Selective White Phosphorus Activation and Functionalization with Inorganic Grignard Reagents
Gilch, Franziska; Brossette, Jan; Westermair, Franz F.; Silva, Wagner; Balázs, Gábor; Gschwind, Ruth M.; Zipse, Hendrik; Wolf, Robert; Chemical Science  (2026) –; doi:10.1039/D6SC01229A

data_1577051
_publ_section_title
;
 Selective White Phosphorus Activation and Functionalization with
 Inorganic Grignard Reagents
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D6SC01229A
_journal_year                    2026
_chemical_formula_moiety         '1.996(C74 H95.72 Fe2 Mg2 N4 O4)'
_chemical_formula_sum            'C147.72 H190.66 Fe4 Mg4 N8 O8'
_chemical_formula_weight         2526.98
_chemical_name_systematic        DepBDIMgFp*
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-15
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7308)
;
_audit_update_record
;
2026-02-09 deposited with the CCDC.	2026-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.1557(2)
_cell_length_b                   24.7875(2)
_cell_length_c                   23.36720(10)
_cell_measurement_reflns_used    66689
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      72.9130
_cell_measurement_theta_min      2.5400
_cell_volume                     13991.33(17)
_computing_cell_refinement       'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection
'CrysAlisPro system (CCD 43.91a 64-bit (release 29-09-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     35.00  66.00   0.50    0.63    --   62.92-112.00  88.00   62
  2  \w     35.00  63.00   0.50    0.63    --   73.03-112.00  88.00   56
  3  \w     58.00  93.00   0.50    0.63    --   75.56-112.00  88.00   70
  4  \w     35.00  82.00   0.50    0.63    --   73.03 -95.00  30.00   94
  5  \w     42.00  83.00   0.50    0.63    --   75.56 -95.00 -90.00   82
  6  \w     29.00 100.00   0.50    0.63    --   62.92   0.00 -30.00  142
  7  \w    -90.00 -24.00   0.50    0.63    --  -63.82 125.00 -90.00  132
  8  \w    -90.00 -65.00   0.50    0.63    --  -76.65 112.00-179.00   50
  9  \w    -92.00 -34.00   0.50    0.63    --  -73.46 112.00-179.00  116
 10  \w    -80.00 -25.00   0.50    0.63    --  -63.82 112.00-179.00  110
 11  \w    -76.00 -41.00   0.50    0.63    --  -76.65   0.00  60.00   70
 12  \w   -114.00 -83.00   0.50    0.63    --  -76.65   0.00  60.00   62
 13  \w   -118.00 -75.00   0.50    0.63    --  -76.65-125.00-120.00   86
 14  \w     56.00 120.00   0.50    0.05    --   75.56  15.00-120.00  128
 15  \w     25.00  70.00   0.50    0.05    --   62.92 -95.00 120.00   90
 16  \w     33.00 100.00   0.50    0.05    --   62.92   0.00 150.00  134
 17  \w     28.00  90.00   0.50    0.05    --   62.92   0.00 -90.00  124
 18  \w     27.00  71.00   0.50    0.05    --   62.92 -95.00 150.00   88
 19  \w     33.00  67.00   0.50    0.05    --   62.92 -95.00 -90.00   68
 20  \w    -82.00 -23.00   0.50    0.05    --  -64.13 125.00 120.00  118
 21  \w    -48.00 -22.00   0.50    0.05    --  -64.13 125.00   0.00   52
 22  \w    -90.00 -56.00   0.50    0.05    --  -64.13 125.00   0.00   68
 23  \w   -100.00 -33.00   0.50    0.05    --  -64.13   0.00-120.00  134
 24  \w     35.00  80.00   0.50    0.05    --   73.03 -95.00-180.00   90
 25  \w   -104.00 -75.00   0.50    0.05    --  -76.85-125.00-180.00   58
 26  \w   -103.00 -36.00   0.50    0.05    --  -76.85 125.00  60.00  134
 27  \w    -69.00 -36.00   0.50    0.05    --  -76.85 125.00 150.00   66
 28  \w   -122.00 -96.00   0.50    0.05    --  -76.85 -15.00 -30.00   52
 29  \w   -118.00 -73.00   0.50    0.05    --  -76.85-125.00   0.00   90
 30  \w   -103.00 -75.00   0.50    0.05    --  -76.85 125.00 150.00   56
 31  \w    -60.00 -35.00   0.50    0.05    --  -76.85 125.00-120.00   50
 32  \w   -118.00 -76.00   0.50    0.05    --  -76.85-125.00  60.00   84
 33  \w    -64.00 -38.00   0.50    0.05    --  -76.85 125.00  30.00   52
 34  \w   -102.00 -76.00   0.50    0.05    --  -76.85 125.00  30.00   52
 35  \w   -103.00 -78.00   0.50    0.05    --  -76.85 125.00-120.00   50
 36  \w    -88.00 -45.00   0.50    0.05    --  -76.85 -15.00 -30.00   86
 37  \w   -103.00 -40.00   0.50    0.05    --  -76.85 125.00 -60.00  126
 38  \w   -118.00 -73.00   0.50    0.05    --  -76.85-125.00 -30.00   90
 39  \w   -103.00 -36.00   0.50    0.05    --  -76.85 125.00  90.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0435180000
_diffrn_orient_matrix_UB_12      -0.0331289000
_diffrn_orient_matrix_UB_13      -0.0329679000
_diffrn_orient_matrix_UB_21      -0.0450051000
_diffrn_orient_matrix_UB_22      -0.0187803000
_diffrn_orient_matrix_UB_23      -0.0422718000
_diffrn_orient_matrix_UB_31      0.0121846000
_diffrn_orient_matrix_UB_32      0.0491037000
_diffrn_orient_matrix_UB_33      -0.0383917000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            205165
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.499
_diffrn_reflns_theta_min         2.554
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.878
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.36a (Rigaku Oxford Diffraction, 2022)
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_crystal_colour            'clear yellowish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       block
_exptl_crystal_F_000             5396
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 8579 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0037(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1849
_refine_ls_number_reflns         27115
_refine_ls_number_restraints     702
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0374
_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/[\s^2^(Fo^2^)+(0.0508P)^2^+1.6497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                23142
_reflns_number_total             27115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc01229a2.cif
_cod_data_source_block           fg112_pca21
_cod_database_code               1577051
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C148H188Fe4Mg4N8O8
_shelx_estimated_absorpt_t_max   0.675
_shelx_estimated_absorpt_t_min   0.336
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H04R,H04S,H04T} of C04D, All C(H,H) groups
 At 1.5 times of:
  {H04D,H04E,H04F} of C043, {H22,HS,HT} of C03X, {H25,HV,HW} of C040, {H04A,
  H04B,H04C} of C042, {H26,HX,HY} of C044, {H27,HZ,H35} of C047, {H04I,H04J,
  H04K} of C046, {H04L,H04M,H04N} of C04A, {H21,HQ,HR} of C03W, {H01L,H01M,
  H01N} of C01P, {H01C,H01D,H01E} of C01W, {H01O,H01P,H01Q} of C01X, {H01R,H01S,
  H01T} of C01Y, {H02A,H02B,H02C} of C024, {H02D,H02E,H02F} of C029, {H02G,H02H,
  H02I} of C02B, {H02J,H02K,H02L} of C02E, {H4,HA,HB} of C02G, {H02R,H02S,H02T}
  of C02J, {H02O,H02P,H02Q} of C02I, {H02W,H02X,H02Y} of C02N, {H01F,H01G,H01H}
  of C01F, {H01I,H01J,H01K} of C01L, {H03I,H03J,H03K} of C03J, {H03L,H03M,H03N}
  of C03K, {H14,HL,HM} of C036, {H18,HN,HO} of C03O, {H03S,H03T,H03U} of C03R,
  {H8,HC,HD} of C02Q, {H13,HF,HG} of C02Z, {H03A,H03B,H03C} of C030, {H03Y,HH,
  HI} of C031, {H1BA,H1BB,H1BC} of C1B, {H1DA,H1DB,H1DC} of C1D, {H3,H53,H54}
  of C04T, {H35A,H35B,H35C} of C35, {H31A,H31B,H31C} of C31, {H32A,H32B,H32C}
  of C32, {H36A,H36B,H36C} of C36, {H34A,H34B,H34C} of C34, {H1FA,H1FB,H1FC} of
  C1F, {H28A,H28B,H28C} of C28, {H26A,H26B,H26C} of C26, {H04O,H04P,H04Q} of
  C04C, {H30,H36,H37} of C04F, {H04Z,H42,H43} of C04M, {H04U,H04V,H04W} of C04K,
   {H04X,H04Y,H41} of C04L, {H32,H39,H40} of C04J, {H33,H44,H45} of C04N, {H1,
  H47,H48} of C04P, {H34,H49,H50} of C04Q, {H2,H51,H52} of C04S, {H39A,H39B,
  H39C} of C39, {H25A,H25B,H25C} of C25, {H22A,H22B,H22C} of C22, {H1AA,H1AB,
  H1AC} of C1A
2. Restrained distances
 C014-C016 \\sim C24-C27
 with sigma of 0.02
 C014-C019 \\sim C24-C0
 with sigma of 0.02
 C014-C040 \\sim C24-C26
 with sigma of 0.02
 C016-C02O \\sim C27-C21
 with sigma of 0.02
 C016-C044 \\sim C27-C28
 with sigma of 0.02
 C019-C03P \\sim C0-C23
 with sigma of 0.02
 C019-C047 \\sim C0-C25
 with sigma of 0.02
 C02O-C03P \\sim C21-C23
 with sigma of 0.02
 C02O-C39 \\sim C21-C1A
 with sigma of 0.02
 C03P-C04N \\sim C23-C22
 with sigma of 0.02
 Fe2-C014 \\sim Fe2-C24
 with sigma of 0.04
 Fe2-C016 \\sim Fe2-C27
 with sigma of 0.04
 Fe2-C019 \\sim Fe2-C0
 with sigma of 0.04
 Fe2-C02O \\sim Fe2-C21
 with sigma of 0.04
 Fe2-C03P \\sim Fe2-C23
 with sigma of 0.04
 Fe2-C040 \\sim Fe2-C26
 with sigma of 0.04
 Fe2-C044 \\sim Fe2-C28
 with sigma of 0.04
 Fe2-C047 \\sim Fe2-C25
 with sigma of 0.04
 Fe2-C04N \\sim Fe2-C22
 with sigma of 0.04
 Fe2-C39 \\sim Fe2-C1A
 with sigma of 0.04
 C014-C02O \\sim C24-C21
 with sigma of 0.04
 C014-C03P \\sim C24-C23
 with sigma of 0.04
 C014-C044 \\sim C24-C28
 with sigma of 0.04
 C014-C047 \\sim C24-C25
 with sigma of 0.04
 C016-C019 \\sim C27-C0
 with sigma of 0.04
 C016-C03P \\sim C27-C23
 with sigma of 0.04
 C016-C040 \\sim C27-C26
 with sigma of 0.04
 C016-C39 \\sim C27-C1A
 with sigma of 0.04
 C019-C02O \\sim C0-C21
 with sigma of 0.04
 C019-C040 \\sim C0-C26
 with sigma of 0.04
 C019-C04N \\sim C0-C22
 with sigma of 0.04
 C02O-C044 \\sim C21-C28
 with sigma of 0.04
 C02O-C04N \\sim C21-C22
 with sigma of 0.04
 C03P-C047 \\sim C23-C25
 with sigma of 0.04
 C03P-C39 \\sim C23-C1A
 with sigma of 0.04
 C04O-C04S \\sim C04O-C04T
 with sigma of 0.02
 C02W-C04O \\sim C02W-C29
 with sigma of 0.02
 C04O-C04S \\sim C29-C04S
 with sigma of 0.02
 C04O-C04T \\sim C29-C04T
 with sigma of 0.02
 C03C-C04I \\sim C03C-C33
 with sigma of 0.02
 C04I-C04Q \\sim C33-C32
 with sigma of 0.02
 C03C-C04Q \\sim C03C-C32
 with sigma of 0.04
 Mg4-O8 \\sim Mg4-O01E
 with sigma of 0.02
 O8-C13 \\sim O01E-C13
 with sigma of 0.02
 C01J-C01M \\sim C1C-C1E
 with sigma of 0.02
 C01J-C03E \\sim C1C-C38
 with sigma of 0.02
 C01J-C04A \\sim C1C-C1D
 with sigma of 0.02
 C01M-C02F \\sim C1E-C1G
 with sigma of 0.02
 C01M-C042 \\sim C1E-C1F
 with sigma of 0.02
 C02F-C03B \\sim C1G-C37
 with sigma of 0.02
 C02F-C04L \\sim C1G-C35
 with sigma of 0.02
 C03B-C03E \\sim C37-C38
 with sigma of 0.02
 C03B-C04M \\sim C37-C36
 with sigma of 0.02
 C03E-C04K \\sim C38-C1B
 with sigma of 0.02
 Fe4-C01J \\sim Fe4-C1C
 with sigma of 0.04
 Fe4-C01M \\sim Fe4-C1E
 with sigma of 0.04
 Fe4-C02F \\sim Fe4-C1G
 with sigma of 0.04
 Fe4-C03B \\sim Fe4-C37
 with sigma of 0.04
 Fe4-C03E \\sim Fe4-C38
 with sigma of 0.04
 Fe4-C042 \\sim Fe4-C1F
 with sigma of 0.04
 Fe4-C04A \\sim Fe4-C1D
 with sigma of 0.04
 Fe4-C04K \\sim Fe4-C1B
 with sigma of 0.04
 Fe4-C04L \\sim Fe4-C35
 with sigma of 0.04
 Fe4-C04M \\sim Fe4-C36
 with sigma of 0.04
 C01J-C02F \\sim C1C-C1G
 with sigma of 0.04
 C01J-C03B \\sim C1C-C37
 with sigma of 0.04
 C01J-C042 \\sim C1C-C1F
 with sigma of 0.04
 C01J-C04K \\sim C1C-C1B
 with sigma of 0.04
 C01M-C03B \\sim C1E-C37
 with sigma of 0.04
 C01M-C03E \\sim C1E-C38
 with sigma of 0.04
 C01M-C04A \\sim C1E-C1D
 with sigma of 0.04
 C01M-C04L \\sim C1E-C35
 with sigma of 0.04
 C02F-C03E \\sim C1G-C38
 with sigma of 0.04
 C02F-C042 \\sim C1G-C1F
 with sigma of 0.04
 C02F-C04M \\sim C1G-C36
 with sigma of 0.04
 C03B-C04K \\sim C37-C1B
 with sigma of 0.04
 C03B-C04L \\sim C37-C35
 with sigma of 0.04
 C03E-C04A \\sim C38-C1D
 with sigma of 0.04
 C03E-C04M \\sim C38-C36
 with sigma of 0.04
 C04D-C04P \\sim C04D-C34
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C04S \\sim C04O \\sim C02W \\sim C03V \\sim C02K \\sim C03D \\sim C02X \\sim
C03G \\sim C03R \\sim C01U: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C04L \\sim C02F \\sim C04M \\sim C03B \\sim C03E \\sim C04K \\sim C01J \\sim
C04A \\sim C01M \\sim C042: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C03Y \\sim C048 \\sim C041 \\sim C04E \\sim C03H \\sim C028 \\sim C03U \\sim
C04J: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
C014 \\sim C016 \\sim C019 \\sim C02O \\sim C03P \\sim C040 \\sim C044 \\sim
C047 \\sim C04N \\sim C39 \\sim C21 \\sim C1A \\sim C22 \\sim C23 \\sim C0
\\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
C02W \\sim C01U \\sim C02X \\sim C03G \\sim C03R \\sim C03D \\sim C02K \\sim
C03V \\sim C04O \\sim C04S: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
C04S \\sim C04O \\sim C02W: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C36 \\sim C04M \\sim C37 \\sim C1G \\sim C35 \\sim C1E \\sim C04L \\sim C1F
\\sim C042 \\sim C38 \\sim C04K \\sim C1B \\sim C1D \\sim C04A \\sim C1C \\sim
C01J: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within
2A
C03Y \\sim C30 \\sim C31: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
C31 \\sim C30 \\sim C03Y: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
4. Others
 Sof(C21)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C23)=Sof(C0)=Sof(C24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=1-FVAR(1)
 Sof(C014)=Sof(C016)=Sof(C019)=Sof(C02O)=Sof(C03P)=Sof(C040)=Sof(H25)=Sof(HV)=
 Sof(HW)=Sof(C044)=Sof(H26)=Sof(HX)=Sof(HY)=Sof(C047)=Sof(H27)=Sof(HZ)=Sof(H35)=
 Sof(C04N)=Sof(H33)=Sof(H44)=Sof(H45)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 FVAR(1)
 Sof(C04T)=Sof(H3)=Sof(H53)=Sof(H54)=1-FVAR(2)
 Sof(C04S)=Sof(H2)=Sof(H51)=Sof(H52)=FVAR(2)
 Sof(C29)=Sof(H29A)=Sof(H29B)=1-FVAR(3)
 Sof(C04O)=Sof(H04)=Sof(H46)=FVAR(3)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=1-FVAR(4)
 Sof(C04I)=Sof(H31)=Sof(H38)=Sof(C04Q)=Sof(H34)=Sof(H49)=Sof(H50)=FVAR(4)
 Sof(H23)=1-FVAR(5)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C30)=Sof(H30A)=Sof(H30B)=FVAR(5)
 Sof(H20)=Sof(HP)=Sof(C04J)=Sof(H32)=Sof(H39)=Sof(H40)=FVAR(6)
 Sof(O01E)=1-FVAR(7)
 Sof(O8)=FVAR(7)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C37)=Sof(C38)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C1C)=Sof(C1D)=
 Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=Sof(C1E)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(H1FC)=
 Sof(C1G)=1-FVAR(8)
 Sof(C01J)=Sof(C01M)=Sof(C02F)=Sof(C03B)=Sof(C03E)=Sof(C042)=Sof(H04A)=
 Sof(H04B)=Sof(H04C)=Sof(C04A)=Sof(H04L)=Sof(H04M)=Sof(H04N)=Sof(C04K)=
 Sof(H04U)=Sof(H04V)=Sof(H04W)=Sof(C04L)=Sof(H04X)=Sof(H04Y)=Sof(H41)=Sof(C04M)=
 Sof(H04Z)=Sof(H42)=Sof(H43)=FVAR(8)
 Sof(H04T)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=1-FVAR(9)
 Sof(H04R)=Sof(H04S)=Sof(C04P)=Sof(H1)=Sof(H47)=Sof(H48)=FVAR(9)
5.a Secondary CH2 refined with riding coordinates:
 C01Q(H01A,H01B), C020(H02Z,H), C02H(H02M,H02N), C02R(H10,HE), C032(H03Z,HJ),
 C033(H03,HK), C03G(H03E,H03F), C03I(H03G,H03H), C03Q(H03Q,H03R), C03U(H20,HP),
 C03Z(H24,HU), C045(H04G,H04H), C04D(H04R,H04S), C04I(H31,H38), C04O(H04,H46),
 C29(H29A,H29B), C33(H33A,H33B), C30(H30A,H30B)
5.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C010(H010), C6(H6), C9(H9), C027(H027), C16(H16), C02D(H02),
 C02K(H02U), C02L(H02V), C02M(H5), C02P(H7), C02S(H11), C02V(H12), C037(H037),
 C038(H038), C03A(H15), C03D(H03D), C03L(H03O), C03M(H17), C03N(H03P),
 C03S(H03V), C03T(H03W), C03V(H03X), C03Y(H23), C041(H041), C048(H048),
 C049(H049), C04B(H28), C04D(H04T), C04E(H29)
5.c Idealised Me refined as rotating group:
 C01F(H01F,H01G,H01H), C01L(H01I,H01J,H01K), C01P(H01L,H01M,H01N), C01W(H01C,
 H01D,H01E), C01X(H01O,H01P,H01Q), C01Y(H01R,H01S,H01T), C024(H02A,H02B,H02C),
 C029(H02D,H02E,H02F), C02B(H02G,H02H,H02I), C02E(H02J,H02K,H02L), C02G(H4,HA,
 HB), C02I(H02O,H02P,H02Q), C02J(H02R,H02S,H02T), C02N(H02W,H02X,H02Y), C02Q(H8,
 HC,HD), C02Z(H13,HF,HG), C030(H03A,H03B,H03C), C031(H03Y,HH,HI), C036(H14,HL,
 HM), C03J(H03I,H03J,H03K), C03K(H03L,H03M,H03N), C03O(H18,HN,HO), C03R(H03S,
 H03T,H03U), C03W(H21,HQ,HR), C03X(H22,HS,HT), C040(H25,HV,HW), C042(H04A,H04B,
 H04C), C043(H04D,H04E,H04F), C044(H26,HX,HY), C046(H04I,H04J,H04K), C047(H27,
 HZ,H35), C04A(H04L,H04M,H04N), C04C(H04O,H04P,H04Q), C04F(H30,H36,H37),
 C04J(H32,H39,H40), C04K(H04U,H04V,H04W), C04L(H04X,H04Y,H41), C04M(H04Z,H42,
 H43), C04N(H33,H44,H45), C04P(H1,H47,H48), C04Q(H34,H49,H50), C04S(H2,H51,H52),
  C39(H39A,H39B,H39C), C1A(H1AA,H1AB,H1AC), C22(H22A,H22B,H22C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C04T(H3,H53,H54), C32(H32A,
 H32B,H32C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C1B(H1BA,H1BB,H1BC), C1D(H1DA,H1DB,H1DC), C1F(H1FA,H1FB,H1FC), C34(H34A,H34B,
 H34C)
;
_shelx_res_checksum              51563
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.661
_oxdiff_exptl_absorpt_empirical_full_min 0.675