Cooperative loading of multisite receptors with lanthanide containers: an approach for organized luminescent metallopolymers.
Babel, Lucille; Guénée, Laure; Besnard, Céline; Eliseeva, Svetlana V.; Petoud, Stéphane; Piguet, Claude; Chemical science 9 (2018) 325–335; doi:10.1039/c7sc03710d

data_1547878
_publ_section_title
;
 Cooperative loading of multisite receptors with lanthanide containers: an
 approach for organized luminescent metallopolymers.
;
_journal_issue                   2
_journal_name_full               'Chemical science'
_journal_page_first              325
_journal_page_last               335
_journal_paper_doi               10.1039/c7sc03710d
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C30 H26 F9 O9 S3 Y'
_chemical_formula_sum            'C30 H26 F9 O9 S3 Y'
_chemical_formula_weight         886.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.264(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5124(3)
_cell_length_b                   18.3614(5)
_cell_length_c                   18.9788(5)
_cell_measurement_reflns_used    7641
_cell_measurement_temperature    180.00(14)
_cell_measurement_theta_max      28.7350
_cell_measurement_theta_min      2.4340
_cell_volume                     3625.29(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4679
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details
;
  1 omega  -34.00   49.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4530   38.0000  -60.0000 83

  2 omega  -32.00   20.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4530   38.0000 -120.0000 52

  3 omega  -57.00  -15.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3905  -38.0000   30.0000 42

  4 omega  -20.00   31.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4530  -99.0000  -30.0000 51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0566854000
_diffrn_orient_matrix_UB_12      0.0010444000
_diffrn_orient_matrix_UB_13      -0.0252654000
_diffrn_orient_matrix_UB_21      -0.0018353000
_diffrn_orient_matrix_UB_22      -0.0386004000
_diffrn_orient_matrix_UB_23      -0.0004660000
_diffrn_orient_matrix_UB_31      -0.0378424000
_diffrn_orient_matrix_UB_32      0.0003192000
_diffrn_orient_matrix_UB_33      0.0280838000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21728
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.418
_diffrn_reflns_theta_min         2.250
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.877
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.624
_exptl_crystal_description       prism
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.3761
_exptl_crystal_size_mid          0.2202
_exptl_crystal_size_min          0.1982
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.076
_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     542
_refine_ls_number_reflns         8819
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0457P)^2^+1.6695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6378
_reflns_number_total             8819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03710d2.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
'Adding full bibliography for 1547877--1547880.cif.'
_cod_original_cell_volume        3625.30(16)
_cod_database_code               1547878
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C30 H26 F9 O9 S3'
_reflns_odcompleteness_completeness 99.95
_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
2. Restrained distances
 S42B-C41B
 1.72 with sigma of 0.02
 S42B-C43B
 1.69 with sigma of 0.02
 C43B-C44B
 1.335 with sigma of 0.02
 C45B-C44B
 1.42 with sigma of 0.02
 C45B-C41B
 1.38 with sigma of 0.02
 S42A-C41A
 1.72 with sigma of 0.02
 S42A-C43A
 1.69 with sigma of 0.02
 C44A-C43A
 1.335 with sigma of 0.02
 C44A-C45A
 1.42 with sigma of 0.02
 C41A-C45A
 1.38 with sigma of 0.02
 S30A-C29
 1.72 with sigma of 0.02
 S30A-C31A
 1.69 with sigma of 0.02
 C32A-C31A
 1.33 with sigma of 0.02
 C32A-C33A
 1.42 with sigma of 0.02
 C29-C33A
 1.38 with sigma of 0.02
 S30B-C29
 1.72 with sigma of 0.02
 S30B-C31B
 1.69 with sigma of 0.02
 C31B-C32B
 1.33 with sigma of 0.02
 C32B-C33B
 1.42 with sigma of 0.02
 C33B-C29
 1.38 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C41A) = Uanis(C41B)
Uanis(C33B) = Uanis(S30A)
4. Rigid body (RIGU) restrains
 C41A, S42A, C44A, C43A, C45A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C45B, S42B, C41B, C44B, C43B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33A, C29, C32A, C31A, S30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C32B, C31B, S30B, C33B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C45B)=Sof(H45B)=Sof(S42B)=Sof(C41B)=Sof(C44B)=Sof(H44B)=Sof(C43B)=
 Sof(H43B)=1-FVAR(1)
 Sof(C41A)=Sof(S42A)=Sof(C44A)=Sof(H44A)=Sof(C43A)=Sof(H43A)=Sof(C45A)=
 Sof(H45A)=FVAR(1)
 Sof(C32B)=Sof(H32B)=Sof(C31B)=Sof(H31B)=Sof(S30B)=Sof(C33B)=Sof(H33B)=1-FVAR(2)
 Sof(S30A)=Sof(C33A)=Sof(H33A)=Sof(C32A)=Sof(H32A)=Sof(C31A)=Sof(H31A)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B)
6.b Aromatic/amide H refined with riding coordinates:
 C45B(H45B), C33A(H33A), C46(H46), C44B(H44B), C34(H34), C43B(H43B), C22(H22),
 C32B(H32B), C31B(H31B), C44A(H44A), C43A(H43A), C45A(H45A), C21(H21), C20(H20),
  C19(H19), C32A(H32A), C31A(H31A), C33B(H33B)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              32473
_olex2_submission_special_instructions 'No special instructions were received'