Scandium calix[<i>n</i>]arenes (<i>n</i> = 4, 6, 8): structural, cytotoxicity and ring opening polymerization studies.
Alshamrani, Abdullah Fahad A.; Santoro, Orlando; Prior, Timothy J.; Alamri, Mohammed A.; Stasiuk, Graeme J.; Elsegood, Mark R. J.; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8302–8306; doi:10.1039/d1dt01330k

data_7707551
_publ_section_title
;
 Scandium calix[<i>n</i>]arenes (<i>n</i> = 4, 6, 8): structural,
 cytotoxicity and ring opening polymerization studies.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8302
_journal_page_last               8306
_journal_paper_doi               10.1039/d1dt01330k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C100 H140 O16 S6 Sc4, 4[C2H6SO]'
_chemical_formula_sum            'C100 H140 O16 S6 Sc4'
_chemical_formula_weight         1970.31
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-05-25 deposited with the CCDC.	2021-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                103.3612(14)
_cell_angle_beta                 107.4938(12)
_cell_angle_gamma                101.4307(14)
_cell_formula_units_Z            1
_cell_length_a                   12.72128(15)
_cell_length_b                   13.4172(2)
_cell_length_c                   19.4141(3)
_cell_measurement_reflns_used    29917
_cell_measurement_temperature    99.9(7)
_cell_measurement_theta_max      70.0640
_cell_measurement_theta_min      3.6340
_cell_volume                     2944.19(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_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      99.9(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_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    -89.00  89.00   0.50    0.50    --    0.00   0.00-180.00  356
  2  \w    -84.00  94.00   0.50    2.00    --    5.00  49.00 -60.00  356
  3  \w   -179.00  -1.00   0.50    2.00    --  -90.00  54.00  19.18  356
  4  \w   -179.00  -1.00   0.50    2.00    --  -90.00  59.00-104.40  356
  5  \w   -179.00  -1.00   0.50    2.00    --  -90.00  39.00 -30.00  356
  6  \w   -179.00  -1.00   0.50    2.00    --  -90.00  51.00 102.32  356
  7  \w   -179.00  -1.00   0.50    2.00    --  -90.00  59.00  63.65  356
  8  \w   -179.00  -1.00   0.50    2.00    --  -90.00  59.00-168.45  356
  9  \w   -179.00  -8.00   0.50    2.00    --  -90.00  59.00 -63.55  342
 10  \w   -170.00-139.00   0.50    2.00    --  -90.00  59.00 -32.17   62
 11  \w   -179.00  -1.00   0.50    2.00    --  -90.00   0.00-180.00  356
 12  \w   -134.00 -92.00   0.50    2.00    --  -90.00  59.00 -32.17   84
 13  \w    -70.00 -26.00   0.50    2.00    --  -90.00  59.00 -32.17   88
 14  \w   -122.00 -96.00   0.50    2.00    --  -90.00  39.00 -30.00   52
 15  \w   -115.00 -89.00   0.50    2.00    --  -90.00  59.00 143.22   52
 16  \w    -67.00 -41.00   0.50    2.00    --  -90.00  59.00 143.22   52
 17  \w   -170.00-119.00   0.50    2.00    --  -90.00  59.00   1.28  102
 18  \w   -179.00 -77.00   0.50    2.00    --  -90.00  49.00-120.00  204
 19  \w   -171.00 -14.00   0.50    2.00    --  -90.00  53.00 135.80  314
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0788096000
_diffrn_orient_matrix_UB_12      0.0383038000
_diffrn_orient_matrix_UB_13      0.0844059000
_diffrn_orient_matrix_UB_21      -0.1066384000
_diffrn_orient_matrix_UB_22      -0.0176622000
_diffrn_orient_matrix_UB_23      0.0227679000
_diffrn_orient_matrix_UB_31      0.0016221000
_diffrn_orient_matrix_UB_32      -0.1158109000
_diffrn_orient_matrix_UB_33      -0.0045229000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54284
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.061
_diffrn_reflns_theta_min         3.536
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.00035(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         11001
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0564P)^2^+1.4977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10271
_reflns_number_total             11001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01330k2.cif
_cod_data_source_block           structure1
_cod_depositor_comments
'Adding full bibliography for 7707550--7707558.cif.'
_cod_original_cell_volume        2944.18(8)
_cod_database_code               7707551
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H52 O4 Sc (C2 H6 O S)'
_chemical_oxdiff_usercomment     Calix[4]ScOTf
_cell_oxdiff_angle_alpha         103.3612(14)
_cell_oxdiff_angle_beta          107.4938(12)
_cell_oxdiff_angle_gamma         101.4307(14)
_cell_oxdiff_length_a            12.72128(15)
_cell_oxdiff_length_b            13.4172(2)
_cell_oxdiff_length_c            19.4141(3)
_cell_oxdiff_measurement_reflns_used 29917
_cell_oxdiff_volume              2944.18(8)
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.826
_reflns_odcompleteness_completeness 98.43
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C56B \\sim C56A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C51B \\sim C51A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C55B \\sim C55A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C52A \\sim C52B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
S3B \\sim S3A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
S1A \\sim S1B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C10B \\sim C10A \\sim C9A \\sim C9B \\sim C8A \\sim C8B: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 O8, S3B, C55B, C55A, S3A, C56B, C56A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, S1A, S1B, C51B, C51A, C52A, C52B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, H5, C7, C8A, C9A, C10A, C8B, C9B, C10B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(S1B)=Sof(C51B)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52B)=Sof(H52D)=
 Sof(H52E)=Sof(H52F)=1-FVAR(1)
 Sof(S1A)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52A)=Sof(H52A)=
 Sof(H52B)=Sof(H52C)=FVAR(1)
 Sof(S3B)=Sof(C55B)=Sof(H55D)=Sof(H55E)=Sof(H55F)=Sof(C56B)=Sof(H56D)=
 Sof(H56E)=Sof(H56F)=1-FVAR(2)
 Sof(S3A)=Sof(C55A)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C56A)=Sof(H56A)=
 Sof(H56B)=Sof(H56C)=FVAR(2)
 Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=
 Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(3)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C33(H33A,H33B), C44(H44A,H44B)
5.b Me refined with riding coordinates:
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C8B(H8BA,H8BB,
 H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C51A(H51A,H51B,H51C),
 C52A(H52A,H52B,H52C), C51B(H51D,H51E,H51F), C52B(H52D,H52E,H52F), C55A(H55A,
 H55B,H55C), C56A(H56A,H56B,H56C), C55B(H55D,H55E,H55F), C56B(H56D,H56E,H56F)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C14(H14), C16(H16), C25(H25), C27(H27), C36(H36), C38(H38)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 156 electrons were 
found in a volume of 604\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[C2H6SO] per Unit Cell 
which account for 168 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60068
_shelx_fab_checksum              52614
_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 3.668
_oxdiff_exptl_absorpt_empirical_full_min 0.737