Trends in benzene inverse sandwich complexes of the alkaline-earth metals Mg, Ca, Sr and Ba.
Jędrzkiewicz, Dawid; Morasch, Michael; Townrow, Oliver P. E.; Rösch, Bastian; Langer, Jens; Mathe, Zachary; Harder, Sjoerd; Chemical science 16 (2025) 17793–17802; doi:10.1039/d5sc05373k

data_1575569
_publ_section_title
;
 Trends in benzene inverse sandwich complexes of the alkaline-earth metals
 Mg, Ca, Sr and Ba.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              17793
_journal_page_last               17802
_journal_paper_doi               10.1039/d5sc05373k
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C172 H276 K4 N8'
_chemical_formula_sum            'C172 H276 K4 N8'
_chemical_formula_weight         2612.39
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-03-28 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                70.6596(17)
_cell_angle_beta                 73.3726(16)
_cell_angle_gamma                85.7978(15)
_cell_formula_units_Z            2
_cell_length_a                   18.0046(3)
_cell_length_b                   19.7746(4)
_cell_length_c                   27.2387(5)
_cell_measurement_reflns_used    43804
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.6540
_cell_measurement_theta_min      3.4850
_cell_volume                     8765.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.971
_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    -70.00  32.00   1.00    6.00    --  -41.44  57.00-180.00  102
  2  \w    -74.00  35.00   1.00    6.00    --  -41.44  77.00  30.00  109
  3  \w   -114.00 -13.00   1.00    6.00    --  -41.44 -57.00 -90.00  101
  4  \w      9.00  42.00   1.00    6.00    --   41.44  76.00-114.38   33
  5  \w     28.00 137.00   1.00   24.00    --  104.37 -77.00 -30.00  109
  6  \w     31.00 112.00   1.00   24.00    --  104.37-125.00-180.00   81
  7  \w     31.00 112.00   1.00   24.00    --  104.37-125.00   0.00   81
  8  \w     79.00 177.00   1.00   24.00    --  104.37  45.00 -60.00   98
  9  \w    103.00 178.00   1.00   24.00    --  104.37  77.00 150.00   75
 10  \w     76.00 178.00   1.00   24.00    --  104.37  30.00-120.00  102
 11  \w     32.00 133.00   1.00   24.00    --  104.37 -61.00 150.00  101
 12  \w     22.00 106.00   1.00   24.00    --  104.37 -94.00-120.00   84
 13  \w     31.00 130.00   1.00   24.00    --  104.37 -45.00   0.00   99
 14  \w   -114.00 -13.00   1.00    6.00    --  -41.44 -57.00  60.00  101
 15  \w      9.00  42.00   1.00    6.00    --   41.44  76.00  52.42   33
 16  \w      8.00  42.00   1.00    6.00    --   41.44  79.00-177.15   34
 17  \w     75.00 177.00   1.00   24.00    --  104.37  61.00 -30.00  102
 18  \w     79.00 177.00   1.00   24.00    --  104.37  45.00 150.00   98
 19  \w     75.00 177.00   1.00   24.00    --  104.37  61.00  90.00  102
 20  \w     52.00 178.00   1.00   24.00    --  104.37  15.00  90.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0082601000
_diffrn_orient_matrix_UB_12      0.0583017000
_diffrn_orient_matrix_UB_13      -0.0520345000
_diffrn_orient_matrix_UB_21      0.0883336000
_diffrn_orient_matrix_UB_22      0.0141089000
_diffrn_orient_matrix_UB_23      -0.0190541000
_diffrn_orient_matrix_UB_31      0.0103817000
_diffrn_orient_matrix_UB_32      -0.0567696000
_diffrn_orient_matrix_UB_33      -0.0287023000
_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  0.0316
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            98411
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.804
_diffrn_reflns_theta_min         3.402
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.246
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.990
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2437
_refine_ls_number_reflns         33930
_refine_ls_number_restraints     9244
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0874P)^2^+3.5074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28206
_reflns_number_total             33930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05373k2.cif
_cod_data_source_block           hasj190821a
_cod_depositor_comments
'Adding full bibliography for 1575569--1575577.cif.'
_cod_database_code               1575569
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C49H75KN2
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.799
_diffrn_oxdiff_digest_hkl
;
013bed2bcea97e8d7fec0b5a68614885ccc363
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C198-C194
 2.55 with sigma of 0.005
 N5A-C87 \\sim N5-C87
 with sigma of 0.02
 N5A-C204 \\sim N5-C98 \\sim N7-C141 \\sim N7-C227 \\sim N4-C71 \\sim N4-C188
 with sigma of 0.02
 C204-C209 \\sim C98-C103 \\sim C99-C98 \\sim C205-C204 \\sim C76-C71 \\sim
C189-C188 \\sim C193-C188
 \\sim C72-C71 \\sim C142-C141 \\sim C228-C227 \\sim C232-C227 \\sim C146-C141
 with sigma of 0.02
 C208-C209 \\sim C103-C102 \\sim C205-C206 \\sim C99-C100 \\sim C76-C75 \\sim
C189-C190 \\sim C192-
 C193 \\sim C73-C72 \\sim C228-C229 \\sim C143-C142 \\sim C231-C232 \\sim
C146-C145
 with sigma of 0.02
 C102-C101 \\sim C207-C208 \\sim C207-C206 \\sim C101-C100 \\sim C74-C73 \\sim
C191-C192 \\sim C75-C74
 \\sim C190-C191 \\sim C229-C230 \\sim C144-C143 \\sim C230-C231 \\sim C145-C144
 with sigma of 0.02
 C109-C103 \\sim C213-C209 \\sim C205-C210 \\sim C99-C104 \\sim C77-C72 \\sim
C199-C193 \\sim C82-C76
 \\sim C194-C189 \\sim C178-C29 \\sim C34-C29 \\sim C61-C56 \\sim C56-C183
\\sim C173-C13 \\sim C18-C13 ~
 C233-C228 \\sim C147-C142 \\sim C152-C146 \\sim C238-C232 \\sim C218-C115
\\sim C120-C115 \\sim C168-
 C162 \\sim C243-C162
 with sigma of 0.02
 C171-C168 \\sim C243-C244 \\sim C169-C168 \\sim C243-C246 \\sim C236-C233
\\sim C148-C147 \\sim C234-
 C233 \\sim C150-C147 \\sim C241-C238 \\sim C153-C152 \\sim C155-C152 \\sim
C239-C238 \\sim C123-C120 ~
 C218-C221 \\sim C121-C120 \\sim C218-C219 \\sim C210-C105 \\sim C105-C104
\\sim C107-C104 \\sim C210-
 C211 \\sim C112-C109 \\sim C213-C216 \\sim C110-C109 \\sim C214-C213 \\sim
C197-C194 \\sim C85-C82 ~
 C195-C194 \\sim C83-C82 \\sim C200-C199 \\sim C78-C77 \\sim C202-C199 \\sim
C80-C77 \\sim C173-C174 ~
 C19-C18 \\sim C21-C18 \\sim C176-C173 \\sim C128-C125 \\sim C225-C125 \\sim
C223-C125 \\sim C126-C125
 \\sim C62-C61 \\sim C184-C183 \\sim C64-C61 \\sim C186-C183 \\sim C35-C34
\\sim C181-C178 \\sim C178-C179
 \\sim C37-C34
 with sigma of 0.02
 C36-C35 \\sim C182-C181 \\sim C180-C179 \\sim C38-C37 \\sim C175-C174 \\sim
C20-C19 \\sim C176-C177 ~
 C22-C21 \\sim C245-C244 \\sim C172-C171 \\sim C246-C247 \\sim C170-C169 \\sim
C237-C236 \\sim C149-
 C148 \\sim C151-C150 \\sim C235-C234 \\sim C240-C239 \\sim C156-C155 \\sim
C242-C241 \\sim C154-C153 ~
 C124-C123 \\sim C222-C221 \\sim C220-C219 \\sim C122-C121 \\sim C129-C128
\\sim C226-C225 \\sim C127-
 C126 \\sim C224-C223 \\sim C113-C112 \\sim C217-C216 \\sim C215-C214 \\sim
C111-C110 \\sim C212-C211 ~
 C108-C107 \\sim C203-C202 \\sim C81-C80 \\sim C201-C200 \\sim C79-C78 \\sim
C84-C83 \\sim C196-C195 ~
 C198-C197 \\sim C86-C85 \\sim C187-C186 \\sim C65-C64 \\sim C185-C184 \\sim
C63-C62
 with sigma of 0.02
 C198-C194 \\sim C194-C196 \\sim C86-C82 \\sim C82-C84
 with sigma of 0.01
 C197-C83 \\sim C85-C195
 with sigma of 0.01
 C197-C189 \\sim C189-C195
 with sigma of 0.01
 C111-C109 \\sim C109-C113 \\sim C215-C213 \\sim C213-C217
 with sigma of 0.01
 C216-C214 \\sim C112-C110
 with sigma of 0.01
3. Restrained planarity
 C204, C205, C206, C207, C208, C209
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C13 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C173 \\sim C174
\\sim C175 \\sim C176 \\sim C177: within 4A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 4A
C162 \\sim C168 \\sim C169 \\sim C170 \\sim C171 \\sim C172 \\sim C243 \\sim
C244 \\sim C245 \\sim C246 \\sim C247: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C125 \\sim C126 \\sim C127 \\sim C128 \\sim C129 \\sim C223 \\sim C224 \\sim
C225 \\sim C226: within 3A with sigma of 0.03 and sigma for terminal atoms of
0.06 within 3A
N7 \\sim C141 \\sim C142 \\sim C143 \\sim C144 \\sim C145 \\sim C146 \\sim C147
\\sim C148 \\sim C149 \\sim C150 \\sim C151 \\sim C152 \\sim C153 \\sim C154
\\sim C155 \\sim C156 \\sim C227 \\sim C228 \\sim C229 \\sim C230 \\sim C231
\\sim C232 \\sim C233 \\sim C234 \\sim C235 \\sim C236 \\sim C237 \\sim C238
\\sim C239 \\sim C240 \\sim C241 \\sim C242: within 4A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 4A
N4 \\sim C87 \\sim K3 \\sim N5 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim
C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim
C83 \\sim C84 \\sim C85 \\sim C86 \\sim C98 \\sim C99 \\sim C100 \\sim C101
\\sim C102 \\sim C103 \\sim C104 \\sim C107 \\sim C108 \\sim C109 \\sim C110
\\sim C111 \\sim C112 \\sim C113 \\sim K3A \\sim N5A \\sim C188 \\sim C189
\\sim C190 \\sim C191 \\sim C192 \\sim C193 \\sim C194 \\sim C195 \\sim C196
\\sim C197 \\sim C198 \\sim C199 \\sim C200 \\sim C201 \\sim C202 \\sim C203
\\sim C204 \\sim C205 \\sim C206 \\sim C207 \\sim C208 \\sim C209 \\sim C210
\\sim C211 \\sim C212 \\sim C213 \\sim C214 \\sim C215 \\sim C216 \\sim C217:
within 4A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 4A
C56 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C183 \\sim C184
\\sim C185 \\sim C186 \\sim C187: within 3A with sigma of 0.03 and sigma for
terminal atoms of 0.06 within 3A
C115 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C218 \\sim
C219 \\sim C220 \\sim C221 \\sim C222: within 4A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 4A
5. Rigid body (RIGU) restrains
 C194, C197, C198
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C214, C215
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C110, C111
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C227, C228, C229, C233, C234, C235, C236, C237
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C173)=Sof(H173)=Sof(C174)=Sof(H17i)=Sof(H17j)=Sof(C175)=Sof(H17k)=
 Sof(H17l)=Sof(H17m)=Sof(C176)=Sof(H17s)=Sof(H17t)=Sof(C177)=Sof(H17n)=
 Sof(H17o)=Sof(H17p)=1-FVAR(1)
 Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19a)=Sof(H19b)=Sof(C20)=Sof(H20a)=Sof(H20b)=
 Sof(H20c)=Sof(C21)=Sof(H21a)=Sof(H21b)=Sof(C22)=Sof(H22a)=Sof(H22b)=Sof(H22c)=
 FVAR(1)
 Sof(C178)=Sof(H178)=Sof(C179)=Sof(H17q)=Sof(H17r)=Sof(C180)=Sof(H18a)=
 Sof(H18b)=Sof(H18c)=Sof(C181)=Sof(H18o)=Sof(H18n)=Sof(C182)=Sof(H18p)=
 Sof(H18q)=Sof(H18r)=1-FVAR(2)
 Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35b)=Sof(H35a)=Sof(C36)=Sof(H36a)=Sof(H36b)=
 Sof(H36c)=Sof(C37)=Sof(H37a)=Sof(H37b)=Sof(C38)=Sof(H38a)=Sof(H38b)=Sof(H38c)=
 FVAR(2)
 Sof(C243)=Sof(H243)=Sof(C244)=Sof(H24k)=Sof(H24l)=Sof(C245)=Sof(H24m)=
 Sof(H24n)=Sof(H24o)=Sof(C246)=Sof(H24p)=Sof(H24q)=Sof(C247)=Sof(H24r)=
 Sof(H24s)=Sof(H24t)=1-FVAR(3)
 Sof(C168)=Sof(H168)=Sof(C169)=Sof(H16k)=Sof(H16l)=Sof(C170)=Sof(H17a)=
 Sof(H17b)=Sof(H17c)=Sof(C171)=Sof(H17e)=Sof(H17d)=Sof(C172)=Sof(H17f)=
 Sof(H17g)=Sof(H17h)=FVAR(3)
 Sof(H12f)=Sof(C223)=Sof(H22d)=Sof(H22e)=Sof(C224)=Sof(H22f)=Sof(H22g)=
 Sof(H22h)=Sof(C225)=Sof(H22i)=Sof(H22j)=Sof(C226)=Sof(H22k)=Sof(H22l)=
 Sof(H22m)=1-FVAR(4)
 Sof(H125)=Sof(C126)=Sof(H12l)=Sof(H12m)=Sof(C127)=Sof(H12n)=Sof(H12o)=
 Sof(H12p)=Sof(C128)=Sof(H12q)=Sof(H12r)=Sof(C129)=Sof(H12s)=Sof(H12t)=
 Sof(H12u)=FVAR(4)
 Sof(C227)=Sof(C228)=Sof(C229)=Sof(H229)=Sof(C230)=Sof(H230)=Sof(C231)=
 Sof(H231)=Sof(C232)=Sof(C233)=Sof(H233)=Sof(C234)=Sof(H23d)=Sof(H23c)=
 Sof(C235)=Sof(H23e)=Sof(H23f)=Sof(H23g)=Sof(C236)=Sof(H23h)=Sof(H23i)=
 Sof(C237)=Sof(H23j)=Sof(H23k)=Sof(H23l)=Sof(C238)=Sof(H238)=Sof(C239)=
 Sof(H23a)=Sof(H23b)=Sof(C240)=Sof(H24c)=Sof(H24d)=Sof(H24e)=Sof(C241)=
 Sof(H24f)=Sof(H24g)=Sof(C242)=Sof(H24h)=Sof(H24i)=Sof(H24j)=1-FVAR(5)
 Sof(C141)=Sof(C142)=Sof(C143)=Sof(H143)=Sof(C144)=Sof(H144)=Sof(C145)=
 Sof(H145)=Sof(C146)=Sof(C147)=Sof(H147)=Sof(C148)=Sof(H14d)=Sof(H14e)=
 Sof(C149)=Sof(H14f)=Sof(H14g)=Sof(H14h)=Sof(C150)=Sof(H15b)=Sof(H15a)=
 Sof(C151)=Sof(H15c)=Sof(H15d)=Sof(H15e)=Sof(C152)=Sof(H152)=Sof(C153)=
 Sof(H15f)=Sof(H15g)=Sof(C154)=Sof(H15h)=Sof(H15i)=Sof(H15j)=Sof(C155)=
 Sof(H15k)=Sof(H15l)=Sof(C156)=Sof(H15m)=Sof(H15n)=Sof(H15o)=FVAR(5)
 Sof(H10f)=Sof(H10g)=Sof(K3A)=Sof(N5A)=Sof(C188)=Sof(C189)=Sof(C190)=Sof(H190)=
 Sof(C191)=Sof(H191)=Sof(C192)=Sof(H192)=Sof(C193)=Sof(C194)=Sof(H194)=
 Sof(C195)=Sof(H19h)=Sof(H19i)=Sof(C196)=Sof(H19j)=Sof(H19k)=Sof(H19l)=
 Sof(C197)=Sof(H19c)=Sof(H19d)=Sof(C198)=Sof(H19e)=Sof(H19f)=Sof(H19g)=
 Sof(C199)=Sof(H199)=Sof(C200)=Sof(H20i)=Sof(H20j)=Sof(C201)=Sof(H20k)=
 Sof(H20l)=Sof(H20m)=Sof(C202)=Sof(H20g)=Sof(H20h)=Sof(C203)=Sof(H20d)=
 Sof(H20e)=Sof(H20f)=Sof(C204)=Sof(C205)=Sof(C206)=Sof(H206)=Sof(C207)=
 Sof(H207)=Sof(C208)=Sof(H208)=Sof(C209)=Sof(C210)=Sof(H210)=Sof(C211)=
 Sof(H21m)=Sof(H21n)=Sof(C212)=Sof(H21o)=Sof(H21p)=Sof(H21q)=Sof(C213)=
 Sof(H213)=Sof(C214)=Sof(H21r)=Sof(H21s)=Sof(C215)=Sof(H21j)=Sof(H21k)=
 Sof(H21l)=Sof(C216)=Sof(H21c)=Sof(H21d)=Sof(C217)=Sof(H21e)=Sof(H21f)=
 Sof(H21g)=1-FVAR(6)
 Sof(H10d)=Sof(H10e)=Sof(K3)=Sof(N5)=Sof(C71)=Sof(C72)=Sof(C73)=Sof(H73)=
 Sof(C74)=Sof(H74)=Sof(C75)=Sof(H75)=Sof(C76)=Sof(C77)=Sof(H77)=Sof(C78)=
 Sof(H78a)=Sof(H78b)=Sof(C79)=Sof(H79a)=Sof(H79b)=Sof(H79c)=Sof(C80)=Sof(H80a)=
 Sof(H80b)=Sof(C81)=Sof(H81a)=Sof(H81b)=Sof(H81c)=Sof(C82)=Sof(H82)=Sof(C83)=
 Sof(H83a)=Sof(H83b)=Sof(C84)=Sof(H84a)=Sof(H84b)=Sof(H84c)=Sof(C85)=Sof(H85a)=
 Sof(H85b)=Sof(C86)=Sof(H86a)=Sof(H86b)=Sof(H86c)=Sof(C98)=Sof(C99)=Sof(C100)=
 Sof(H100)=Sof(C101)=Sof(H101)=Sof(C102)=Sof(H102)=Sof(C103)=Sof(C104)=
 Sof(H104)=Sof(C107)=Sof(H10k)=Sof(H10l)=Sof(C108)=Sof(H10m)=Sof(H10n)=
 Sof(H10o)=Sof(C109)=Sof(H109)=Sof(C110)=Sof(H11d)=Sof(H11e)=Sof(C111)=
 Sof(H11f)=Sof(H11g)=Sof(H11h)=Sof(C112)=Sof(H11j)=Sof(H11i)=Sof(C113)=
 Sof(H11k)=Sof(H11l)=Sof(H11m)=FVAR(6)
 Sof(C183)=Sof(H183)=Sof(C184)=Sof(H18d)=Sof(H18e)=Sof(C185)=Sof(H18f)=
 Sof(H18g)=Sof(H18h)=Sof(C186)=Sof(H18i)=Sof(H18j)=Sof(C187)=Sof(H18k)=
 Sof(H18l)=Sof(H18m)=1-FVAR(7)
 Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62a)=Sof(H62b)=Sof(C63)=Sof(H63a)=Sof(H63b)=
 Sof(H63c)=Sof(C64)=Sof(H64a)=Sof(H64b)=Sof(C65)=Sof(H65a)=Sof(H65b)=Sof(H65c)=
 FVAR(7)
 Sof(C218)=Sof(H218)=Sof(C219)=Sof(H21h)=Sof(H21i)=Sof(C220)=Sof(H22s)=
 Sof(H22t)=Sof(H22u)=Sof(C221)=Sof(H22n)=Sof(H22o)=Sof(C222)=Sof(H22p)=
 Sof(H22q)=Sof(H22r)=1-FVAR(8)
 Sof(C120)=Sof(H120)=Sof(C121)=Sof(H12a)=Sof(H12b)=Sof(C122)=Sof(H12c)=
 Sof(H12d)=Sof(H12e)=Sof(C123)=Sof(H12g)=Sof(H12h)=Sof(C124)=Sof(H12i)=
 Sof(H12j)=Sof(H12k)=FVAR(8)
7.a Ternary CH refined with riding coordinates:
 C23(H23), C39(H39), C66(H66), C125(H125), C125(H12f), C163(H163), C18(H18),
 C34(H34), C61(H61), C77(H77), C82(H82), C104(H104), C109(H109), C120(H120),
 C147(H147), C152(H152), C168(H168), C173(H173), C178(H178), C183(H183),
 C194(H194), C199(H199), C210(H210), C213(H213), C218(H218), C233(H233),
 C238(H238), C243(H243)
7.b Secondary CH2 refined with riding coordinates:
 C24(H24b,H24a), C26(H26a,H26b), C40(H40a,H40b), C42(H42a,H42b), C67(H67a,
 H67b), C69(H69a,H69b), C105(H10d,H10e), C105(H10f,H10g), C164(H16a,H16b),
 C166(H16f,H16g), C19(H19a,H19b), C21(H21a,H21b), C35(H35b,H35a), C37(H37a,
 H37b), C62(H62a,H62b), C64(H64a,H64b), C78(H78a,H78b), C80(H80a,H80b),
 C83(H83a,H83b), C85(H85a,H85b), C107(H10k,H10l), C110(H11d,H11e), C112(H11j,
 H11i), C121(H12a,H12b), C123(H12g,H12h), C126(H12l,H12m), C128(H12q,H12r),
 C148(H14d,H14e), C150(H15b,H15a), C153(H15f,H15g), C155(H15k,H15l), C169(H16k,
 H16l), C171(H17e,H17d), C174(H17i,H17j), C176(H17s,H17t), C179(H17q,H17r),
 C181(H18o,H18n), C184(H18d,H18e), C186(H18i,H18j), C195(H19h,H19i), C197(H19c,
 H19d), C200(H20i,H20j), C202(H20g,H20h), C211(H21m,H21n), C214(H21r,H21s),
 C216(H21c,H21d), C219(H21h,H21i), C221(H22n,H22o), C223(H22d,H22e), C225(H22i,
 H22j), C234(H23d,H23c), C236(H23h,H23i), C239(H23a,H23b), C241(H24f,H24g),
 C244(H24k,H24l), C246(H24p,H24q)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C14(H14), C15(H15), C16(H16), C30(H30), C31(H31), C32(H32), C45(H45),
 C57(H57), C58(H58), C59(H59), C88(H88), C116(H116), C117(H117), C118(H118),
 C131(H131), C159(H159), C160(H160), C161(H161), C73(H73), C74(H74), C75(H75),
 C100(H100), C101(H101), C102(H102), C143(H143), C144(H144), C145(H145),
 C190(H190), C191(H191), C192(H192), C206(H206), C207(H207), C208(H208),
 C229(H229), C230(H230), C231(H231)
7.d Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C9(H9a,H9b,H9c), C10(H10a,
 H10b,H10c), C11(H11a,H11b,H11c), C25(H25a,H25b,H25c), C27(H27a,H27b,H27c),
 C41(H41a,H41b,H41c), C43(H43a,H43b,H43c), C48(H48a,H48b,H48c), C49(H49a,H49b,
 H49c), C50(H50a,H50b,H50c), C52(H52a,H52b,H52c), C53(H53a,H53b,H53c), C54(H54a,
 H54b,H54c), C68(H68a,H68b,H68c), C70(H70a,H70b,H70c), C91(H91a,H91b,H91c),
 C92(H92a,H92b,H92c), C93(H93a,H93b,H93c), C95(H95a,H95c,H95b), C96(H96a,H96b,
 H96c), C97(H97a,H97b,H97c), C106(H10h,H10i,H10j), C134(H13a,H13b,H13c),
 C135(H13d,H13e,H13f), C136(H13g,H13h,H13i), C138(H13j,H13k,H13l), C139(H13m,
 H13n,H13o), C140(H14a,H14b,H14c), C165(H16c,H16d,H16e), C167(H16h,H16i,H16j),
 C20(H20a,H20b,H20c), C22(H22a,H22b,H22c), C36(H36a,H36b,H36c), C38(H38a,H38b,
 H38c), C63(H63a,H63b,H63c), C65(H65a,H65b,H65c), C79(H79a,H79b,H79c), C81(H81a,
 H81b,H81c), C84(H84a,H84b,H84c), C86(H86a,H86b,H86c), C108(H10m,H10n,H10o),
 C111(H11f,H11g,H11h), C113(H11k,H11l,H11m), C122(H12c,H12d,H12e), C124(H12i,
 H12j,H12k), C127(H12n,H12o,H12p), C129(H12s,H12t,H12u), C149(H14f,H14g,H14h),
 C151(H15c,H15d,H15e), C154(H15h,H15i,H15j), C156(H15m,H15n,H15o), C170(H17a,
 H17b,H17c), C172(H17f,H17g,H17h), C175(H17k,H17l,H17m), C177(H17n,H17o,H17p),
 C180(H18a,H18b,H18c), C182(H18p,H18q,H18r), C185(H18f,H18g,H18h), C187(H18k,
 H18l,H18m), C196(H19j,H19k,H19l), C198(H19e,H19f,H19g), C201(H20k,H20l,H20m),
 C203(H20d,H20e,H20f), C212(H21o,H21p,H21q), C215(H21j,H21k,H21l), C217(H21e,
 H21f,H21g), C220(H22s,H22t,H22u), C222(H22p,H22q,H22r), C224(H22f,H22g,H22h),
 C226(H22k,H22l,H22m), C235(H23e,H23f,H23g), C237(H23j,H23k,H23l), C240(H24c,
 H24d,H24e), C242(H24h,H24i,H24j), C245(H24m,H24n,H24o), C247(H24r,H24s,H24t)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              21532
_shelx_fab_checksum              9407
_olex2_date_sample_data_collection 2019-08-21
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.564
_oxdiff_exptl_absorpt_empirical_full_min 0.755