Self-assembly of M4L4 Tetrahedral Cages Incorporating Pendant P=S and P=Se Functionalised Ligands
Butler, Patrick; Kruger, Paul; Ward, Jas S.; Chemical Communications  (2019) –; doi:10.1039/C9CC05443J

data_7123952
_publ_section_title
;
 Self-assembly of M4L4 Tetrahedral Cages Incorporating Pendant P=S and
 P=Se Functionalised Ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05443J
_journal_year                    2019
_chemical_formula_moiety         'C18 H18 N3 P S4'
_chemical_formula_sum            'C18 H18 N3 P S4'
_chemical_formula_weight         435.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-03 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                91.015(3)
_cell_angle_beta                 92.969(4)
_cell_angle_gamma                98.585(4)
_cell_formula_units_Z            4
_cell_length_a                   9.7504(5)
_cell_length_b                   10.5449(3)
_cell_length_c                   19.9570(7)
_cell_measurement_reflns_used    8388
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6820
_cell_measurement_theta_min      4.5520
_cell_volume                     2025.53(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_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    -30.00  54.00   1.00    2.00    --   37.04 -57.00 150.00   84
  2  \w      8.00 108.00   1.00    2.00    --   37.04  19.00  60.00  100
  3  \w      1.00  76.00   1.00    2.00    --   37.04 -99.00 120.00   75
  4  \w    -30.00  54.00   1.00    2.00    --   37.04 -57.00 -60.00   84
  5  \w     23.00  90.00   1.00    2.00    --   37.04-125.00  30.00   67
  6  \w     18.00 106.00   1.00    2.00    --   37.04  38.00 120.00   88
  7  \w    -30.00  54.00   1.00    2.00    --   37.04 -57.00-120.00   84
  8  \w      1.00  76.00   1.00    2.00    --   37.04 -99.00-120.00   75
  9  \w     43.00 128.00   1.00   20.00    --  111.00 -50.00 120.00   85
 10  \w     41.00 113.00   1.00   20.00    --  111.00-111.00   0.00   72
 11  \w     44.00 131.00   1.00   20.00    --  111.00 -64.00 -90.00   87
 12  \w     42.00 130.00   1.00   20.00    --  111.00 -38.00  30.00   88
 13  \w     86.00 178.00   1.00   20.00    --  111.00  25.00-150.00   92
 14  \w     42.00 130.00   1.00   20.00    --  111.00 -38.00-120.00   88
 15  \w     65.00 178.00   1.00   20.00    --  111.00  12.00  30.00  113
 16  \w     84.00 178.00   1.00   20.00    --  111.00  77.00  30.00   94
 17  \w     92.00 178.00   1.00   20.00    --  111.00  38.00  90.00   86
 18  \w     42.00 109.00   1.00   20.00    --  111.00 -92.00 150.00   67
 19  \w     43.00 138.00   1.00   20.00    --  111.00 -77.00  30.00   95
 20  \w     42.00 109.00   1.00   20.00    --  111.00 -92.00-120.00   67
 21  \w   -105.00 -10.00   1.00    2.00    --  -37.04 -77.00   0.00   95
 22  \w   -105.00 -10.00   1.00    2.00    --  -37.04 -77.00 -90.00   95
 23  \w     18.00 106.00   1.00    2.00    --   37.04  38.00-150.00   88
 24  \w     10.00 105.00   1.00    2.00    --   37.04  77.00-150.00   95
 25  \w    -34.00  66.00   1.00    2.00    --   37.04 -19.00  30.00  100
 26  \w      4.00  33.00   1.00    2.00    --   37.04  89.00 123.18   29
 27  \w     86.00 178.00   1.00   20.00    --  111.00  25.00 -90.00   92
 28  \w     84.00 178.00   1.00   20.00    --  111.00  77.00   0.00   94
 29  \w     84.00 178.00   1.00   20.00    --  111.00  77.00 -30.00   94
 30  \w     86.00 178.00   1.00   20.00    --  111.00  25.00-180.00   92
 31  \w     94.00 178.00   1.00   20.00    --  111.00  50.00-150.00   84
 32  \w     92.00 178.00   1.00   20.00    --  111.00  38.00 -60.00   86
 33  \w     84.00 159.00   1.00   20.00    --  111.00  77.00-120.00   75
 34  \w     86.00 178.00   1.00   20.00    --  111.00  25.00 150.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0674446000
_diffrn_orient_matrix_UB_12      -0.0127244000
_diffrn_orient_matrix_UB_13      -0.0718073000
_diffrn_orient_matrix_UB_21      0.1003848000
_diffrn_orient_matrix_UB_22      0.1183583000
_diffrn_orient_matrix_UB_23      -0.0202583000
_diffrn_orient_matrix_UB_31      0.1048086000
_diffrn_orient_matrix_UB_32      -0.0876036000
_diffrn_orient_matrix_UB_33      -0.0203031000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27571
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.993
_diffrn_reflns_theta_min         4.242
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.116
_exptl_absorpt_correction_T_max  0.76727
_exptl_absorpt_correction_T_min  0.75475
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN evaporation'
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.047
_exptl_crystal_size_rad          0.036
_refine_diff_density_max         1.750
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0894
_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^)+(0.1308P)^2^+5.2849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2449
_refine_ls_wR_factor_ref         0.2565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6441
_reflns_number_total             8041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05443j2.cif
_cod_data_source_block           '[3b]'
_cod_database_code               7123952
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C18 H18 N3 P S4'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Rotating group:
 N3(H3A,H3B), N4(H4A,H4B), N2A(H2AA,H2AB), N3A(H3AA,H3AB)
2.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C24(H24), C25(H25), C31(H31), C32(H32), C34(H34),
 C35(H35), C41(H41), C42(H42), C44(H44), C45(H45), C21A(H21A), C22A(H22A),
 C24A(H24A), C25A(H25A), C31A(H31A), C32A(H32A), C34A(H34A), C35A(H35A),
 C41A(H41A), C42A(H42A), C44A(H44A), C45A(H45A)
;
_shelx_res_checksum              72477
_ins_header
;
TITL PB-5-227_c4_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   9.750379  10.544871  19.957043  91.0154  92.9692  98.5851
ZERR    4.00   0.000538   0.000319   0.000654   0.0026   0.0035   0.0035
LATT  1
SFAC C H N P S
UNIT 72.00 72.00 12.00 4.00 16.00
TREF
HKLF 4
END
;
_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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.770