# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_TcNOCpPPh3_Br
_database_code_depnum_ccdc_archive 'CCDC 1491441'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'Bromido-hapto5-cyclopentadienyltriphenylphosphinenitrosyl technetium(I)'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H20 Br N O P Tc'
_chemical_formula_sum            'C23 H20 Br N O P Tc'
_chemical_formula_weight         535.28

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.001(1)
_cell_length_b                   13.607(1)
_cell_length_c                   17.541(1)
_cell_angle_alpha                90
_cell_angle_beta                 126.91(1)
_cell_angle_gamma                90
_cell_volume                     4198.8(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9956
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.79

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_F_000             2128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    2.679
_shelx_estimated_absorpt_T_min   0.379
_shelx_estimated_absorpt_T_max   0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5453
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker,2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61770
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.315
_diffrn_reflns_theta_max         27.918
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5012
_reflns_number_gt                4503
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0257P)²+19.1468P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5012
_refine_ls_number_parameters     262
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_restrained_S_all      1.278
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Br2 Br 0.17171(5) 0.19594(6) 0.24738(7) 0.01935(19) Uani 0.5 1 d . . P . .
Br1 Br 0.15359(6) -0.00629(8) 0.39391(9) 0.0371(2) Uani 0.5 1 d . . P . .
N10 N 0.1759(5) 0.1534(7) 0.2636(7) 0.0374(12) Uani 0.5 1 d D . P . .
O10 O 0.1802(6) 0.2282(6) 0.2570(7) 0.0374(12) Uani 0.5 1 d D . P . .
Tc1 Tc 0.16771(2) 0.01693(2) 0.26555(2) 0.02018(9) Uani 1 1 d D . . . .
P1 P 0.30219(4) 0.01156(6) 0.37278(6) 0.01371(16) Uani 1 1 d . . . . .
C21 C 0.34975(18) 0.1166(2) 0.4533(2) 0.0168(6) Uani 1 1 d . . . . .
C31 C 0.34408(18) 0.0064(2) 0.3093(2) 0.0173(6) Uani 1 1 d . . . . .
C11 C 0.34373(18) -0.0940(2) 0.4535(2) 0.0149(6) Uani 1 1 d . . . . .
C14 C 0.4080(2) -0.2580(3) 0.5730(3) 0.0241(7) Uani 1 1 d . . . . .
H14 H 0.4295 -0.3125 0.6129 0.029 Uiso 1 1 calc R U . . .
C26 C 0.4127(2) 0.1612(3) 0.4672(3) 0.0237(7) Uani 1 1 d . . . . .
H26 H 0.4305 0.1389 0.4338 0.028 Uiso 1 1 calc R U . . .
C16 C 0.42029(19) -0.0936(2) 0.5321(2) 0.0181(7) Uani 1 1 d . . . . .
H16 H 0.4502 -0.0387 0.5448 0.022 Uiso 1 1 calc R U . . .
C12 C 0.29994(19) -0.1771(3) 0.4362(3) 0.0211(7) Uani 1 1 d . . . . .
H12 H 0.2486 -0.1775 0.3847 0.025 Uiso 1 1 calc R U . . .
C36 C 0.3234(2) 0.0797(3) 0.2413(3) 0.0257(8) Uani 1 1 d . . . . .
H36 H 0.2908 0.1301 0.2313 0.031 Uiso 1 1 calc R U . . .
C13 C 0.3320(2) -0.2593(3) 0.4949(3) 0.0246(8) Uani 1 1 d . . . . .
H13 H 0.3026 -0.3148 0.4817 0.030 Uiso 1 1 calc R U . . .
C34 C 0.4009(2) 0.0014(3) 0.2036(3) 0.0288(8) Uani 1 1 d . . . . .
H34 H 0.4201 -0.0004 0.1686 0.035 Uiso 1 1 calc R U . . .
C15 C 0.4520(2) -0.1754(3) 0.5917(3) 0.0234(7) Uani 1 1 d . . . . .
H15 H 0.5030 -0.1747 0.6442 0.028 Uiso 1 1 calc R U . . .
C4 C 0.1595(2) -0.1212(3) 0.1859(3) 0.0344(10) Uani 1 1 d . . . . .
H4 H 0.1987 -0.1719 0.2103 0.041 Uiso 1 1 calc R U . . .
C33 C 0.4210(2) -0.0708(3) 0.2704(3) 0.0269(8) Uani 1 1 d . . . . .
H33 H 0.4533 -0.1214 0.2798 0.032 Uiso 1 1 calc R U . . .
C32 C 0.3931(2) -0.0679(3) 0.3236(2) 0.0197(7) Uani 1 1 d . . . . .
H32 H 0.4074 -0.1162 0.3691 0.024 Uiso 1 1 calc R U . . .
C25 C 0.4490(2) 0.2393(3) 0.5311(3) 0.0328(9) Uani 1 1 d . . . . .
H25 H 0.4913 0.2686 0.5406 0.039 Uiso 1 1 calc R U . . .
C35 C 0.3522(2) 0.0762(3) 0.1887(3) 0.0298(9) Uani 1 1 d . . . . .
H35 H 0.3386 0.1245 0.1434 0.036 Uiso 1 1 calc R U . . .
C22 C 0.3230(2) 0.1514(3) 0.5028(3) 0.0270(8) Uani 1 1 d . . . . .
H22 H 0.2809 0.1223 0.4938 0.032 Uiso 1 1 calc R U . . .
C24 C 0.4224(2) 0.2731(3) 0.5798(3) 0.0357(10) Uani 1 1 d . . . . .
H24 H 0.4467 0.3251 0.6223 0.043 Uiso 1 1 calc R U . . .
C23 C 0.3595(2) 0.2301(3) 0.5659(3) 0.0340(9) Uani 1 1 d . . . . .
H23 H 0.3414 0.2536 0.5987 0.041 Uiso 1 1 calc R U . . .
C1 C 0.0834(3) 0.0105(4) 0.1043(3) 0.0464(13) Uani 1 1 d . . . . .
H1 H 0.0608 0.0678 0.0621 0.056 Uiso 1 1 calc R U . . .
C2 C 0.0509(2) -0.0404(4) 0.1413(4) 0.0465(13) Uani 1 1 d . . . . .
H2 H 0.0022 -0.0260 0.1292 0.056 Uiso 1 1 calc R U . . .
C5 C 0.1503(3) -0.0379(4) 0.1312(3) 0.0401(11) Uani 1 1 d . . . . .
H5 H 0.1816 -0.0212 0.1103 0.048 Uiso 1 1 calc R U . . .
C3 C 0.0989(3) -0.1224(3) 0.1922(3) 0.0399(11) Uani 1 1 d . . . . .
H3 H 0.0890 -0.1742 0.2222 0.048 Uiso 1 1 calc R U . . .
N10A N 0.1597(5) 0.0078(7) 0.3564(6) 0.0374(12) Uani 0.5 1 d D . P . .
O10A O 0.1446(5) -0.0068(7) 0.4190(6) 0.0374(12) Uani 0.5 1 d D . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Br2 N10 0.628(9) . ?
Br2 Tc1 2.4651(10) . ?
Br1 O10A 0.580(7) . ?
Br1 N10A 0.771(8) . ?
Br1 Tc1 2.4711(14) . ?
N10 O10 1.036(10) . ?
N10 Tc1 1.867(9) . ?
Tc1 N10A 1.709(9) . ?
Tc1 C1 2.268(4) . ?
Tc1 C5 2.274(4) . ?
Tc1 C3 2.281(4) . ?
Tc1 C4 2.283(4) . ?
Tc1 C2 2.287(4) . ?
Tc1 P1 2.3691(9) . ?
P1 C31 1.824(3) . ?
P1 C11 1.830(3) . ?
P1 C21 1.832(3) . ?
C21 C26 1.392(5) . ?
C21 C22 1.392(5) . ?
C31 C32 1.387(5) . ?
C31 C36 1.404(5) . ?
C11 C12 1.395(5) . ?
C11 C16 1.396(5) . ?
C14 C13 1.386(5) . ?
C14 C15 1.389(5) . ?
C14 H14 0.9300 . ?
C26 C25 1.396(5) . ?
C26 H26 0.9300 . ?
C16 C15 1.393(5) . ?
C16 H16 0.9300 . ?
C12 C13 1.391(5) . ?
C12 H12 0.9300 . ?
C36 C35 1.400(5) . ?
C36 H36 0.9300 . ?
C13 H13 0.9300 . ?
C34 C33 1.382(5) . ?
C34 C35 1.385(6) . ?
C34 H34 0.9300 . ?
C15 H15 0.9300 . ?
C4 C3 1.402(7) . ?
C4 C5 1.418(7) . ?
C4 H4 0.9800 . ?
C33 C32 1.395(5) . ?
C33 H33 0.9300 . ?
C32 H32 0.9300 . ?
C25 C24 1.374(6) . ?
C25 H25 0.9300 . ?
C35 H35 0.9300 . ?
C22 C23 1.396(5) . ?
C22 H22 0.9300 . ?
C24 C23 1.383(6) . ?
C24 H24 0.9300 . ?
C23 H23 0.9300 . ?
C1 C2 1.402(8) . ?
C1 C5 1.412(7) . ?
C1 H1 0.9800 . ?
C2 C3 1.423(7) . ?
C2 H2 0.9800 . ?
C5 H5 0.9800 . ?
C3 H3 0.9800 . ?
N10A O10A 1.339(9) . ?

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
N10 Br2 Tc1 15.4(8) . . ?
O10A Br1 N10A 164.4(11) . . ?
O10A Br1 Tc1 168.1(9) . . ?
N10A Br1 Tc1 7.5(7) . . ?
Br2 N10 O10 16.2(7) . . ?
Br2 N10 Tc1 159.5(11) . . ?
O10 N10 Tc1 174.7(10) . . ?
N10A Tc1 N10 98.8(4) . . ?
N10A Tc1 C1 133.9(3) . . ?
N10 Tc1 C1 91.8(3) . . ?
N10A Tc1 C5 153.5(3) . . ?
N10 Tc1 C5 105.4(3) . . ?
C1 Tc1 C5 36.23(19) . . ?
N10A Tc1 C3 93.5(3) . . ?
N10 Tc1 C3 148.7(3) . . ?
C1 Tc1 C3 59.72(18) . . ?
C5 Tc1 C3 60.07(18) . . ?
N10A Tc1 C4 119.7(3) . . ?
N10 Tc1 C4 141.3(3) . . ?
C1 Tc1 C4 60.04(17) . . ?
C5 Tc1 C4 36.26(17) . . ?
C3 Tc1 C4 35.76(17) . . ?
N10A Tc1 C2 100.2(3) . . ?
N10 Tc1 C2 112.8(3) . . ?
C1 Tc1 C2 35.9(2) . . ?
C5 Tc1 C2 60.50(19) . . ?
C3 Tc1 C2 36.28(17) . . ?
C4 Tc1 C2 60.35(16) . . ?
N10A Tc1 P1 92.1(3) . . ?
N10 Tc1 P1 87.5(3) . . ?
C1 Tc1 P1 133.26(15) . . ?
C5 Tc1 P1 99.50(13) . . ?
C3 Tc1 P1 120.77(12) . . ?
C4 Tc1 P1 93.61(11) . . ?
C2 Tc1 P1 153.95(13) . . ?
N10A Tc1 Br2 102.9(3) . . ?
N10 Tc1 Br2 5.1(3) . . ?
C1 Tc1 Br2 86.71(13) . . ?
C5 Tc1 Br2 100.78(13) . . ?
C3 Tc1 Br2 144.25(13) . . ?
C4 Tc1 Br2 136.89(12) . . ?
C2 Tc1 Br2 108.71(14) . . ?
P1 Tc1 Br2 90.49(3) . . ?
N10A Tc1 Br1 3.4(3) . . ?
N10 Tc1 Br1 102.1(3) . . ?
C1 Tc1 Br1 132.42(15) . . ?
C5 Tc1 Br1 150.13(13) . . ?
C3 Tc1 Br1 90.22(14) . . ?
C4 Tc1 Br1 116.44(13) . . ?
C2 Tc1 Br1 98.07(15) . . ?
P1 Tc1 Br1 93.04(3) . . ?
Br2 Tc1 Br1 106.14(4) . . ?
C31 P1 C11 103.97(15) . . ?
C31 P1 C21 103.66(15) . . ?
C11 P1 C21 103.16(15) . . ?
C31 P1 Tc1 111.37(11) . . ?
C11 P1 Tc1 116.34(11) . . ?
C21 P1 Tc1 116.80(11) . . ?
C26 C21 C22 119.4(3) . . ?
C26 C21 P1 121.5(3) . . ?
C22 C21 P1 119.1(3) . . ?
C32 C31 C36 119.5(3) . . ?
C32 C31 P1 122.7(3) . . ?
C36 C31 P1 117.9(3) . . ?
C12 C11 C16 118.9(3) . . ?
C12 C11 P1 120.6(2) . . ?
C16 C11 P1 120.5(2) . . ?
C13 C14 C15 119.9(3) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C21 C26 C25 120.2(4) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C15 C16 C11 120.1(3) . . ?
C15 C16 H16 119.9 . . ?
C11 C16 H16 119.9 . . ?
C13 C12 C11 120.9(3) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C35 C36 C31 119.6(4) . . ?
C35 C36 H36 120.2 . . ?
C31 C36 H36 120.2 . . ?
C14 C13 C12 119.8(3) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C33 C34 C35 120.0(4) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C14 C15 C16 120.4(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C3 C4 C5 107.9(4) . . ?
C3 C4 Tc1 72.1(2) . . ?
C5 C4 Tc1 71.5(2) . . ?
C3 C4 H4 125.9 . . ?
C5 C4 H4 125.9 . . ?
Tc1 C4 H4 125.9 . . ?
C34 C33 C32 120.2(4) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C31 C32 C33 120.4(3) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C24 C25 C26 120.1(4) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C34 C35 C36 120.4(4) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C21 C22 C23 119.9(4) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C25 C24 C23 120.3(4) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C23 C22 120.1(4) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C2 C1 C5 109.5(4) . . ?
C2 C1 Tc1 72.8(3) . . ?
C5 C1 Tc1 72.1(2) . . ?
C2 C1 H1 125.2 . . ?
C5 C1 H1 125.2 . . ?
Tc1 C1 H1 125.2 . . ?
C1 C2 C3 106.6(4) . . ?
C1 C2 Tc1 71.3(2) . . ?
C3 C2 Tc1 71.6(2) . . ?
C1 C2 H2 126.6 . . ?
C3 C2 H2 126.6 . . ?
Tc1 C2 H2 126.6 . . ?
C1 C5 C4 107.1(4) . . ?
C1 C5 Tc1 71.7(3) . . ?
C4 C5 Tc1 72.2(2) . . ?
C1 C5 H5 126.3 . . ?
C4 C5 H5 126.3 . . ?
Tc1 C5 H5 126.3 . . ?
C4 C3 C2 108.9(4) . . ?
C4 C3 Tc1 72.2(2) . . ?
C2 C3 Tc1 72.1(2) . . ?
C4 C3 H3 125.5 . . ?
C2 C3 H3 125.5 . . ?
Tc1 C3 H3 125.5 . . ?
Br1 N10A O10A 6.7(5) . . ?
Br1 N10A Tc1 169.1(10) . . ?
O10A N10A Tc1 171.9(9) . . ?
Br1 O10A N10A 8.9(6) . . ?

_refine_diff_density_max         0.535
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.117

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TcNOCpPPh3_CO
_database_code_depnum_ccdc_archive 'CCDC 1491442'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;        
hapto5-cyclopentadienylcarbonyl
triphenylphosphinenitrosyl technetium(I)
;
_chemical_name_common            '[Tc(NO)(CO)(PPh3)]BF4'
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H20 N O P Tc, B F4'
_chemical_formula_sum            'C24 H20 B F4 N O2 P Tc'
_chemical_formula_weight         570.19

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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'

_cell_length_a                   9.270(1)
_cell_length_b                   17.374(1)
_cell_length_c                   14.270(1)
_cell_angle_alpha                90
_cell_angle_beta                 100.29(1)
_cell_angle_gamma                90
_cell_volume                     2261.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9576
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      26.42

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.763
_shelx_estimated_absorpt_T_min   0.750
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6734
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker,2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47238
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.344
_diffrn_reflns_theta_max         26.417
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4651
_reflns_number_gt                4007
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0256P)²+3.5769P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4651
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0667
_refine_ls_wR_factor_gt          0.0622
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Tc1 Tc 0.52113(2) 0.12824(2) 0.66175(2) 0.01504(7) Uani 1 1 d . . . . .
P1 P 0.73724(6) 0.18412(3) 0.61907(4) 0.01007(12) Uani 1 1 d . . . . .
C21 C 0.8891(2) 0.17112(13) 0.71723(16) 0.0126(4) Uani 1 1 d . . . . .
O20 O 0.6145(2) -0.02295(10) 0.58431(14) 0.0269(4) Uani 1 1 d . . . . .
C31 C 0.7931(2) 0.14139(12) 0.51450(16) 0.0129(4) Uani 1 1 d . . . . .
C12 C 0.5981(2) 0.32739(13) 0.59586(16) 0.0141(5) Uani 1 1 d . . . . .
H12 H 0.5164 0.3023 0.6141 0.017 Uiso 1 1 calc R U . . .
C22 C 0.9588(2) 0.23312(13) 0.76765(17) 0.0162(5) Uani 1 1 d . . . . .
H22 H 0.9387 0.2840 0.7448 0.019 Uiso 1 1 calc R U . . .
C16 C 0.8450(2) 0.32322(13) 0.56263(17) 0.0150(5) Uani 1 1 d . . . . .
H16 H 0.9312 0.2951 0.5576 0.018 Uiso 1 1 calc R U . . .
C20 C 0.5789(2) 0.03365(13) 0.61231(17) 0.0139(5) Uani 1 1 d . . . . .
C36 C 0.6885(3) 0.13573(13) 0.43117(17) 0.0174(5) Uani 1 1 d . . . . .
H36 H 0.5907 0.1521 0.4312 0.021 Uiso 1 1 calc R U . . .
C13 C 0.5909(3) 0.40565(13) 0.57386(17) 0.0159(5) Uani 1 1 d . . . . .
H13 H 0.5039 0.4338 0.5767 0.019 Uiso 1 1 calc R U . . .
C14 C 0.7101(3) 0.44215(13) 0.54803(17) 0.0168(5) Uani 1 1 d . . . . .
H14 H 0.7056 0.4957 0.5343 0.020 Uiso 1 1 calc R U . . .
O10 O 0.3231(2) 0.18259(12) 0.48597(15) 0.0356(5) Uani 1 1 d . . . . .
C15 C 0.8368(3) 0.40116(13) 0.54195(18) 0.0176(5) Uani 1 1 d . . . . .
H15 H 0.9180 0.4267 0.5236 0.021 Uiso 1 1 calc R U . . .
C11 C 0.7257(2) 0.28603(12) 0.59097(16) 0.0115(4) Uani 1 1 d . . . . .
N10 N 0.4038(2) 0.16096(13) 0.55183(17) 0.0249(5) Uani 1 1 d . . . . .
C34 C 0.8678(3) 0.08174(13) 0.34818(18) 0.0205(5) Uani 1 1 d . . . . .
H34 H 0.8932 0.0611 0.2916 0.025 Uiso 1 1 calc R U . . .
C25 C 1.0218(3) 0.08417(14) 0.83319(18) 0.0196(5) Uani 1 1 d . . . . .
H25 H 1.0444 0.0332 0.8551 0.023 Uiso 1 1 calc R U . . .
C26 C 0.9225(3) 0.09617(13) 0.75034(18) 0.0168(5) Uani 1 1 d . . . . .
H26 H 0.8765 0.0535 0.7156 0.020 Uiso 1 1 calc R U . . .
C3 C 0.5928(3) 0.16962(15) 0.81701(18) 0.0231(5) Uani 1 1 d . . . . .
H3 H 0.6883 0.1949 0.8436 0.028 Uiso 1 1 calc R U . . .
C24 C 1.0892(3) 0.14655(16) 0.88512(18) 0.0229(6) Uani 1 1 d . . . . .
H24 H 1.1561 0.1382 0.9429 0.027 Uiso 1 1 calc R U . . .
C2 C 0.5645(3) 0.09032(16) 0.81689(19) 0.0281(6) Uani 1 1 d . . . . .
H2 H 0.6347 0.0494 0.8454 0.034 Uiso 1 1 calc R U . . .
C23 C 1.0580(3) 0.22065(15) 0.85178(18) 0.0222(5) Uani 1 1 d . . . . .
H23 H 1.1045 0.2632 0.8865 0.027 Uiso 1 1 calc R U . . .
C35 C 0.7258(3) 0.10651(14) 0.34862(18) 0.0193(5) Uani 1 1 d . . . . .
H35 H 0.6541 0.1034 0.2922 0.023 Uiso 1 1 calc R U . . .
C32 C 0.9363(3) 0.11676(14) 0.51345(18) 0.0190(5) Uani 1 1 d . . . . .
H32 H 1.0087 0.1203 0.5695 0.023 Uiso 1 1 calc R U . . .
C33 C 0.9724(3) 0.08706(14) 0.42998(19) 0.0234(6) Uani 1 1 d . . . . .
H33 H 1.0698 0.0703 0.4293 0.028 Uiso 1 1 calc R U . . .
C4 C 0.3518(3) 0.15235(18) 0.7551(2) 0.0300(6) Uani 1 1 d . . . . .
H4 H 0.2455 0.1632 0.7316 0.036 Uiso 1 1 calc R U . . .
C1 C 0.4126(3) 0.07986(16) 0.7788(2) 0.0303(6) Uani 1 1 d . . . . .
H1 H 0.3574 0.0302 0.7764 0.036 Uiso 1 1 calc R U . . .
C5 C 0.4619(3) 0.20792(15) 0.77770(19) 0.0261(6) Uani 1 1 d . . . . .
H5 H 0.4481 0.2649 0.7725 0.031 Uiso 1 1 calc R U . . .
F1 F 0.13506(17) 0.09886(9) 0.23831(12) 0.0320(4) Uani 1 1 d . . . . .
F2 F 0.37833(16) 0.10543(9) 0.23236(12) 0.0296(4) Uani 1 1 d . . . . .
F3 F 0.21689(18) 0.06077(9) 0.10531(12) 0.0319(4) Uani 1 1 d . . . . .
F4 F 0.21912(17) 0.18766(9) 0.14311(12) 0.0323(4) Uani 1 1 d . . . . .
B1 B 0.2362(3) 0.11323(15) 0.1801(2) 0.0180(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Tc1 N10 1.832(2) . ?
Tc1 C20 1.903(2) . ?
Tc1 C1 2.261(3) . ?
Tc1 C4 2.271(3) . ?
Tc1 C2 2.276(3) . ?
Tc1 C5 2.298(3) . ?
Tc1 C3 2.311(3) . ?
Tc1 P1 2.4006(6) . ?
P1 C11 1.814(2) . ?
P1 C21 1.814(2) . ?
P1 C31 1.822(2) . ?
C21 C22 1.389(3) . ?
C21 C26 1.401(3) . ?
O20 C20 1.133(3) . ?
C31 C36 1.397(3) . ?
C31 C32 1.397(3) . ?
C12 C13 1.394(3) . ?
C12 C11 1.396(3) . ?
C12 H12 0.9500 . ?
C22 C23 1.393(3) . ?
C22 H22 0.9500 . ?
C16 C15 1.385(3) . ?
C16 C11 1.402(3) . ?
C16 H16 0.9500 . ?
C36 C35 1.382(3) . ?
C36 H36 0.9500 . ?
C13 C14 1.380(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(3) . ?
C14 H14 0.9500 . ?
O10 N10 1.155(3) . ?
C15 H15 0.9500 . ?
C34 C33 1.381(4) . ?
C34 C35 1.386(4) . ?
C34 H34 0.9500 . ?
C25 C26 1.378(3) . ?
C25 C24 1.396(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C3 C2 1.402(4) . ?
C3 C5 1.410(4) . ?
C3 H3 1.0000 . ?
C24 C23 1.385(4) . ?
C24 H24 0.9500 . ?
C2 C1 1.427(4) . ?
C2 H2 1.0000 . ?
C23 H23 0.9500 . ?
C35 H35 0.9500 . ?
C32 C33 1.393(4) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C4 C1 1.397(4) . ?
C4 C5 1.400(4) . ?
C4 H4 1.0000 . ?
C1 H1 1.0000 . ?
C5 H5 1.0000 . ?
F1 B1 1.382(3) . ?
F2 B1 1.400(3) . ?
F3 B1 1.390(3) . ?
F4 B1 1.395(3) . ?

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
N10 Tc1 C20 96.54(10) . . ?
N10 Tc1 C1 118.28(11) . . ?
C20 Tc1 C1 98.32(10) . . ?
N10 Tc1 C4 94.47(10) . . ?
C20 Tc1 C4 130.27(10) . . ?
C1 Tc1 C4 35.90(11) . . ?
N10 Tc1 C2 153.82(10) . . ?
C20 Tc1 C2 95.63(10) . . ?
C1 Tc1 C2 36.68(11) . . ?
C4 Tc1 C2 60.24(10) . . ?
N10 Tc1 C5 104.35(10) . . ?
C20 Tc1 C5 155.05(10) . . ?
C1 Tc1 C5 59.79(10) . . ?
C4 Tc1 C5 35.68(10) . . ?
C2 Tc1 C5 59.83(9) . . ?
N10 Tc1 C3 138.53(10) . . ?
C20 Tc1 C3 124.92(10) . . ?
C1 Tc1 C3 59.79(10) . . ?
C4 Tc1 C3 59.41(10) . . ?
C2 Tc1 C3 35.59(10) . . ?
C5 Tc1 C3 35.62(9) . . ?
N10 Tc1 P1 92.97(7) . . ?
C20 Tc1 P1 87.27(7) . . ?
C1 Tc1 P1 147.10(8) . . ?
C4 Tc1 P1 140.31(8) . . ?
C2 Tc1 P1 110.70(8) . . ?
C5 Tc1 P1 104.87(7) . . ?
C3 Tc1 P1 90.42(7) . . ?
C11 P1 C21 107.41(10) . . ?
C11 P1 C31 103.34(10) . . ?
C21 P1 C31 106.66(10) . . ?
C11 P1 Tc1 115.58(7) . . ?
C21 P1 Tc1 108.75(7) . . ?
C31 P1 Tc1 114.51(7) . . ?
C22 C21 C26 119.5(2) . . ?
C22 C21 P1 121.89(17) . . ?
C26 C21 P1 118.06(17) . . ?
C36 C31 C32 119.0(2) . . ?
C36 C31 P1 118.04(17) . . ?
C32 C31 P1 122.88(18) . . ?
C13 C12 C11 119.9(2) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C21 C22 C23 120.0(2) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C15 C16 C11 119.7(2) . . ?
C15 C16 H16 120.1 . . ?
C11 C16 H16 120.1 . . ?
O20 C20 Tc1 178.9(2) . . ?
C35 C36 C31 120.7(2) . . ?
C35 C36 H36 119.7 . . ?
C31 C36 H36 119.7 . . ?
C14 C13 C12 120.0(2) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.5(2) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C16 C15 C14 120.2(2) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C12 C11 C16 119.8(2) . . ?
C12 C11 P1 120.55(17) . . ?
C16 C11 P1 119.68(16) . . ?
O10 N10 Tc1 175.6(2) . . ?
C33 C34 C35 120.0(2) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C26 C25 C24 120.3(2) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 120.2(2) . . ?
C25 C26 H26 119.9 . . ?
C21 C26 H26 119.9 . . ?
C2 C3 C5 108.4(2) . . ?
C2 C3 Tc1 70.83(15) . . ?
C5 C3 Tc1 71.68(15) . . ?
C2 C3 H3 125.8 . . ?
C5 C3 H3 125.8 . . ?
Tc1 C3 H3 125.8 . . ?
C23 C24 C25 119.5(2) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C3 C2 C1 107.3(2) . . ?
C3 C2 Tc1 73.58(15) . . ?
C1 C2 Tc1 71.08(15) . . ?
C3 C2 H2 126.2 . . ?
C1 C2 H2 126.2 . . ?
Tc1 C2 H2 126.2 . . ?
C24 C23 C22 120.4(2) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C36 C35 C34 120.0(2) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C33 C32 C31 119.8(2) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C34 C33 C32 120.5(2) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C1 C4 C5 108.7(2) . . ?
C1 C4 Tc1 71.63(15) . . ?
C5 C4 Tc1 73.19(15) . . ?
C1 C4 H4 125.6 . . ?
C5 C4 H4 125.6 . . ?
Tc1 C4 H4 125.6 . . ?
C4 C1 C2 107.8(2) . . ?
C4 C1 Tc1 72.47(15) . . ?
C2 C1 Tc1 72.24(15) . . ?
C4 C1 H1 125.9 . . ?
C2 C1 H1 125.9 . . ?
Tc1 C1 H1 125.9 . . ?
C4 C5 C3 107.8(2) . . ?
C4 C5 Tc1 71.12(15) . . ?
C3 C5 Tc1 72.70(15) . . ?
C4 C5 H5 126.0 . . ?
C3 C5 H5 126.0 . . ?
Tc1 C5 H5 126.0 . . ?
F1 B1 F3 109.6(2) . . ?
F1 B1 F4 110.6(2) . . ?
F3 B1 F4 109.1(2) . . ?
F1 B1 F2 109.7(2) . . ?
F3 B1 F2 109.0(2) . . ?
F4 B1 F2 108.9(2) . . ?

_refine_diff_density_max         0.762
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.073

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TcNOCpPPh3_Phenyl
_database_code_depnum_ccdc_archive 'CCDC 1491443'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;        
hapto5-cyclopentadienylphenyl
triphenylphosphinenitrosyl technetium(I)
;
_chemical_name_common            ' [Tc(NO)(Cp)(Ph)(PPh3)]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H25 N O Tc P'
_chemical_formula_sum            'C29 H25 N O P Tc'
_chemical_formula_weight         532.47

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'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.179(1)
_cell_length_b                   13.937(1)
_cell_length_c                   10.048(7)
_cell_angle_alpha                90
_cell_angle_beta                 112.89(2)
_cell_angle_gamma                90
_cell_volume                     1184.2(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9603
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      27.92

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_F_000             544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.698
_shelx_estimated_absorpt_T_min   0.845
_shelx_estimated_absorpt_T_max   0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6948
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2014/5
(Bruker, 2014)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46079
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.408
_diffrn_reflns_theta_max         27.909
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5631
_reflns_number_gt                5576
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.918
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0261P)²+1.1186P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2640 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5631
_refine_ls_number_parameters     298
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0141
_refine_ls_wR_factor_ref         0.0361
_refine_ls_wR_factor_gt          0.0358
_refine_ls_goodness_of_fit_ref   0.714
_refine_ls_restrained_S_all      0.714
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Tc1 Tc 0.47432(2) 0.15151(2) 0.39654(2) 0.01053(4) Uani 1 1 d . . . . .
N10 N 0.6213(2) 0.22265(13) 0.52351(18) 0.0142(3) Uani 1 1 d . . . . .
O10 O 0.7129(2) 0.27165(12) 0.61652(17) 0.0235(3) Uani 1 1 d . . . . .
C1 C 0.2564(2) 0.05463(16) 0.2967(2) 0.0166(4) Uani 1 1 d . . . . .
H1 H 0.2275 0.0167 0.2055 0.020 Uiso 1 1 calc R U . . .
C2 C 0.1996(2) 0.1482(2) 0.3090(2) 0.0182(3) Uani 1 1 d . . . . .
H2 H 0.1261 0.1878 0.2274 0.022 Uiso 1 1 calc R U . . .
C3 C 0.2544(3) 0.17179(15) 0.4574(3) 0.0211(5) Uani 1 1 d . . . . .
H3 H 0.2274 0.2312 0.4988 0.025 Uiso 1 1 calc R U . . .
C4 C 0.3462(3) 0.09326(18) 0.5381(3) 0.0221(5) Uani 1 1 d . . . . .
H4 H 0.3931 0.0878 0.6458 0.027 Uiso 1 1 calc R U . . .
C5 C 0.3475(2) 0.02061(16) 0.4396(2) 0.0189(4) Uani 1 1 d . . . . .
H5 H 0.3930 -0.0452 0.4658 0.023 Uiso 1 1 calc R U . . .
P1 P 0.45835(6) 0.24288(3) 0.19398(5) 0.00949(9) Uani 1 1 d . . . . .
C11 C 0.3732(2) 0.36324(14) 0.1817(2) 0.0112(3) Uani 1 1 d . . . . .
C12 C 0.3494(2) 0.42059(15) 0.0605(2) 0.0149(4) Uani 1 1 d . . . . .
H12 H 0.3840 0.3986 -0.0118 0.018 Uiso 1 1 calc R U . . .
C13 C 0.2755(3) 0.50945(17) 0.0449(3) 0.0182(5) Uani 1 1 d . . . . .
H13 H 0.2562 0.5468 -0.0393 0.022 Uiso 1 1 calc R U . . .
C14 C 0.2299(2) 0.54347(15) 0.1536(2) 0.0184(4) Uani 1 1 d . . . . .
H14 H 0.1802 0.6044 0.1437 0.022 Uiso 1 1 calc R U . . .
C15 C 0.2569(3) 0.48842(16) 0.2762(2) 0.0178(4) Uani 1 1 d . . . . .
H15 H 0.2275 0.5122 0.3509 0.021 Uiso 1 1 calc R U . . .
C16 C 0.3272(2) 0.39819(15) 0.2899(2) 0.0141(4) Uani 1 1 d . . . . .
H16 H 0.3439 0.3603 0.3731 0.017 Uiso 1 1 calc R U . . .
C21 C 0.3293(2) 0.18492(14) 0.0264(2) 0.0109(3) Uani 1 1 d . . . . .
C22 C 0.1837(2) 0.22257(15) -0.0663(2) 0.0137(4) Uani 1 1 d . . . . .
H22 H 0.1475 0.2820 -0.0443 0.016 Uiso 1 1 calc R U . . .
C23 C 0.0918(2) 0.17261(14) -0.1913(2) 0.0159(4) Uani 1 1 d . . . . .
H23 H -0.0067 0.1984 -0.2545 0.019 Uiso 1 1 calc R U . . .
C26 C 0.3795(2) 0.09654(15) -0.0061(2) 0.0136(4) Uani 1 1 d . . . . .
H26 H 0.4770 0.0699 0.0576 0.016 Uiso 1 1 calc R U . . .
C25 C 0.2879(2) 0.04734(15) -0.1307(2) 0.0163(4) Uani 1 1 d . . . . .
H25 H 0.3234 -0.0123 -0.1528 0.020 Uiso 1 1 calc R U . . .
C24 C 0.1434(3) 0.08556(16) -0.2239(2) 0.0170(4) Uani 1 1 d . . . . .
H24 H 0.0807 0.0520 -0.3093 0.020 Uiso 1 1 calc R U . . .
C31 C 0.6379(2) 0.27122(14) 0.1624(2) 0.0110(3) Uani 1 1 d . . . . .
C32 C 0.7699(2) 0.30690(14) 0.2781(2) 0.0127(4) Uani 1 1 d . . . . .
H32 H 0.7677 0.3106 0.3717 0.015 Uiso 1 1 calc R U . . .
C33 C 0.9040(2) 0.33694(15) 0.2570(2) 0.0147(4) Uani 1 1 d . . . . .
H33 H 0.9931 0.3603 0.3363 0.018 Uiso 1 1 calc R U . . .
C34 C 0.9077(2) 0.33279(15) 0.1197(2) 0.0163(4) Uani 1 1 d . . . . .
H34 H 0.9985 0.3544 0.1050 0.020 Uiso 1 1 calc R U . . .
C35 C 0.7782(3) 0.29688(16) 0.0044(3) 0.0161(4) Uani 1 1 d . . . . .
H35 H 0.7808 0.2935 -0.0890 0.019 Uiso 1 1 calc R U . . .
C36 C 0.6443(2) 0.26575(15) 0.0257(2) 0.0143(4) Uani 1 1 d . . . . .
H36 H 0.5568 0.2406 -0.0533 0.017 Uiso 1 1 calc R U . . .
C41 C 0.6360(2) 0.05413(15) 0.3592(2) 0.0125(4) Uani 1 1 d . . . . .
C42 C 0.5938(3) -0.04034(16) 0.3071(2) 0.0157(4) Uani 1 1 d . . . . .
H42 H 0.4859 -0.0590 0.2741 0.019 Uiso 1 1 calc R U . . .
C46 C 0.7975(2) 0.07653(15) 0.4010(2) 0.0141(4) Uani 1 1 d . . . . .
H46 H 0.8322 0.1394 0.4351 0.017 Uiso 1 1 calc R U . . .
C43 C 0.7052(3) -0.10745(16) 0.3023(2) 0.0179(4) Uani 1 1 d . . . . .
H43 H 0.6720 -0.1706 0.2688 0.021 Uiso 1 1 calc R U . . .
C44 C 0.8642(3) -0.08281(16) 0.3461(2) 0.0182(4) Uani 1 1 d . . . . .
H44 H 0.9398 -0.1284 0.3430 0.022 Uiso 1 1 calc R U . . .
C45 C 0.9091(2) 0.01009(16) 0.3942(2) 0.0165(4) Uani 1 1 d . . . . .
H45 H 1.0165 0.0288 0.4229 0.020 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Tc1 N10 1.758(2) . ?
Tc1 C41 2.149(2) . ?
Tc1 C5 2.294(2) . ?
Tc1 C1 2.296(3) . ?
Tc1 C4 2.316(2) . ?
Tc1 C2 2.326(3) . ?
Tc1 C3 2.343(3) . ?
Tc1 P1 2.3565(13) . ?
N10 O10 1.198(2) . ?
C1 C2 1.428(4) . ?
C1 C5 1.433(3) . ?
C1 H1 1.0000 . ?
C2 C3 1.415(3) . ?
C2 H2 1.0000 . ?
C3 C4 1.426(3) . ?
C3 H3 1.0000 . ?
C4 C5 1.418(3) . ?
C4 H4 1.0000 . ?
C5 H5 1.0000 . ?
P1 C21 1.827(2) . ?
P1 C11 1.834(2) . ?
P1 C31 1.839(3) . ?
C11 C16 1.398(3) . ?
C11 C12 1.401(3) . ?
C12 C13 1.391(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.396(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.396(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.398(3) . ?
C21 C22 1.401(3) . ?
C22 C23 1.396(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(3) . ?
C23 H23 0.9500 . ?
C26 C25 1.388(3) . ?
C26 H26 0.9500 . ?
C25 C24 1.398(3) . ?
C25 H25 0.9500 . ?
C24 H24 0.9500 . ?
C31 C36 1.400(3) . ?
C31 C32 1.404(3) . ?
C32 C33 1.392(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.394(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.391(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.396(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.410(3) . ?
C41 C42 1.414(3) . ?
C42 C43 1.401(3) . ?
C42 H42 0.9500 . ?
C46 C45 1.402(3) . ?
C46 H46 0.9500 . ?
C43 C44 1.393(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.388(3) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?

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
N10 Tc1 C41 95.49(10) . . ?
N10 Tc1 C5 127.87(9) . . ?
C41 Tc1 C5 88.07(10) . . ?
N10 Tc1 C1 160.22(8) . . ?
C41 Tc1 C1 95.49(11) . . ?
C5 Tc1 C1 36.38(8) . . ?
N10 Tc1 C4 100.47(10) . . ?
C41 Tc1 C4 115.83(9) . . ?
C5 Tc1 C4 35.83(9) . . ?
C1 Tc1 C4 59.87(9) . . ?
N10 Tc1 C2 134.33(9) . . ?
C41 Tc1 C2 129.95(10) . . ?
C5 Tc1 C2 60.03(10) . . ?
C1 Tc1 C2 35.98(10) . . ?
C4 Tc1 C2 59.38(9) . . ?
N10 Tc1 C3 103.79(10) . . ?
C41 Tc1 C3 147.71(8) . . ?
C5 Tc1 C3 59.64(9) . . ?
C1 Tc1 C3 59.49(10) . . ?
C4 Tc1 C3 35.64(8) . . ?
C2 Tc1 C3 35.28(9) . . ?
N10 Tc1 P1 95.42(7) . . ?
C41 Tc1 P1 90.34(6) . . ?
C5 Tc1 P1 136.64(6) . . ?
C1 Tc1 P1 100.91(7) . . ?
C4 Tc1 P1 147.54(7) . . ?
C2 Tc1 P1 89.42(6) . . ?
C3 Tc1 P1 112.94(6) . . ?
O10 N10 Tc1 174.24(16) . . ?
C2 C1 C5 107.80(19) . . ?
C2 C1 Tc1 73.16(13) . . ?
C5 C1 Tc1 71.76(12) . . ?
C2 C1 H1 125.9 . . ?
C5 C1 H1 125.9 . . ?
Tc1 C1 H1 125.9 . . ?
C3 C2 C1 108.1(2) . . ?
C3 C2 Tc1 73.00(11) . . ?
C1 C2 Tc1 70.86(11) . . ?
C3 C2 H2 125.8 . . ?
C1 C2 H2 125.8 . . ?
Tc1 C2 H2 125.8 . . ?
C2 C3 C4 108.1(2) . . ?
C2 C3 Tc1 71.72(12) . . ?
C4 C3 Tc1 71.17(12) . . ?
C2 C3 H3 125.9 . . ?
C4 C3 H3 125.9 . . ?
Tc1 C3 H3 125.9 . . ?
C5 C4 C3 108.4(2) . . ?
C5 C4 Tc1 71.25(13) . . ?
C3 C4 Tc1 73.19(13) . . ?
C5 C4 H4 125.7 . . ?
C3 C4 H4 125.7 . . ?
Tc1 C4 H4 125.7 . . ?
C4 C5 C1 107.6(2) . . ?
C4 C5 Tc1 72.92(13) . . ?
C1 C5 Tc1 71.86(12) . . ?
C4 C5 H5 126.0 . . ?
C1 C5 H5 126.0 . . ?
Tc1 C5 H5 126.0 . . ?
C21 P1 C11 103.63(10) . . ?
C21 P1 C31 103.84(10) . . ?
C11 P1 C31 100.31(10) . . ?
C21 P1 Tc1 110.93(8) . . ?
C11 P1 Tc1 115.72(7) . . ?
C31 P1 Tc1 120.42(7) . . ?
C16 C11 C12 119.02(19) . . ?
C16 C11 P1 121.06(16) . . ?
C12 C11 P1 119.89(15) . . ?
C13 C12 C11 120.63(19) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 119.7(2) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C15 C14 C13 120.1(2) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 120.05(19) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C11 120.38(19) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
C26 C21 C22 119.41(18) . . ?
C26 C21 P1 116.76(16) . . ?
C22 C21 P1 123.80(16) . . ?
C23 C22 C21 119.86(19) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C24 C23 C22 120.40(19) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C26 C21 120.46(19) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
C26 C25 C24 120.0(2) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C23 C24 C25 119.87(19) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C36 C31 C32 118.67(18) . . ?
C36 C31 P1 122.71(15) . . ?
C32 C31 P1 118.43(16) . . ?
C33 C32 C31 120.66(19) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 120.10(19) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C35 C34 C33 119.8(2) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C36 120.2(2) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C36 C31 120.59(19) . . ?
C35 C36 H36 119.7 . . ?
C31 C36 H36 119.7 . . ?
C46 C41 C42 114.90(18) . . ?
C46 C41 Tc1 121.73(16) . . ?
C42 C41 Tc1 122.98(15) . . ?
C43 C42 C41 122.4(2) . . ?
C43 C42 H42 118.8 . . ?
C41 C42 H42 118.8 . . ?
C45 C46 C41 122.9(2) . . ?
C45 C46 H46 118.6 . . ?
C41 C46 H46 118.6 . . ?
C44 C43 C42 120.9(2) . . ?
C44 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C45 C44 C43 118.22(19) . . ?
C45 C44 H44 120.9 . . ?
C43 C44 H44 120.9 . . ?
C44 C45 C46 120.6(2) . . ?
C44 C45 H45 119.7 . . ?
C46 C45 H45 119.7 . . ?

_refine_diff_density_max         0.274
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.048

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TcNOBr3OPPh3
_database_code_depnum_ccdc_archive 'CCDC 1491444'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-07-22 downloaded from the CCDC.
;


# start Validation Reply Form
_vrf_PLAT342_TcNOBr3OPPh3        
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............   0.02043 Ang.  
RESPONSE: It arises from the limited quality of the crystals. 
;
_vrf_PLAT910_TcNOBr3OPPh3        
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)
RESPONSE: It arises also from the limited quality of the crystals. 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;
Tribromidobistriphenylphosphine
oxid nitrosyl technetium(II)
;
_chemical_name_common            '[Tc(NO)Br3(OPPh3)2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 Br3  N O3 P2 Tc, C0.5 H1 Cl1'
_chemical_formula_sum            'C36.50 H31 Br3 Cl N O3 P2 Tc'
_chemical_formula_weight         966.74

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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'

_cell_length_a                   12.5510(10)
_cell_length_b                   14.3940(10)
_cell_length_c                   44.488(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.550(10)
_cell_angle_gamma                90
_cell_volume                     7967.5(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    18145
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      24.37

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_F_000             3808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    3.552
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            47263
_diffrn_reflns_av_unetI/netI     0.1783
_diffrn_reflns_av_R_equivalents  0.1777
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         3.152
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             13834
_reflns_number_gt                5626
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0671P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13834
_refine_ls_number_parameters     881
_refine_ls_number_restraints     99
_refine_ls_R_factor_all          0.1770
_refine_ls_R_factor_gt           0.0673
_refine_ls_wR_factor_ref         0.1782
_refine_ls_wR_factor_gt          0.1388
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_restrained_S_all      0.866
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Tc1 Tc 0.31149(8) 0.33930(6) 0.08141(2) 0.0585(3) Uani 1 1 d D . . . .
Br11 Br 0.25565(14) 0.45867(11) 0.04162(4) 0.1041(5) Uani 1 1 d . . . . .
Br12 Br 0.35573(12) 0.21145(9) 0.11918(3) 0.0816(4) Uani 1 1 d . . . . .
Br13 Br 0.50453(11) 0.37941(11) 0.08263(3) 0.0902(5) Uani 1 1 d . . . . .
P11 P 0.3772(3) 0.1793(3) 0.02747(8) 0.0756(10) Uani 1 1 d . . . . .
P12 P 0.0651(3) 0.2758(2) 0.08616(7) 0.0672(9) Uani 1 1 d . . . . .
O10 O 0.2912(7) 0.4653(6) 0.1295(2) 0.094(3) Uani 1 1 d D . . . .
O12 O 0.1593(7) 0.2920(6) 0.0730(2) 0.082(2) Uani 1 1 d . . . . .
O11 O 0.3285(7) 0.2466(6) 0.04663(16) 0.079(2) Uani 1 1 d . . . . .
N10 N 0.2957(7) 0.4195(7) 0.1107(2) 0.062(3) Uani 1 1 d D . . . .
C121 C 0.4875(12) 0.1151(9) 0.0482(3) 0.074(4) Uani 1 1 d . . . . .
C122 C 0.5908(13) 0.1265(11) 0.0428(3) 0.100(5) Uani 1 1 d . . . . .
H122 H 0.6047 0.1665 0.0273 0.120 Uiso 1 1 calc R U . . .
C123 C 0.6781(13) 0.0797(12) 0.0597(4) 0.108(5) Uani 1 1 d . . . . .
H123 H 0.7481 0.0868 0.0554 0.130 Uiso 1 1 calc R U . . .
C124 C 0.6558(16) 0.0249(13) 0.0823(4) 0.118(6) Uani 1 1 d . U . . .
H124 H 0.7118 -0.0046 0.0944 0.141 Uiso 1 1 calc R U . . .
C125 C 0.5530(15) 0.0110(11) 0.0881(4) 0.108(5) Uani 1 1 d . U . . .
H125 H 0.5403 -0.0305 0.1033 0.130 Uiso 1 1 calc R U . . .
C126 C 0.4667(13) 0.0573(10) 0.0720(3) 0.102(5) Uani 1 1 d . . . . .
H126 H 0.3973 0.0501 0.0768 0.122 Uiso 1 1 calc R U . . .
C111 C 0.4245(11) 0.2370(11) -0.0032(3) 0.084(4) Uani 1 1 d . . . . .
C116 C 0.4502(13) 0.3299(12) -0.0022(3) 0.102(5) Uani 1 1 d . . . . .
H116 H 0.4421 0.3631 0.0153 0.122 Uiso 1 1 calc R U . . .
C112 C 0.4374(14) 0.1860(14) -0.0292(3) 0.123(6) Uani 1 1 d . . . . .
H112 H 0.4208 0.1230 -0.0305 0.148 Uiso 1 1 calc R U . . .
C115 C 0.4884(15) 0.3776(13) -0.0265(4) 0.123(6) Uani 1 1 d . . . . .
H115 H 0.5046 0.4406 -0.0253 0.147 Uiso 1 1 calc R U . . .
C114 C 0.5002(15) 0.3280(16) -0.0513(4) 0.126(6) Uani 1 1 d . . . . .
H114 H 0.5250 0.3577 -0.0676 0.151 Uiso 1 1 calc R U . . .
C113 C 0.4763(17) 0.2326(18) -0.0534(4) 0.149(8) Uani 1 1 d . . . . .
H113 H 0.4863 0.2001 -0.0709 0.179 Uiso 1 1 calc R U . . .
C141 C 0.0513(10) 0.1539(8) 0.0926(2) 0.064(3) Uani 1 1 d . . . . .
C142 C 0.1163(10) 0.0919(8) 0.0794(3) 0.069(3) Uani 1 1 d . . . . .
H142 H 0.1692 0.1135 0.0684 0.083 Uiso 1 1 calc R U . . .
C143 C 0.1011(11) -0.0014(9) 0.0830(3) 0.080(4) Uani 1 1 d . . . . .
H143 H 0.1432 -0.0435 0.0739 0.096 Uiso 1 1 calc R U . . .
C146 C -0.0280(11) 0.1198(10) 0.1094(3) 0.082(4) Uani 1 1 d . . . . .
H146 H -0.0723 0.1617 0.1178 0.098 Uiso 1 1 calc R U . . .
C145 C -0.0415(12) 0.0272(10) 0.1138(3) 0.088(4) Uani 1 1 d . . . . .
H145 H -0.0923 0.0056 0.1256 0.106 Uiso 1 1 calc R U . . .
C144 C 0.0235(13) -0.0341(9) 0.1001(3) 0.088(4) Uani 1 1 d . . . . .
H144 H 0.0148 -0.0977 0.1024 0.106 Uiso 1 1 calc R U . . .
C151 C 0.0573(9) 0.3352(8) 0.1207(2) 0.060(3) Uani 1 1 d . . . . .
C156 C 0.1042(9) 0.2976(9) 0.1472(3) 0.067(3) Uani 1 1 d . . . . .
H156 H 0.1371 0.2398 0.1471 0.080 Uiso 1 1 calc R U . . .
C152 C 0.0122(10) 0.4219(8) 0.1209(3) 0.076(4) Uani 1 1 d . . . . .
H152 H -0.0199 0.4482 0.1028 0.091 Uiso 1 1 calc R U . . .
C153 C 0.0145(12) 0.4711(10) 0.1483(4) 0.091(4) Uani 1 1 d . . . . .
H153 H -0.0157 0.5301 0.1484 0.110 Uiso 1 1 calc R U . . .
C154 C 0.0611(12) 0.4324(14) 0.1746(4) 0.098(5) Uani 1 1 d . . . . .
H154 H 0.0642 0.4652 0.1927 0.117 Uiso 1 1 calc R U . . .
C155 C 0.1038(11) 0.3436(12) 0.1743(3) 0.086(4) Uani 1 1 d . . . . .
H155 H 0.1322 0.3151 0.1924 0.103 Uiso 1 1 calc R U . . .
C161 C -0.0452(11) 0.3118(8) 0.0589(3) 0.077(3) Uani 1 1 d . U . . .
C162 C -0.1524(11) 0.3053(9) 0.0649(3) 0.091(4) Uani 1 1 d . U . . .
H162 H -0.1676 0.2838 0.0836 0.109 Uiso 1 1 calc R U . . .
C163 C -0.2345(13) 0.3312(11) 0.0429(4) 0.112(5) Uani 1 1 d . U . . .
H163 H -0.3050 0.3268 0.0470 0.135 Uiso 1 1 calc R U . . .
C166 C -0.0266(14) 0.3410(15) 0.0313(3) 0.148(8) Uani 1 1 d . U . . .
H166 H 0.0436 0.3442 0.0268 0.177 Uiso 1 1 calc R U . . .
C164 C -0.2162(16) 0.3620(15) 0.0161(4) 0.155(8) Uani 1 1 d . U . . .
H164 H -0.2737 0.3804 0.0020 0.187 Uiso 1 1 calc R U . . .
C165 C -0.1138(16) 0.3673(19) 0.0088(5) 0.200(12) Uani 1 1 d . U . . .
H165 H -0.1012 0.3874 -0.0103 0.240 Uiso 1 1 calc R U . . .
Tc2 Tc 0.16663(7) 0.31638(6) 0.31050(2) 0.0538(3) Uani 1 1 d D . . . .
Br21 Br 0.26432(11) 0.34315(9) 0.36295(3) 0.0730(4) Uani 1 1 d D . . . .
Br22 Br 0.08565(9) 0.30165(9) 0.25594(3) 0.0668(3) Uani 1 1 d D . . . .
P21 P 0.1356(2) 0.54723(19) 0.28950(6) 0.0484(7) Uani 1 1 d . . . . .
P22 P 0.4253(2) 0.27640(18) 0.29617(6) 0.0493(7) Uani 1 1 d . . . . .
O22 O 0.3130(5) 0.3161(5) 0.29373(16) 0.0572(18) Uani 1 1 d . . . . .
O21 O 0.1816(5) 0.4588(4) 0.30420(14) 0.0475(17) Uani 1 1 d . . . . .
C211 C 0.1838(8) 0.5618(7) 0.2534(2) 0.051(3) Uani 1 1 d . . . . .
C212 C 0.2638(8) 0.5027(7) 0.2464(3) 0.054(3) Uani 1 1 d . . . . .
H212 H 0.2895 0.4556 0.2597 0.065 Uiso 1 1 calc R U . . .
C213 C 0.3049(9) 0.5148(7) 0.2195(3) 0.063(3) Uani 1 1 d . . . . .
H213 H 0.3599 0.4761 0.2149 0.075 Uiso 1 1 calc R U . . .
C214 C 0.2665(9) 0.5827(8) 0.1991(3) 0.061(3) Uani 1 1 d . . . . .
H214 H 0.2924 0.5876 0.1805 0.073 Uiso 1 1 calc R U . . .
C215 C 0.1469(9) 0.6337(7) 0.2333(2) 0.053(3) Uani 1 1 d . . . . .
H215 H 0.0942 0.6743 0.2382 0.064 Uiso 1 1 calc R U . . .
C216 C 0.1882(9) 0.6441(9) 0.2067(3) 0.070(3) Uani 1 1 d . . . . .
H216 H 0.1642 0.6922 0.1936 0.084 Uiso 1 1 calc R U . . .
C221 C 0.1819(7) 0.6424(7) 0.3138(2) 0.047(3) Uani 1 1 d . . . . .
C222 C 0.2583(8) 0.6252(8) 0.3392(2) 0.056(3) Uani 1 1 d . . . . .
H222 H 0.2831 0.5650 0.3433 0.067 Uiso 1 1 calc R U . . .
C223 C 0.1473(9) 0.7333(7) 0.3076(3) 0.059(3) Uani 1 1 d . . . . .
H223 H 0.0980 0.7464 0.2906 0.071 Uiso 1 1 calc R U . . .
C224 C 0.2965(10) 0.6969(10) 0.3580(3) 0.072(3) Uani 1 1 d . . . . .
H224 H 0.3470 0.6843 0.3747 0.087 Uiso 1 1 calc R U . . .
C225 C 0.1876(9) 0.8034(8) 0.3270(3) 0.065(3) Uani 1 1 d . . . . .
H225 H 0.1641 0.8640 0.3229 0.078 Uiso 1 1 calc R U . . .
C226 C 0.2621(9) 0.7869(9) 0.3526(3) 0.068(3) Uani 1 1 d . . . . .
H226 H 0.2876 0.8349 0.3656 0.082 Uiso 1 1 calc R U . . .
C227 C 0.4466(10) -0.0130(9) 0.3387(3) 0.079(4) Uani 1 1 d . . . . .
H227 H 0.4491 -0.0718 0.3474 0.095 Uiso 1 1 calc R U . . .
C231 C -0.0075(8) 0.5521(7) 0.2831(2) 0.050(3) Uani 1 1 d . . . . .
C232 C -0.1750(10) 0.5745(10) 0.3033(3) 0.080(4) Uani 1 1 d . . . . .
H232 H -0.2121 0.5951 0.3188 0.097 Uiso 1 1 calc R U . . .
C233 C -0.2297(10) 0.5383(10) 0.2778(3) 0.086(4) Uani 1 1 d . . . . .
H233 H -0.3040 0.5317 0.2762 0.103 Uiso 1 1 calc R U . . .
C234 C -0.0629(9) 0.5812(7) 0.3065(3) 0.060(3) Uani 1 1 d . . . . .
H234 H -0.0255 0.6051 0.3243 0.073 Uiso 1 1 calc R U . . .
C235 C -0.1771(11) 0.5119(11) 0.2549(3) 0.090(4) Uani 1 1 d . . . . .
H235 H -0.2155 0.4895 0.2371 0.108 Uiso 1 1 calc R U . . .
C236 C -0.0656(9) 0.5176(9) 0.2575(3) 0.068(3) Uani 1 1 d . . . . .
H236 H -0.0303 0.4977 0.2416 0.082 Uiso 1 1 calc R U . . .
C241 C 0.4590(9) 0.2672(6) 0.2584(2) 0.052(3) Uani 1 1 d . . . . .
C242 C 0.3790(9) 0.2685(7) 0.2350(2) 0.058(3) Uani 1 1 d . . . . .
H242 H 0.3083 0.2764 0.2386 0.069 Uiso 1 1 calc R U . . .
C243 C 0.4016(11) 0.2579(9) 0.2047(3) 0.077(4) Uani 1 1 d . . . . .
H243 H 0.3468 0.2568 0.1884 0.093 Uiso 1 1 calc R U . . .
C244 C 0.5073(13) 0.2493(8) 0.2004(3) 0.080(4) Uani 1 1 d . . . . .
H244 H 0.5249 0.2435 0.1808 0.096 Uiso 1 1 calc R U . . .
C245 C 0.5672(11) 0.2618(9) 0.2537(3) 0.081(4) Uani 1 1 d . . . . .
H245 H 0.6228 0.2665 0.2696 0.097 Uiso 1 1 calc R U . . .
C246 C 0.5870(12) 0.2493(9) 0.2244(4) 0.089(4) Uani 1 1 d . . . . .
H246 H 0.6576 0.2404 0.2207 0.107 Uiso 1 1 calc R U . . .
C251 C 0.5183(9) 0.3528(8) 0.3184(3) 0.064(3) Uani 1 1 d . . . . .
C252 C 0.4893(10) 0.4431(8) 0.3222(3) 0.067(3) Uani 1 1 d . . . . .
H252 H 0.4227 0.4640 0.3131 0.081 Uiso 1 1 calc R U . . .
C253 C 0.6185(10) 0.3230(9) 0.3315(3) 0.091(5) Uani 1 1 d . . . . .
H253 H 0.6394 0.2617 0.3292 0.110 Uiso 1 1 calc R U . . .
C254 C 0.6879(11) 0.3847(10) 0.3482(3) 0.096(5) Uani 1 1 d . . . . .
H254 H 0.7560 0.3653 0.3566 0.115 Uiso 1 1 calc R U . . .
C255 C 0.6554(10) 0.4750(9) 0.3522(3) 0.077(4) Uani 1 1 d . . . . .
H255 H 0.7007 0.5165 0.3637 0.093 Uiso 1 1 calc R U . . .
C256 C 0.5560(12) 0.5025(9) 0.3391(3) 0.080(4) Uani 1 1 d . . . . .
H256 H 0.5337 0.5632 0.3418 0.097 Uiso 1 1 calc R U . . .
C261 C 0.4394(8) 0.1627(7) 0.3130(2) 0.050(3) Uani 1 1 d . . . . .
C262 C 0.4490(10) 0.1521(8) 0.3440(3) 0.075(4) Uani 1 1 d . . . . .
H262 H 0.4516 0.2038 0.3567 0.090 Uiso 1 1 calc R U . . .
C263 C 0.4548(11) 0.0633(9) 0.3561(3) 0.085(4) Uani 1 1 d . . . . .
H263 H 0.4646 0.0563 0.3771 0.102 Uiso 1 1 calc R U . . .
C265 C 0.4343(9) -0.0027(7) 0.3071(3) 0.070(4) Uani 1 1 d . . . . .
H265 H 0.4282 -0.0551 0.2947 0.084 Uiso 1 1 calc R U . . .
C266 C 0.4312(9) 0.0851(8) 0.2940(3) 0.063(3) Uani 1 1 d . . . . .
H266 H 0.4238 0.0921 0.2731 0.076 Uiso 1 1 calc R U . . .
Cl98 Cl 0.1353(10) 0.6880(6) 0.1184(2) 0.150(4) Uani 0.5 1 d . . P . .
Cl99 Cl 0.2263(12) 0.7566(7) 0.0693(3) 0.176(5) Uani 0.5 1 d . . P . .
C99 C 0.217(4) 0.6806(19) 0.0913(8) 0.165(19) Uani 0.5 1 d . . P . .
H99A H 0.2885 0.6689 0.1016 0.199 Uiso 0.5 1 calc R U P . .
H99B H 0.1954 0.6253 0.0795 0.199 Uiso 0.5 1 calc R U P . .
C131 C 0.2809(11) 0.0943(11) 0.0118(3) 0.088(4) Uani 1 1 d . . . . .
C132 C 0.2951(16) -0.0022(13) 0.0164(4) 0.136(7) Uani 1 1 d . . . . .
H132 H 0.3567 -0.0239 0.0282 0.163 Uiso 1 1 calc R U . . .
C136 C 0.1899(14) 0.1294(17) -0.0037(4) 0.151(8) Uani 1 1 d . . . . .
H136 H 0.1794 0.1933 -0.0051 0.181 Uiso 1 1 calc R U . . .
C135 C 0.1092(16) 0.0660(19) -0.0179(5) 0.160(9) Uani 1 1 d . U . . .
H135 H 0.0468 0.0894 -0.0289 0.192 Uiso 1 1 calc R U . . .
C133 C 0.218(2) -0.0660(17) 0.0034(6) 0.181(9) Uani 1 1 d . U . . .
H133 H 0.2263 -0.1296 0.0065 0.217 Uiso 1 1 calc R U . . .
C134 C 0.123(3) -0.027(2) -0.0155(7) 0.203(12) Uani 1 1 d . U . . .
H134 H 0.0729 -0.0671 -0.0258 0.244 Uiso 1 1 calc R U . . .
Cl88 Cl 0.2349(10) 0.0623(10) 0.4088(4) 0.172(5) Uani 0.5 1 d . . P . .
Cl89 Cl 0.1125(16) 0.1380(18) 0.4455(5) 0.306(11) Uani 0.5 1 d . . P . .
C88 C 0.194(4) 0.158(5) 0.4181(13) 0.26(4) Uani 0.5 1 d . . P . .
H88A H 0.1541 0.1885 0.4007 0.315 Uiso 0.5 1 calc R U P . .
H88B H 0.2540 0.1972 0.4260 0.315 Uiso 0.5 1 calc R U P . .
Br24 Br 0.1447(3) 0.1561(3) 0.31769(11) 0.0745(6) Uani 0.373(3) 1 d D . P A 1
N20 N 0.1768(15) 0.1935(7) 0.3169(4) 0.0745(6) Uani 0.627(3) 1 d D U P A 2
O20 O 0.1649(14) 0.1212(7) 0.3158(4) 0.0745(6) Uani 0.627(3) 1 d D U P A 2
Br23 Br -0.00469(18) 0.32928(18) 0.32834(6) 0.0745(6) Uani 0.627(3) 1 d . . P A
.
O23 O -0.0366(11) 0.3609(14) 0.3288(3) 0.0745(6) Uani 0.373(3) 1 d D . P A 2
N23 N 0.0394(16) 0.334(3) 0.3251(8) 0.0745(6) Uani 0.373(3) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Tc1 N10 1.770(9) . ?
Tc1 O12 2.016(8) . ?
Tc1 O11 2.076(7) . ?
Tc1 Br13 2.4843(17) . ?
Tc1 Br11 2.5003(16) . ?
Tc1 Br12 2.5045(15) . ?
P11 O11 1.475(8) . ?
P11 C111 1.766(15) . ?
P11 C131 1.795(14) . ?
P11 C121 1.813(13) . ?
P12 O12 1.407(9) . ?
P12 C151 1.774(11) . ?
P12 C161 1.792(12) . ?
P12 C141 1.790(12) . ?
O10 N10 1.074(9) . ?
C121 C122 1.360(18) . ?
C121 C126 1.396(18) . ?
C122 C123 1.417(18) . ?
C122 H122 0.9300 . ?
C123 C124 1.33(2) . ?
C123 H123 0.9300 . ?
C124 C125 1.36(2) . ?
C124 H124 0.9300 . ?
C125 C126 1.388(19) . ?
C125 H125 0.9300 . ?
C126 H126 0.9300 . ?
C111 C116 1.375(19) . ?
C111 C112 1.398(19) . ?
C116 C115 1.42(2) . ?
C116 H116 0.9300 . ?
C112 C113 1.41(2) . ?
C112 H112 0.9300 . ?
C115 C114 1.34(2) . ?
C115 H115 0.9300 . ?
C114 C113 1.41(2) . ?
C114 H114 0.9300 . ?
C113 H113 0.9300 . ?
C141 C142 1.389(15) . ?
C141 C146 1.409(17) . ?
C142 C143 1.369(16) . ?
C142 H142 0.9300 . ?
C143 C144 1.395(18) . ?
C143 H143 0.9300 . ?
C146 C145 1.360(17) . ?
C146 H146 0.9300 . ?
C145 C144 1.396(19) . ?
C145 H145 0.9300 . ?
C144 H144 0.9300 . ?
C151 C156 1.359(15) . ?
C151 C152 1.370(15) . ?
C156 C155 1.375(17) . ?
C156 H156 0.9300 . ?
C152 C153 1.408(17) . ?
C152 H152 0.9300 . ?
C153 C154 1.36(2) . ?
C153 H153 0.9300 . ?
C154 C155 1.39(2) . ?
C154 H154 0.9300 . ?
C155 H155 0.9300 . ?
C161 C166 1.346(17) . ?
C161 C162 1.409(17) . ?
C162 C163 1.376(17) . ?
C162 H162 0.9300 . ?
C163 C164 1.32(2) . ?
C163 H163 0.9300 . ?
C166 C165 1.43(2) . ?
C166 H166 0.9300 . ?
C164 C165 1.37(2) . ?
C164 H164 0.9300 . ?
C165 H165 0.9300 . ?
Tc2 N20 1.793(10) . ?
Tc2 N23 1.818(12) . ?
Tc2 O22 2.071(7) . ?
Tc2 O21 2.080(6) . ?
Tc2 Br24 2.351(4) . ?
Tc2 Br23 2.395(2) . ?
Tc2 Br22 2.5144(15) . ?
Tc2 Br21 2.5191(15) . ?
P21 O21 1.511(6) . ?
P21 C231 1.783(10) . ?
P21 C221 1.793(9) . ?
P21 C211 1.800(11) . ?
P22 O22 1.512(7) . ?
P22 C241 1.788(11) . ?
P22 C261 1.800(10) . ?
P22 C251 1.800(11) . ?
C211 C212 1.383(14) . ?
C211 C215 1.406(14) . ?
C212 C213 1.377(15) . ?
C212 H212 0.9300 . ?
C213 C214 1.376(15) . ?
C213 H213 0.9300 . ?
C214 C216 1.397(15) . ?
C214 H214 0.9300 . ?
C215 C216 1.361(14) . ?
C215 H215 0.9300 . ?
C216 H216 0.9300 . ?
C221 C223 1.394(13) . ?
C221 C222 1.407(13) . ?
C222 C224 1.374(15) . ?
C222 H222 0.9300 . ?
C223 C225 1.381(14) . ?
C223 H223 0.9300 . ?
C224 C226 1.376(16) . ?
C224 H224 0.9300 . ?
C225 C226 1.397(16) . ?
C225 H225 0.9300 . ?
C226 H226 0.9300 . ?
C227 C263 1.341(17) . ?
C227 C265 1.402(16) . ?
C227 H227 0.9300 . ?
C231 C236 1.364(14) . ?
C231 C234 1.389(14) . ?
C232 C233 1.350(17) . ?
C232 C234 1.399(15) . ?
C232 H232 0.9300 . ?
C233 C235 1.339(17) . ?
C233 H233 0.9300 . ?
C234 H234 0.9300 . ?
C235 C236 1.391(16) . ?
C235 H235 0.9300 . ?
C236 H236 0.9300 . ?
C241 C242 1.351(14) . ?
C241 C245 1.405(16) . ?
C242 C243 1.420(15) . ?
C242 H242 0.9300 . ?
C243 C244 1.371(17) . ?
C243 H243 0.9300 . ?
C244 C246 1.364(18) . ?
C244 H244 0.9300 . ?
C245 C246 1.371(17) . ?
C245 H245 0.9300 . ?
C246 H246 0.9300 . ?
C251 C252 1.367(14) . ?
C251 C253 1.384(15) . ?
C252 C256 1.353(15) . ?
C252 H252 0.9300 . ?
C253 C254 1.388(16) . ?
C253 H253 0.9300 . ?
C254 C255 1.380(17) . ?
C254 H254 0.9300 . ?
C255 C256 1.365(16) . ?
C255 H255 0.9300 . ?
C256 H256 0.9300 . ?
C261 C262 1.378(15) . ?
C261 C266 1.395(14) . ?
C262 C263 1.385(16) . ?
C262 H262 0.9300 . ?
C263 H263 0.9300 . ?
C265 C266 1.390(15) . ?
C265 H265 0.9300 . ?
C266 H266 0.9300 . ?
Cl98 C99 1.68(3) . ?
Cl99 C99 1.48(3) . ?
C99 H99A 0.9700 . ?
C99 H99B 0.9700 . ?
C131 C136 1.35(2) . ?
C131 C132 1.41(2) . ?
C132 C133 1.40(2) . ?
C132 H132 0.9300 . ?
C136 C135 1.45(2) . ?
C136 H136 0.9300 . ?
C135 C134 1.36(3) . ?
C135 H135 0.9300 . ?
C133 C134 1.47(3) . ?
C133 H133 0.9300 . ?
C134 H134 0.9300 . ?
Cl88 C88 1.54(8) . ?
Cl89 C88 1.72(6) . ?
C88 H88A 0.9700 . ?
C88 H88B 0.9700 . ?
N20 O20 1.052(11) . ?
Br23 N23 0.593(16) . ?
Br23 O23 0.608(16) . ?
O23 N23 1.063(13) . ?

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
N10 Tc1 O12 99.3(4) . . ?
N10 Tc1 O11 179.1(4) . . ?
O12 Tc1 O11 80.3(3) . . ?
N10 Tc1 Br13 92.1(3) . . ?
O12 Tc1 Br13 168.5(3) . . ?
O11 Tc1 Br13 88.3(2) . . ?
N10 Tc1 Br11 91.4(3) . . ?
O12 Tc1 Br11 85.9(2) . . ?
O11 Tc1 Br11 87.8(2) . . ?
Br13 Tc1 Br11 92.15(7) . . ?
N10 Tc1 Br12 91.3(3) . . ?
O12 Tc1 Br12 89.9(2) . . ?
O11 Tc1 Br12 89.5(2) . . ?
Br13 Tc1 Br12 91.52(6) . . ?
Br11 Tc1 Br12 175.37(7) . . ?
O11 P11 C111 110.1(6) . . ?
O11 P11 C131 111.3(6) . . ?
C111 P11 C131 107.3(7) . . ?
O11 P11 C121 112.7(5) . . ?
C111 P11 C121 108.8(7) . . ?
C131 P11 C121 106.4(7) . . ?
O12 P12 C151 115.3(6) . . ?
O12 P12 C161 106.6(6) . . ?
C151 P12 C161 108.8(6) . . ?
O12 P12 C141 109.5(6) . . ?
C151 P12 C141 108.4(5) . . ?
C161 P12 C141 108.0(6) . . ?
P12 O12 Tc1 143.7(6) . . ?
P11 O11 Tc1 160.8(5) . . ?
O10 N10 Tc1 175.4(10) . . ?
C122 C121 C126 119.0(13) . . ?
C122 C121 P11 122.0(11) . . ?
C126 C121 P11 118.9(12) . . ?
C121 C122 C123 122.4(15) . . ?
C121 C122 H122 118.8 . . ?
C123 C122 H122 118.8 . . ?
C124 C123 C122 117.2(17) . . ?
C124 C123 H123 121.4 . . ?
C122 C123 H123 121.4 . . ?
C123 C124 C125 121.8(18) . . ?
C123 C124 H124 119.1 . . ?
C125 C124 H124 119.1 . . ?
C124 C125 C126 121.7(17) . . ?
C124 C125 H125 119.2 . . ?
C126 C125 H125 119.2 . . ?
C125 C126 C121 117.8(16) . . ?
C125 C126 H126 121.1 . . ?
C121 C126 H126 121.1 . . ?
C116 C111 C112 119.2(15) . . ?
C116 C111 P11 122.2(11) . . ?
C112 C111 P11 118.7(13) . . ?
C111 C116 C115 123.1(15) . . ?
C111 C116 H116 118.4 . . ?
C115 C116 H116 118.4 . . ?
C111 C112 C113 118.2(18) . . ?
C111 C112 H112 120.9 . . ?
C113 C112 H112 120.9 . . ?
C114 C115 C116 117.2(17) . . ?
C114 C115 H115 121.4 . . ?
C116 C115 H115 121.4 . . ?
C115 C114 C113 122.1(18) . . ?
C115 C114 H114 118.9 . . ?
C113 C114 H114 118.9 . . ?
C114 C113 C112 120.2(18) . . ?
C114 C113 H113 119.9 . . ?
C112 C113 H113 119.9 . . ?
C142 C141 C146 119.7(11) . . ?
C142 C141 P12 119.1(10) . . ?
C146 C141 P12 121.1(10) . . ?
C143 C142 C141 118.9(13) . . ?
C143 C142 H142 120.6 . . ?
C141 C142 H142 120.6 . . ?
C142 C143 C144 120.8(13) . . ?
C142 C143 H143 119.6 . . ?
C144 C143 H143 119.6 . . ?
C145 C146 C141 121.8(14) . . ?
C145 C146 H146 119.1 . . ?
C141 C146 H146 119.1 . . ?
C146 C145 C144 117.7(14) . . ?
C146 C145 H145 121.1 . . ?
C144 C145 H145 121.1 . . ?
C145 C144 C143 121.1(13) . . ?
C145 C144 H144 119.5 . . ?
C143 C144 H144 119.5 . . ?
C156 C151 C152 119.4(11) . . ?
C156 C151 P12 119.6(9) . . ?
C152 C151 P12 120.8(9) . . ?
C151 C156 C155 121.2(13) . . ?
C151 C156 H156 119.4 . . ?
C155 C156 H156 119.4 . . ?
C151 C152 C153 120.0(13) . . ?
C151 C152 H152 120.0 . . ?
C153 C152 H152 120.0 . . ?
C154 C153 C152 119.9(14) . . ?
C154 C153 H153 120.0 . . ?
C152 C153 H153 120.0 . . ?
C153 C154 C155 119.5(14) . . ?
C153 C154 H154 120.2 . . ?
C155 C154 H154 120.2 . . ?
C156 C155 C154 119.8(14) . . ?
C156 C155 H155 120.1 . . ?
C154 C155 H155 120.1 . . ?
C166 C161 C162 118.6(13) . . ?
C166 C161 P12 119.7(12) . . ?
C162 C161 P12 121.6(9) . . ?
C163 C162 C161 119.4(13) . . ?
C163 C162 H162 120.3 . . ?
C161 C162 H162 120.3 . . ?
C164 C163 C162 122.1(17) . . ?
C164 C163 H163 118.9 . . ?
C162 C163 H163 118.9 . . ?
C161 C166 C165 120.7(16) . . ?
C161 C166 H166 119.6 . . ?
C165 C166 H166 119.6 . . ?
C163 C164 C165 120.9(18) . . ?
C163 C164 H164 119.5 . . ?
C165 C164 H164 119.5 . . ?
C164 C165 C166 118.2(18) . . ?
C164 C165 H165 120.9 . . ?
C166 C165 H165 120.9 . . ?
N20 Tc2 N23 97.2(13) . . ?
N20 Tc2 O22 90.4(6) . . ?
N23 Tc2 O22 172.2(12) . . ?
N20 Tc2 O21 170.8(6) . . ?
N23 Tc2 O21 90.7(12) . . ?
O22 Tc2 O21 81.6(3) . . ?
O22 Tc2 Br24 99.9(2) . . ?
O21 Tc2 Br24 178.4(2) . . ?
N20 Tc2 Br23 94.1(6) . . ?
N23 Tc2 Br23 3.8(12) . . ?
O22 Tc2 Br23 175.4(2) . . ?
O21 Tc2 Br23 93.95(19) . . ?
Br24 Tc2 Br23 84.53(12) . . ?
N20 Tc2 Br22 94.7(6) . . ?
N23 Tc2 Br22 95.4(11) . . ?
O22 Tc2 Br22 85.25(19) . . ?
O21 Tc2 Br22 89.15(18) . . ?
Br24 Tc2 Br22 90.51(12) . . ?
Br23 Tc2 Br22 93.43(8) . . ?
N20 Tc2 Br21 89.3(6) . . ?
N23 Tc2 Br21 89.5(11) . . ?
O22 Tc2 Br21 89.27(19) . . ?
O21 Tc2 Br21 86.13(18) . . ?
Br24 Tc2 Br21 94.33(12) . . ?
Br23 Tc2 Br21 91.73(8) . . ?
Br22 Tc2 Br21 173.24(6) . . ?
O21 P21 C231 114.9(4) . . ?
O21 P21 C221 107.9(4) . . ?
C231 P21 C221 107.8(5) . . ?
O21 P21 C211 109.3(5) . . ?
C231 P21 C211 107.7(5) . . ?
C221 P21 C211 109.1(5) . . ?
O22 P22 C241 107.1(5) . . ?
O22 P22 C261 114.4(4) . . ?
C241 P22 C261 107.6(5) . . ?
O22 P22 C251 109.9(5) . . ?
C241 P22 C251 110.1(5) . . ?
C261 P22 C251 107.8(5) . . ?
P22 O22 Tc2 146.9(5) . . ?
P21 O21 Tc2 148.5(4) . . ?
C212 C211 C215 119.8(10) . . ?
C212 C211 P21 118.0(8) . . ?
C215 C211 P21 122.2(8) . . ?
C213 C212 C211 119.0(10) . . ?
C213 C212 H212 120.5 . . ?
C211 C212 H212 120.5 . . ?
C212 C213 C214 121.6(11) . . ?
C212 C213 H213 119.2 . . ?
C214 C213 H213 119.2 . . ?
C213 C214 C216 119.1(11) . . ?
C213 C214 H214 120.4 . . ?
C216 C214 H214 120.4 . . ?
C216 C215 C211 120.2(11) . . ?
C216 C215 H215 119.9 . . ?
C211 C215 H215 119.9 . . ?
C215 C216 C214 120.1(11) . . ?
C215 C216 H216 119.9 . . ?
C214 C216 H216 119.9 . . ?
C223 C221 C222 119.1(9) . . ?
C223 C221 P21 122.0(8) . . ?
C222 C221 P21 118.9(8) . . ?
C224 C222 C221 120.2(11) . . ?
C224 C222 H222 119.9 . . ?
C221 C222 H222 119.9 . . ?
C225 C223 C221 118.9(11) . . ?
C225 C223 H223 120.5 . . ?
C221 C223 H223 120.5 . . ?
C226 C224 C222 121.7(12) . . ?
C226 C224 H224 119.2 . . ?
C222 C224 H224 119.2 . . ?
C223 C225 C226 122.5(11) . . ?
C223 C225 H225 118.8 . . ?
C226 C225 H225 118.8 . . ?
C224 C226 C225 117.6(11) . . ?
C224 C226 H226 121.2 . . ?
C225 C226 H226 121.2 . . ?
C263 C227 C265 118.9(12) . . ?
C263 C227 H227 120.5 . . ?
C265 C227 H227 120.5 . . ?
C236 C231 C234 118.1(10) . . ?
C236 C231 P21 122.4(8) . . ?
C234 C231 P21 119.1(8) . . ?
C233 C232 C234 120.4(12) . . ?
C233 C232 H232 119.8 . . ?
C234 C232 H232 119.8 . . ?
C235 C233 C232 120.0(12) . . ?
C235 C233 H233 120.0 . . ?
C232 C233 H233 120.0 . . ?
C231 C234 C232 119.8(11) . . ?
C231 C234 H234 120.1 . . ?
C232 C234 H234 120.1 . . ?
C233 C235 C236 120.8(12) . . ?
C233 C235 H235 119.6 . . ?
C236 C235 H235 119.6 . . ?
C231 C236 C235 120.8(11) . . ?
C231 C236 H236 119.6 . . ?
C235 C236 H236 119.6 . . ?
C242 C241 C245 121.3(11) . . ?
C242 C241 P22 118.8(9) . . ?
C245 C241 P22 119.9(9) . . ?
C241 C242 C243 120.7(11) . . ?
C241 C242 H242 119.6 . . ?
C243 C242 H242 119.6 . . ?
C244 C243 C242 117.4(12) . . ?
C244 C243 H243 121.3 . . ?
C242 C243 H243 121.3 . . ?
C246 C244 C243 120.9(13) . . ?
C246 C244 H244 119.5 . . ?
C243 C244 H244 119.5 . . ?
C246 C245 C241 116.8(13) . . ?
C246 C245 H245 121.6 . . ?
C241 C245 H245 121.6 . . ?
C244 C246 C245 122.6(13) . . ?
C244 C246 H246 118.7 . . ?
C245 C246 H246 118.7 . . ?
C252 C251 C253 118.9(11) . . ?
C252 C251 P22 119.1(9) . . ?
C253 C251 P22 122.0(9) . . ?
C256 C252 C251 121.0(11) . . ?
C256 C252 H252 119.5 . . ?
C251 C252 H252 119.5 . . ?
C251 C253 C254 119.9(12) . . ?
C251 C253 H253 120.0 . . ?
C254 C253 H253 120.0 . . ?
C255 C254 C253 119.8(12) . . ?
C255 C254 H254 120.1 . . ?
C253 C254 H254 120.1 . . ?
C256 C255 C254 119.1(12) . . ?
C256 C255 H255 120.4 . . ?
C254 C255 H255 120.4 . . ?
C252 C256 C255 121.2(12) . . ?
C252 C256 H256 119.4 . . ?
C255 C256 H256 119.4 . . ?
C262 C261 C266 120.5(10) . . ?
C262 C261 P22 120.6(8) . . ?
C266 C261 P22 118.7(8) . . ?
C261 C262 C263 118.9(11) . . ?
C261 C262 H262 120.5 . . ?
C263 C262 H262 120.5 . . ?
C227 C263 C262 122.4(13) . . ?
C227 C263 H263 118.8 . . ?
C262 C263 H263 118.8 . . ?
C266 C265 C227 120.5(11) . . ?
C266 C265 H265 119.7 . . ?
C227 C265 H265 119.7 . . ?
C265 C266 C261 118.7(11) . . ?
C265 C266 H266 120.7 . . ?
C261 C266 H266 120.7 . . ?
Cl99 C99 Cl98 122(2) . . ?
Cl99 C99 H99A 106.7 . . ?
Cl98 C99 H99A 106.7 . . ?
Cl99 C99 H99B 106.7 . . ?
Cl98 C99 H99B 106.7 . . ?
H99A C99 H99B 106.6 . . ?
C136 C131 C132 121.6(16) . . ?
C136 C131 P11 115.1(15) . . ?
C132 C131 P11 123.2(13) . . ?
C133 C132 C131 121(2) . . ?
C133 C132 H132 119.4 . . ?
C131 C132 H132 119.4 . . ?
C131 C136 C135 119(2) . . ?
C131 C136 H136 120.6 . . ?
C135 C136 H136 120.6 . . ?
C134 C135 C136 121(3) . . ?
C134 C135 H135 119.6 . . ?
C136 C135 H135 119.6 . . ?
C132 C133 C134 117(3) . . ?
C132 C133 H133 121.6 . . ?
C134 C133 H133 121.6 . . ?
C135 C134 C133 120(3) . . ?
C135 C134 H134 119.8 . . ?
C133 C134 H134 119.8 . . ?
Cl88 C88 Cl89 107(3) . . ?
Cl88 C88 H88A 110.3 . . ?
Cl89 C88 H88A 110.3 . . ?
Cl88 C88 H88B 110.3 . . ?
Cl89 C88 H88B 110.3 . . ?
H88A C88 H88B 108.6 . . ?
O20 N20 Tc2 164.2(18) . . ?
N23 Br23 O23 124(4) . . ?
N23 Br23 Tc2 12(4) . . ?
O23 Br23 Tc2 133.8(19) . . ?
Br23 O23 N23 27(2) . . ?
Br23 N23 O23 28(2) . . ?
Br23 N23 Tc2 164(5) . . ?
O23 N23 Tc2 162(3) . . ?

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
C116 H116 Br11 0.93 3.07 3.800(16) 136.1 .
C116 H116 Br13 0.93 3.00 3.811(14) 146.3 .
C166 H166 Br11 0.93 3.13 3.899(17) 141.8 .
C212 H212 O22 0.93 2.51 3.420(13) 166.3 .
C215 H215 Br22 0.93 2.95 3.868(11) 171.5 2
C223 H223 Br22 0.93 3.00 3.916(12) 169.8 2
C242 H242 Br22 0.93 3.02 3.944(12) 175.4 .
C262 H262 Br21 0.93 3.13 3.762(12) 126.8 .
C99 H99B Br11 0.97 3.08 3.95(3) 149.6 .

_refine_diff_density_max         0.668
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.111

