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_7708486
_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
'C272 H329 Cl2 Li10 N4 O30 Pb8, 5(C2 H3 N), 9[CH3CN]'
_chemical_formula_sum            'C282 H340 Cl2 Li10 N9 O30 Pb8'
_chemical_formula_weight         6133.43
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-09
_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                69.691(2)
_cell_angle_beta                 72.882(2)
_cell_angle_gamma                85.7680(10)
_cell_formula_units_Z            2
_cell_length_a                   23.1594(4)
_cell_length_b                   25.7268(4)
_cell_length_c                   28.7875(6)
_cell_measurement_reflns_used    78872
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8890
_cell_measurement_theta_min      2.9440
_cell_volume                     15365.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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 2014/5 (Sheldrick, 2014)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -106.00  19.00   1.00   17.50    --  -16.70 -57.00 -30.00  125
  2  \w   -106.00  22.00   1.00   17.50    --  -16.70 -72.00  60.00  128
  3  \w   -106.00  17.00   1.00   17.50    --  -16.70 -38.00-150.00  123
  4  \w    -55.00  73.00   1.00   17.50    --  -16.70  72.00 -30.00  128
  5  \w   -106.00  17.00   1.00   17.50    --  -16.70 -38.00  60.00  123
  6  \w   -106.00  22.00   1.00   17.50    --  -16.70 -72.00-150.00  128
  7  \w    -52.00  31.00   1.00   17.50    --  -16.70  57.00 -90.00   83
  8  \w    -55.00  73.00   1.00   17.50    --  -16.70  72.00 150.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_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      0.0254116000
_diffrn_orient_matrix_UB_12      0.0115471000
_diffrn_orient_matrix_UB_13      -0.0215851000
_diffrn_orient_matrix_UB_21      0.0131301000
_diffrn_orient_matrix_UB_22      0.0083228000
_diffrn_orient_matrix_UB_23      0.0157796000
_diffrn_orient_matrix_UB_31      0.0144866000
_diffrn_orient_matrix_UB_32      -0.0257390000
_diffrn_orient_matrix_UB_33      0.0061184000
_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  0.0644
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            327875
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.899
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    4.441
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
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    1.326
_exptl_crystal_description       irregular
_exptl_crystal_F_000             6110
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.926
_refine_diff_density_min         -1.582
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3093
_refine_ls_number_reflns         62724
_refine_ls_number_restraints     3492
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0943P)^2^+82.5990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1749
_refine_ls_wR_factor_ref         0.2026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                41423
_reflns_number_total             62724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02790e2.cif
_cod_data_source_block           2017ncs0767z
_cod_database_code               7708486
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pb (MeCN)(C66 H78 O6)'
_chemical_oxdiff_usercomment     Pb[6]
_shelx_estimated_absorpt_t_max   0.665
_shelx_estimated_absorpt_t_min   0.403
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 O(H) groups
2. Restrained distances
 H30-O25
 1.7 with sigma of 0.05
 H30-O30
 0.9 with sigma of 0.0125
 O4-H4
 0.85 with sigma of 0.01
 Li2-H4
 2.317229 with sigma of 0.02
 C34-H4
 1.856066 with sigma of 0.02
 C188-C192 \\sim C188-C193 \\sim C188-C194 \\sim C192-C193 \\sim C192-C194
\\sim C193-C194
 with sigma of 0.04
 C191-C188 \\sim C191-C192 \\sim C191-C193 \\sim C191-C194
 with sigma of 0.02
 C204-C201 \\sim C204-C205 \\sim C204-C206 \\sim C204-C207
 with sigma of 0.02
 C201-C205 \\sim C201-C206 \\sim C205-C206 \\sim C205-C207 \\sim C206-C207
 with sigma of 0.04
 C96-C100 \\sim C96-C102 \\sim C100-C101 \\sim C100-C102 \\sim C101-C102
 with sigma of 0.04
 C99-C96 \\sim C99-C100 \\sim C99-C101 \\sim C99-C102
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C206) = Uiso(C205) = Uiso(C207)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Rotating group:
 O30(H30)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C33(H33A,H33B), C44(H44A,H44B), C55(H55A,
 H55B), C66(H66A,H66B), C81(H81A,H81B), C92(H92A,H92B), C103(H10M,H10N),
 C114(H11L,H11M), C125(H12J,H12K), C136(H13J,H13K), C151(H15D,H15E), C162(H16G,
 H16H), C173(H17A,H17B), C184(H18J,H18K), C197(H19D,H19E), C208(H20D,H20E),
 C221(H22F,H22G), C232(H23G,H23H), C243(H24J,H24K), C254(H25J,H25K), C265(H26J,
 H26K), C276(H27J,H27K)
5.c 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), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C102(H10J,H10K,H10L)
5.d Me refined as rotating group:
 C89(H89A,H89B,H89C), C100(H10D,H10E,H10F), C101(H10G,H10H,H10I), C112(H11F,
 H11G,H11H), C181(H18A,H18B,H18C), C182(H18D,H18E,H18F), C183(H18G,H18H,H18I),
 C262(H26A,H26B,H26C), C263(H26D,H26E,H26F), C264(H26G,H26H,H26I), C192(H19F,
 H19G,H19H), C193(H19I,H19J,H19K), C194(H19L,H19M,H19N), C205(H20F,H20G,H20H),
 C206(H20I,H20J,H20K), C207(H20L,H20M,H20N)
5.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C14(H14), C16(H16), C25(H25), C27(H27), C36(H36), C38(H38),
 C49(H49), C58(H58), C60(H60), C73(H73), C75(H75), C84(H84), C86(H86), C95(H95),
  C97(H97), C106(H106), C108(H108), C117(H117), C119(H119), C128(H128),
 C130(H130), C143(H143), C145(H145), C154(H154), C156(H156), C165(H165),
 C167(H167), C176(H176), C178(H178), C187(H187), C189(H189), C200(H200),
 C202(H202), C213(H213), C215(H215), C224(H224), C226(H226), C235(H235),
 C237(H237), C246(H246), C248(H248), C257(H257), C259(H259), C268(H268),
 C270(H270)
5.f Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C),
 C80(H80A,H80B,H80C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C111(H11C,H11D,
 H11E), C113(H11I,H11J,H11K), C122(H12A,H12B,H12C), C123(H12D,H12E,H12F),
 C124(H12G,H12H,H12I), C133(H13A,H13B,H13C), C134(H13D,H13E,H13F), C135(H13G,
 H13H,H13I), C148(H14A,H14B,H14C), C149(H14D,H14E,H14F), C150(H15A,H15B,H15C),
 C159(H15F,H15G,H15H), C160(H16A,H16B,H16C), C161(H16D,H16E,H16F), C370(H37A,
 H37B,H37C), C371(H37D,H37E,H37F), C372(H37G,H37H,H37I), C218(H21D,H21E,H21F),
 C219(H21G,H21H,H21I), C220(H22C,H22D,H22E), C229(H22H,H22I,H22J), C230(H23A,
 H23B,H23C), C231(H23D,H23E,H23F), C240(H24A,H24B,H24C), C241(H24D,H24E,H24F),
 C242(H24G,H24H,H24I), C251(H25A,H25B,H25C), C252(H25D,H25E,H25F), C253(H25G,
 H25H,H25I), C273(H27A,H27B,H27C), C274(H27D,H27E,H27F), C275(H27G,H27H,H27I),
 C306(H30J,H30K,H30L), C308(H30M,H30N,H30O), C310(H31J,H31K,H31L), C312(H31D,
 H31E,H31F), C314(H31M,H31N,H31O), C316(H31P,H31Q,H31R), C302(H30D,H30E,H30F),
 C304(H30G,H30H,H30I), C318(H31G,H31H,H31I)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 396 electrons were 
found in a volume of 3605\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
9[CH3CN] per Unit Cell 
which account for 396 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2555
_shelx_hkl_checksum              46708
_shelx_fab_checksum              31521
_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 1.566
_oxdiff_exptl_absorpt_empirical_full_min 0.727