Phosphorylated-calix[4]arene double-deckers of single rare earth metal ions.
Hosseinzadeh, Marjan; Sanz, Sergio; van Leusen, Jan; Izarova, Natalya V.; Brechin, Euan K.; Dalgarno, Scott J.; Kögerler, Paul; Chemical communications (Cambridge, England) 57 (2021) 8087–8090; doi:10.1039/d1cc02910j

data_7128677
_publ_section_title
;
 Phosphorylated-calix[4]arene double-deckers of single rare earth metal
 ions.
;
_journal_issue                   65
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8087
_journal_page_last               8090
_journal_paper_doi               10.1039/d1cc02910j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C120 H184 Dy O32 P8, 2(C F3 O3 S)'
_chemical_formula_sum            'C123 H184 Dy F9 O41 P8 S3'
_chemical_formula_weight         2996.13
_chemical_name_common            DyL2
_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             2021-05-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-21 deposited with the CCDC.	2021-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                77.616(7)
_cell_angle_beta                 75.227(7)
_cell_angle_gamma                86.972(16)
_cell_formula_units_Z            2
_cell_length_a                   16.141(4)
_cell_length_b                   24.753(6)
_cell_length_c                   25.146(7)
_cell_measurement_reflns_used    9206
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      58.561
_cell_measurement_theta_min      2.873
_cell_volume                     9489(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            126160
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        59.174
_diffrn_reflns_theta_max         59.174
_diffrn_reflns_theta_min         1.827
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.621
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1082 before and 0.0843 after correction.
The Ratio of minimum to maximum transmission is 0.7407.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3130
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.119
_refine_diff_density_max         1.172
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1502
_refine_ls_number_reflns         27054
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0844
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1600P)^2^+10.3791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2372
_refine_ls_wR_factor_ref         0.2608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19152
_reflns_number_total             27054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02910j2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7128677.cif.'
_cod_original_cell_volume        9488(4)
_cod_database_code               7128677
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.673
_shelx_estimated_absorpt_t_min   0.404
_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. Restrained distances
 C96-C95 = C97-C95 = C98-C95 = C99-C95 = C95-C101 = C95-C100
 1.54 with sigma of 0.02
 C35-C29 = C34-C29 = C33-C29 = C31-C29 = C32-C29 = C30-C29
 1.54 with sigma of 0.02
 C43-C40 = C44-C40 = C45-C40 = C46-C40 = C41-C40 = C42-C40
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C95) = Uanis(C98) = Uanis(C96) = Uanis(C100) = Uanis(C101) = Uanis(C97) =
Uanis(C99)
Uanis(C104) = Uanis(C102) = Uanis(C105) = Uanis(C103)
Uanis(C107) = Uanis(C109) = Uanis(C106) = Uanis(C108)
Uanis(C124) = Uanis(C125)
Uanis(C29) = Uanis(C34) = Uanis(C31) = Uanis(C30) = Uanis(C35) = Uanis(C32) =
Uanis(C33)
Uanis(C40) = Uanis(C43) = Uanis(C45) = Uanis(C41) = Uanis(C46) = Uanis(C42) =
Uanis(C44)
Uanis(F4) = Uanis(F5) = Uanis(F6)
Uanis(C50) = Uanis(C48) = Uanis(C49) = Uanis(C47)
Uanis(C128) = Uanis(C129)
Uanis(C62) = Uanis(C61)
Uanis(O38) = Uanis(O36) = Uanis(O37)
4. Others
 Fixed Sof: C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C32(0.5) H32A(0.5)
 H32B(0.5) H32C(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C42(0.5) H42A(0.5)
 H42B(0.5) H42C(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5) C46(0.5) H46A(0.5)
 H46B(0.5) H46C(0.5) C96(0.75) H96A(0.75) H96B(0.75) H96C(0.75) C98(0.75)
 H98A(0.75) H98B(0.75) H98C(0.75) C100(0.75) H10S(0.75) H10T(0.75) H10U(0.75)
 C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5)
 C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5)
 C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5)
 C97(0.25) H97A(0.25) H97B(0.25) H97C(0.25) C99(0.25) H99A(0.25) H99B(0.25)
 H99C(0.25) C101(0.25) H10V(0.25) H10W(0.25) H10X(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B), C51(H51A,H51B),
 C53(H53A,H53B), C55(H55A,H55B), C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B),
  C63(H63A,H63B), C65(H65A,H65B), C73(H73A,H73B), C80(H80A,H80B), C87(H87A,
 H87B), C94(H94A,H94B), C114(H11J,H11K), C116(H11O,H11P), C118(H11T,H11U),
 C120(H12A,H12B), C122(H12F,H12G), C124(H12K,H12L), C126(H12P,H12Q), C128(H12U,
 H12V)
5.b Me refined with riding coordinates:
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C96(H96A,H96B,H96C), C98(H98A,
 H98B,H98C), C100(H10S,H10T,H10U), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C),
 C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C45(H45A,H45B,
 H45C), C97(H97A,H97B,H97C), C99(H99A,H99B,H99C), C101(H10V,H10W,H10X)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C11(H11), C16(H16), C18(H18), C23(H23), C25(H25),
 C68(H68), C70(H70), C75(H75), C77(H77), C82(H82), C84(H84), C89(H89), C91(H91)
5.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,
 H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C),
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C103(H10A,H10B,
 H10C), C104(H10D,H10E,H10F), C105(H10G,H10H,H10I), C107(H10J,H10K,H10L),
 C108(H10M,H10N,H10O), C109(H10P,H10Q,H10R), C111(H11A,H11B,H11C), C112(H11D,
 H11E,H11F), C113(H11G,H11H,H11I), C115(H11L,H11M,H11N), C117(H11Q,H11R,H11S),
 C119(H11V,H11W,H11X), C121(H12C,H12D,H12E), C123(H12H,H12I,H12J), C125(H12M,
 H12N,H12O), C127(H12R,H12S,H12T), C129(H12W,H12X,H12Y)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              59851
_shelx_hkl_checksum              95703
_shelx_fab_checksum              18240
_olex2_submission_special_instructions 'No special instructions were received'