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_7123951
_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 O3 P Se'
_chemical_formula_sum            'C18 H18 N3 O3 P Se'
_chemical_formula_weight         434.28
_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             2018-09-09
_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                77.237(6)
_cell_angle_beta                 78.194(6)
_cell_angle_gamma                66.810(7)
_cell_formula_units_Z            2
_cell_length_a                   9.8993(7)
_cell_length_b                   10.0421(7)
_cell_length_c                   10.7965(8)
_cell_measurement_reflns_used    5454
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6670
_cell_measurement_theta_min      4.8420
_cell_volume                     953.87(13)
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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     24.00  90.00   1.00    7.00    --   36.95-125.00 150.00   66
  2  \w      5.00  33.00   1.00    7.00    --   36.95 -57.00  60.00   28
  3  \w     11.00  64.00   1.00    7.00    --   36.95 -77.00 -60.00   53
  4  \w    -32.00  55.00   1.00    7.00    --   36.95 -38.00   0.00   87
  5  \w     33.00  82.00   1.00    7.00    --   36.95  57.00-120.00   49
  6  \w     55.00 104.00   1.00    7.00    --   36.95  57.00 -90.00   49
  7  \w     24.00  84.00   1.00    7.00    --   36.95-125.00-120.00   60
  8  \w     24.00 105.00   1.00    7.00    --   36.95  38.00-180.00   81
  9  \w     53.00 101.00   1.00    7.00    --   36.95  38.00 -30.00   48
 10  \w     50.00  81.00   1.00    7.00    --   36.95-125.00  30.00   31
 11  \w     52.00 128.00   1.00   22.00    --  111.00 -50.00  30.00   76
 12  \w    114.00 140.00   1.00   22.00    --  111.00  50.00   0.00   26
 13  \w     42.00  70.00   1.00   22.00    --  111.00-111.00  60.00   28
 14  \w     85.00 112.00   1.00   22.00    --  111.00-111.00  60.00   27
 15  \w     88.00 113.00   1.00   22.00    --  111.00-111.00 -60.00   25
 16  \w     87.00 129.00   1.00   22.00    --  111.00  25.00  90.00   42
 17  \w     94.00 134.00   1.00   22.00    --  111.00 -72.00-161.81   40
 18  \w     79.00 105.00   1.00   22.00    --  111.00-119.00   1.00   26
 19  \w    119.00 177.00   1.00   22.00    --  111.00  64.00 -30.00   58
 20  \w    141.00 178.00   1.00   22.00    --  111.00  64.00 -60.00   37
 21  \w     43.00  69.00   1.00   22.00    --  111.00 -92.00  90.00   26
 22  \w     44.00  70.00   1.00   22.00    --  111.00-111.00 -60.00   26
 23  \w     48.00  74.00   1.00   22.00    --  111.00-119.00   1.00   26
 24  \w     86.00 112.00   1.00   22.00    --  111.00  77.00  60.00   26
 25  \w    138.00 176.00   1.00   22.00    --  111.00  77.00  60.00   38
 26  \w     60.00 106.00   1.00   22.00    --  111.00 -92.00-150.00   46
 27  \w     42.00  68.00   1.00   22.00    --  111.00-111.00  30.00   26
 28  \w     88.00 113.00   1.00   22.00    --  111.00-111.00  30.00   25
 29  \w     42.00 113.00   1.00   22.00    --  111.00-111.00 150.00   71
 30  \w     79.00 110.00   1.00   22.00    --  111.00  12.00 -90.00   31
 31  \w    104.00 170.00   1.00   22.00    --  111.00  38.00  30.00   66
 32  \w     98.00 124.00   1.00   22.00    --  111.00  64.00 -60.00   26
 33  \w     53.00  78.00   1.00   22.00    --  111.00 -92.00 150.00   25
 34  \w     54.00 110.00   1.00   22.00    --  111.00-111.00-150.00   56
 35  \w    131.00 178.00   1.00   22.00    --  111.00  50.00 150.00   47
 36  \w    129.00 155.00   1.00   22.00    --  111.00  12.00 -90.00   26
 37  \w    141.00 168.00   1.00   22.00    --  111.00  50.00-120.00   27
 38  \w     48.00 118.00   1.00   22.00    --  111.00 -38.00 150.00   70
 39  \w     60.00  87.00   1.00   22.00    --  111.00 -92.00 -60.00   27
 40  \w     73.00 100.00   1.00   22.00    --  111.00 -92.00  60.00   27
 41  \w     92.00 178.00   1.00   22.00    --  111.00  38.00 120.00   86
 42  \w     51.00  85.00   1.00   22.00    --  111.00 -72.00-161.81   34
 43  \w     60.00  85.00   1.00   22.00    --  111.00 -92.00 -30.00   25
 44  \w     85.00 110.00   1.00   22.00    --  111.00-111.00-120.00   25
 45  \w    106.00 132.00   1.00   22.00    --  111.00 111.00  60.00   26
 46  \w     97.00 123.00   1.00   22.00    --  111.00  25.00 -90.00   26
 47  \w     50.00 128.00   1.00   22.00    --  111.00 -70.00 -46.75   78
;
_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      0.0882804000
_diffrn_orient_matrix_UB_12      0.0484388000
_diffrn_orient_matrix_UB_13      0.0715148000
_diffrn_orient_matrix_UB_21      0.0212892000
_diffrn_orient_matrix_UB_22      0.1101364000
_diffrn_orient_matrix_UB_23      -0.1194662000
_diffrn_orient_matrix_UB_31      -0.1446324000
_diffrn_orient_matrix_UB_32      0.1186259000
_diffrn_orient_matrix_UB_33      0.0489262000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9196
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.857
_diffrn_reflns_theta_min         4.235
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.512
_exptl_crystal_description       plate
_exptl_crystal_F_000             440
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN evaporation'
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0720P)^2^+0.3318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3563
_reflns_number_total             3851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05443j2.cif
_cod_data_source_block           '[2b]'
_cod_database_code               7123951
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.730
_reflns_odcompleteness_completeness 98.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H) groups, All N(H,H) groups
2.a Rotating group:
 N1(H1A,H1B), N2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), C21(H21), C22(H22), C24(H24),
 C25(H25), C31(H31), C32(H32), C34(H34), C35(H35)
;
_shelx_res_checksum              85450
_ins_header
;
TITL PB-4-146_NH2_c2_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   9.899314  10.042122  10.796461  77.2372  78.1940  66.8097
ZERR    2.00   0.000698   0.000704   0.000770   0.0060   0.0060   0.0067
LATT  1
SFAC C H N O P Se
UNIT 36.00 36.00 6.00 6.00 2.00 2.00
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 1.351
_oxdiff_exptl_absorpt_empirical_full_min 0.754