# Supplementary Information (SI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_ba_ss24
_database_code_depnum_ccdc_archive 'CCDC 2525134'
loop_
_audit_author_name
_audit_author_address
'Joachim Ballmann'
;Heidelberg University
Germany
;
_audit_update_record             
;
2026-01-22 deposited with the CCDC.	2026-03-02 downloaded from the CCDC.
;
_audit_creation_date             2025-02-16
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
loop_
_audit_author_email
joachim.ballmann@uni-heidelberg.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Br), C46 H66 P4, 1[C4H10O]'
_chemical_formula_sum            'C50 H76 Br2 O P4'
_chemical_formula_weight         976.80
_chemical_melting_point          ?
_chemical_oxdiff_formula         C50H76Br2OP4
_chemical_oxdiff_usercomment     ss447
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   12.5338(2)
_cell_length_b                   15.7508(2)
_cell_length_c                   14.4968(3)
_cell_angle_alpha                90
_cell_angle_beta                 115.625(2)
_cell_angle_gamma                90
_cell_volume                     2580.43(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    19846
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.7530
_cell_measurement_theta_min      3.9180
_shelx_estimated_absorpt_T_max   0.905
_shelx_estimated_absorpt_T_min   0.685
_exptl_absorpt_coefficient_mu    3.408
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.127a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1028
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 0 1 0.0104
3 -6 -7 0.0354
-3 -7 7 0.0569
-7 -1 -1 0.0070
-1 6 -6 0.0462
-3 6 8 0.0645
3 8 -6 0.0526

_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7.1174 0.0873 0.5527 -0.1295 -0.9915 0.0091
3.1864 -6.3546 -7.3477 0.6435 -0.0861 0.7606
-2.9618 -6.8105 7.0052 0.6341 -0.0808 -0.7690
-6.9850 -1.1479 -0.7538 0.2325 0.9726 0.0091
-1.2464 6.0433 -6.0986 -0.5012 0.5881 0.6347
-2.7936 6.0007 7.6165 -0.6184 0.0135 -0.7858
3.0627 7.8094 -5.9802 -0.7436 0.0205 0.6683

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38166
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.096
_diffrn_reflns_theta_min         3.912
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  71.00   1.00    5.00    --    0.00  77.00 150.00   96
  2  ω    -21.00  69.00   1.00    5.00    --    0.00  57.00 -90.00   90
  3  ω    -31.00  69.00   1.00    5.00    --    0.00  77.00  30.00  100
  4  ω    -38.00  -7.00   1.00    5.00    --   14.00 130.00  25.30   31
  5  ω    -16.00   9.00   1.00   18.00    --   30.00 105.00 -88.34   25
  6  ω     -2.00  25.00   1.00   18.00    --   38.00  94.00 -63.05   27
  7  ω      3.00  28.00   1.00   18.00    --   42.00  91.00  56.05   25
  8  ω     10.00  35.00   1.00   18.00    --   46.00  85.00 138.81   25
  9  ω     11.00  38.00   1.00   18.00    --   46.00  84.00 -73.01   27
 10  ω     17.00  42.00   1.00   18.00    --   50.00  80.00 -14.08   25
 11  ω     16.00  41.00   1.00   18.00    --   50.00  81.00-142.69   25
 12  ω     16.00  41.00   1.00   18.00    --   50.00  81.00  31.75   25
 13  ω     17.00  44.00   1.00   18.00    --   50.00  80.00 115.94   27
 14  ω     16.00  41.00   1.00   18.00    --   50.00  81.00 173.54   25
 15  ω     17.00  42.00   1.00   18.00    --   50.00  80.00  62.66   25
 16  ω    -10.00  86.00   1.00   18.00    --   54.47 -77.00  60.00   96
 17  ω     23.00 106.00   1.00   18.00    --   54.47-125.00 -60.00   83
 18  ω      1.00  58.00   1.00   18.00    --   54.47 -99.00-150.00   57
 19  ω    -15.00  75.00   1.00   18.00    --   54.47 -57.00 -60.00   90
 20  ω     71.00 126.00   1.00   18.00    --   62.00  74.00 -37.73   55
 21  ω     81.00 108.00   1.00   18.00    --   62.00  75.00 100.45   27
 22  ω     31.00  66.00   1.00   18.00    --   62.00  76.00-176.79   35
 23  ω     32.00  58.00   1.00   18.00    --   62.00  74.00 -37.73   26
 24  ω     31.00  60.00   1.00   18.00    --   62.00  77.00 -20.57   29
 25  ω     69.00 122.00   1.00   18.00    --   62.00  76.00-176.79   53
 26  ω     31.00 116.00   1.00   18.00    --   62.00  76.00 151.43   85
 27  ω     31.00  70.00   1.00   18.00    --   62.00  75.00 100.45   39
 28  ω     31.00  58.00   1.00   18.00    --   62.00  76.00-124.99   27
 29  ω     30.00  56.00   1.00   18.00    --   62.00  77.00  69.40   26
 30  ω     31.00 133.00   1.00   18.00    --   62.00  75.00  22.07  102
 31  ω     31.00 133.00   1.00   18.00    --   62.00  75.00 -73.91  102
 32  ω     66.00 125.00   1.00   18.00    --   62.00  77.00  69.40   59
 33  ω     30.00 132.00   1.00   18.00    --   62.00  77.00-113.17  102
 34  ω     77.00 103.00   1.00   30.00    --  108.94  77.00-180.00   26
 35  ω     84.00 160.00   1.00   30.00    --  108.94  64.00 150.00   76
 36  ω     84.00 169.00   1.00   30.00    --  108.94  64.00 120.00   85
 37  ω     77.00 103.00   1.00   30.00    --  108.94  77.00   0.00   26
 38  ω     84.00 166.00   1.00   30.00    --  108.94  64.00 -90.00   82
 39  ω     77.00 103.00   1.00   30.00    --  108.94  77.00 -60.00   26
 40  ω     84.00 177.00   1.00   30.00    --  108.94  64.00-150.00   93
 41  ω     82.00 145.00   1.00   30.00    --  108.94  38.00 -90.00   63
 42  ω     84.00 177.00   1.00   30.00    --  108.94  64.00  90.00   93
 43  ω     84.00 177.00   1.00   30.00    --  108.94  64.00  60.00   93
 44  ω     84.00 166.00   1.00   30.00    --  108.94  64.00   0.00   82
 45  ω     84.00 122.00   1.00   30.00    --  108.94  64.00-180.00   38
 46  ω     77.00 103.00   1.00   30.00    --  108.94  77.00 150.00   26
 47  ω    101.00 176.00   1.00   30.00    --  108.94 111.00 150.00   75
 48  ω     84.00 165.00   1.00   30.00    --  108.94  64.00 -60.00   81
 49  ω     36.00 102.00   1.00   30.00    --  108.94 -92.00  60.00   66
 50  ω     77.00 103.00   1.00   30.00    --  108.94  77.00  90.00   26
 51  ω     39.00 123.00   1.00   30.00    --  108.94 -50.00  60.00   84
 52  ω     59.00 112.00   1.00   30.00    --  108.94-111.00-150.00   53
 53  ω     77.00 103.00   1.00   30.00    --  108.94  77.00  30.00   26
 54  ω    136.00 163.00   1.00   30.00    --  108.94  77.00-120.00   27
 55  ω     77.00 103.00   1.00   30.00    --  108.94  77.00 120.00   26
 56  ω     84.00 110.00   1.00   30.00    --  108.94  64.00 -30.00   26
 57  ω     77.00 104.00   1.00   30.00    --  108.94  77.00  60.00   27
 58  ω     77.00 103.00   1.00   30.00    --  108.94  77.00-120.00   26
 59  ω     36.00 108.00   1.00   30.00    --  108.94 -92.00-120.00   72
 60  ω     78.00 105.00   1.00   30.00    --  108.94  77.00-150.00   27
 61  ω     84.00 171.00   1.00   30.00    --  108.94  64.00  30.00   87
 62  ω     77.00 178.00   1.00   30.00    --  108.94  77.00 -30.00  101
 63  ω     75.00 112.00   1.00   30.00    --  108.94-111.00   0.00   37
 64  ω     77.00 103.00   1.00   30.00    --  108.94  77.00 -90.00   26
 65  ω     41.00 133.00   1.00   30.00    --  108.94 -64.00-120.00   92
 66  ω    131.00 158.00   1.00   30.00    --  108.94  77.00-180.00   27
 67  ω     82.00 109.00   1.00   30.00    --  108.94 -92.00  90.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0161791000
_diffrn_orient_matrix_UB_12      -0.0970421000
_diffrn_orient_matrix_UB_13      -0.0106696000
_diffrn_orient_matrix_UB_21      -0.1350236000
_diffrn_orient_matrix_UB_22      0.0118539000
_diffrn_orient_matrix_UB_23      -0.0570926000
_diffrn_orient_matrix_UB_31      0.0091925000
_diffrn_orient_matrix_UB_32      0.0034656000
_diffrn_orient_matrix_UB_33      -0.1025238000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4507
_reflns_number_total             4956
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4956
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0416
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0663P)²+1.9381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1157
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C18(H18), C21(H21)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Br1 Br 0.82535(2) 0.65722(2) 0.42599(2) 0.04523(12) Uani 1 1 d . . . . .
P1 P 0.74155(5) 0.35748(4) 0.41439(5) 0.03633(16) Uani 1 1 d . . . . .
P2 P 0.39740(5) 0.32524(4) 0.38913(5) 0.03487(16) Uani 1 1 d . . . . .
C1 C 0.6905(2) 0.25927(15) 0.3466(2) 0.0398(6) Uani 1 1 d . . . . .
C2 C 0.7508(3) 0.20147(17) 0.3136(2) 0.0484(7) Uani 1 1 d . . . . .
H2 H 0.830528 0.211699 0.325813 0.058 Uiso 1 1 calc R U . . .
C3 C 0.6929(3) 0.12923(19) 0.2630(3) 0.0548(8) Uani 1 1 d . . . . .
H3 H 0.733243 0.089023 0.240714 0.066 Uiso 1 1 calc R U . . .
C4 C 0.5762(3) 0.11479(18) 0.2445(3) 0.0538(7) Uani 1 1 d . . . . .
H4 H 0.537269 0.065277 0.207999 0.065 Uiso 1 1 calc R U . . .
C5 C 0.5149(3) 0.17084(17) 0.2778(2) 0.0467(6) Uani 1 1 d . . . . .
H5 H 0.435073 0.159778 0.264561 0.056 Uiso 1 1 calc R U . . .
C6 C 0.5724(2) 0.24412(15) 0.3313(2) 0.0398(6) Uani 1 1 d . . . . .
C7 C 0.5282(2) 0.31044(15) 0.3744(2) 0.0368(5) Uani 1 1 d . . . . .
C8 C 0.6060(2) 0.37913(15) 0.4210(2) 0.0353(5) Uani 1 1 d . . . . .
C9 C 0.56265(19) 0.44461(14) 0.46324(18) 0.0319(5) Uani 1 1 d . . . . .
C10 C 0.6152(2) 0.52108(14) 0.51040(18) 0.0330(5) Uani 1 1 d . . . . .
H10 H 0.691550 0.536081 0.516827 0.040 Uiso 1 1 calc R U . . .
C11 C 0.5555(2) 0.57454(14) 0.54750(19) 0.0325(5) Uani 1 1 d . . . . .
C12 C 0.8672(2) 0.33975(17) 0.5368(2) 0.0455(6) Uani 1 1 d . . . . .
H12 H 0.935320 0.322141 0.522595 0.055 Uiso 1 1 calc R U . . .
C13 C 0.9036(3) 0.4200(2) 0.6004(3) 0.0573(8) Uani 1 1 d . . . . .
H13A H 0.912444 0.466327 0.559114 0.086 Uiso 1 1 calc R U . . .
H13B H 0.979083 0.410549 0.660287 0.086 Uiso 1 1 calc R U . . .
H13C H 0.842800 0.435113 0.623010 0.086 Uiso 1 1 calc R U . . .
C14 C 0.8420(3) 0.2667(2) 0.5940(3) 0.0617(8) Uani 1 1 d . . . . .
H14A H 0.771860 0.280177 0.604750 0.093 Uiso 1 1 calc R U . . .
H14B H 0.910123 0.258503 0.660276 0.093 Uiso 1 1 calc R U . . .
H14C H 0.827676 0.214535 0.553464 0.093 Uiso 1 1 calc R U . . .
C15 C 0.7796(2) 0.43568(16) 0.3412(2) 0.0426(6) Uani 1 1 d . . . . .
H15 H 0.805032 0.488618 0.383273 0.051 Uiso 1 1 calc R U . . .
C16 C 0.6720(3) 0.4573(2) 0.2431(3) 0.0618(8) Uani 1 1 d . . . . .
H16A H 0.650482 0.408246 0.196978 0.093 Uiso 1 1 calc R U . . .
H16B H 0.690194 0.505756 0.209935 0.093 Uiso 1 1 calc R U . . .
H16C H 0.605665 0.471869 0.258880 0.093 Uiso 1 1 calc R U . . .
C17 C 0.8829(3) 0.4055(2) 0.3211(3) 0.0540(7) Uani 1 1 d . . . . .
H17A H 0.950580 0.392516 0.386290 0.081 Uiso 1 1 calc R U . . .
H17B H 0.905017 0.450185 0.285594 0.081 Uiso 1 1 calc R U . . .
H17C H 0.859781 0.354329 0.278482 0.081 Uiso 1 1 calc R U . . .
C18 C 0.3748(2) 0.24686(17) 0.4724(2) 0.0446(6) Uani 1 1 d . . . . .
H18 H 0.329990 0.275311 0.506481 0.053 Uiso 1 1 calc R U . . .
C19 C 0.4947(3) 0.2207(2) 0.5556(3) 0.0628(9) Uani 1 1 d . . . . .
H19A H 0.536908 0.186588 0.525389 0.094 Uiso 1 1 calc R U . . .
H19B H 0.483376 0.187127 0.607572 0.094 Uiso 1 1 calc R U . . .
H19C H 0.541117 0.271562 0.587395 0.094 Uiso 1 1 calc R U . . .
C20 C 0.3021(4) 0.1699(2) 0.4135(3) 0.0773(12) Uani 1 1 d . . . . .
H20A H 0.224212 0.189030 0.363003 0.116 Uiso 1 1 calc R U . . .
H20B H 0.292094 0.130458 0.461436 0.116 Uiso 1 1 calc R U . . .
H20C H 0.343409 0.141196 0.378398 0.116 Uiso 1 1 calc R U . . .
C21 C 0.2645(2) 0.33009(17) 0.2693(2) 0.0439(6) Uani 1 1 d . . . . .
H21 H 0.246571 0.270945 0.241765 0.053 Uiso 1 1 calc R U . . .
C22 C 0.1580(3) 0.3611(2) 0.2854(3) 0.0620(8) Uani 1 1 d . . . . .
H22A H 0.150716 0.327194 0.339021 0.093 Uiso 1 1 calc R U . . .
H22B H 0.085900 0.355143 0.221450 0.093 Uiso 1 1 calc R U . . .
H22C H 0.169282 0.420961 0.305990 0.093 Uiso 1 1 calc R U . . .
C23 C 0.2850(3) 0.3830(2) 0.1915(2) 0.0554(7) Uani 1 1 d . . . . .
H23A H 0.303115 0.441578 0.216210 0.083 Uiso 1 1 calc R U . . .
H23B H 0.213601 0.382334 0.126403 0.083 Uiso 1 1 calc R U . . .
H23C H 0.351515 0.359483 0.181328 0.083 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
P1 C1 1.796(3) . ?
P1 C8 1.776(2) . ?
P1 C12 1.814(3) . ?
P1 C15 1.818(3) . ?
P2 C7 1.758(2) . ?
P2 C11 1.793(2) 3_666 ?
P2 C18 1.833(3) . ?
P2 C21 1.815(3) . ?
C1 C2 1.394(3) . ?
C1 C6 1.418(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.378(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.404(4) . ?
C6 C7 1.445(3) . ?
C7 C8 1.417(3) . ?
C8 C9 1.422(3) . ?
C9 C10 1.401(3) . ?
C9 C11 1.452(3) 3_666 ?
C10 H10 0.9500 . ?
C10 C11 1.381(3) . ?
C12 H12 1.0000 . ?
C12 C13 1.514(4) . ?
C12 C14 1.529(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.517(4) . ?
C15 C17 1.522(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18 1.0000 . ?
C18 C19 1.522(4) . ?
C18 C20 1.535(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21 1.0000 . ?
C21 C22 1.531(4) . ?
C21 C23 1.511(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

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
C1 P1 C12 110.85(13) . . ?
C1 P1 C15 112.70(12) . . ?
C8 P1 C1 94.12(11) . . ?
C8 P1 C12 115.03(12) . . ?
C8 P1 C15 113.57(12) . . ?
C12 P1 C15 109.82(13) . . ?
C7 P2 C11 93.51(11) . 3_666 ?
C7 P2 C18 114.13(12) . . ?
C7 P2 C21 114.02(13) . . ?
C11 P2 C18 111.47(12) 3_666 . ?
C11 P2 C21 114.57(12) 3_666 . ?
C21 P2 C18 108.64(13) . . ?
C2 C1 P1 129.2(2) . . ?
C2 C1 C6 121.4(2) . . ?
C6 C1 P1 109.35(17) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 C1 118.9(3) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.5(3) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 119.2 . . ?
C3 C4 C5 121.6(3) . . ?
C5 C4 H4 119.2 . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.1(3) . . ?
C6 C5 H5 120.4 . . ?
C1 C6 C7 112.4(2) . . ?
C5 C6 C1 118.4(2) . . ?
C5 C6 C7 129.2(2) . . ?
C6 C7 P2 134.49(19) . . ?
C8 C7 P2 109.06(17) . . ?
C8 C7 C6 116.4(2) . . ?
C7 C8 P1 107.77(17) . . ?
C7 C8 C9 116.5(2) . . ?
C9 C8 P1 135.65(19) . . ?
C8 C9 C11 111.4(2) . 3_666 ?
C10 C9 C8 130.3(2) . . ?
C10 C9 C11 118.3(2) . 3_666 ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.6(2) . . ?
C11 C10 H10 120.2 . . ?
C9 C11 P2 109.41(16) 3_666 3_666 ?
C10 C11 P2 128.50(18) . 3_666 ?
C10 C11 C9 122.1(2) . 3_666 ?
P1 C12 H12 107.4 . . ?
C13 C12 P1 111.9(2) . . ?
C13 C12 H12 107.4 . . ?
C13 C12 C14 112.1(3) . . ?
C14 C12 P1 110.5(2) . . ?
C14 C12 H12 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
P1 C15 H15 107.7 . . ?
C16 C15 P1 110.36(19) . . ?
C16 C15 H15 107.7 . . ?
C16 C15 C17 112.1(3) . . ?
C17 C15 P1 111.09(19) . . ?
C17 C15 H15 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
P2 C18 H18 107.7 . . ?
C19 C18 P2 108.86(19) . . ?
C19 C18 H18 107.7 . . ?
C19 C18 C20 111.9(3) . . ?
C20 C18 P2 112.9(2) . . ?
C20 C18 H18 107.7 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
P2 C21 H21 107.3 . . ?
C22 C21 P2 111.5(2) . . ?
C22 C21 H21 107.3 . . ?
C23 C21 P2 110.9(2) . . ?
C23 C21 H21 107.3 . . ?
C23 C21 C22 112.2(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 C3 179.5(2) . . . . ?
P1 C1 C6 C5 178.8(2) . . . . ?
P1 C1 C6 C7 -0.4(3) . . . . ?
P1 C8 C9 C10 5.3(5) . . . . ?
P1 C8 C9 C11 -175.3(2) . . . 3_666 ?
P2 C7 C8 P1 175.03(13) . . . . ?
P2 C7 C8 C9 -3.0(3) . . . . ?
C1 P1 C8 C7 1.6(2) . . . . ?
C1 P1 C8 C9 179.0(3) . . . . ?
C1 P1 C12 C13 -173.8(2) . . . . ?
C1 P1 C12 C14 -48.1(2) . . . . ?
C1 P1 C15 C16 61.2(2) . . . . ?
C1 P1 C15 C17 -63.7(2) . . . . ?
C1 C2 C3 C4 0.6(5) . . . . ?
C1 C6 C7 P2 -174.6(2) . . . . ?
C1 C6 C7 C8 1.7(4) . . . . ?
C2 C1 C6 C5 -2.8(4) . . . . ?
C2 C1 C6 C7 178.0(3) . . . . ?
C2 C3 C4 C5 -1.5(5) . . . . ?
C3 C4 C5 C6 0.2(5) . . . . ?
C4 C5 C6 C1 1.9(4) . . . . ?
C4 C5 C6 C7 -179.1(3) . . . . ?
C5 C6 C7 P2 6.3(5) . . . . ?
C5 C6 C7 C8 -177.4(3) . . . . ?
C6 C1 C2 C3 1.6(5) . . . . ?
C6 C7 C8 P1 -2.1(3) . . . . ?
C6 C7 C8 C9 179.9(2) . . . . ?
C7 P2 C18 C19 32.9(2) . . . . ?
C7 P2 C18 C20 -92.0(3) . . . . ?
C7 P2 C21 C22 -168.2(2) . . . . ?
C7 P2 C21 C23 -42.4(2) . . . . ?
C7 C8 C9 C10 -177.5(3) . . . . ?
C7 C8 C9 C11 2.0(3) . . . 3_666 ?
C8 P1 C1 C2 -178.9(3) . . . . ?
C8 P1 C1 C6 -0.7(2) . . . . ?
C8 P1 C12 C13 -68.5(2) . . . . ?
C8 P1 C12 C14 57.2(2) . . . . ?
C8 P1 C15 C16 -44.3(2) . . . . ?
C8 P1 C15 C17 -169.2(2) . . . . ?
C8 C9 C10 C11 -178.9(2) . . . . ?
C9 C10 C11 P2 179.71(19) . . . 3_666 ?
C9 C10 C11 C9 -1.8(4) . . . 3_666 ?
C11 P2 C7 C6 178.8(3) 3_666 . . . ?
C11 P2 C7 C8 2.4(2) 3_666 . . . ?
C11 P2 C18 C19 -71.5(2) 3_666 . . . ?
C11 P2 C18 C20 163.6(2) 3_666 . . . ?
C11 P2 C21 C22 -62.1(2) 3_666 . . . ?
C11 P2 C21 C23 63.8(2) 3_666 . . . ?
C11 C9 C10 C11 1.7(4) 3_666 . . . ?
C12 P1 C1 C2 -60.1(3) . . . . ?
C12 P1 C1 C6 118.1(2) . . . . ?
C12 P1 C8 C7 -113.7(2) . . . . ?
C12 P1 C8 C9 63.7(3) . . . . ?
C12 P1 C15 C16 -174.6(2) . . . . ?
C12 P1 C15 C17 60.4(2) . . . . ?
C15 P1 C1 C2 63.4(3) . . . . ?
C15 P1 C1 C6 -118.4(2) . . . . ?
C15 P1 C8 C7 118.55(19) . . . . ?
C15 P1 C8 C9 -64.0(3) . . . . ?
C15 P1 C12 C13 61.1(2) . . . . ?
C15 P1 C12 C14 -173.2(2) . . . . ?
C18 P2 C7 C6 63.4(3) . . . . ?
C18 P2 C7 C8 -113.0(2) . . . . ?
C18 P2 C21 C22 63.3(2) . . . . ?
C18 P2 C21 C23 -170.9(2) . . . . ?
C21 P2 C7 C6 -62.3(3) . . . . ?
C21 P2 C7 C8 121.3(2) . . . . ?
C21 P2 C18 C19 161.3(2) . . . . ?
C21 P2 C18 C20 36.4(3) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 74 electrons were 
found in a volume of 374Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[C4H10O] per formula unit 
which account for 84 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.169 0.000 0.500 186.7 37.2 '1 ether'
2 0.130 0.500 0.000 186.7 37.2 '1 ether'

_smtbx_masks_void_probe_radius   1.4
_smtbx_masks_void_truncation_radius 1.1
_olex2_date_sample_data_collection 2025-02-14
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
# start Validation Reply Form
_vrf_FORMU01_ba_ss24             
;
PROBLEM:There is a discrepancy between the atom counts
RESPONSE: Disordered Et2O (one molecule per formula unit) was treated with 
OLEX2 solvent masks. Hence, the moiety formula, sum formula, F000, mue and 
rho are expected to differ. See following G-alerts/G-infos.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_ba_ss25
_database_code_depnum_ccdc_archive 'CCDC 2525136'
loop_
_audit_author_name
_audit_author_address
'Joachim Ballmann'
;Heidelberg University
Germany
;
_audit_update_record             
;
2026-01-22 deposited with the CCDC.	2026-03-02 downloaded from the CCDC.
;
_audit_creation_date             2025-05-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_shelx_SHELXL_version_number     2019/3
loop_
_audit_author_email
joachim.ballmann@uni-heidelberg.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H70 P4, 4(Br), 2[CH4O]'
_chemical_formula_sum            'C56 H78 Br4 O2 P4'
_chemical_formula_weight         1226.70
_chemical_melting_point          ?
_chemical_oxdiff_formula         C56H78Br4O2P4
_chemical_oxdiff_usercomment     ss483
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   23.0439(3)
_cell_length_b                   8.59720(10)
_cell_length_c                   30.0718(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.5950(10)
_cell_angle_gamma                90
_cell_volume                     5814.25(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18474
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.7830
_cell_measurement_theta_min      3.9290
_shelx_estimated_absorpt_T_max   0.765
_shelx_estimated_absorpt_T_min   0.539
_exptl_absorpt_coefficient_mu    4.707
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.127a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2520
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 4 14 0.0555
11 3 -9 0.0348
5 -4 -14 0.0462
-5 5 0 0.0455
-10 -2 -10 0.0411
-9 -4 -1 0.0446
1 -2 18 0.0281
5 -1 16 0.0158
2 -6 0 0.0468
-5 2 -15 0.0360

_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.3649 3.7187 13.9734 0.4671 0.1415 0.8728
10.6776 3.4721 -9.1681 -0.8603 -0.2545 0.4418
5.3267 -3.7322 -13.9423 -0.4640 -0.1406 -0.8746
-5.2992 5.2014 -0.1079 0.1701 -0.5805 0.7963
-9.8121 -2.1421 -9.5734 0.4368 -0.6307 -0.6415
-9.4269 -4.2137 -0.7564 0.6269 -0.0796 -0.7751
0.6791 -1.7054 17.9265 0.3302 0.9345 0.1331
5.0805 -0.6546 16.3284 0.0247 0.9528 0.3027
2.3427 -5.5075 0.3743 0.0104 0.5039 -0.8637
-5.2322 2.1705 -14.7515 -0.0250 -0.9994 -0.0232

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            38736
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.970
_diffrn_reflns_theta_min         3.011
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00 -24.00   1.00    5.00    --    0.00 -57.00  60.00   42
  2  ω     16.00  67.00   1.00    5.00    --    0.00  77.00   0.00   51
  3  ω    -17.00  69.00   1.00    5.00    --    0.00  57.00-150.00   86
  4  ω    -21.00  13.00   1.00    5.00    --    0.00 -57.00  60.00   34
  5  ω    -31.00  -4.00   1.00    5.00    --    0.00  77.00   0.00   27
  6  ω    -33.00  -6.00   1.00    5.00    --   10.00 108.00  85.40   27
  7  ω    -29.00  -3.00   1.00    5.00    --   22.00 118.00-160.73   26
  8  ω     -3.00  24.00   1.00   10.00    --   38.00  95.00 133.37   27
  9  ω      4.00  31.00   1.00   10.00    --   42.00  89.00  85.29   27
 10  ω      2.00  27.00   1.00   10.00    --   42.00  92.00 -93.79   25
 11  ω     11.00  36.00   1.00   10.00    --   46.00  83.00 -13.50   25
 12  ω     10.00  35.00   1.00   10.00    --   46.00  85.00-142.71   25
 13  ω     16.00  41.00   1.00   10.00    --   50.00  81.00-153.76   25
 14  ω     16.00  41.00   1.00   10.00    --   50.00  82.00  12.44   25
 15  ω     23.00 100.00   1.00   10.00    --   54.47-125.00-150.00   77
 16  ω      2.00  73.00   1.00   10.00    --   54.47 -99.00   0.00   71
 17  ω    -11.00  72.00   1.00   10.00    --   54.47 -57.00-150.00   83
 18  ω     -3.00  75.00   1.00   10.00    --   54.47 -57.00  30.00   78
 19  ω     23.00  51.00   1.00   10.00    --   54.47  77.00  90.00   28
 20  ω     26.00  53.00   1.00   10.00    --   58.00  77.00-103.23   27
 21  ω     91.00 128.00   1.00   10.00    --   58.00  77.00-103.23   37
 22  ω    101.00 128.00   1.00   10.00    --   58.00  76.00 -63.32   27
 23  ω     27.00  53.00   1.00   10.00    --   58.00  76.00 -63.32   26
 24  ω     31.00 131.00   1.00   10.00    --   62.00  77.00 -38.02  100
 25  ω     30.00  68.00   1.00   10.00    --   62.00  77.00  41.81   38
 26  ω     33.00 113.00   1.00   10.00    --   62.00  72.00   9.54   80
 27  ω     31.00 108.00   1.00   10.00    --   62.00  77.00-134.19   77
 28  ω     31.00 131.00   1.00   10.00    --   62.00  76.00 171.05  100
 29  ω     80.00 124.00   1.00   10.00    --   62.00  77.00  41.81   44
 30  ω     69.00 125.00   1.00   10.00    --   62.00  77.00  98.56   56
 31  ω     31.00  56.00   1.00   10.00    --   62.00  77.00 128.77   25
 32  ω     89.00 114.00   1.00   10.00    --   62.00  77.00 128.77   25
 33  ω     30.00  64.00   1.00   10.00    --   62.00  77.00  98.56   34
 34  ω     43.00  78.00   1.00   10.00    --   66.00  49.00 -54.93   35
 35  ω     75.00 110.00   1.00   15.00    --  108.94-111.00  90.00   35
 36  ω     84.00 173.00   1.00   15.00    --  108.94  64.00   0.00   89
 37  ω     84.00 117.00   1.00   15.00    --  108.94  64.00 -60.00   33
 38  ω    143.00 177.00   1.00   15.00    --  108.94 111.00-120.00   34
 39  ω     85.00 167.00   1.00   15.00    --  108.94  64.00-150.00   82
 40  ω     77.00 103.00   1.00   15.00    --  108.94  77.00 -30.00   26
 41  ω    112.00 177.00   1.00   15.00    --  108.94  77.00 -60.00   65
 42  ω     84.00 174.00   1.00   15.00    --  108.94  64.00 120.00   90
 43  ω     78.00 104.00   1.00   15.00    --  108.94  77.00 -60.00   26
 44  ω     41.00 133.00   1.00   15.00    --  108.94 -64.00 -30.00   92
 45  ω     37.00 109.00   1.00   15.00    --  108.94 -92.00 -60.00   72
 46  ω    109.00 177.00   1.00   15.00    --  108.94  77.00  30.00   68
 47  ω     78.00 103.00   1.00   15.00    --  108.94  77.00  30.00   25
 48  ω     77.00 157.00   1.00   15.00    --  108.94  77.00  60.00   80
 49  ω     84.00 123.00   1.00   15.00    --  108.94  64.00  30.00   39
 50  ω    114.00 166.00   1.00   15.00    --  108.94  64.00 -30.00   52
 51  ω     84.00 111.00   1.00   15.00    --  108.94  64.00 -30.00   27
 52  ω     77.00 103.00   1.00   15.00    --  108.94  77.00-150.00   26
 53  ω     77.00 163.00   1.00   15.00    --  108.94  77.00 -90.00   86
 54  ω     77.00 166.00   1.00   15.00    --  108.94  77.00-120.00   89
 55  ω     44.00 108.00   1.00   15.00    --  108.94-111.00-180.00   64
 56  ω     78.00 105.00   1.00   15.00    --  108.94  77.00 120.00   27
 57  ω     84.00 144.00   1.00   15.00    --  108.94  64.00  90.00   60
 58  ω     53.00 106.00   1.00   15.00    --  108.94-111.00 -90.00   53
 59  ω     77.00 177.00   1.00   15.00    --  108.94  77.00 150.00  100
 60  ω     77.00 165.00   1.00   15.00    --  108.94  77.00-180.00   88
 61  ω     77.00 103.00   1.00   15.00    --  108.94  77.00   0.00   26
 62  ω     84.00 110.00   1.00   15.00    --  108.94  64.00-180.00   26
 63  ω     36.00  83.00   1.00   15.00    --  108.94 -92.00-150.00   47
 64  ω    132.00 177.00   1.00   15.00    --  108.94  77.00  90.00   45
 65  ω     84.00 110.00   1.00   15.00    --  108.94  64.00  60.00   26
 66  ω     77.00 103.00   1.00   15.00    --  108.94  77.00  90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0568561000
_diffrn_orient_matrix_UB_12      -0.0248359000
_diffrn_orient_matrix_UB_13      0.0182094000
_diffrn_orient_matrix_UB_21      0.0373887000
_diffrn_orient_matrix_UB_22      -0.0726091000
_diffrn_orient_matrix_UB_23      0.0438054000
_diffrn_orient_matrix_UB_31      0.0080906000
_diffrn_orient_matrix_UB_32      0.1617959000
_diffrn_orient_matrix_UB_33      0.0225088000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4944
_reflns_number_total             5572
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.117
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5572
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0531
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0929P)²+13.1958P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1592
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C22(H22), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Br1 Br 0.68662(2) 0.51593(5) 0.43888(2) 0.04720(16) Uani 1 1 d . . . . .
P1 P 0.49771(4) 0.48741(10) 0.39465(3) 0.0335(2) Uani 1 1 d . . . . .
P2 P 0.67162(3) 0.36980(10) 0.58603(3) 0.0352(2) Uani 1 1 d . . . . .
C1 C 0.50493(15) 0.4881(4) 0.45550(11) 0.0339(7) Uani 1 1 d . . . . .
C2 C 0.55474(14) 0.4528(4) 0.48893(11) 0.0354(7) Uani 1 1 d . . . . .
H2 H 0.591044 0.422209 0.481416 0.043 Uiso 1 1 calc R U . . .
C3 C 0.54932(14) 0.4642(4) 0.53406(11) 0.0341(7) Uani 1 1 d . . . . .
C4 C 0.59501(14) 0.4337(4) 0.57534(11) 0.0351(7) Uani 1 1 d . . . . .
C5 C 0.57948(14) 0.4578(4) 0.61579(11) 0.0360(7) Uani 1 1 d . . . . .
C6 C 0.62548(14) 0.4371(4) 0.65726(11) 0.0367(7) Uani 1 1 d . . . . .
C7 C 0.62209(16) 0.4639(4) 0.70141(12) 0.0410(8) Uani 1 1 d . . . . .
H7 H 0.586444 0.503906 0.707954 0.049 Uiso 1 1 calc R U . . .
C8 C 0.67184(16) 0.4320(5) 0.73774(11) 0.0417(7) Uani 1 1 d . . . . .
C9 C 0.66973(19) 0.4547(5) 0.78361(13) 0.0499(9) Uani 1 1 d . . . . .
H9 H 0.635006 0.497140 0.791094 0.060 Uiso 1 1 calc R U . . .
C10 C 0.71771(19) 0.4160(6) 0.81775(13) 0.0551(10) Uani 1 1 d . . . . .
H10 H 0.715998 0.431791 0.848703 0.066 Uiso 1 1 calc R U . . .
C11 C 0.7696(2) 0.3526(5) 0.80693(13) 0.0551(10) Uani 1 1 d . . . . .
H11 H 0.802018 0.323238 0.830766 0.066 Uiso 1 1 calc R U . . .
C12 C 0.77357(17) 0.3332(5) 0.76299(13) 0.0502(9) Uani 1 1 d . . . . .
H12 H 0.809240 0.293944 0.756289 0.060 Uiso 1 1 calc R U . . .
C13 C 0.72495(16) 0.3711(5) 0.72696(12) 0.0427(8) Uani 1 1 d . . . . .
C14 C 0.72852(15) 0.3519(4) 0.68065(12) 0.0424(8) Uani 1 1 d . . . . .
H14 H 0.764274 0.315922 0.673321 0.051 Uiso 1 1 calc R U . . .
C15 C 0.68028(15) 0.3856(4) 0.64683(11) 0.0385(7) Uani 1 1 d . . . . .
C16 C 0.50577(14) 0.2981(4) 0.37030(11) 0.0366(7) Uani 1 1 d . . . . .
H16 H 0.502239 0.313069 0.336834 0.044 Uiso 1 1 calc R U . . .
C17 C 0.45604(18) 0.1889(5) 0.37618(15) 0.0529(9) Uani 1 1 d . . . . .
H17A H 0.457866 0.172928 0.408719 0.079 Uiso 1 1 calc R U . . .
H17B H 0.460667 0.088783 0.361763 0.079 Uiso 1 1 calc R U . . .
H17C H 0.417563 0.234692 0.361837 0.079 Uiso 1 1 calc R U . . .
C18 C 0.56705(17) 0.2284(5) 0.38958(15) 0.0507(9) Uani 1 1 d . . . . .
H18A H 0.597605 0.308047 0.390039 0.076 Uiso 1 1 calc R U . . .
H18B H 0.574019 0.141205 0.370419 0.076 Uiso 1 1 calc R U . . .
H18C H 0.568850 0.191286 0.420664 0.076 Uiso 1 1 calc R U . . .
C19 C 0.54411(15) 0.6358(4) 0.37735(12) 0.0407(7) Uani 1 1 d . . . . .
H19 H 0.585823 0.595547 0.384289 0.049 Uiso 1 1 calc R U . . .
C20 C 0.5274(2) 0.6690(7) 0.32667(15) 0.0658(12) Uani 1 1 d . . . . .
H20A H 0.526507 0.571289 0.309733 0.099 Uiso 1 1 calc R U . . .
H20B H 0.556853 0.739194 0.318386 0.099 Uiso 1 1 calc R U . . .
H20C H 0.488071 0.717887 0.319100 0.099 Uiso 1 1 calc R U . . .
C21 C 0.5435(2) 0.7840(5) 0.40550(18) 0.0669(12) Uani 1 1 d . . . . .
H21A H 0.503463 0.828916 0.398675 0.100 Uiso 1 1 calc R U . . .
H21B H 0.571721 0.859363 0.397816 0.100 Uiso 1 1 calc R U . . .
H21C H 0.555000 0.758699 0.438004 0.100 Uiso 1 1 calc R U . . .
C22 C 0.67904(15) 0.1696(4) 0.56984(11) 0.0394(7) Uani 1 1 d . . . . .
H22 H 0.721574 0.139065 0.581170 0.047 Uiso 1 1 calc R U . . .
C23 C 0.66407(17) 0.1482(5) 0.51788(12) 0.0456(8) Uani 1 1 d . . . . .
H23A H 0.621100 0.159647 0.506350 0.068 Uiso 1 1 calc R U . . .
H23B H 0.676509 0.044338 0.510296 0.068 Uiso 1 1 calc R U . . .
H23C H 0.685034 0.227069 0.503827 0.068 Uiso 1 1 calc R U . . .
C24 C 0.64175(18) 0.0653(5) 0.59288(13) 0.0471(8) Uani 1 1 d . . . . .
H24A H 0.652873 0.081203 0.625924 0.071 Uiso 1 1 calc R U . . .
H24B H 0.648568 -0.043538 0.585835 0.071 Uiso 1 1 calc R U . . .
H24C H 0.599602 0.090733 0.581844 0.071 Uiso 1 1 calc R U . . .
C25 C 0.71832(17) 0.5033(4) 0.56302(13) 0.0428(8) Uani 1 1 d . . . . .
H25 H 0.712178 0.481257 0.529673 0.051 Uiso 1 1 calc R U . . .
C26 C 0.6985(2) 0.6710(5) 0.56798(19) 0.0654(12) Uani 1 1 d . . . . .
H26A H 0.656506 0.682251 0.552911 0.098 Uiso 1 1 calc R U . . .
H26B H 0.722564 0.741736 0.553836 0.098 Uiso 1 1 calc R U . . .
H26C H 0.703777 0.696583 0.600376 0.098 Uiso 1 1 calc R U . . .
C27 C 0.78387(18) 0.4723(6) 0.58429(15) 0.0582(11) Uani 1 1 d . . . . .
H27A H 0.791399 0.491740 0.617161 0.087 Uiso 1 1 calc R U . . .
H27B H 0.808795 0.541416 0.570458 0.087 Uiso 1 1 calc R U . . .
H27C H 0.793402 0.363788 0.578873 0.087 Uiso 1 1 calc R U . . .
Br3 Br 0.500000 0.70164(10) 0.750000 0.0731(2) Uani 1 2 d S T P . .
Br2 Br 0.500000 0.000000 0.500000 0.0877(3) Uani 1 2 d S . 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
P1 C1 1.801(3) . ?
P1 C5 1.800(3) 5_666 ?
P1 C16 1.811(3) . ?
P1 C19 1.812(4) . ?
P2 C4 1.809(3) . ?
P2 C15 1.801(3) . ?
P2 C22 1.807(4) . ?
P2 C25 1.811(4) . ?
C1 C2 1.385(5) . ?
C1 C3 1.414(5) 5_666 ?
C2 H2 0.9500 . ?
C2 C3 1.393(5) . ?
C3 C4 1.466(4) . ?
C4 C5 1.357(4) . ?
C5 C6 1.461(4) . ?
C6 C7 1.366(5) . ?
C6 C15 1.436(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.427(5) . ?
C8 C9 1.405(5) . ?
C8 C13 1.432(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.376(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.415(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.355(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.416(5) . ?
C13 C14 1.422(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.364(5) . ?
C16 H16 1.0000 . ?
C16 C17 1.521(5) . ?
C16 C18 1.527(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19 1.0000 . ?
C19 C20 1.515(5) . ?
C19 C21 1.531(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C23 1.536(5) . ?
C22 C24 1.511(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25 1.0000 . ?
C25 C26 1.529(6) . ?
C25 C27 1.530(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?

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
C1 P1 C16 114.78(15) . . ?
C1 P1 C19 111.09(16) . . ?
C5 P1 C1 92.59(15) 5_666 . ?
C5 P1 C16 110.44(16) 5_666 . ?
C5 P1 C19 112.83(16) 5_666 . ?
C16 P1 C19 113.43(16) . . ?
C4 P2 C25 112.19(17) . . ?
C15 P2 C4 92.60(15) . . ?
C15 P2 C22 110.47(17) . . ?
C15 P2 C25 113.36(17) . . ?
C22 P2 C4 112.77(16) . . ?
C22 P2 C25 113.70(17) . . ?
C2 C1 P1 128.0(3) . . ?
C2 C1 C3 122.4(3) . 5_666 ?
C3 C1 P1 109.7(2) 5_666 . ?
C1 C2 H2 121.5 . . ?
C1 C2 C3 117.1(3) . . ?
C3 C2 H2 121.5 . . ?
C1 C3 C4 111.7(3) 5_666 . ?
C2 C3 C1 120.5(3) . 5_666 ?
C2 C3 C4 127.7(3) . . ?
C3 C4 P2 134.3(2) . . ?
C5 C4 P2 109.0(2) . . ?
C5 C4 C3 116.8(3) . . ?
C4 C5 P1 109.1(2) . 5_666 ?
C4 C5 C6 117.6(3) . . ?
C6 C5 P1 133.3(3) . 5_666 ?
C7 C6 C5 128.6(3) . . ?
C7 C6 C15 120.2(3) . . ?
C15 C6 C5 111.1(3) . . ?
C6 C7 H7 119.8 . . ?
C6 C7 C8 120.3(3) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 C13 118.7(3) . . ?
C9 C8 C7 122.1(4) . . ?
C9 C8 C13 119.2(3) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.3(4) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.9 . . ?
C9 C10 C11 120.2(4) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 H11 119.6 . . ?
C12 C11 C10 120.8(4) . . ?
C12 C11 H11 119.6 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.5(4) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 C8 118.9(3) . . ?
C12 C13 C14 121.2(3) . . ?
C14 C13 C8 119.9(3) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.6(3) . . ?
C15 C14 H14 120.2 . . ?
C6 C15 P2 109.7(2) . . ?
C14 C15 P2 129.3(3) . . ?
C14 C15 C6 121.0(3) . . ?
P1 C16 H16 107.4 . . ?
C17 C16 P1 111.2(2) . . ?
C17 C16 H16 107.4 . . ?
C17 C16 C18 111.8(3) . . ?
C18 C16 P1 111.5(2) . . ?
C18 C16 H16 107.4 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P1 C19 H19 107.3 . . ?
C20 C19 P1 112.6(3) . . ?
C20 C19 H19 107.3 . . ?
C20 C19 C21 111.6(4) . . ?
C21 C19 P1 110.5(3) . . ?
C21 C19 H19 107.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
P2 C22 H22 107.5 . . ?
C23 C22 P2 112.0(3) . . ?
C23 C22 H22 107.5 . . ?
C24 C22 P2 110.2(2) . . ?
C24 C22 H22 107.5 . . ?
C24 C22 C23 111.8(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
P2 C25 H25 107.3 . . ?
C26 C25 P2 110.2(3) . . ?
C26 C25 H25 107.3 . . ?
C26 C25 C27 114.3(4) . . ?
C27 C25 P2 110.1(3) . . ?
C27 C25 H25 107.3 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 C3 179.1(3) . . . . ?
P1 C5 C6 C7 -4.1(6) 5_666 . . . ?
P1 C5 C6 C15 177.7(3) 5_666 . . . ?
P2 C4 C5 P1 -177.35(17) . . . 5_666 ?
P2 C4 C5 C6 3.0(4) . . . . ?
C1 P1 C16 C17 64.7(3) . . . . ?
C1 P1 C16 C18 -60.9(3) . . . . ?
C1 P1 C19 C20 -164.5(3) . . . . ?
C1 P1 C19 C21 -38.9(3) . . . . ?
C1 C2 C3 C1 -0.8(6) . . . 5_666 ?
C1 C2 C3 C4 -179.9(3) . . . . ?
C1 C3 C4 P2 179.5(3) 5_666 . . . ?
C1 C3 C4 C5 -1.3(5) 5_666 . . . ?
C2 C3 C4 P2 -1.3(6) . . . . ?
C2 C3 C4 C5 177.9(3) . . . . ?
C3 C1 C2 C3 0.8(6) 5_666 . . . ?
C3 C4 C5 P1 3.2(4) . . . 5_666 ?
C3 C4 C5 C6 -176.4(3) . . . . ?
C4 P2 C15 C6 0.4(3) . . . . ?
C4 P2 C15 C14 178.2(4) . . . . ?
C4 P2 C22 C23 70.6(3) . . . . ?
C4 P2 C22 C24 -54.5(3) . . . . ?
C4 P2 C25 C26 36.4(4) . . . . ?
C4 P2 C25 C27 163.5(3) . . . . ?
C4 C5 C6 C7 175.4(4) . . . . ?
C4 C5 C6 C15 -2.8(5) . . . . ?
C5 P1 C1 C2 178.9(3) 5_666 . . . ?
C5 P1 C1 C3 -2.6(3) 5_666 . . 5_666 ?
C5 P1 C16 C17 -38.4(3) 5_666 . . . ?
C5 P1 C16 C18 -163.9(3) 5_666 . . . ?
C5 P1 C19 C20 -62.1(3) 5_666 . . . ?
C5 P1 C19 C21 63.5(3) 5_666 . . . ?
C5 C6 C7 C8 178.2(4) . . . . ?
C5 C6 C15 P2 1.1(4) . . . . ?
C5 C6 C15 C14 -176.9(3) . . . . ?
C6 C7 C8 C9 -178.6(4) . . . . ?
C6 C7 C8 C13 -0.2(6) . . . . ?
C7 C6 C15 P2 -177.3(3) . . . . ?
C7 C6 C15 C14 4.7(6) . . . . ?
C7 C8 C9 C10 177.0(4) . . . . ?
C7 C8 C13 C12 -177.4(4) . . . . ?
C7 C8 C13 C14 3.6(6) . . . . ?
C8 C9 C10 C11 -0.1(7) . . . . ?
C8 C13 C14 C15 -2.8(6) . . . . ?
C9 C8 C13 C12 1.0(6) . . . . ?
C9 C8 C13 C14 -178.0(4) . . . . ?
C9 C10 C11 C12 1.9(7) . . . . ?
C10 C11 C12 C13 -2.2(7) . . . . ?
C11 C12 C13 C8 0.8(6) . . . . ?
C11 C12 C13 C14 179.8(4) . . . . ?
C12 C13 C14 C15 178.3(4) . . . . ?
C13 C8 C9 C10 -1.3(6) . . . . ?
C13 C14 C15 P2 -178.9(3) . . . . ?
C13 C14 C15 C6 -1.3(6) . . . . ?
C15 P2 C4 C3 177.3(4) . . . . ?
C15 P2 C4 C5 -1.9(3) . . . . ?
C15 P2 C22 C23 172.7(2) . . . . ?
C15 P2 C22 C24 47.6(3) . . . . ?
C15 P2 C25 C26 -66.9(4) . . . . ?
C15 P2 C25 C27 60.2(3) . . . . ?
C15 C6 C7 C8 -3.8(6) . . . . ?
C16 P1 C1 C2 65.0(4) . . . . ?
C16 P1 C1 C3 -116.6(3) . . . 5_666 ?
C16 P1 C19 C20 64.5(3) . . . . ?
C16 P1 C19 C21 -169.9(3) . . . . ?
C19 P1 C1 C2 -65.4(4) . . . . ?
C19 P1 C1 C3 113.1(3) . . . 5_666 ?
C19 P1 C16 C17 -166.2(3) . . . . ?
C19 P1 C16 C18 68.3(3) . . . . ?
C22 P2 C4 C3 -69.2(4) . . . . ?
C22 P2 C4 C5 111.6(3) . . . . ?
C22 P2 C15 C6 -115.1(3) . . . . ?
C22 P2 C15 C14 62.7(4) . . . . ?
C22 P2 C25 C26 165.8(3) . . . . ?
C22 P2 C25 C27 -67.1(3) . . . . ?
C25 P2 C4 C3 60.8(4) . . . . ?
C25 P2 C4 C5 -118.5(3) . . . . ?
C25 P2 C15 C6 116.0(3) . . . . ?
C25 P2 C15 C14 -66.2(4) . . . . ?
C25 P2 C22 C23 -58.5(3) . . . . ?
C25 P2 C22 C24 176.3(2) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 136 electrons were 
found in a volume of 1368Å³ in 1 void per unit cell. 
This is consistent with the presence of 
2[CH4O] per Asymmetric Unit 
which account for 144 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.461 0.250 342.1 34.2 '2 MeOH'
2 0.000 0.539 0.750 342.1 34.4 '2 MeOH'
3 0.500 0.039 0.750 342.1 34.4 '2 MeOH'
4 0.500 0.961 0.250 342.1 34.2 '2 MeOH'

_smtbx_masks_void_probe_radius   1.1
_smtbx_masks_void_truncation_radius 1.8
_olex2_date_sample_data_collection 2025-05-03
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
# start Validation Reply Form
_vrf_FORMU01_ba_ss25             
;
PROBLEM:There is a discrepancy between the atom counts
RESPONSE: Disordered MeOH (1 equiv. per asymm. unit, 2 equiv per molecule) 
was treated with OLEX2 solvent masks. Hence, the moiety formula, sum formula, 
F000, mue and rho are expected to differ. See following G-alerts/G-infos.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_ba_ss23
_database_code_depnum_ccdc_archive 'CCDC 2525135'
loop_
_audit_author_name
_audit_author_address
'Joachim Ballmann'
;Heidelberg University
Germany
;
_audit_update_record             
;
2026-01-22 deposited with the CCDC.	2026-03-02 downloaded from the CCDC.
;
_audit_creation_date             2025-02-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
loop_
_audit_author_email
joachim.ballmann@uni-heidelberg.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(Br), C46 H66 P4, 8[H2O]'
_chemical_formula_sum            'C46 H82 Br4 O8 P4'
_chemical_formula_weight         1206.63
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         C46H80Br4O7P4
_chemical_oxdiff_usercomment     ss438
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_H-M_alt        'P 32 2 1'
_space_group_name_Hall           'P 32 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'

_cell_length_a                   12.4139(3)
_cell_length_b                   12.4139(3)
_cell_length_c                   32.4727(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4333.8(2)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    9492
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      69.6180
_cell_measurement_theta_min      4.0760
_shelx_estimated_absorpt_T_max   0.795
_shelx_estimated_absorpt_T_min   0.620
_exptl_absorpt_coefficient_mu    4.800
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.127a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1866
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 0 12 0.0393
-5 -2 -3 0.0071
-2 4 -19 0.0505
-5 4 16 0.0259
5 -8 5 0.0272
4 -2 -19 0.0197
-1 -4 15 0.0319
4 4 -4 0.0470
5 3 6 0.0373
0 6 12 0.0360

_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.6284 0.2690 11.8720 -0.4539 0.8329 0.3165
-5.4729 -2.2677 -3.3033 0.4704 -0.8652 0.1733
-1.6924 3.6317 -18.8209 0.0828 -0.1480 -0.9855
-4.7574 4.3823 15.8925 -0.7887 -0.4302 0.4391
4.7895 -7.7757 4.8120 0.6703 0.3632 0.6471
3.5183 -2.0798 -18.9366 0.6260 0.3423 -0.7007
-0.9143 -4.4911 14.6764 0.1791 -0.2634 0.9479
3.8208 4.1099 -3.7128 -0.4725 0.6880 -0.5508
4.9625 2.7030 5.5357 -0.5640 0.8194 -0.1024
-0.3566 5.9149 11.9669 -0.9711 0.2321 0.0554

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            33705
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.199
_diffrn_reflns_theta_min         4.084
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -29.00  12.00   1.00   10.00    --    0.00  77.00  90.00   41
  2  ω     34.00  70.00   1.00   10.00    --    0.00  77.00  90.00   36
  3  ω    -22.00   7.00   1.00   10.00    --   14.00 104.00 159.61   29
  4  ω    -25.00  17.00   1.00   10.00    --   14.00 102.00  18.08   42
  5  ω    -27.00  -2.00   1.00   10.00    --   18.00 109.00-124.46   25
  6  ω    -26.00   2.00   1.00   10.00    --   22.00 118.00-173.91   28
  7  ω      2.00  28.00   1.00   34.00    --   38.00  92.00-121.62   26
  8  ω     -1.00  27.00   1.00   34.00    --   38.00  93.00 120.36   28
  9  ω      0.00  26.00   1.00   34.00    --   38.00  92.00 -15.11   26
 10  ω     -1.00  26.00   1.00   34.00    --   38.00  93.00  74.94   27
 11  ω     29.00 124.00   1.00   34.00    --   54.34  38.00-180.00   95
 12  ω     27.00 124.00   1.00   34.00    --   54.34  77.00-120.00   97
 13  ω     40.00 123.00   1.00   34.00    --   54.34  57.00  30.00   83
 14  ω     40.00 112.00   1.00   34.00    --   54.34  57.00 -60.00   72
 15  ω    108.00 134.00   1.00   34.00    --   74.00 122.00 -36.87   26
 16  ω    102.00 151.00   1.00   54.00    --   82.00 118.00  96.41   49
 17  ω    102.00 130.00   1.00   54.00    --   82.00 119.00-149.98   28
 18  ω    116.00 155.00   1.00   54.00    --   90.00 137.00-106.58   39
 19  ω    100.00 139.00   1.00   54.00    --  102.00 116.00  -8.65   39
 20  ω    136.00 162.00   1.00   54.00    --  102.00 120.00  16.46   26
 21  ω     98.00 163.00   1.00   54.00    --  106.00 119.00-171.56   65
 22  ω    110.00 173.00   1.00   54.00    --  106.00 114.00  74.13   63
 23  ω    110.00 170.00   1.00   54.00    --  106.00 109.00 129.44   60
 24  ω     99.00 153.00   1.00   54.00    --  108.67 139.00-112.95   54
 25  ω    108.00 178.00   1.00   54.00    --  108.67  38.00-180.00   70
 26  ω    104.00 143.00   1.00   54.00    --  108.67 149.00 -59.41   39
 27  ω    108.00 177.00   1.00   54.00    --  108.67 143.00 -26.73   69
 28  ω    114.00 178.00   1.00   54.00    --  108.67 140.00 157.34   64
 29  ω    104.00 177.00   1.00   54.00    --  108.67 143.00  97.44   73
 30  ω    103.00 177.00   1.00   54.00    --  108.67 138.00-145.78   74
 31  ω    124.00 177.00   1.00   54.00    --  108.67 143.00 -87.30   53
 32  ω     83.00 162.00   1.00   54.00    --  108.67  38.00 -90.00   79
 33  ω    105.00 177.00   1.00   54.00    --  108.67 143.00  27.80   72
 34  ω     89.00 170.00   1.00   54.00    --  108.67  64.00 -60.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0231353000
_diffrn_orient_matrix_UB_12      -0.1157125000
_diffrn_orient_matrix_UB_13      -0.0246465000
_diffrn_orient_matrix_UB_21      0.1391321000
_diffrn_orient_matrix_UB_22      0.0410114000
_diffrn_orient_matrix_UB_23      0.0032687000
_diffrn_orient_matrix_UB_31      -0.0254349000
_diffrn_orient_matrix_UB_32      -0.0738897000
_diffrn_orient_matrix_UB_33      0.0403917000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.741
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                4892
_reflns_number_total             5564
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.358
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 
;
 Flack x determined using 1855 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         5564
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0499
_refine_ls_restrained_S_all      1.030
_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)+(0.0763P)²+3.9971P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1368
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Br1(0.5)
3.a Ternary CH refined with riding coordinates:
 C18(H18), C15(H15), C12(H12), C21(H21)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C5(H5), C2(H2), C4(H4), C3(H3)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C17(H17A,H17B,
 H17C), C22(H22A,H22B,H22C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C23(H23A,
 H23B,H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Br3 Br 0.52449(10) 0.52449(10) 0.500000 0.0459(3) Uani 1 2 d S T P . .
Br2 Br 0.93103(7) 0.44185(9) 0.47977(2) 0.0513(3) Uani 1 1 d . . . . .
P1 P 0.37045(16) 0.52049(17) 0.27646(5) 0.0311(3) Uani 1 1 d . . . . .
P2 P 0.22107(16) 0.45369(16) 0.39718(4) 0.0318(4) Uani 1 1 d . . . . .
Br1 Br 0.95871(19) 0.0119(2) 0.36707(6) 0.0666(5) Uani 0.5 1 d . . P A -1
C10 C 0.0392(6) 0.3555(7) 0.29135(18) 0.0323(14) Uani 1 1 d . . . . .
H10 H 0.064310 0.370693 0.263319 0.039 Uiso 1 1 calc R U . . .
C1 C 0.5034(6) 0.5894(6) 0.31033(19) 0.0317(13) Uani 1 1 d . . . . .
C11 C -0.0882(7) 0.2896(6) 0.30263(17) 0.0314(13) Uani 1 1 d . . . . .
C9 C 0.1256(6) 0.3969(6) 0.32309(18) 0.0301(13) Uani 1 1 d . . . . .
C5 C 0.5494(7) 0.6106(6) 0.38331(19) 0.0358(15) Uani 1 1 d . . . . .
H5 H 0.523241 0.598481 0.411255 0.043 Uiso 1 1 calc R U . . .
C2 C 0.6272(7) 0.6493(7) 0.3001(2) 0.0400(16) Uani 1 1 d . . . . .
H2 H 0.653806 0.659303 0.272213 0.048 Uiso 1 1 calc R U . . .
C6 C 0.4640(6) 0.5690(6) 0.35101(19) 0.0327(13) Uani 1 1 d . . . . .
C18 C 0.2402(7) 0.3482(7) 0.4308(2) 0.0397(16) Uani 1 1 d . . . . .
H18 H 0.315570 0.398451 0.448190 0.048 Uiso 1 1 calc R U . . .
C8 C 0.2616(6) 0.4658(6) 0.31886(18) 0.0308(13) Uani 1 1 d . . . . .
C15 C 0.3551(7) 0.6347(6) 0.24591(18) 0.0347(14) Uani 1 1 d . . . . .
H15 H 0.274832 0.590826 0.230389 0.042 Uiso 1 1 calc R U . . .
C12 C 0.3679(7) 0.3965(7) 0.2458(2) 0.0372(15) Uani 1 1 d . . . . .
H12 H 0.445148 0.433984 0.228648 0.045 Uiso 1 1 calc R U . . .
C7 C 0.3291(6) 0.5017(6) 0.35422(18) 0.0333(14) Uani 1 1 d . . . . .
C4 C 0.6757(7) 0.6712(7) 0.3726(2) 0.0408(16) Uani 1 1 d . . . . .
H4 H 0.737101 0.696580 0.393566 0.049 Uiso 1 1 calc R U . . .
C16 C 0.4631(7) 0.6915(8) 0.2144(2) 0.0432(17) Uani 1 1 d . . . . .
H16A H 0.542683 0.731316 0.229129 0.065 Uiso 1 1 calc R U . . .
H16B H 0.456611 0.753655 0.197631 0.065 Uiso 1 1 calc R U . . .
H16C H 0.458355 0.625651 0.196571 0.065 Uiso 1 1 calc R U . . .
C21 C 0.2233(7) 0.5854(7) 0.42256(19) 0.0401(16) Uani 1 1 d . . . . .
H21 H 0.155871 0.550464 0.443780 0.048 Uiso 1 1 calc R U . . .
C3 C 0.7112(7) 0.6941(8) 0.3321(2) 0.0482(19) Uani 1 1 d . . . . .
H3 H 0.797247 0.742917 0.325910 0.058 Uiso 1 1 calc R U . . .
C14 C 0.2554(8) 0.3361(8) 0.2163(2) 0.0483(18) Uani 1 1 d . . . . .
H14A H 0.179072 0.286521 0.232165 0.073 Uiso 1 1 calc R U . . .
H14B H 0.266366 0.282134 0.196720 0.073 Uiso 1 1 calc R U . . .
H14C H 0.249451 0.401230 0.201153 0.073 Uiso 1 1 calc R U . . .
C20 C 0.2607(8) 0.2582(8) 0.4065(2) 0.0476(19) Uani 1 1 d . . . . .
H20A H 0.192637 0.214951 0.386761 0.071 Uiso 1 1 calc R U . . .
H20B H 0.263283 0.197458 0.425155 0.071 Uiso 1 1 calc R U . . .
H20C H 0.339809 0.303090 0.391635 0.071 Uiso 1 1 calc R U . . .
C17 C 0.3515(9) 0.7314(8) 0.2738(2) 0.0492(18) Uani 1 1 d . . . . .
H17A H 0.277826 0.691015 0.291560 0.074 Uiso 1 1 calc R U . . .
H17B H 0.347836 0.794991 0.256972 0.074 Uiso 1 1 calc R U . . .
H17C H 0.426552 0.770570 0.290960 0.074 Uiso 1 1 calc R U . . .
C22 C 0.3474(8) 0.6640(8) 0.4459(2) 0.055(2) Uani 1 1 d . . . . .
H22A H 0.374233 0.608779 0.457910 0.082 Uiso 1 1 calc R U . . .
H22B H 0.335550 0.711156 0.467888 0.082 Uiso 1 1 calc R U . . .
H22C H 0.411034 0.721725 0.426702 0.082 Uiso 1 1 calc R U . . .
C13 C 0.3713(9) 0.3004(8) 0.2739(2) 0.0505(19) Uani 1 1 d . . . . .
H13A H 0.447591 0.340042 0.290445 0.076 Uiso 1 1 calc R U . . .
H13B H 0.369692 0.233761 0.257262 0.076 Uiso 1 1 calc R U . . .
H13C H 0.298832 0.265303 0.292232 0.076 Uiso 1 1 calc R U . . .
C19 C 0.1277(9) 0.2831(9) 0.4594(2) 0.055(2) Uani 1 1 d . . . . .
H19A H 0.115336 0.345618 0.473739 0.082 Uiso 1 1 calc R U . . .
H19B H 0.142172 0.233182 0.479657 0.082 Uiso 1 1 calc R U . . .
H19C H 0.053391 0.228885 0.443189 0.082 Uiso 1 1 calc R U . . .
C23 C 0.1928(14) 0.6583(10) 0.3936(3) 0.086(4) Uani 1 1 d . . . . .
H23A H 0.261027 0.701431 0.373889 0.129 Uiso 1 1 calc R U . . .
H23B H 0.180971 0.719547 0.408991 0.129 Uiso 1 1 calc R U . . .
H23C H 0.116132 0.602283 0.378727 0.129 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
P1 C1 1.803(7) . ?
P1 C8 1.807(6) . ?
P1 C15 1.817(7) . ?
P1 C12 1.820(7) . ?
P2 C11 1.792(7) 6 ?
P2 C18 1.810(7) . ?
P2 C7 1.817(7) . ?
P2 C21 1.819(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.418(10) . ?
C10 C9 1.387(9) . ?
C1 C2 1.373(10) . ?
C1 C6 1.387(8) . ?
C11 C9 1.389(8) 6 ?
C9 C8 1.469(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(9) . ?
C5 C4 1.402(10) . ?
C2 H2 0.9500 . ?
C2 C3 1.378(10) . ?
C6 C7 1.453(9) . ?
C18 H18 1.0000 . ?
C18 C20 1.490(11) . ?
C18 C19 1.529(10) . ?
C8 C7 1.359(9) . ?
C15 H15 1.0000 . ?
C15 C16 1.548(9) . ?
C15 C17 1.524(10) . ?
C12 H12 1.0000 . ?
C12 C14 1.544(11) . ?
C12 C13 1.520(10) . ?
C4 H4 0.9500 . ?
C4 C3 1.370(10) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 H21 1.0000 . ?
C21 C22 1.549(11) . ?
C21 C23 1.480(12) . ?
C3 H3 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

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
C1 P1 C8 92.8(3) . . ?
C1 P1 C15 113.0(3) . . ?
C1 P1 C12 111.1(3) . . ?
C8 P1 C15 111.0(3) . . ?
C8 P1 C12 113.9(3) . . ?
C15 P1 C12 113.4(3) . . ?
C11 P2 C18 113.6(3) 6 . ?
C11 P2 C7 92.6(3) 6 . ?
C11 P2 C21 109.9(3) 6 . ?
C18 P2 C7 111.0(3) . . ?
C18 P2 C21 115.4(3) . . ?
C7 P2 C21 112.1(3) . . ?
C11 C10 H10 121.5 . . ?
C9 C10 H10 121.5 . . ?
C9 C10 C11 117.0(5) . . ?
C2 C1 P1 128.3(5) . . ?
C2 C1 C6 121.8(6) . . ?
C6 C1 P1 109.8(5) . . ?
C10 C11 P2 127.8(4) . 6 ?
C9 C11 P2 110.1(5) 6 6 ?
C9 C11 C10 121.8(6) 6 . ?
C10 C9 C11 121.2(6) . 6 ?
C10 C9 C8 126.6(5) . . ?
C11 C9 C8 112.2(6) 6 . ?
C6 C5 H5 121.6 . . ?
C6 C5 C4 116.9(6) . . ?
C4 C5 H5 121.6 . . ?
C1 C2 H2 121.6 . . ?
C1 C2 C3 116.8(6) . . ?
C3 C2 H2 121.6 . . ?
C1 C6 C5 121.0(6) . . ?
C1 C6 C7 111.9(6) . . ?
C5 C6 C7 127.1(6) . . ?
P2 C18 H18 108.0 . . ?
C20 C18 P2 110.9(5) . . ?
C20 C18 H18 108.0 . . ?
C20 C18 C19 112.3(7) . . ?
C19 C18 P2 109.5(5) . . ?
C19 C18 H18 108.0 . . ?
C9 C8 P1 135.7(4) . . ?
C7 C8 P1 107.3(5) . . ?
C7 C8 C9 116.9(5) . . ?
P1 C15 H15 108.4 . . ?
C16 C15 P1 108.2(5) . . ?
C16 C15 H15 108.4 . . ?
C17 C15 P1 110.2(4) . . ?
C17 C15 H15 108.4 . . ?
C17 C15 C16 113.2(6) . . ?
P1 C12 H12 107.7 . . ?
C14 C12 P1 112.3(5) . . ?
C14 C12 H12 107.7 . . ?
C13 C12 P1 109.9(5) . . ?
C13 C12 H12 107.7 . . ?
C13 C12 C14 111.4(7) . . ?
C6 C7 P2 133.9(5) . . ?
C8 C7 P2 107.9(5) . . ?
C8 C7 C6 118.2(6) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 C5 120.4(7) . . ?
C3 C4 H4 119.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
P2 C21 H21 106.8 . . ?
C22 C21 P2 110.5(6) . . ?
C22 C21 H21 106.8 . . ?
C23 C21 P2 111.6(5) . . ?
C23 C21 H21 106.8 . . ?
C23 C21 C22 113.8(8) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 C2 122.8(7) . . ?
C4 C3 H3 118.6 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 C3 179.9(6) . . . . ?
P1 C1 C6 C5 178.4(5) . . . . ?
P1 C1 C6 C7 -1.5(7) . . . . ?
P1 C8 C7 P2 177.4(3) . . . . ?
P1 C8 C7 C6 -1.2(8) . . . . ?
C10 C9 C8 P1 -1.8(12) . . . . ?
C10 C9 C8 C7 177.5(7) . . . . ?
C1 P1 C8 C9 179.5(7) . . . . ?
C1 P1 C8 C7 0.2(5) . . . . ?
C1 P1 C15 C16 69.0(5) . . . . ?
C1 P1 C15 C17 -55.3(6) . . . . ?
C1 P1 C12 C14 -179.7(5) . . . . ?
C1 P1 C12 C13 55.7(6) . . . . ?
C1 C2 C3 C4 6.1(13) . . . . ?
C1 C6 C7 P2 -176.4(6) . . . . ?
C1 C6 C7 C8 1.8(9) . . . . ?
C11 P2 C18 C20 62.3(6) 6 . . . ?
C11 P2 C18 C19 -62.1(6) 6 . . . ?
C11 P2 C7 C6 -178.2(7) 6 . . . ?
C11 P2 C7 C8 3.4(6) 6 . . . ?
C11 P2 C21 C22 -171.2(5) 6 . . . ?
C11 P2 C21 C23 -43.4(8) 6 . . . ?
C11 C10 C9 C11 -2.1(9) . . . 6 ?
C11 C10 C9 C8 179.5(6) . . . . ?
C11 C9 C8 P1 179.7(6) 6 . . . ?
C11 C9 C8 C7 -1.1(9) 6 . . . ?
C9 C10 C11 P2 176.0(5) . . . 6 ?
C9 C10 C11 C9 2.6(9) . . . 6 ?
C9 C8 C7 P2 -2.0(8) . . . . ?
C9 C8 C7 C6 179.4(6) . . . . ?
C5 C6 C7 P2 3.8(11) . . . . ?
C5 C6 C7 C8 -178.0(7) . . . . ?
C5 C4 C3 C2 -6.5(13) . . . . ?
C2 C1 C6 C5 1.1(10) . . . . ?
C2 C1 C6 C7 -178.7(6) . . . . ?
C6 C1 C2 C3 -3.4(11) . . . . ?
C6 C5 C4 C3 3.9(11) . . . . ?
C18 P2 C7 C6 -61.7(8) . . . . ?
C18 P2 C7 C8 120.0(5) . . . . ?
C18 P2 C21 C22 58.7(6) . . . . ?
C18 P2 C21 C23 -173.5(7) . . . . ?
C8 P1 C1 C2 177.8(7) . . . . ?
C8 P1 C1 C6 0.7(5) . . . . ?
C8 P1 C15 C16 171.7(5) . . . . ?
C8 P1 C15 C17 47.4(6) . . . . ?
C8 P1 C12 C14 77.2(6) . . . . ?
C8 P1 C12 C13 -47.4(6) . . . . ?
C15 P1 C1 C2 -68.0(7) . . . . ?
C15 P1 C1 C6 115.0(5) . . . . ?
C15 P1 C8 C9 63.6(8) . . . . ?
C15 P1 C8 C7 -115.7(5) . . . . ?
C15 P1 C12 C14 -51.1(6) . . . . ?
C15 P1 C12 C13 -175.7(5) . . . . ?
C12 P1 C1 C2 60.8(7) . . . . ?
C12 P1 C1 C6 -116.3(5) . . . . ?
C12 P1 C8 C9 -65.9(8) . . . . ?
C12 P1 C8 C7 114.8(5) . . . . ?
C12 P1 C15 C16 -58.6(6) . . . . ?
C12 P1 C15 C17 177.2(5) . . . . ?
C7 P2 C18 C20 -40.5(6) . . . . ?
C7 P2 C18 C19 -164.9(5) . . . . ?
C7 P2 C21 C22 -69.7(6) . . . . ?
C7 P2 C21 C23 58.1(8) . . . . ?
C4 C5 C6 C1 -1.3(10) . . . . ?
C4 C5 C6 C7 178.5(7) . . . . ?
C21 P2 C18 C20 -169.4(5) . . . . ?
C21 P2 C18 C19 66.2(6) . . . . ?
C21 P2 C7 C6 69.0(8) . . . . ?
C21 P2 C7 C8 -109.3(6) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 231 electrons were 
found in a volume of 1039Å³ in 1 void per unit cell. 
This is consistent with the presence of 
8[H2O] per formula unit 
which account for 240 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.058 1039.2 230.6 '24 water'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.4
_olex2_date_sample_data_collection 2025-02-11
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
# start Validation Reply Form
_vrf_FORMU01_ba_ss23             
;
PROBLEM:There is a discrepancy between the atom counts
RESPONSE: Disordered water (4 molecules per asymmetric unit, 8 molecules per 
formual unit) was treated with OLEX2 solvent masks. Hence, the moiety formula, 
sum formula, F000, mue and rho are expected to differ. See following G-alerts/G-infos.
;
# end Validation Reply Form
