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_1567581
_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         'Cl, C53 H77 N2 O, H2 O'
_chemical_formula_sum            'C53 H79 Cl N2 O2'
_chemical_formula_weight         811.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 107.607(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0058(6)
_cell_length_b                   18.6532(8)
_cell_length_c                   20.2559(8)
_cell_measurement_reflns_used    2088
_cell_measurement_temperature    150.3(5)
_cell_measurement_theta_max      24.4110
_cell_measurement_theta_min      2.4990
_cell_volume                     4683.9(4)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.3(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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     39.00 101.00   1.00  120.00    --   25.25 178.00 -30.00   62
  2  \w    -48.00  69.00   1.00  120.00    --   25.25 -19.00 -30.00  117
  3  \w   -103.00 -39.00   1.00  120.00    --  -27.12-178.00 -90.00   64
  4  \w      4.00  29.00   1.00  120.00    --   25.25  57.00   0.00   25
;
_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      -0.0185569000
_diffrn_orient_matrix_UB_12      0.0353530000
_diffrn_orient_matrix_UB_13      0.0024136000
_diffrn_orient_matrix_UB_21      -0.0426662000
_diffrn_orient_matrix_UB_22      -0.0053110000
_diffrn_orient_matrix_UB_23      -0.0311415000
_diffrn_orient_matrix_UB_31      -0.0333100000
_diffrn_orient_matrix_UB_32      -0.0129191000
_diffrn_orient_matrix_UB_33      0.0193822000
_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  0.1072
_diffrn_reflns_av_unetI/netI     0.1931
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22574
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.972
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.997
_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 violet'
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         9580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.1626
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0141P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4449
_reflns_number_total             9580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01895k2.cif
_cod_data_source_block           1HCl
_cod_database_code               1567581
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H70 N4 O1 Cl'
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.968
_reflns_odcompleteness_completeness 67.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1.a Free rotating group:
 O1W(H1WA,H1WB)
1.b Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C48(H48), C51(H51)
1.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C26(H26A,H26B), C28(H28A,H28B), C36(H36A,H36B),
 C38(H38A,H38B)
1.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), C44(H44), C45(H45), C46(H46)
1.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), C27(H27A,H27B,H27C), C29(H29A,
 H29B,H29C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              66160
_shelx_hkl_checksum              22130
_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 1.128
_oxdiff_exptl_absorpt_empirical_full_min 0.902