 123.5(4) ?
C12 C13 C14 . . 120.6(6) ?
C12 C13 H13 . . 119.7 ?
C14 C13 H13 . . 119.7 ?
C15 C16 C11 . . 120.7(5) ?
C15 C16 H16 . . 119.6 ?
C11 C16 H16 . . 119.6 ?
C42 C41 C46 . . 120.2(5) ?
C42 C41 P2 . . 119.6(4) ?
C46 C41 P2 . . 120.2(4) ?
C31 C36 C35 . . 120.4(7) ?
C31 C36 H36 . . 119.8 ?
C35 C36 H36 . . 119.8 ?
C16 C15 C14 . . 119.9(5) ?
C16 C15 H15 . . 120.1 ?
C14 C15 H15 . . 120.1 ?
C13 C14 C15 . . 119.7(5) ?
C13 C14 H14 . . 120.2 ?
C15 C14 H14 . . 120.2 ?
C4A N1 P2 . . 130.1(4) ?
C4B N1 P2 . . 121.1(6) ?
C4A N1 P1 . . 122.9(4) ?
C4B N1 P1 . . 128.7(6) ?
P2 N1 P1 . . 103.9(2) ?
C44 C45 C46 . . 120.5(6) ?
C44 C45 H45 . . 119.7 ?
C46 C45 H45 . . 119.7 ?
C25 C24 C23 . . 120.3(6) ?
C25 C24 H24 . . 119.9 ?
C23 C24 H24 . . 119.9 ?
C13 C12 C11 . . 120.2(5) ?
C13 C12 H12 . . 119.9 ?
C11 C12 H12 . . 119.9 ?
C24 C25 C26 . . 120.3(5) ?
C24 C25 H25 . . 119.8 ?
C26 C25 H25 . . 119.8 ?
C24 C23 C22 . . 119.6(6) ?
C24 C23 H23 . . 120.2 ?
C22 C23 H23 . . 120.2 ?
C41 C42 C43 . . 120.4(6) ?
C41 C42 H42 . . 119.8 ?
C43 C42 H42 . . 119.8 ?
C42 C43 C44 . . 118.9(6) ?
C42 C43 H43 . . 120.5 ?
C44 C43 H43 . . 120.5 ?
C34 C33 C32 . . 120.4(7) ?
C34 C33 H33 . . 119.8 ?
C32 C33 H33 . . 119.8 ?
O3A C3A Re1 . . 176(2) ?
O3B C3B Re1 . . 174.9(14) ?
C5B C4B N1 . . 106.8(12) ?
C5B C4B H4B1 . . 110.4 ?
N1 C4B H4B1 . . 110.4 ?
C5B C4B H4B2 . . 110.4 ?
N1 C4B H4B2 . . 110.4 ?
H4B1 C4B H4B2 . . 108.6 ?
C6B C5B C4B . . 108.5(16) ?
C6B C5B H5B1 . . 110 ?
C4B C5B H5B1 . . 110 ?
C6B C5B H5B2 . . 110 ?
C4B C5B H5B2 . . 110 ?
H5B1 C5B H5B2 . . 108.4 ?
C5B C6B H6B1 . . 109.5 ?
C5B C6B H6B2 . . 109.5 ?
H6B1 C6B H6B2 . . 109.5 ?
C5B C6B H6B3 . . 109.5 ?
H6B1 C6B H6B3 . . 109.5 ?
H6B2 C6B H6B3 . . 109.5 ?
N1 C4A C5A . . 110.2(7) ?
N1 C4A H4A1 . . 109.6 ?
C5A C4A H4A1 . . 109.6 ?
N1 C4A H4A2 . . 109.6 ?
C5A C4A H4A2 . . 109.6 ?
H4A1 C4A H4A2 . . 108.1 ?
C4A C5A C6A . . 111.5(9) ?
C4A C5A H5A1 . . 109.3 ?
C6A C5A H5A1 . . 109.3 ?
C4A C5A H5A2 . . 109.3 ?
C6A C5A H5A2 . . 109.3 ?
H5A1 C5A H5A2 . . 108 ?
C5A C6A H6A1 . . 109.5 ?
C5A C6A H6A2 . . 109.5 ?
H6A1 C6A H6A2 . . 109.5 ?
C5A C6A H6A3 . . 109.5 ?
H6A1 C6A H6A3 . . 109.5 ?
H6A2 C6A H6A3 . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Re1 C3B . 1.866(15) y
Re1 C2 . 1.952(5) y
Re1 C1 . 1.962(6) y
Re1 C3A . 1.968(18) y
Re1 P2 . 2.4375(14) y
Re1 P1 . 2.4583(15) y
Re1 Br2 . 2.617(3) y
Re1 Br1 . 2.619(2) y
P2 N1 . 1.702(5) ?
P2 C31 . 1.820(5) ?
P2 C41 . 1.828(5) ?
P2 P1 . 2.6897(18) ?
P1 N1 . 1.713(4) ?
P1 C21 . 1.804(5) ?
P1 C11 . 1.824(5) ?
C2 O2 . 1.146(6) ?
C34 C33 . 1.361(10) ?
C34 C35 . 1.366(10) ?
C34 H34 . 0.95 ?
C35 C36 . 1.387(9) ?
C35 H35 . 0.95 ?
O1 C1 . 1.142(6) ?
C32 C31 . 1.392(7) ?
C32 C33 . 1.406(8) ?
C32 H32 . 0.95 ?
C44 C45 . 1.370(9) ?
C44 C43 . 1.400(9) ?
C44 H44 . 0.95 ?
C46 C45 . 1.388(8) ?
C46 C41 . 1.393(8) ?
C46 H46 . 0.95 ?
C31 C36 . 1.386(8) ?
C11 C16 . 1.392(7) ?
C11 C12 . 1.402(7) ?
C26 C25 . 1.382(8) ?
C26 C21 . 1.408(7) ?
C26 H26 . 0.95 ?
C22 C23 . 1.394(8) ?
C22 C21 . 1.395(7) ?
C22 H22 . 0.95 ?
C13 C12 . 1.375(7) ?
C13 C14 . 1.383(8) ?
C13 H13 . 0.95 ?
C16 C15 . 1.379(7) ?
C16 H16 . 0.95 ?
C41 C42 . 1.385(8) ?
C36 H36 . 0.95 ?
C15 C14 . 1.394(8) ?
C15 H15 . 0.95 ?
C14 H14 . 0.95 ?
N1 C4A . 1.478(9) ?
N1 C4B . 1.619(18) ?
C45 H45 . 0.95 ?
C24 C25 . 1.376(9) ?
C24 C23 . 1.386(8) ?
C24 H24 . 0.95 ?
C12 H12 . 0.95 ?
C25 H25 . 0.95 ?
C23 H23 . 0.95 ?
C42 C43 . 1.388(8) ?
C42 H42 . 0.95 ?
C43 H43 . 0.95 ?
C33 H33 . 0.95 ?
C3A O3A . 1.12(2) ?
C3B O3B . 1.20(2) ?
C4B C5B . 1.52(2) ?
C4B H4B1 . 0.99 ?
C4B H4B2 . 0.99 ?
C5B C6B . 1.50(4) ?
C5B H5B1 . 0.99 ?
C5B H5B2 . 0.99 ?
C6B H6B1 . 0.98 ?
C6B H6B2 . 0.98 ?
C6B H6B3 . 0.98 ?
C4A C5A . 1.500(13) ?
C4A H4A1 . 0.99 ?
C4A H4A2 . 0.99 ?
C5A C6A . 1.52(3) ?
C5A H5A1 . 0.99 ?
C5A H5A2 . 0.99 ?
C6A H6A1 . 0.98 ?
C6A H6A2 . 0.98 ?
C6A H6A3 . 0.98 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C12 H12 O3B 1 0.95 2.51 3.39(2) 155.1
C14 H14 Br1 1_655 0.95 2.81 3.524(6) 133
C46 H46 Br1 1 0.95 2.63 3.519(6) 156.8
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C3B Re1 P2 N1 . . . . 88.4(4) ?
C2 Re1 P2 N1 . . . . 176.3(2) ?
C3A Re1 P2 N1 . . . . -89.3(5) ?
P1 Re1 P2 N1 . . . . -3.19(18) ?
Br2 Re1 P2 N1 . . . . 91.86(19) ?
Br1 Re1 P2 N1 . . . . -89.13(19) ?
C3B Re1 P2 C31 . . . . -27.4(4) ?
C2 Re1 P2 C31 . . . . 60.6(2) ?
C3A Re1 P2 C31 . . . . 154.9(5) ?
P1 Re1 P2 C31 . . . . -119.0(2) ?
Br2 Re1 P2 C31 . . . . -23.9(2) ?
Br1 Re1 P2 C31 . . . . 155.1(2) ?
C3B Re1 P2 C41 . . . . -156.7(4) ?
C2 Re1 P2 C41 . . . . -68.8(3) ?
C3A Re1 P2 C41 . . . . 25.6(5) ?
P1 Re1 P2 C41 . . . . 111.7(2) ?
Br2 Re1 P2 C41 . . . . -153.2(2) ?
Br1 Re1 P2 C41 1 . . . 25.8(2) ?
Br1 Re1 P2 C41 . . . . 25.8(2) ?
C3B Re1 P2 P1 . . . . 91.5(3) ?
C2 Re1 P2 P1 . . . . 179.50(15) ?
C3A Re1 P2 P1 . . . . -86.2(4) ?
Br2 Re1 P2 P1 . . . . 95.04(7) ?
Br1 Re1 P2 P1 1 . . . -85.94(7) ?
Br1 Re1 P2 P1 . . . . -85.94(7) ?
C3B Re1 P1 N1 . . . . -83.7(4) ?
C2 Re1 P1 N1 . . . . 1.5(5) ?
C1 Re1 P1 N1 . . . . -174.5(2) ?
C3A Re1 P1 N1 . . . . 98.9(4) ?
P2 Re1 P1 N1 . . . . 3.16(18) ?
Br2 Re1 P1 N1 . . . . -85.59(19) ?
Br1 Re1 P1 N1 1 . . . 100.87(19) ?
Br1 Re1 P1 N1 . . . . 100.87(19) ?
C3B Re1 P1 C21 . . . . 163.2(4) ?
C2 Re1 P1 C21 . . . . -111.5(5) ?
C1 Re1 P1 C21 . . . . 72.4(2) ?
C3A Re1 P1 C21 . . . . -14.2(4) ?
P2 Re1 P1 C21 . . . . -109.92(19) ?
Br2 Re1 P1 C21 . . . . 161.3(2) ?
Br1 Re1 P1 C21 1 . . . -12.22(19) ?
Br1 Re1 P1 C21 . . . . -12.22(19) ?
C3B Re1 P1 C11 . . . . 28.6(4) ?
C2 Re1 P1 C11 . . . . 113.8(5) ?
C1 Re1 P1 C11 . . . . -62.3(3) ?
C3A Re1 P1 C11 . . . . -148.8(5) ?
P2 Re1 P1 C11 . . . . 115.4(2) ?
Br2 Re1 P1 C11 . . . . 26.7(2) ?
Br1 Re1 P1 C11 1 . . . -146.9(2) ?
Br1 Re1 P1 C11 . . . . -146.9(2) ?
C3B Re1 P1 P2 . . . . -86.8(3) ?
C2 Re1 P1 P2 . . . . -1.6(5) ?
C1 Re1 P1 P2 . . . . -177.70(16) ?
C3A Re1 P1 P2 . . . . 95.7(4) ?
Br2 Re1 P1 P2 . . . . -88.75(7) ?
Br1 Re1 P1 P2 1 . . . 97.70(7) ?
Br1 Re1 P1 P2 . . . . 97.70(7) ?
C31 P2 P1 N1 . . . . -78.3(4) ?
C41 P2 P1 N1 . . . . 69.0(4) ?
Re1 P2 P1 N1 . . . . -174.9(3) ?
N1 P2 P1 C21 . . . . -80.7(4) ?
C31 P2 P1 C21 . . . . -159.0(3) ?
C41 P2 P1 C21 . . . . -11.7(3) ?
Re1 P2 P1 C21 . . . . 104.5(2) ?
N1 P2 P1 C11 . . . . 59.8(4) ?
C31 P2 P1 C11 . . . . -18.6(3) ?
C41 P2 P1 C11 . . . . 128.7(3) ?
Re1 P2 P1 C11 . . . . -115.1(2) ?
N1 P2 P1 Re1 . . . . 174.9(3) ?
C31 P2 P1 Re1 . . . . 96.5(2) ?
C41 P2 P1 Re1 . . . . -116.2(2) ?
C33 C34 C35 C36 . . . . -0.1(9) ?
C33 C32 C31 C36 . . . . 0.0(8) ?
C33 C32 C31 P2 . . . . 172.7(4) ?
N1 P2 C31 C36 . . . . -19.3(5) ?
C41 P2 C31 C36 . . . . -132.0(5) ?
Re1 P2 C31 C36 . . . . 86.5(5) ?
P1 P2 C31 C36 . . . . 21.2(6) ?
N1 P2 C31 C32 . . . . 168.4(4) ?
C41 P2 C31 C32 . . . . 55.7(4) ?
Re1 P2 C31 C32 . . . . -85.8(4) ?
P1 P2 C31 C32 . . . . -151.1(3) ?
N1 P1 C11 C16 . . . . -77.7(4) ?
C21 P1 C11 C16 . . . . 34.9(5) ?
Re1 P1 C11 C16 . . . . 174.8(3) ?
P2 P1 C11 C16 . . . . -111.0(4) ?
N1 P1 C11 C12 . . . . 98.5(4) ?
C21 P1 C11 C12 . . . . -148.8(4) ?
Re1 P1 C11 C12 . . . . -8.9(5) ?
P2 P1 C11 C12 . . . . 65.3(5) ?
C23 C22 C21 C26 . . . . 0.4(8) ?
C23 C22 C21 P1 . . . . 177.4(5) ?
C25 C26 C21 C22 . . . . -2.4(9) ?
C25 C26 C21 P1 . . . . -179.3(5) ?
N1 P1 C21 C22 . . . . 165.6(4) ?
C11 P1 C21 C22 . . . . 55.7(5) ?
Re1 P1 C21 C22 . . . . -89.6(4) ?
P2 P1 C21 C22 . . . . -154.8(4) ?
N1 P1 C21 C26 . . . . -17.6(6) ?
C11 P1 C21 C26 . . . . -127.4(5) ?
Re1 P1 C21 C26 . . . . 87.2(5) ?
P2 P1 C21 C26 . . . . 22.1(6) ?
C12 C11 C16 C15 . . . . -0.3(7) ?
P1 C11 C16 C15 . . . . 176.0(4) ?
C45 C46 C41 C42 . . . . -0.4(8) ?
C45 C46 C41 P2 . . . . -179.8(4) ?
N1 P2 C41 C42 . . . . -77.5(4) ?
C31 P2 C41 C42 . . . . 39.0(5) ?
Re1 P2 C41 C42 . . . . 172.5(3) ?
P1 P2 C41 C42 . . . . -114.4(4) ?
N1 P2 C41 C46 . . . . 101.9(5) ?
C31 P2 C41 C46 . . . . -141.6(4) ?
Re1 P2 C41 C46 . . . . -8.1(5) ?
P1 P2 C41 C46 . . . . 65.0(5) ?
C32 C31 C36 C35 . . . . 0.2(8) ?
P2 C31 C36 C35 . . . . -171.9(4) ?
C34 C35 C36 C31 . . . . -0.2(9) ?
C11 C16 C15 C14 . . . . 0.4(8) ?
C12 C13 C14 C15 . . . . -0.2(9) ?
C16 C15 C14 C13 . . . . -0.1(9) ?
C31 P2 N1 C4A . . . . -78.0(6) ?
C41 P2 N1 C4A . . . . 32.3(7) ?
Re1 P2 N1 C4A . . . . 164.4(6) ?
P1 P2 N1 C4A . . . . 160.1(8) ?
C31 P2 N1 C4B . . . . -32.4(8) ?
C41 P2 N1 C4B . . . . 77.9(8) ?
Re1 P2 N1 C4B . . . . -150.0(7) ?
P1 P2 N1 C4B . . . . -154.3(9) ?
C31 P2 N1 P1 . . . . 121.9(3) ?
C41 P2 N1 P1 . . . . -127.7(3) ?
Re1 P2 N1 P1 . . . . 4.3(2) ?
C21 P1 N1 C4A . . . . -45.5(6) ?
C11 P1 N1 C4A . . . . 62.3(6) ?
Re1 P1 N1 C4A . . . . -166.2(5) ?
P2 P1 N1 C4A . . . . -161.9(7) ?
C21 P1 N1 C4B . . . . -92.0(9) ?
C11 P1 N1 C4B . . . . 15.8(9) ?
Re1 P1 N1 C4B . . . . 147.4(8) ?
P2 P1 N1 C4B . . . . 151.6(9) ?
C21 P1 N1 P2 . . . . 116.4(3) ?
C11 P1 N1 P2 . . . . -135.8(3) ?
Re1 P1 N1 P2 . . . . -4.3(2) ?
C43 C44 C45 C46 . . . . 1.3(9) ?
C41 C46 C45 C44 . . . . -0.4(9) ?
C14 C13 C12 C11 . . . . 0.3(9) ?
C16 C11 C12 C13 . . . . 0.0(8) ?
P1 C11 C12 C13 . . . . -176.4(4) ?
C23 C24 C25 C26 . . . . 1.1(10) ?
C21 C26 C25 C24 . . . . 1.7(10) ?
C25 C24 C23 C22 . . . . -3.1(10) ?
C21 C22 C23 C24 . . . . 2.3(9) ?
C46 C41 C42 C43 . . . . 0.4(8) ?
P2 C41 C42 C43 . . . . 179.8(4) ?
C41 C42 C43 C44 . . . . 0.4(8) ?
C45 C44 C43 C42 . . . . -1.3(8) ?
C35 C34 C33 C32 . . . . 0.3(9) ?
C31 C32 C33 C34 . . . . -0.2(8) ?
C2 Re1 Br1 Br1 . . . 1 0.00(6) ?
C1 Re1 Br1 Br1 . . . 1 0.00(6) ?
C3A Re1 Br1 Br1 . . . 1 0.0(14) ?
P2 Re1 Br1 Br1 . . . 1 0.00(6) ?
P1 Re1 Br1 Br1 . . . 1 0.00(6) ?
C4A N1 C4B C5B . . . . -7.6(9) ?
P2 N1 C4B C5B . . . . -124.3(10) ?
P1 N1 C4B C5B . . . . 88.3(12) ?
N1 C4B C5B C6B . . . . -176.0(19) ?
C4B N1 C4A C5A . . . . 9.0(10) ?
P2 N1 C4A C5A . . . . 99.9(7) ?
P1 N1 C4A C5A . . . . -103.3(7) ?
N1 C4A C5A C6A . . . . 170.2(13) ?
