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_1567583
_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 H2 Cl2, 2(F6 P), C53 H76 N2 O'
_chemical_formula_sum            'C54 H78 Cl2 F12 N2 O P2'
_chemical_formula_weight         1132.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 97.129(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1520(8)
_cell_length_b                   31.9515(18)
_cell_length_c                   14.2567(7)
_cell_measurement_reflns_used    3631
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      21.4940
_cell_measurement_theta_min      2.1140
_cell_volume                     5492.7(6)
_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 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -20.00  67.00   1.00  120.00    --   25.25 -99.00  60.00   87
  2  \w    -96.00  -6.00   1.00  120.00    --  -27.12 -57.00  90.00   90
  3  \w   -104.00 -35.00   1.00  120.00    --  -27.12 178.00-150.00   69
  4  \w   -100.00  46.00   1.00  120.00    --  -27.12   0.00-150.00  146
  5  \w    -96.00  -6.00   1.00  120.00    --  -27.12 -57.00-180.00   90
;
_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      -0.0583550000
_diffrn_orient_matrix_UB_12      0.0024277000
_diffrn_orient_matrix_UB_13      -0.0090420000
_diffrn_orient_matrix_UB_21      0.0071973000
_diffrn_orient_matrix_UB_22      0.0203203000
_diffrn_orient_matrix_UB_23      -0.0183329000
_diffrn_orient_matrix_UB_31      0.0006106000
_diffrn_orient_matrix_UB_32      -0.0086289000
_diffrn_orient_matrix_UB_33      -0.0457852000
_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  0.1883
_diffrn_reflns_av_unetI/netI     0.2034
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47920
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.923
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.990
_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 light yellow'
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       needle
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         11219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.2151
_refine_ls_R_factor_gt           0.0942
_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^)+(0.0850P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2009
_refine_ls_wR_factor_ref         0.2575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4613
_reflns_number_total             11219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01895k2.cif
_cod_data_source_block           1(PF6)2
_cod_database_code               1567583
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H40 N2 O1 P F6'
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.807
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C48(H48), C51(H51)
1.b Secondary CH2 refined with riding coordinates:
 C1CL(H1CA,H1CB), C7(H7A,H7B), C10(H10A,H10B), C26(H26A,H26B), C28(H28A,H28B),
 C36(H36A,H36B), C38(H38A,H38B)
1.c 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.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24B,H24A,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              28007
_shelx_hkl_checksum              49188
_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 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.635