#------------------------------------------------------------------------------
#$Date: 2021-10-29 02:47:56 +0300 (Fri, 29 Oct 2021) $
#$Revision: 270125 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708634.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7708634
loop_
_publ_author_name
'Kama, Dumisani Vincent'
'Frei, Angelo'
'Brink, Alice'
'Braband, Henrik'
'Alberto, Roger'
'Roodt, Andreas'
_publ_section_title
;
 New approach for the synthesis of water soluble fac-[MI(CO)3]+
 bis(diarylphosphino)alkylamine complexes (M=99Tc, Re)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03234H
_journal_year                    2021
_chemical_formula_moiety         'C37 H39 Cl N O3 P2 Tc'
_chemical_formula_sum            'C37 H39 Cl N O3 P2 Tc'
_chemical_formula_weight         741.08
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-10-12
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-12 deposited with the CCDC.	2021-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                92.434(3)
_cell_angle_beta                 111.683(3)
_cell_angle_gamma                104.288(3)
_cell_formula_units_Z            1
_cell_length_a                   9.6184(3)
_cell_length_b                   9.8959(4)
_cell_length_c                   10.6919(4)
_cell_measurement_reflns_used    6867
_cell_measurement_temperature    182.9(6)
_cell_measurement_theta_max      29.0160
_cell_measurement_theta_min      3.0180
_cell_volume                     906.27(6)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      182.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega 10.00 64.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 57.0000 -90.0000 54 #__ type_ start__ end____ width___ exp.time_ 2 omega 13.00 89.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 57.0000 -30.0000 76 #__ type_ start__ end____ width___ exp.time_ 3 omega 1.00 63.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 57.0000 -150.0000 62 #__ type_ start__ end____ width___ exp.time_ 4 omega -25.00 23.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 -48.0000 -19.0000 48 #__ type_ start__ end____ width___ exp.time_ 5 omega -12.00 89.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 60.0000 104.2145 101 #__ type_ start__ end____ width___ exp.time_ 6 omega 53.00 79.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 38.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 7 omega -38.00 48.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -58.0000 52.5966 86 #__ type_ start__ end____ width___ exp.time_ 8 omega -39.00 48.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -59.0000 -138.5858 87 #__ type_ start__ end____ width___ exp.time_ 9 omega -54.00 45.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -57.0000 -34.2645 99 #__ type_ start__ end____ width___ exp.time_ 10 omega -28.00 9.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -60.0000 143.0809 37'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0253209000
_diffrn_orient_matrix_UB_12      -0.0631475000
_diffrn_orient_matrix_UB_13      0.0243561000
_diffrn_orient_matrix_UB_21      -0.0343061000
_diffrn_orient_matrix_UB_22      0.0352275000
_diffrn_orient_matrix_UB_23      0.0346041000
_diffrn_orient_matrix_UB_31      -0.0709241000
_diffrn_orient_matrix_UB_32      -0.0191637000
_diffrn_orient_matrix_UB_33      -0.0585064000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15248
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         3.021
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       cube
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.099
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.38(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8390
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0522P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                7693
_reflns_number_total             8390
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03234h2.cif
_cod_data_source_block           tdk150615
_cod_database_code               7708634
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.879
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.62(4)
 0.38(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C3)
Uanis(C1) = Uanis(C4)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43), C45(H45),
  C46(H46)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C47(H47A,H47B,
 H47C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
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
C1 C -0.0312(9) 0.9105(9) 0.7836(7) 0.0557(14) Uani 1 1 d . . . . .
H1 H -0.081828 0.826898 0.813307 0.067 Uiso 1 1 calc R . . . .
C2 C -0.1537(9) 0.9889(9) 0.7302(8) 0.0560(19) Uani 1 1 d . . . . .
H2A H -0.245181 0.928150 0.656690 0.067 Uiso 1 1 calc R . . . .
H2B H -0.112804 1.071165 0.694589 0.067 Uiso 1 1 calc R . . . .
C3 C -0.1991(9) 1.0348(10) 0.8451(7) 0.0646(17) Uani 1 1 d . . . . .
H3A H -0.273363 1.088852 0.811725 0.077 Uiso 1 1 calc R . . . .
H3B H -0.248331 0.952118 0.875215 0.077 Uiso 1 1 calc R . . . .
C4 C -0.0552(9) 1.1239(8) 0.9640(7) 0.0557(14) Uani 1 1 d . . . . .
H4A H -0.009689 1.208878 0.934560 0.067 Uiso 1 1 calc R . . . .
H4B H -0.085604 1.151745 1.035952 0.067 Uiso 1 1 calc R . . . .
C5 C 0.0605(10) 1.0480(10) 1.0169(7) 0.068(2) Uani 1 1 d . . . . .
H5A H 0.019143 0.970138 1.057213 0.081 Uiso 1 1 calc R . . . .
H5B H 0.152515 1.110652 1.088417 0.081 Uiso 1 1 calc R . . . .
C6 C 0.1080(10) 0.9906(10) 0.9095(8) 0.0646(17) Uani 1 1 d . . . . .
H6A H 0.170937 1.068307 0.884091 0.077 Uiso 1 1 calc R . . . .
H6B H 0.171552 0.928480 0.947745 0.077 Uiso 1 1 calc R . . . .
C7 C 0.2002(8) 0.8202(7) 0.3339(7) 0.0391(14) Uani 1 1 d . . . . .
C8 C 0.1392(7) 0.5491(7) 0.4193(7) 0.0393(14) Uani 1 1 d . . . . .
C9 C -0.0822(8) 0.6833(7) 0.3383(6) 0.0372(14) Uani 1 1 d . . . . .
C11 C 0.2217(6) 1.1078(6) 0.6595(6) 0.0317(12) Uani 1 1 d . . . . .
C12 C 0.3775(6) 1.1097(7) 0.7216(6) 0.0372(13) Uani 1 1 d . . . . .
H12 H 0.406227 1.027593 0.714151 0.045 Uiso 1 1 calc R . . . .
C13 C 0.4896(7) 1.2328(7) 0.7941(6) 0.0417(14) Uani 1 1 d . . . . .
H13 H 0.592874 1.231394 0.834713 0.050 Uiso 1 1 calc R . . . .
C14 C 0.4545(7) 1.3577(7) 0.8088(6) 0.0403(14) Uani 1 1 d . . . . .
C15 C 0.3013(8) 1.3559(7) 0.7498(7) 0.0494(17) Uani 1 1 d . . . . .
H15 H 0.273776 1.438591 0.757969 0.059 Uiso 1 1 calc R . . . .
C16 C 0.1857(7) 1.2324(6) 0.6778(6) 0.0417(14) Uani 1 1 d . . . . .
H16 H 0.082021 1.233629 0.641155 0.050 Uiso 1 1 calc R . . . .
C17 C 0.5825(8) 1.4915(7) 0.8878(8) 0.058(2) Uani 1 1 d . . . . .
H17A H 0.570309 1.567623 0.835683 0.087 Uiso 1 1 calc GR . . . .
H17B H 0.682511 1.476979 0.904475 0.087 Uiso 1 1 calc GR . . . .
H17C H 0.575419 1.514494 0.972943 0.087 Uiso 1 1 calc GR . . . .
C21 C -0.0784(6) 0.9988(6) 0.4429(5) 0.0284(11) Uani 1 1 d . . . . .
C22 C -0.0480(7) 1.1088(7) 0.3712(6) 0.0394(14) Uani 1 1 d . . . . .
H22 H 0.054789 1.158990 0.390659 0.047 Uiso 1 1 calc R . . . .
C23 C -0.1677(8) 1.1451(7) 0.2714(6) 0.0442(15) Uani 1 1 d . . . . .
H23 H -0.144047 1.220520 0.226571 0.053 Uiso 1 1 calc R . . . .
C24 C -0.3229(7) 1.0702(7) 0.2374(6) 0.0405(14) Uani 1 1 d . . . . .
C25 C -0.3531(7) 0.9592(7) 0.3049(6) 0.0435(15) Uani 1 1 d . . . . .
H25 H -0.456168 0.907575 0.282497 0.052 Uiso 1 1 calc R . . . .
C26 C -0.2338(7) 0.9206(7) 0.4069(6) 0.0365(13) Uani 1 1 d . . . . .
H26 H -0.257936 0.843930 0.450071 0.044 Uiso 1 1 calc R . . . .
C27 C -0.4517(9) 1.1101(10) 0.1295(8) 0.069(2) Uani 1 1 d . . . . .
H27A H -0.549935 1.044446 0.115503 0.103 Uiso 1 1 calc GR . . . .
H27B H -0.435618 1.108189 0.046110 0.103 Uiso 1 1 calc GR . . . .
H27C H -0.452103 1.203352 0.157856 0.103 Uiso 1 1 calc GR . . . .
C31 C -0.1543(6) 0.5599(6) 0.5958(5) 0.0299(11) Uani 1 1 d . . . . .
C32 C -0.2925(7) 0.5854(7) 0.5863(6) 0.0360(13) Uani 1 1 d . . . . .
H32 H -0.292607 0.675769 0.613929 0.043 Uiso 1 1 calc R . . . .
C33 C -0.4304(7) 0.4781(7) 0.5361(7) 0.0433(15) Uani 1 1 d . . . . .
H33 H -0.522190 0.496677 0.531415 0.052 Uiso 1 1 calc R . . . .
C34 C -0.4337(7) 0.3432(8) 0.4927(6) 0.0431(16) Uani 1 1 d . . . . .
C35 C -0.2939(8) 0.3164(7) 0.5049(7) 0.0512(18) Uani 1 1 d . . . . .
H35 H -0.293414 0.225467 0.479634 0.061 Uiso 1 1 calc R . . . .
C36 C -0.1550(8) 0.4249(7) 0.5545(7) 0.0448(15) Uani 1 1 d . . . . .
H36 H -0.062640 0.406838 0.560024 0.054 Uiso 1 1 calc R . . . .
C37 C -0.5864(9) 0.2262(9) 0.4301(8) 0.068(2) Uani 1 1 d . . . . .
H37A H -0.641171 0.237130 0.337517 0.102 Uiso 1 1 calc GR . . . .
H37B H -0.649385 0.231107 0.480980 0.102 Uiso 1 1 calc GR . . . .
H37C H -0.564853 0.136385 0.432329 0.102 Uiso 1 1 calc GR . . . .
C41 C 0.1388(6) 0.6549(6) 0.8214(6) 0.0333(12) Uani 1 1 d . . . . .
C42 C 0.0667(7) 0.5649(7) 0.8894(6) 0.0426(14) Uani 1 1 d . . . . .
H42 H -0.040325 0.522999 0.848055 0.051 Uiso 1 1 calc R . . . .
C43 C 0.1500(8) 0.5348(8) 1.0184(7) 0.0521(19) Uani 1 1 d . . . . .
H43 H 0.100264 0.472872 1.061941 0.063 Uiso 1 1 calc R . . . .
C44 C 0.3124(8) 0.6020(7) 1.0802(7) 0.0458(16) Uani 1 1 d . . . . .
C45 C 0.3813(7) 0.6907(7) 1.0136(6) 0.0424(15) Uani 1 1 d . . . . .
H45 H 0.488153 0.733629 1.054942 0.051 Uiso 1 1 calc R . . . .
C46 C 0.2985(7) 0.7199(7) 0.8862(6) 0.0368(13) Uani 1 1 d . . . . .
H46 H 0.349389 0.782602 0.843997 0.044 Uiso 1 1 calc R . . . .
C47 C 0.4029(10) 0.5677(10) 1.2171(8) 0.065(2) Uani 1 1 d . . . . .
H47A H 0.511810 0.593337 1.233646 0.097 Uiso 1 1 calc GR . . . .
H47B H 0.367149 0.468444 1.218519 0.097 Uiso 1 1 calc GR . . . .
H47C H 0.387387 0.619412 1.286485 0.097 Uiso 1 1 calc GR . . . .
N1 N 0.0104(5) 0.8550(5) 0.6746(5) 0.0283(10) Uani 1 1 d . . . . .
O1 O 0.2409(6) 0.8663(6) 0.2553(5) 0.0631(14) Uani 1 1 d . . . . .
O2 O 0.1417(6) 0.4418(5) 0.3864(6) 0.0587(14) Uani 1 1 d . . . . .
O3 O -0.1981(6) 0.6488(6) 0.2585(5) 0.0608(14) Uani 1 1 d . . . . .
P1 P 0.07849(16) 0.94423(16) 0.56488(14) 0.0281(3) Uani 1 1 d . . . . .
P2 P 0.03337(15) 0.69262(15) 0.65225(14) 0.0272(3) Uani 1 1 d . . . . .
Cl1 Cl 0.41611(19) 0.78511(19) 0.61812(19) 0.0459(4) Uani 1 1 d . . . . .
Tc1 Tc 0.13088(2) 0.73816(2) 0.47177(2) 0.03042(13) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
C2 C1 H1 105.3 . . ?
C6 C1 H1 105.3 . . ?
C6 C1 C2 113.5(6) . . ?
N1 C1 H1 105.3 . . ?
N1 C1 C2 112.5(6) . . ?
N1 C1 C6 114.0(6) . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
C1 C2 C3 109.9(6) . . ?
H2A C2 H2B 108.2 . . ?
C3 C2 H2A 109.7 . . ?
C3 C2 H2B 109.7 . . ?
C2 C3 H3A 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 C2 110.2(6) . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C5 C4 C3 111.8(7) . . ?
C5 C4 H4A 109.3 . . ?
C5 C4 H4B 109.3 . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C4 C5 C6 113.5(7) . . ?
H5A C5 H5B 107.7 . . ?
C6 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
C1 C6 C5 112.3(7) . . ?
C1 C6 H6A 109.1 . . ?
C1 C6 H6B 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
O1 C7 Tc1 179.2(6) . . ?
O2 C8 Tc1 178.3(7) . . ?
O3 C9 Tc1 175.5(6) . . ?
C12 C11 P1 118.9(4) . . ?
C16 C11 C12 117.1(5) . . ?
C16 C11 P1 124.0(4) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.3(6) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 118.7 . . ?
C14 C13 C12 122.6(6) . . ?
C14 C13 H13 118.7 . . ?
C13 C14 C17 120.8(6) . . ?
C15 C14 C13 117.3(6) . . ?
C15 C14 C17 121.9(6) . . ?
C14 C15 H15 119.4 . . ?
C14 C15 C16 121.1(6) . . ?
C16 C15 H15 119.4 . . ?
C11 C16 C15 121.4(6) . . ?
C11 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 C21 C26 118.0(5) . . ?
C22 C21 P1 121.2(4) . . ?
C26 C21 P1 120.4(5) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 C21 121.4(6) . . ?
C23 C22 H22 119.3 . . ?
C22 C23 H23 119.6 . . ?
C22 C23 C24 120.8(6) . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C27 120.6(7) . . ?
C25 C24 C23 117.9(5) . . ?
C25 C24 C27 121.5(6) . . ?
C24 C25 H25 118.9 . . ?
C24 C25 C26 122.3(6) . . ?
C26 C25 H25 118.9 . . ?
C21 C26 C25 119.4(6) . . ?
C21 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C32 C31 C36 119.4(5) . . ?
C32 C31 P2 125.2(4) . . ?
C36 C31 P2 115.4(4) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 C31 120.6(6) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 119.6 . . ?
C32 C33 C34 120.9(6) . . ?
C34 C33 H33 119.6 . . ?
C33 C34 C35 118.7(5) . . ?
C33 C34 C37 121.2(6) . . ?
C35 C34 C37 120.1(7) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 C34 120.4(7) . . ?
C36 C35 H35 119.8 . . ?
C31 C36 C35 120.0(6) . . ?
C31 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C41 C46 118.3(5) . . ?
C42 C41 P2 122.9(4) . . ?
C46 C41 P2 118.8(5) . . ?
C41 C42 H42 118.9 . . ?
C41 C42 C43 122.2(6) . . ?
C43 C42 H42 118.9 . . ?
C42 C43 H43 121.1 . . ?
C42 C43 C44 117.7(7) . . ?
C44 C43 H43 121.1 . . ?
C43 C44 C47 118.0(7) . . ?
C45 C44 C43 119.6(6) . . ?
C45 C44 C47 122.4(6) . . ?
C44 C45 H45 118.8 . . ?
C44 C45 C46 122.4(6) . . ?
C46 C45 H45 118.8 . . ?
C41 C46 H46 120.1 . . ?
C45 C46 C41 119.8(6) . . ?
C45 C46 H46 120.1 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C1 N1 P1 129.2(5) . . ?
C1 N1 P2 126.0(5) . . ?
P2 N1 P1 103.9(3) . . ?
C11 P1 C21 104.3(3) . . ?
C11 P1 P2 127.1(2) . . ?
C11 P1 Tc1 126.33(18) . . ?
C21 P1 P2 122.6(2) . . ?
C21 P1 Tc1 113.60(18) . . ?
N1 P1 C11 108.3(2) . . ?
N1 P1 C21 108.7(2) . . ?
N1 P1 P2 37.71(16) . . ?
N1 P1 Tc1 94.21(17) . . ?
Tc1 P1 P2 56.55(5) . . ?
C31 P2 C41 103.0(3) . . ?
C31 P2 P1 124.31(19) . . ?
C31 P2 Tc1 113.68(18) . . ?
C41 P2 P1 126.38(19) . . ?
C41 P2 Tc1 127.2(2) . . ?
N1 P2 C31 109.9(2) . . ?
N1 P2 C41 106.5(2) . . ?
N1 P2 P1 38.37(17) . . ?
N1 P2 Tc1 95.59(18) . . ?
Tc1 P2 P1 57.27(5) . . ?
C7 Tc1 C8 93.9(3) . . ?
C7 Tc1 P1 99.6(2) . . ?
C7 Tc1 P2 165.8(2) . . ?
C7 Tc1 Cl1 85.9(2) . . ?
C8 Tc1 P1 165.7(2) . . ?
C8 Tc1 P2 100.2(2) . . ?
C8 Tc1 Cl1 85.48(19) . . ?
C9 Tc1 C7 89.3(3) . . ?
C9 Tc1 C8 86.9(3) . . ?
C9 Tc1 P1 88.77(18) . . ?
C9 Tc1 P2 89.47(19) . . ?
C9 Tc1 Cl1 170.63(17) . . ?
P1 Tc1 Cl1 99.94(5) . . ?
P2 Tc1 P1 66.18(5) . . ?
P2 Tc1 Cl1 97.19(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.519(10) . ?
C1 C6 1.512(10) . ?
C1 N1 1.490(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.534(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.520(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.452(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.520(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O1 1.120(8) . ?
C7 Tc1 1.959(7) . ?
C8 O2 1.113(8) . ?
C8 Tc1 1.960(7) . ?
C9 O3 1.082(8) . ?
C9 Tc1 1.938(7) . ?
C11 C12 1.392(8) . ?
C11 C16 1.385(8) . ?
C11 P1 1.809(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.378(8) . ?
C13 H13 0.9300 . ?
C13 C14 1.376(9) . ?
C14 C15 1.368(9) . ?
C14 C17 1.522(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.393(8) . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 C22 1.392(8) . ?
C21 C26 1.399(8) . ?
C21 P1 1.811(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.386(9) . ?
C23 H23 0.9300 . ?
C23 C24 1.393(9) . ?
C24 C25 1.370(9) . ?
C24 C27 1.499(9) . ?
C25 H25 0.9300 . ?
C25 C26 1.407(8) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C31 C32 1.381(8) . ?
C31 C36 1.387(8) . ?
C31 P2 1.818(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.381(8) . ?
C33 H33 0.9300 . ?
C33 C34 1.383(10) . ?
C34 C35 1.395(10) . ?
C34 C37 1.521(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.392(9) . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C41 C42 1.387(9) . ?
C41 C46 1.394(8) . ?
C41 P2 1.824(6) . ?
C42 H42 0.9300 . ?
C42 C43 1.404(9) . ?
C43 H43 0.9300 . ?
C43 C44 1.416(9) . ?
C44 C45 1.353(10) . ?
C44 C47 1.504(10) . ?
C45 H45 0.9300 . ?
C45 C46 1.386(8) . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
N1 P1 1.719(5) . ?
N1 P2 1.694(5) . ?
P1 P2 2.688(2) . ?
P1 Tc1 2.4717(15) . ?
P2 Tc1 2.4513(15) . ?
Cl1 Tc1 2.5155(17) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 56.4(10) . . . . ?
C1 N1 P1 C11 41.8(6) . . . . ?
C1 N1 P1 C21 -71.0(5) . . . . ?
C1 N1 P1 P2 169.4(6) . . . . ?
C1 N1 P1 Tc1 172.3(5) . . . . ?
C1 N1 P2 C31 69.5(5) . . . . ?
C1 N1 P2 C41 -41.3(5) . . . . ?
C1 N1 P2 P1 -169.8(6) . . . . ?
C1 N1 P2 Tc1 -172.8(5) . . . . ?
C2 C1 C6 C5 48.3(11) . . . . ?
C2 C1 N1 P1 56.5(8) . . . . ?
C2 C1 N1 P2 -136.3(6) . . . . ?
C2 C3 C4 C5 -58.7(10) . . . . ?
C3 C4 C5 C6 55.0(11) . . . . ?
C4 C5 C6 C1 -49.4(12) . . . . ?
C6 C1 C2 C3 -52.4(10) . . . . ?
C6 C1 N1 P1 -74.5(8) . . . . ?
C6 C1 N1 P2 92.7(8) . . . . ?
C11 C12 C13 C14 0.0(10) . . . . ?
C12 C11 C16 C15 2.9(10) . . . . ?
C12 C11 P1 C21 -154.6(5) . . . . ?
C12 C11 P1 N1 89.8(5) . . . . ?
C12 C11 P1 P2 52.4(6) . . . . ?
C12 C11 P1 Tc1 -20.1(6) . . . . ?
C12 C13 C14 C15 1.0(10) . . . . ?
C12 C13 C14 C17 -178.9(7) . . . . ?
C13 C14 C15 C16 0.0(10) . . . . ?
C14 C15 C16 C11 -2.0(11) . . . . ?
C16 C11 C12 C13 -1.9(9) . . . . ?
C16 C11 P1 C21 27.3(6) . . . . ?
C16 C11 P1 N1 -88.4(6) . . . . ?
C16 C11 P1 P2 -125.8(5) . . . . ?
C16 C11 P1 Tc1 161.8(4) . . . . ?
C17 C14 C15 C16 179.9(7) . . . . ?
C21 C22 C23 C24 -1.5(10) . . . . ?
C22 C21 C26 C25 -2.7(9) . . . . ?
C22 C21 P1 C11 43.6(5) . . . . ?
C22 C21 P1 N1 159.0(5) . . . . ?
C22 C21 P1 P2 -161.8(4) . . . . ?
C22 C21 P1 Tc1 -97.6(5) . . . . ?
C22 C23 C24 C25 -0.4(10) . . . . ?
C22 C23 C24 C27 179.9(6) . . . . ?
C23 C24 C25 C26 0.7(10) . . . . ?
C24 C25 C26 C21 0.9(10) . . . . ?
C26 C21 C22 C23 3.1(9) . . . . ?
C26 C21 P1 C11 -143.8(5) . . . . ?
C26 C21 P1 N1 -28.4(5) . . . . ?
C26 C21 P1 P2 10.8(6) . . . . ?
C26 C21 P1 Tc1 75.0(5) . . . . ?
C27 C24 C25 C26 -179.6(6) . . . . ?
C31 C32 C33 C34 -0.8(9) . . . . ?
C32 C31 C36 C35 -0.4(9) . . . . ?
C32 C31 P2 C41 106.8(5) . . . . ?
C32 C31 P2 N1 -6.3(6) . . . . ?
C32 C31 P2 P1 -46.6(6) . . . . ?
C32 C31 P2 Tc1 -112.1(5) . . . . ?
C32 C33 C34 C35 2.1(9) . . . . ?
C32 C33 C34 C37 -176.6(6) . . . . ?
C33 C34 C35 C36 -2.6(10) . . . . ?
C34 C35 C36 C31 1.8(10) . . . . ?
C36 C31 C32 C33 -0.1(9) . . . . ?
C36 C31 P2 C41 -76.1(5) . . . . ?
C36 C31 P2 N1 170.8(4) . . . . ?
C36 C31 P2 P1 130.5(4) . . . . ?
C36 C31 P2 Tc1 65.1(5) . . . . ?
C37 C34 C35 C36 176.1(6) . . . . ?
C41 C42 C43 C44 1.2(11) . . . . ?
C42 C41 C46 C45 1.6(9) . . . . ?
C42 C41 P2 C31 -12.2(6) . . . . ?
C42 C41 P2 N1 103.4(5) . . . . ?
C42 C41 P2 P1 140.5(5) . . . . ?
C42 C41 P2 Tc1 -146.0(5) . . . . ?
C42 C43 C44 C45 -0.5(11) . . . . ?
C42 C43 C44 C47 -178.6(7) . . . . ?
C43 C44 C45 C46 0.5(10) . . . . ?
C44 C45 C46 C41 -1.1(10) . . . . ?
C46 C41 C42 C43 -1.7(10) . . . . ?
C46 C41 P2 C31 168.3(5) . . . . ?
C46 C41 P2 N1 -76.2(5) . . . . ?
C46 C41 P2 P1 -39.1(6) . . . . ?
C46 C41 P2 Tc1 34.4(6) . . . . ?
C47 C44 C45 C46 178.5(7) . . . . ?
N1 C1 C2 C3 176.3(7) . . . . ?
N1 C1 C6 C5 178.8(8) . . . . ?
P1 C11 C12 C13 179.8(5) . . . . ?
P1 C11 C16 C15 -178.9(5) . . . . ?
P1 C21 C22 C23 175.8(5) . . . . ?
P1 C21 C26 C25 -175.5(4) . . . . ?
P1 N1 P2 C31 -120.6(3) . . . . ?
P1 N1 P2 C41 128.5(3) . . . . ?
P1 N1 P2 Tc1 -2.9(2) . . . . ?
P2 C31 C32 C33 177.0(5) . . . . ?
P2 C31 C36 C35 -177.7(5) . . . . ?
P2 C41 C42 C43 178.7(6) . . . . ?
P2 C41 C46 C45 -178.8(5) . . . . ?
P2 N1 P1 C11 -127.7(3) . . . . ?
P2 N1 P1 C21 119.6(3) . . . . ?
P2 N1 P1 Tc1 2.9(2) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.62(4)
2 0.38(4)
