Reductive cyclotrimerization of CO and isonitriles with a highly reactive CaI synthon
Thum, Stefan; Mai, Jonathan; Schmidt, Marcel A.; Langer, Jens; Harder, Sjoerd; Chemical Science 16 (2025) 12058–12067; doi:10.1039/D5SC02829A

data_1574741
_publ_section_title
;
 Reductive cyclotrimerization of CO and isonitriles with a highly reactive
 CaI synthon
;
_journal_issue                   26
_journal_name_full               'Chemical Science'
_journal_page_first              12058
_journal_page_last               12067
_journal_paper_doi               10.1039/D5SC02829A
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C169 H258 Ca4 N8 O9, 3(C5 H12)'
_chemical_formula_sum            'C184 H294 Ca4 N8 O9'
_chemical_formula_weight         2922.57
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-03
_audit_creation_method
;
Olex2 1.5
(compiled 2025.02.27 svn.r83f5de26 for OlexSys, GUI svn.r7172)
;
_audit_update_record
;
2025-03-04 deposited with the CCDC.	2025-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                77.9900(10)
_cell_angle_beta                 77.6940(10)
_cell_angle_gamma                75.3370(10)
_cell_formula_units_Z            2
_cell_length_a                   18.2798(2)
_cell_length_b                   18.3492(2)
_cell_length_c                   27.9435(3)
_cell_measurement_reflns_used    38782
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.3160
_cell_measurement_theta_min      3.1350
_cell_volume                     8740.62(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (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 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 0.997
_diffrn_measured_fraction_theta_max 0.969
_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   -114.00 -13.00   1.00    7.00    --  -41.15 -57.00 120.00  101
  2  \w    -74.00  35.00   1.00    7.00    --  -41.15  77.00-120.00  109
  3  \w    -21.00  74.00   1.00    7.00    --   41.15 -77.00   0.00   95
  4  \w     21.00 107.00   1.00   28.00    --  104.04 -94.00-120.00   86
  5  \w     31.00 109.00   1.00   28.00    --  104.04-111.00-180.00   78
  6  \w     76.00 178.00   1.00   28.00    --  104.04  30.00  60.00  102
  7  \w     28.00 132.00   1.00   28.00    --  104.04 -30.00   0.00  104
  8  \w     32.00 133.00   1.00   28.00    --  104.04 -61.00-120.00  101
  9  \w     31.00 109.00   1.00   28.00    --  104.04-111.00  30.00   78
 10  \w     28.00 132.00   1.00   28.00    --  104.04 -30.00 120.00  104
 11  \w     51.00 178.00   1.00   28.00    --  104.04  15.00   0.00  127
 12  \w     28.00 137.00   1.00   28.00    --  104.04 -77.00   0.00  109
 13  \w   -114.00 -13.00   1.00    7.00    --  -41.15 -57.00-120.00  101
 14  \w   -114.00 -13.00   1.00    7.00    --  -41.15 -57.00   0.00  101
 15  \w    -33.00  66.00   1.00    7.00    --   41.15 -38.00  60.00   99
 16  \w     76.00 142.00   1.00   28.00    --  104.04  30.00-180.00   66
;
_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      -0.0374601000
_diffrn_orient_matrix_UB_12      -0.0571135000
_diffrn_orient_matrix_UB_13      -0.0141174000
_diffrn_orient_matrix_UB_21      0.0250320000
_diffrn_orient_matrix_UB_22      -0.0593054000
_diffrn_orient_matrix_UB_23      0.0445985000
_diffrn_orient_matrix_UB_31      -0.0760546000
_diffrn_orient_matrix_UB_32      0.0309506000
_diffrn_orient_matrix_UB_33      0.0329039000
_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  0.0229
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            82794
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.437
_diffrn_reflns_theta_min         2.776
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_description       block
_exptl_crystal_F_000             3212
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2998
_refine_ls_number_reflns         33569
_refine_ls_number_restraints     14950
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0648
_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^)+(0.1024P)^2^+6.8169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28693
_reflns_number_total             33569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02829a2.cif
_cod_data_source_block           hasj221019a
_cod_depositor_comments
'Adding full bibliography for 1574737--1574741.cif.'
_cod_database_code               1574741
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C184 H294 Ca4 N8 O9'
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.758
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C181-C180 = C182-C181 = C183-C182 = C184-C183 = C176-C175 = C177-C176 = C178-
 C177 = C178-C179 = C174-C173 = C173-C172 = C172-C171 = C171-C170 = C296-C295 =
 C295-C294 = C294-C293 = C293-C292 = C291-C290 = C290-C289 = C289-C288 = C288-
 C287
 1.52 with sigma of 0.005
 C175-C177 = C176-C178 = C184-C182 = C183-C181 = C170-C172 = C171-C173 = C174-
 C172 = C179-C177 = C180-C182 = C296-C294 = C295-C293 = C287-C289 = C288-C290 =
 C289-C291 = C294-C292
 2.54 with sigma of 0.01
 N5-C96 \\sim N5A-C96 \\sim N6A-C221 \\sim N6-C112 \\sim N7A-C247 \\sim N7-C138
\\sim N8-C272 \\sim N8A-
 C261 \\sim N2-C22 \\sim N2-C185
 with sigma of 0.02
 C214-C213 \\sim C94-C93 \\sim C213-C212 \\sim C93-C92 \\sim C136-C135 \\sim
C245-C244 \\sim C244-C243
 \\sim C135-C134
 with sigma of 0.02
 C134-C133 \\sim C243-C242 \\sim C246-C245 \\sim C137-C136 \\sim C212-C211
\\sim C92-C91 \\sim C215-
 C214 \\sim C95-C94
 with sigma of 0.02
 O2-C205 \\sim O2-C47 \\sim O2-C43 \\sim O2-C201 \\sim O9-C128 \\sim O9-C132
\\sim O9A-C237 \\sim O9A-C241
 with sigma of 0.02
 N7A-C243 \\sim N7-C134 \\sim N8-C136 \\sim N8A-C245 \\sim N6A-C214 \\sim
N6-C94 \\sim N5A-C212 \\sim N5-C92
 with sigma of 0.02
 C129-C128 \\sim C132-C131 \\sim C238-C237 \\sim C241-C240 \\sim C205-C204
\\sim C47-C46 \\sim C44-C43
 \\sim C202-C201
 with sigma of 0.02
 C252-C247 \\sim C143-C138 \\sim C248-C247 \\sim C139-C138 \\sim C155-C154
\\sim C273-C272 \\sim C262-
 C261 \\sim C277-C272 \\sim C159-C154 \\sim C266-C261 \\sim C117-C112 \\sim
C226-C221 \\sim C113-C112 ~
 C222-C221 \\sim C186-C185 \\sim C23-C22 \\sim C190-C185 \\sim C27-C22
 with sigma of 0.02
 C45-C44 \\sim C203-C202 \\sim C46-C45 \\sim C204-C203 \\sim C130-C129 \\sim
C131-C130 \\sim C240-C239
 \\sim C239-C238
 with sigma of 0.02
 C69-C68 \\sim C208-C207 \\sim C210-C209 \\sim C71-C70 \\sim C32-C31 \\sim
C195-C194 \\sim C193-C192 ~
 C30-C29 \\sim C35-C34 \\sim C198-C197 \\sim C37-C36 \\sim C200-C199 \\sim
C258-C257 \\sim C151-C150 ~
 C153-C152 \\sim C260-C259 \\sim C148-C147 \\sim C255-C254 \\sim C120-C119
\\sim C229-C228 \\sim C231-
 C230 \\sim C122-C121 \\sim C236-C235 \\sim C127-C126 \\sim C125-C124 \\sim
C234-C233 \\sim C218-C217 ~
 C104-C103 \\sim C106-C105 \\sim C220-C219 \\sim C167-C166 \\sim C284-C283
\\sim C286-C285 \\sim C169-
 C168 \\sim C164-C163 \\sim C281-C164 \\sim C271-C270 \\sim C269-C268 \\sim
C162-C161 \\sim C280-C279
 with sigma of 0.02
 C264-C263 \\sim C157-C156 \\sim C275-C274 \\sim C158-C157 \\sim C265-C264
\\sim C276-C275 \\sim C141-
 C140 \\sim C250-C249 \\sim C142-C141 \\sim C251-C250 \\sim C25-C24 \\sim
C188-C187 \\sim C26-C25 ~
 C189-C188 \\sim C225-C224 \\sim C116-C115 \\sim C115-C114 \\sim C224-C223
 with sigma of 0.02
 C160-C155 \\sim C278-C273 \\sim C267-C262 \\sim C282-C277 \\sim C165-C159
\\sim C266-C165 \\sim C256-
 C252 \\sim C149-C143 \\sim C196-C190 \\sim C33-C27 \\sim C191-C186 \\sim
C28-C23 \\sim C67-C61 \\sim C61-
 C206 \\sim C97-C102 \\sim C97-C216 \\sim C232-C226 \\sim C123-C117 \\sim
C118-C113 \\sim C227-C222 ~
 C253-C248 \\sim C144-C139
 with sigma of 0.02
 C114-C113 \\sim C223-C222 \\sim C117-C116 \\sim C226-C225 \\sim C190-C189
\\sim C27-C26 \\sim C187-
 C186 \\sim C24-C23 \\sim C143-C142 \\sim C252-C251 \\sim C140-C139 \\sim
C249-C248 \\sim C156-C155 ~
 C274-C273 \\sim C263-C262 \\sim C159-C158 \\sim C266-C265 \\sim C277-C276
 with sigma of 0.02
 C163-C160 \\sim C281-C278 \\sim C279-C278 \\sim C161-C160 \\sim C268-C267
\\sim C270-C267 \\sim C166-
 C165 \\sim C283-C282 \\sim C168-C165 \\sim C285-C282 \\sim C207-C206 \\sim
C68-C67 \\sim C209-C206 ~
 C70-C67 \\sim C217-C216 \\sim C103-C102 \\sim C219-C216 \\sim C105-C102 \\sim
C233-C232 \\sim C124-
 C123 \\sim C235-C232 \\sim C126-C123 \\sim C230-C227 \\sim C121-C118 \\sim
C228-C227 \\sim C119-C118 ~
 C145-C144 \\sim C253-C145 \\sim C147-C144 \\sim C254-C253 \\sim C257-C256
\\sim C150-C149 \\sim C152-
 C149 \\sim C259-C256 \\sim C36-C33 \\sim C199-C196 \\sim C197-C196 \\sim
C34-C33 \\sim C29-C28 \\sim C192-
 C191 \\sim C31-C28 \\sim C194-C191
 with sigma of 0.02
 C234-C232 \\sim C232-C236 \\sim C127-C123 \\sim C123-C125
 with sigma of 0.02
 C126-C124 \\sim C235-C233
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O9 \\sim C128 \\sim C129 \\sim C130 \\sim C131 \\sim C132 \\sim O9A \\sim C237
\\sim C238 \\sim C239 \\sim C240 \\sim C241: within 4A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 4A
C175 \\sim C176 \\sim C177 \\sim C178 \\sim C179 \\sim C287 \\sim C288 \\sim
C289 \\sim C290 \\sim C291: within 4A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 4A
N5 \\sim N6 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C112 \\sim
C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim C118 \\sim C119 \\sim
C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim
C127 \\sim N5A \\sim N6A \\sim C211 \\sim C212 \\sim C213 \\sim C214 \\sim C215
\\sim C221 \\sim C222 \\sim C223 \\sim C224 \\sim C225 \\sim C226 \\sim C227
\\sim C228 \\sim C229 \\sim C230 \\sim C231 \\sim C232 \\sim C233 \\sim C234
\\sim C235 \\sim C236: within 4A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 4A
C145 \\sim C146 \\sim Ca4 \\sim O5 \\sim O8 \\sim N7 \\sim N8 \\sim C133 \\sim
C134 \\sim C135 \\sim C136 \\sim C137 \\sim C138 \\sim C139 \\sim C140 \\sim
C141 \\sim C142 \\sim C143 \\sim C144 \\sim C147 \\sim C148 \\sim C149 \\sim
C150 \\sim C151 \\sim C152 \\sim C153 \\sim Ca4A \\sim O5A \\sim O8A \\sim N7A
\\sim N8A \\sim C242 \\sim C243 \\sim C244 \\sim C245 \\sim C246 \\sim C247
\\sim C248 \\sim C249 \\sim C250 \\sim C251 \\sim C252 \\sim C253 \\sim C254
\\sim C255 \\sim C256 \\sim C257 \\sim C258 \\sim C259 \\sim C260 \\sim C261
\\sim C262 \\sim C263 \\sim C264 \\sim C265 \\sim C266 \\sim C267 \\sim C268
\\sim C269 \\sim C270 \\sim C271 \\sim C272 \\sim C273 \\sim C274 \\sim C275
\\sim C276 \\sim C277 \\sim C278 \\sim C279 \\sim C280 \\sim C281 \\sim C282
\\sim C283 \\sim C284 \\sim C285 \\sim C286 \\sim C154 \\sim C155 \\sim C156
\\sim C157 \\sim C158 \\sim C159 \\sim C160 \\sim C161 \\sim C162 \\sim C163
\\sim C165 \\sim C166 \\sim C167 \\sim C168 \\sim C169 \\sim C164: within 4A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 4A
C44 \\sim C45 \\sim C46 \\sim C202 \\sim C203 \\sim C204: within 3A with sigma
of 0.03 and sigma for terminal atoms of 0.06 within 3A
C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim
C185 \\sim C186 \\sim C187 \\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: within 4A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 4A
C180 \\sim C181 \\sim C182 \\sim C183 \\sim C184 \\sim C292 \\sim C293 \\sim
C294 \\sim C295 \\sim C296: within 4A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 4A
C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C216 \\sim C217 \\sim
C218 \\sim C219 \\sim C220: within 4A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 4A
4. Rigid body (RIGU) restrains
 C233, C234
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(C154)+Sof(C155)+Sof(C156)+Sof(H156)+Sof(C157)+Sof(H157)+Sof(C158)+
 Sof(H158)+Sof(C159)+Sof(C160)+Sof(H160)+Sof(C161)+Sof(H16D)+Sof(H16E)+
 Sof(C162)+Sof(H16F)+Sof(H16G)+Sof(H16H)+Sof(C163)+Sof(H16I)+Sof(H16J)+
 Sof(H16K)+Sof(H16Y)+Sof(H)+Sof(HA)]+1*[Sof(H14F)+Sof(H14G)+Sof(H14D)+Sof(H14E)+
 Sof(Ca4)+Sof(O5)+Sof(O8)+Sof(N7)+Sof(N8)+Sof(C133)+Sof(H13I)+Sof(H13J)+
 Sof(H13K)+Sof(C134)+Sof(C135)+Sof(H135)+Sof(C136)+Sof(C137)+Sof(H13L)+
 Sof(H13M)+Sof(H13N)+Sof(C138)+Sof(C139)+Sof(C140)+Sof(H140)+Sof(C141)+
 Sof(H141)+Sof(C142)+Sof(H142)+Sof(C143)+Sof(C144)+Sof(H144)+Sof(C147)+
 Sof(H14K)+Sof(H14L)+Sof(C148)+Sof(H14M)+Sof(H14N)+Sof(H14O)+Sof(C149)+
 Sof(H149)+Sof(C150)+Sof(H15C)+Sof(H15D)+Sof(C151)+Sof(H15E)+Sof(H15F)+
 Sof(H15G)+Sof(C152)+Sof(H15H)+Sof(H15I)+Sof(C153)+Sof(H15J)+Sof(H15K)+
 Sof(H15L)+Sof(Ca4A)+Sof(O5A)+Sof(O8A)+Sof(N7A)+Sof(N8A)+Sof(C242)+Sof(H24A)+
 Sof(H24B)+Sof(H24C)+Sof(C243)+Sof(C244)+Sof(H244)+Sof(C245)+Sof(C246)+
 Sof(H24D)+Sof(H24E)+Sof(H24F)+Sof(C247)+Sof(C248)+Sof(C249)+Sof(H249)+
 Sof(C250)+Sof(H250)+Sof(C251)+Sof(H251)+Sof(C252)+Sof(C253)+Sof(H253)+
 Sof(C254)+Sof(H25A)+Sof(H25B)+Sof(C255)+Sof(H25C)+Sof(H25D)+Sof(H25E)+
 Sof(C256)+Sof(H256)+Sof(C257)+Sof(H25F)+Sof(H25G)+Sof(C258)+Sof(H25H)+
 Sof(H25I)+Sof(H25J)+Sof(C259)+Sof(H25K)+Sof(H25L)+Sof(C260)+Sof(H26A)+
 Sof(H26B)+Sof(H26C)+Sof(C261)+Sof(C262)+Sof(C263)+Sof(H263)+Sof(C264)+
 Sof(H264)+Sof(C265)+Sof(H265)+Sof(C266)+Sof(C267)+Sof(H267)+Sof(C268)+
 Sof(H26D)+Sof(H26E)+Sof(C269)+Sof(H26F)+Sof(H26G)+Sof(H26H)+Sof(C270)+
 Sof(H27A)+Sof(H27B)+Sof(C271)+Sof(H27C)+Sof(H27D)+Sof(H27E)+Sof(H165)+
 Sof(C164)]+1*[Sof(C273)+Sof(C274)+Sof(H274)+Sof(C275)+Sof(H275)+Sof(C276)+
 Sof(H276)+Sof(C277)+Sof(C272)+Sof(C278)+Sof(H278)+Sof(C279)+Sof(H27F)+
 Sof(H27G)+Sof(C280)+Sof(H28A)+Sof(H28B)+Sof(H28C)+Sof(C281)+Sof(H28D)+
 Sof(H28E)+Sof(C282)+Sof(H282)+Sof(C283)+Sof(H28F)+Sof(H28G)+Sof(C284)+
 Sof(H28H)+Sof(H28I)+Sof(H28J)+Sof(C285)+Sof(H28K)+Sof(H28L)+Sof(C286)+
 Sof(H28M)+Sof(H28N)+Sof(H28O)+Sof(C165)+Sof(C166)+Sof(H16L)+Sof(H16M)+
 Sof(C167)+Sof(H16N)+Sof(H16O)+Sof(H16P)+Sof(C168)+Sof(H16Q)+Sof(H16R)+
 Sof(C169)+Sof(H16S)+Sof(H16T)+Sof(H16U)+Sof(H16V)+Sof(H16W)+Sof(H16X)]=1 with
 esd of 0.0001
 Sof(N5A)=Sof(N6A)=Sof(C211)=Sof(H21G)=Sof(H21H)=Sof(H21I)=Sof(C212)=Sof(C213)=
 Sof(H213)=Sof(C214)=Sof(C215)=Sof(H21J)=Sof(H21K)=Sof(H21L)=Sof(C221)=
 Sof(C222)=Sof(C223)=Sof(H223)=Sof(C224)=Sof(H224)=Sof(C225)=Sof(H225)=
 Sof(C226)=Sof(C227)=Sof(H227)=Sof(C228)=Sof(H22D)=Sof(H22E)=Sof(C229)=
 Sof(H22F)=Sof(H22G)=Sof(H22H)=Sof(C230)=Sof(H23A)=Sof(H23B)=Sof(C231)=
 Sof(H23C)=Sof(H23D)=Sof(H23E)=Sof(C232)=Sof(H232)=Sof(C233)=Sof(H23F)=
 Sof(H23G)=Sof(C234)=Sof(H23H)=Sof(H23I)=Sof(H23J)=Sof(C235)=Sof(H23K)=
 Sof(H23L)=Sof(C236)=Sof(H23M)=Sof(H23N)=Sof(H23O)=Sof(O9A)=Sof(C237)=Sof(H23P)=
 Sof(H23Q)=Sof(C238)=Sof(H23R)=Sof(H23S)=Sof(C239)=Sof(H23T)=Sof(H23U)=
 Sof(C240)=Sof(H24G)=Sof(H24H)=Sof(C241)=Sof(H24I)=Sof(H24J)=1-FVAR(1)
 Sof(O9)=Sof(N5)=Sof(N6)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=Sof(C92)=
 Sof(C93)=Sof(H93)=Sof(C94)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=Sof(C112)=
 Sof(C113)=Sof(C114)=Sof(H114)=Sof(C115)=Sof(H115)=Sof(C116)=Sof(H116)=
 Sof(C117)=Sof(C118)=Sof(H118)=Sof(C119)=Sof(H11F)=Sof(H11G)=Sof(C120)=
 Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C121)=Sof(H12D)=Sof(H12E)=Sof(C122)=
 Sof(H12F)=Sof(H12G)=Sof(H12H)=Sof(C123)=Sof(H123)=Sof(C124)=Sof(H12I)=
 Sof(H12J)=Sof(C125)=Sof(H12K)=Sof(H12L)=Sof(H12M)=Sof(C126)=Sof(H12N)=
 Sof(H12O)=Sof(C127)=Sof(H12P)=Sof(H12Q)=Sof(H12R)=Sof(C128)=Sof(H12S)=
 Sof(H12T)=Sof(C129)=Sof(H12U)=Sof(H12V)=Sof(C130)=Sof(H13C)=Sof(H13D)=
 Sof(C131)=Sof(H13E)=Sof(H13F)=Sof(C132)=Sof(H13G)=Sof(H13H)=FVAR(1)
 Sof(C287)=Sof(H28P)=Sof(H28Q)=Sof(H28R)=Sof(C288)=Sof(H28S)=Sof(H28T)=
 Sof(C289)=Sof(H28U)=Sof(H28V)=Sof(C290)=Sof(H29C)=Sof(H29D)=Sof(C291)=
 Sof(H29E)=Sof(H29F)=Sof(H29G)=1-FVAR(2)
 Sof(C175)=Sof(H17M)=Sof(H17N)=Sof(H17O)=Sof(C176)=Sof(H17P)=Sof(H17Q)=
 Sof(C177)=Sof(H17R)=Sof(H17S)=Sof(C178)=Sof(H17T)=Sof(H17U)=Sof(C179)=
 Sof(H17V)=Sof(H17W)=Sof(H17X)=FVAR(2)
 Sof(H14D)=Sof(H14E)=Sof(Ca4)=Sof(O5)=Sof(O8)=Sof(N7)=Sof(N8)=Sof(C133)=
 Sof(H13I)=Sof(H13J)=Sof(H13K)=Sof(C134)=Sof(C135)=Sof(H135)=Sof(C136)=
 Sof(C137)=Sof(H13L)=Sof(H13M)=Sof(H13N)=Sof(C138)=Sof(C139)=Sof(C140)=
 Sof(H140)=Sof(C141)=Sof(H141)=Sof(C142)=Sof(H142)=Sof(C143)=Sof(C144)=
 Sof(H144)=Sof(C147)=Sof(H14K)=Sof(H14L)=Sof(C148)=Sof(H14M)=Sof(H14N)=
 Sof(H14O)=Sof(C149)=Sof(H149)=Sof(C150)=Sof(H15C)=Sof(H15D)=Sof(C151)=
 Sof(H15E)=Sof(H15F)=Sof(H15G)=Sof(C152)=Sof(H15H)=Sof(H15I)=Sof(C153)=
 Sof(H15J)=Sof(H15K)=Sof(H15L)=Sof(C164)=1-FVAR(3)
 Sof(H14F)=Sof(H14G)=Sof(Ca4A)=Sof(O5A)=Sof(O8A)=Sof(N7A)=Sof(N8A)=Sof(C242)=
 Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C243)=Sof(C244)=Sof(H244)=Sof(C245)=
 Sof(C246)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C247)=Sof(C248)=Sof(C249)=
 Sof(H249)=Sof(C250)=Sof(H250)=Sof(C251)=Sof(H251)=Sof(C252)=Sof(C253)=
 Sof(H253)=Sof(C254)=Sof(H25A)=Sof(H25B)=Sof(C255)=Sof(H25C)=Sof(H25D)=
 Sof(H25E)=Sof(C256)=Sof(H256)=Sof(C257)=Sof(H25F)=Sof(H25G)=Sof(C258)=
 Sof(H25H)=Sof(H25I)=Sof(H25J)=Sof(C259)=Sof(H25K)=Sof(H25L)=Sof(C260)=
 Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C261)=Sof(C262)=Sof(C263)=Sof(H263)=
 Sof(C264)=Sof(H264)=Sof(C265)=Sof(H265)=Sof(C266)=Sof(C267)=Sof(H267)=
 Sof(C268)=Sof(H26D)=Sof(H26E)=Sof(C269)=Sof(H26F)=Sof(H26G)=Sof(H26H)=
 Sof(C270)=Sof(H27A)=Sof(H27B)=Sof(C271)=Sof(H27C)=Sof(H27D)=Sof(H27E)=
 Sof(H165)=FVAR(3)
 Sof(C165)=Sof(C166)=Sof(H16L)=Sof(H16M)=Sof(C167)=Sof(H16N)=Sof(H16O)=
 Sof(H16P)=Sof(C168)=Sof(H16Q)=Sof(H16R)=Sof(C169)=Sof(H16S)=Sof(H16T)=
 Sof(H16U)=1-FVAR(4)
 Sof(C273)=Sof(C274)=Sof(H274)=Sof(C275)=Sof(H275)=Sof(C276)=Sof(H276)=
 Sof(C277)=Sof(C272)=Sof(C278)=Sof(H278)=Sof(C279)=Sof(H27F)=Sof(H27G)=
 Sof(C280)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C281)=Sof(H28D)=Sof(H28E)=
 Sof(C282)=Sof(H282)=Sof(C283)=Sof(H28F)=Sof(H28G)=Sof(C284)=Sof(H28H)=
 Sof(H28I)=Sof(H28J)=Sof(C285)=Sof(H28K)=Sof(H28L)=Sof(C286)=Sof(H28M)=
 Sof(H28N)=Sof(H28O)=Sof(H16V)=Sof(H16W)=Sof(H16X)=FVAR(4)
 Sof(C154)=Sof(C155)=Sof(C156)=Sof(H156)=Sof(C157)=Sof(H157)=Sof(C158)=
 Sof(H158)=Sof(C159)=Sof(C160)=Sof(H160)=Sof(C161)=Sof(H16D)=Sof(H16E)=
 Sof(C162)=Sof(H16F)=Sof(H16G)=Sof(H16H)=Sof(C163)=Sof(H16I)=Sof(H16J)=
 Sof(H16K)=Sof(H16Y)=Sof(H)=Sof(HA)=FVAR(5)
 Sof(C201)=Sof(H20F)=Sof(H20G)=Sof(C202)=Sof(H20H)=Sof(H20I)=Sof(C203)=
 Sof(H20J)=Sof(H20K)=Sof(C204)=Sof(H20L)=Sof(H20M)=Sof(C205)=Sof(H20N)=
 Sof(H20O)=1-FVAR(6)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=
 Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=FVAR(6)
 Sof(C185)=Sof(C186)=Sof(C187)=Sof(H187)=Sof(C188)=Sof(H188)=Sof(C189)=
 Sof(H189)=Sof(C190)=Sof(C191)=Sof(H191)=Sof(C192)=Sof(H19D)=Sof(H19E)=
 Sof(C193)=Sof(H19F)=Sof(H19G)=Sof(H19H)=Sof(C194)=Sof(H19I)=Sof(H19J)=
 Sof(C195)=Sof(H19K)=Sof(H19L)=Sof(H19M)=Sof(C196)=Sof(H196)=Sof(C197)=
 Sof(H19N)=Sof(H19O)=Sof(C198)=Sof(H19P)=Sof(H19Q)=Sof(H19R)=Sof(C199)=
 Sof(H19S)=Sof(H19T)=Sof(C200)=Sof(H20C)=Sof(H20D)=Sof(H20E)=1-FVAR(7)
 Sof(C22)=Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=
 Sof(C27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=
 Sof(H37C)=FVAR(7)
 Sof(C206)=Sof(H206)=Sof(C207)=Sof(H20P)=Sof(H20Q)=Sof(C208)=Sof(H20R)=
 Sof(H20S)=Sof(H20T)=Sof(C209)=Sof(H20U)=Sof(H20V)=Sof(C210)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=1-FVAR(8)
 Sof(C67)=Sof(H67)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(H69A)=Sof(H69B)=
 Sof(H69C)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=
 FVAR(8)
 Sof(C292)=Sof(H29H)=Sof(H29I)=Sof(H29J)=Sof(C293)=Sof(H29K)=Sof(H29L)=
 Sof(C294)=Sof(H29M)=Sof(H29N)=Sof(C295)=Sof(H29O)=Sof(H29P)=Sof(C296)=
 Sof(H29Q)=Sof(H29R)=Sof(H29S)=1-FVAR(9)
 Sof(C180)=Sof(H18C)=Sof(H18D)=Sof(H18E)=Sof(C181)=Sof(H18F)=Sof(H18G)=
 Sof(C182)=Sof(H18H)=Sof(H18I)=Sof(C183)=Sof(H18J)=Sof(H18K)=Sof(C184)=
 Sof(H18L)=Sof(H18M)=Sof(H18N)=FVAR(9)
 Sof(C216)=Sof(H216)=Sof(C217)=Sof(H21M)=Sof(H21N)=Sof(C218)=Sof(H21O)=
 Sof(H21P)=Sof(H21Q)=Sof(C219)=Sof(H21R)=Sof(H21S)=Sof(C220)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=1-FVAR(10)
 Sof(C102)=Sof(H102)=Sof(C103)=Sof(H10F)=Sof(H10G)=Sof(C104)=Sof(H10H)=
 Sof(H10I)=Sof(H10J)=Sof(C105)=Sof(H10K)=Sof(H10L)=Sof(C106)=Sof(H10M)=
 Sof(H10N)=Sof(H10O)=FVAR(10)
6.a Riding coordinates:
 C165(H16K), C165(H165)
6.b Ternary CH refined with riding coordinates:
 C12(H12), C17(H17), C62(H62), C78(H78), C83(H83), C107(H107), C28(H28),
 C33(H33), C67(H67), C102(H102), C118(H118), C123(H123), C144(H144), C149(H149),
  C191(H191), C196(H196), C206(H206), C216(H216), C227(H227), C232(H232),
 C253(H253), C256(H256), C267(H267), C278(H278), C282(H282), C160(H160)
6.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C18(H18A,H18B), C20(H20A,H20B), C38(H38A,
 H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
 C63(H63A,H63B), C65(H65A,H65B), C79(H79A,H79B), C81(H81A,H81B), C84(H84A,H84B),
  C86(H86A,H86B), C108(H10A,H10B), C110(H11A,H11B), C145(H14F,H14G), C145(H14D,
 H14E), C29(H29A,H29B), C31(H31A,H31B), C34(H34A,H34B), C36(H36A,H36B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
  C68(H68A,H68B), C70(H70A,H70B), C103(H10F,H10G), C105(H10K,H10L), C119(H11F,
 H11G), C121(H12D,H12E), C124(H12I,H12J), C126(H12N,H12O), C128(H12S,H12T),
 C129(H12U,H12V), C130(H13C,H13D), C131(H13E,H13F), C132(H13G,H13H), C147(H14K,
 H14L), C150(H15C,H15D), C152(H15H,H15I), C192(H19D,H19E), C194(H19I,H19J),
 C197(H19N,H19O), C199(H19S,H19T), C201(H20F,H20G), C202(H20H,H20I), C203(H20J,
 H20K), C204(H20L,H20M), C205(H20N,H20O), C207(H20P,H20Q), C209(H20U,H20V),
 C217(H21M,H21N), C219(H21R,H21S), C228(H22D,H22E), C230(H23A,H23B), C233(H23F,
 H23G), C235(H23K,H23L), C254(H25A,H25B), C257(H25F,H25G), C259(H25K,H25L),
 C268(H26D,H26E), C270(H27A,H27B), C279(H27F,H27G), C281(H28D,H28E), C283(H28F,
 H28G), C285(H28K,H28L), C161(H16D,H16E), C163(H16I,H16J), C237(H23P,H23Q),
 C238(H23R,H23S), C239(H23T,H23U), C240(H24G,H24H), C241(H24I,H24J), C166(H16L,
 H16M), C168(H16Q,H16R), C171(H17D,H17E), C172(H17F,H17G), C173(H17H,H17I),
 C176(H17P,H17Q), C177(H17R,H17S), C178(H17T,H17U), C181(H18F,H18G), C182(H18H,
 H18I), C183(H18J,H18K), C288(H28S,H28T), C289(H28U,H28V), C290(H29C,H29D),
 C293(H29K,H29L), C294(H29M,H29N), C295(H29O,H29P)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C53(H53), C58(H58), C59(H59), C60(H60),
 C74(H74), C75(H75), C76(H76), C98(H98), C99(H99), C100(H100), C24(H24),
 C25(H25), C26(H26), C93(H93), C114(H114), C115(H115), C116(H116), C135(H135),
 C140(H140), C141(H141), C142(H142), C187(H187), C188(H188), C189(H189),
 C213(H213), C223(H223), C224(H224), C225(H225), C244(H244), C249(H249),
 C250(H250), C251(H251), C263(H263), C264(H264), C265(H265), C274(H274),
 C275(H275), C276(H276), C156(H156), C157(H157), C158(H158)
6.e Fitted hexagon refined as free rotating group:
 C273(C274,C275,C276,C277,C272)
6.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C51(H51A,H51B,H51C), C55(H55A,H55B,
 H55C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C80(H80A,H80B,H80C), C82(H82A,
 H82B,H82C), C85(H85A,H85B,H85C), C87(H87A,H87B,H87C), C109(H10C,H10D,H10E),
 C111(H11C,H11D,H11E), C146(H14H,H14I,H14J), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C69(H69A,H69B,H69C), C71(H71A,
 H71B,H71C), C91(H91A,H91B,H91C), C95(H95A,H95B,H95C), C104(H10H,H10I,H10J),
 C106(H10M,H10N,H10O), C120(H12A,H12B,H12C), C122(H12F,H12G,H12H), C125(H12K,
 H12L,H12M), C127(H12P,H12Q,H12R), C133(H13I,H13J,H13K), C137(H13L,H13M,H13N),
 C148(H14M,H14N,H14O), C151(H15E,H15F,H15G), C153(H15J,H15K,H15L), C193(H19F,
 H19G,H19H), C195(H19K,H19L,H19M), C198(H19P,H19Q,H19R), C200(H20C,H20D,H20E),
 C208(H20R,H20S,H20T), C210(H21D,H21E,H21F), C211(H21G,H21H,H21I), C215(H21J,
 H21K,H21L), C218(H21O,H21P,H21Q), C220(H22A,H22B,H22C), C229(H22F,H22G,H22H),
 C231(H23C,H23D,H23E), C234(H23H,H23I,H23J), C236(H23M,H23N,H23O), C242(H24A,
 H24B,H24C), C246(H24D,H24E,H24F), C255(H25C,H25D,H25E), C258(H25H,H25I,H25J),
 C260(H26A,H26B,H26C), C269(H26F,H26G,H26H), C271(H27C,H27D,H27E), C280(H28A,
 H28B,H28C), C284(H28H,H28I,H28J), C286(H28M,H28N,H28O), C162(H16F,H16G,H16H),
 C167(H16N,H16O,H16P), C169(H16S,H16T,H16U), C164(H16Y,H,HA), C164(H16V,H16W,
 H16X), C170(H17A,H17B,H17C), C174(H17J,H17K,H17L), C175(H17M,H17N,H17O),
 C179(H17V,H17W,H17X), C180(H18C,H18D,H18E), C184(H18L,H18M,H18N), C287(H28P,
 H28Q,H28R), C291(H29E,H29F,H29G), C292(H29H,H29I,H29J), C296(H29Q,H29R,H29S)
;
_shelx_res_checksum              72608
_olex2_date_sample_data_collection 2022-10-19
_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 1.387
_oxdiff_exptl_absorpt_empirical_full_min 0.694