Lead calix[n]arenes (n=4, 6, 8): Structures and ring opening homo-/co-polymerization capability for cyclic esters
Xing, Tian; Prior, Timothy J.; Redshaw, Carl; Dalton Transactions  (2021) –; doi:10.1039/D1DT02790E

data_7708489
_publ_section_title
;
 Lead calix[n]arenes (n=4, 6, 8): Structures and ring opening
 homo-/co-polymerization capability for cyclic esters
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02790E
_journal_year                    2021
_chemical_formula_moiety         'C66 H78 Cl0.5 Li O8.5 Pb5, C2 H3 N'
_chemical_formula_sum            'C68 H81 Cl0.5 Li N O8.5 Pb5'
_chemical_formula_weight         2108.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-08-10 deposited with the CCDC.	2021-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.5489(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.7928(2)
_cell_length_b                   33.7801(3)
_cell_length_c                   24.5621(3)
_cell_measurement_reflns_used    67496
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6540
_cell_measurement_theta_min      1.9580
_cell_volume                     15821.3(3)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.904
_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    7.00    --    5.00  -9.00 -57.00  356
  2  \w   -106.00   4.00   0.50    7.00    --  -16.80  -9.00 -57.00  220
  3  \w    -41.00 -16.00   0.50    7.00    --  -16.80   9.00 116.00   50
  4  \w    -19.00   6.00   0.50    7.00    --    5.00   9.00 116.00   50
  5  \w     16.00  41.00   0.50    7.00    --    5.00 -60.00-180.00   50
  6  \w    -53.00  56.00   0.50    7.00    --  -16.80  57.00-180.00  218
  7  \w    -52.00  13.00   0.50    7.00    --  -16.80  60.00-150.00  130
  8  \w    -25.00  20.00   0.50    7.00    --  -16.80 -60.00 120.00   90
  9  \w    -53.00  73.00   0.50    7.00    --  -16.80  57.00 -60.00  252
 10  \w   -106.00  40.00   0.50    7.00    --  -16.80 -38.00-120.00  292
 11  \w    -53.00  16.00   0.50    7.00    --  -16.80  60.00  90.00  138
 12  \w   -106.00  20.00   0.50    7.00    --  -16.80 -60.00-150.00  252
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0359798000
_diffrn_orient_matrix_UB_12      0.0023853000
_diffrn_orient_matrix_UB_13      -0.0143651000
_diffrn_orient_matrix_UB_21      0.0087797000
_diffrn_orient_matrix_UB_22      0.0013222000
_diffrn_orient_matrix_UB_23      -0.0261155000
_diffrn_orient_matrix_UB_31      -0.0035416000
_diffrn_orient_matrix_UB_32      -0.0208085000
_diffrn_orient_matrix_UB_33      -0.0032883000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            211141
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.965
_diffrn_reflns_theta_min         1.721
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    10.668
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.771
_exptl_crystal_description       prism
_exptl_crystal_F_000             7884
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.794
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         24791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+34.1449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18155
_reflns_number_total             24791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02790e2.cif
_cod_data_source_block           2021ncs0003z
_cod_original_formula_sum        'C68 H81 Cl0.50 Li N O8.50 Pb5'
_cod_database_code               7708489
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C70 H70 N4 O8 Pb4'
_chemical_oxdiff_usercomment     calixzrene(6)arene+4Pb(N(TMS)2)2
_cell_oxdiff_angle_alpha         89.9749(6)
_cell_oxdiff_angle_beta          105.5572(7)
_cell_oxdiff_angle_gamma         89.9699(6)
_cell_oxdiff_length_a            19.78996(16)
_cell_oxdiff_length_b            33.7979(2)
_cell_oxdiff_length_c            24.55360(16)
_cell_oxdiff_measurement_reflns_used 67495
_cell_oxdiff_volume              15821.2(2)
_shelx_estimated_absorpt_t_max   0.522
_shelx_estimated_absorpt_t_min   0.447
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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
Uiso(Cl1) = Uiso(O7)
3. Others
 Fixed Sof: Cl1(0.5) O7(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C33(H33A,H33B), C11(H11A,H11B), C44(H44A,H44B), C66(H66A,
 H66B), C22(H22A,H22B)
4.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C47(H47), C27(H27), C60(H60), C16(H16), C5(H5), C38(H38), C14(H14),
 C49(H49), C3(H3), C58(H58), C25(H25)
4.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C41(H41A,H41B,H41C), C63(H63A,H63B,
 H63C), C42(H42A,H42B,H42C), C65(H65A,H65B,H65C), C64(H64A,H64B,H64C), C68(H68A,
 H68B,H68C), C54(H54A,H54B,H54C), C43(H43A,H43B,H43C), C19(H19A,H19B,H19C),
 C10(H10A,H10B,H10C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C9(H9A,H9B,H9C),
  C8(H8A,H8B,H8C), C30(H30A,H30B,H30C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 652 electrons were 
found in a volume of 4076\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
3.75[CH3CN] per Asymmetric Unit 
which account for 660 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              5330
_shelx_hkl_checksum              88603
_shelx_fab_checksum              7140
_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 2.831
_oxdiff_exptl_absorpt_empirical_full_min 0.235