The curious case of a sterically crowded Stenhouse salt
Théry, Valentin; Molton, Florian; Sirach, Selim; Tillet, Neven; Pécaut, Jacques; Tomás-Mendivil, Eder; Martin, David; Chemical Science 13 (2022) 9755–9760; doi:10.1039/D2SC01895K

data_1567582
_publ_section_title
;
 The curious case of a sterically crowded Stenhouse salt
;
_journal_issue                   33
_journal_name_full               'Chemical Science'
_journal_page_first              9755
_journal_page_last               9760
_journal_paper_doi               10.1039/D2SC01895K
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C F3 O3 S, C54 H79 N2 O, 0.5(C4 H10 O)'
_chemical_formula_sum            'C57 H84 F3 N2 O4.5 S'
_chemical_formula_weight         958.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-02-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-30 deposited with the CCDC.	2022-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.096(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3378(9)
_cell_length_b                   16.0403(10)
_cell_length_c                   38.924(2)
_cell_measurement_reflns_used    2748
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      24.4160
_cell_measurement_theta_min      2.4850
_cell_volume                     10782.1(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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      4.00  94.00   1.00  240.00    --   25.25  57.00-150.00   90
  2  \w   -103.00 -39.00   1.00  240.00    --  -27.12-178.00  30.00   64
  3  \w   -100.00  -1.00   1.00  240.00    --  -27.12 -37.00 -90.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0182117000
_diffrn_orient_matrix_UB_12      -0.0170088000
_diffrn_orient_matrix_UB_13      0.0154794000
_diffrn_orient_matrix_UB_21      0.0336361000
_diffrn_orient_matrix_UB_22      0.0238659000
_diffrn_orient_matrix_UB_23      -0.0021836000
_diffrn_orient_matrix_UB_31      -0.0149389000
_diffrn_orient_matrix_UB_32      0.0331167000
_diffrn_orient_matrix_UB_33      0.0095088000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.1286
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            24739
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.024
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.995
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent intense pink'
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       plate
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.539
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         11002
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1844
_refine_ls_R_factor_gt           0.0859
_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/[\s^2^(Fo^2^)+(0.1408P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2195
_refine_ls_wR_factor_ref         0.2793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5218
_reflns_number_total             11002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01895k2.cif
_cod_data_source_block           1MeOTf
_cod_original_cell_volume        10782.0(11)
_cod_original_formula_sum        'C57 H84 F3 N2 O4.50 S'
_cod_database_code               1567582
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C53 H76 N1 O4 F3 S1'
_reflns_odcompleteness_completeness 98.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Restrained distances
 C64-C63
 1.52 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
O61 \\sim C61 \\sim C62 \\sim C63 \\sim C64: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
Uanis(C62) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(O61) \\sim Ueq, Uanis(C63)
\\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Others
 Sof(C26B)=Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=
 Sof(C28B)=Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1)
 Fixed Sof: O61(0.5) C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62B(0.5) H62C(0.5)
 H62A(0.5) C63(0.5) H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5)
4.a :
 O61(C61,C62,C63,C64)
4.b Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C49(H49), C52(H52)
4.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C37(H37A,H37B), C39(H39A,H39B), C26(H26A,H26B),
 C28(H28A,H28B), C26B(H26C,H26D), C28B(H28C,H28D), C61(H61A,H61B), C63(H63A,
 H63B)
4.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C14(H14), C15(H15), C16(H16), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C45(H45), C46(H46), C47(H47)
4.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C36(H36A,H36B,H36C), C38(H38A,
 H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C27B(H27D,H27E,H27F),
 C29B(H29D,H29E,H29F), C62(H62B,H62C,H62A), C64(H64A,H64B,H64C)
;
_shelx_res_checksum              86811
_shelx_hkl_checksum              11427
_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 1.256
_oxdiff_exptl_absorpt_empirical_full_min 0.748