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_1567580
_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         '2(C26.5 H38 N O0.5)'
_chemical_formula_sum            'C53 H76 N2 O'
_chemical_formula_weight         757.15
_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   difmap
_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                109.830(4)
_cell_angle_beta                 93.980(3)
_cell_angle_gamma                103.160(3)
_cell_formula_units_Z            4
_cell_length_a                   14.2247(5)
_cell_length_b                   18.7107(6)
_cell_length_c                   19.0753(10)
_cell_measurement_reflns_used    6745
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.8450
_cell_measurement_theta_min      2.6070
_cell_volume                     4590.5(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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_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    -19.00  98.00   1.00   40.00    --   25.25  19.00 120.00  117
  2  \w     -5.00  42.00   1.00   40.00    --   25.25  79.00-124.00   47
  3  \w    -20.00  67.00   1.00   40.00    --   25.25 -99.00  60.00   87
  4  \w      4.00  94.00   1.00   40.00    --   25.25  57.00-180.00   90
  5  \w    -57.00  39.00   1.00   40.00    --  -27.12  77.00 -60.00   96
  6  \w   -100.00 -52.00   1.00   40.00    --  -27.12 -37.00 -90.00   48
;
_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      0.0008609000
_diffrn_orient_matrix_UB_12      -0.0079148000
_diffrn_orient_matrix_UB_13      0.0338309000
_diffrn_orient_matrix_UB_21      0.0463592000
_diffrn_orient_matrix_UB_22      -0.0075825000
_diffrn_orient_matrix_UB_23      -0.0040174000
_diffrn_orient_matrix_UB_31      0.0232677000
_diffrn_orient_matrix_UB_32      0.0403627000
_diffrn_orient_matrix_UB_33      0.0210447000
_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  0.0518
_diffrn_reflns_av_unetI/netI     0.0957
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41469
_diffrn_reflns_point_group_measured_fraction_full 0.999
_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         1.942
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.998
_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 colourless'
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1617
_refine_ls_number_reflns         18741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0366P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11281
_reflns_number_total             18741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01895k2.cif
_cod_data_source_block           c1
_cod_original_cell_volume        4590.5(3)
_cod_database_code               1567580
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.981
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
;
_shelx_res_checksum              62767
_shelx_hkl_checksum              18038
_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 1.071
_oxdiff_exptl_absorpt_empirical_full_min 0.913