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_7707554
_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         'C148 H204 O20 S8 Sc4, 2(C3 H6 O), 6[C2H6SO]'
_chemical_formula_sum            'C154 H216 O22 S8 Sc4'
_chemical_formula_weight         2855.58
_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                84.7397(6)
_cell_angle_beta                 73.4252(7)
_cell_angle_gamma                63.7025(9)
_cell_formula_units_Z            1
_cell_length_a                   16.60531(16)
_cell_length_b                   16.72546(15)
_cell_length_c                   19.20582(12)
_cell_measurement_reflns_used    53192
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      70.1750
_cell_measurement_theta_min      2.3760
_cell_volume                     4579.57(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_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    -84.00  94.00   0.50    0.50    --    5.00  30.00  30.00  356
  2  \w   -141.00  37.00   0.50    0.50    --  -52.10  48.00 -94.57  356
  3  \w   -141.00  37.00   0.50    0.50    --  -52.10  20.00-150.00  356
  4  \w   -179.00  -1.00   0.50    2.00    --  -90.00  56.00 -65.62  356
  5  \w   -179.00  -1.00   0.50    2.00    --  -90.00  51.00-125.85  356
  6  \w   -179.00  -1.00   0.50    2.00    --  -90.00  59.00  -5.71  356
  7  \w   -179.00 -91.00   0.50    2.00    --  -90.00  59.00 -68.87  176
  8  \w   -167.00 -20.00   0.50    2.00    --  -90.00  59.00 107.90  294
  9  \w   -167.00-138.00   0.50    2.00    --  -90.00  53.00 -18.06   58
 10  \w   -178.00  -1.00   0.50    2.00    --  -90.00  10.00 150.00  354
 11  \w   -178.00-119.00   0.50    2.00    --  -90.00  59.00-112.54  118
 12  \w   -102.00 -48.00   0.50    2.00    --  -90.00  59.00-112.54  108
 13  \w   -143.00  -1.00   0.50    2.00    --  -90.00  39.00   0.00  284
 14  \w   -179.00-149.00   0.50    2.00    --  -90.00  39.00   0.00   60
 15  \w   -179.00-110.00   0.50    2.00    --  -90.00  59.00  77.32  138
 16  \w    -62.00  -1.00   0.50    2.00    --  -90.00  59.00  77.32  122
 17  \w    -58.00 -22.00   0.50    2.00    --  -90.00  51.00-125.85   72
 18  \w   -129.00 -94.00   0.50    2.00    --  -90.00  10.00   0.00   70
 19  \w    -51.00 -25.00   0.50    2.00    --  -90.00  10.00   0.00   52
 20  \w    -60.00 -35.00   0.50    2.00    --  -90.00  59.00 167.88   50
 21  \w   -164.00 -90.00   0.50    2.00    --  -90.00  59.00 135.61  148
 22  \w   -172.00-146.00   0.50    2.00    --  -90.00  59.00-175.78   52
 23  \w    -51.00 -25.00   0.50    2.00    --  -90.00  59.00-175.78   52
 24  \w   -169.00 -77.00   0.50    2.00    --  -90.00  59.00 167.88  184
;
_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      0.0628237000
_diffrn_orient_matrix_UB_12      0.0476543000
_diffrn_orient_matrix_UB_13      -0.0076074000
_diffrn_orient_matrix_UB_21      0.0308361000
_diffrn_orient_matrix_UB_22      -0.0160846000
_diffrn_orient_matrix_UB_23      -0.0831198000
_diffrn_orient_matrix_UB_31      -0.0817382000
_diffrn_orient_matrix_UB_32      0.0896857000
_diffrn_orient_matrix_UB_33      -0.0069866000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            85195
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.402
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         16607
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0645P)^2^+4.8767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15878
_reflns_number_total             16607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01330k2.cif
_cod_data_source_block           2019ncsx0121
_cod_depositor_comments
'Adding full bibliography for 7707550--7707558.cif.'
_cod_original_cell_volume        4579.58(7)
_cod_database_code               7707554
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C152 H218 O22 S8 Sc4'
_chemical_oxdiff_usercomment     '[6]ScOTf'
_cell_oxdiff_angle_alpha         84.7397(6)
_cell_oxdiff_angle_beta          73.4252(7)
_cell_oxdiff_angle_gamma         63.7025(9)
_cell_oxdiff_length_a            16.60531(16)
_cell_oxdiff_length_b            16.72546(15)
_cell_oxdiff_length_c            19.20582(12)
_cell_oxdiff_measurement_reflns_used 53192
_cell_oxdiff_volume              4579.58(6)
_reflns_odcompleteness_completeness 99.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
S2A \\sim S2B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
S3A \\sim S3B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C73 \\sim C74: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(S2A) = Uanis(S2B)
Uanis(S3A) = Uanis(S3B)
3. Rigid body (RIGU) restrains
 S2A, S2B, O8, C73, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S3A, S3B, O9, C75, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(S2B)=Sof(H73D)=Sof(H73E)=Sof(H73F)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(1)
 Sof(S2A)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(1)
 Sof(S3B)=Sof(H75D)=Sof(H75E)=Sof(H75F)=Sof(H76D)=Sof(H76E)=Sof(H76F)=1-FVAR(2)
 Sof(S3A)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(H76A)=Sof(H76B)=Sof(H76C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C33(H33A,H33B), C44(H44A,H44B), C55(H55A,
 H55B), C66(H66A,H66B)
5.b Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), 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), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C73(H73D,H73E,H73F), C74(H74A,
 H74B,H74C), C74(H74D,H74E,H74F), C75(H75A,H75B,H75C), C75(H75D,H75E,H75F),
 C76(H76A,H76B,H76C), C76(H76D,H76E,H76F), C77(H77A,H77B,H77C), C78(H78A,H78B,
 H78C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C)
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),
 C47(H47), C49(H49), C58(H58), C60(H60)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 272 electrons were 
found in a volume of 992\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
6[C2H6SO] per Unit Cell 
which account for 252 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              21369
_shelx_fab_checksum              33445
_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 3.602
_oxdiff_exptl_absorpt_empirical_full_min 0.532