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_1547877
_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 Eu F9 O9 S3'
_chemical_formula_sum            'C30 H26 Eu F9 O9 S3'
_chemical_formula_weight         949.65
_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                 92.9627(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.81000(16)
_cell_length_b                   16.5659(2)
_cell_length_c                   18.3880(2)
_cell_measurement_reflns_used    20796
_cell_measurement_temperature    183(7)
_cell_measurement_theta_max      29.3260
_cell_measurement_theta_min      2.2220
_cell_volume                     3592.68(8)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      183(7)
_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 0.895
_diffrn_measurement_details
;
  1 omega    8.00   34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4530   38.0000   60.0000 26

  2 omega  -14.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3905   57.0000    0.0000 100

  3 omega  -14.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3905   38.0000 -180.0000 101

  4 omega  -32.00    0.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4530   38.0000   60.0000 32

  5 omega  -79.00  -34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4530  -57.0000   60.0000 45

  6 omega  -20.00    6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4530  -99.0000   90.0000 26

  7 omega  -65.00   16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3905  -77.0000 -120.0000 81
;
_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      0.0212067000
_diffrn_orient_matrix_UB_12      0.0350892000
_diffrn_orient_matrix_UB_13      0.0181150000
_diffrn_orient_matrix_UB_21      -0.0527711000
_diffrn_orient_matrix_UB_22      0.0052159000
_diffrn_orient_matrix_UB_23      0.0161622000
_diffrn_orient_matrix_UB_31      0.0195897000
_diffrn_orient_matrix_UB_32      -0.0239639000
_diffrn_orient_matrix_UB_33      0.0300399000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39183
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.513
_diffrn_reflns_theta_min         2.218
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.017
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.488
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.5013
_exptl_crystal_size_mid          0.2665
_exptl_crystal_size_min          0.1021
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         8971
_refine_ls_number_restraints     321
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+2.6019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7552
_reflns_number_total             8971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03710d2.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
'Adding full bibliography for 1547877--1547880.cif.'
_cod_database_code               1547877
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C30 H26 Eu1 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
 C12A-C11B = C12B-C11A = C14A-C13B = C14B-C13A
 1.49 with sigma of 0.02
 O2-C12A = O2-C12B = O2-C13A = O2-C13B
 1.42 with sigma of 0.02
 O11-C11A = O11-C11B = O1-C14A = O1-C14B
 1.42 with sigma of 0.02
 S17B-C16B = S17A-C16A = S28B-C27B = S28A-C27A = S40A-C39A = S40B-C39B
 1.72 with sigma of 0.02
 S17B-C18B = S17A-C18A = S28A-C29A = S28B-C29B = S40A-C41A = S40B-C41B
 1.69 with sigma of 0.02
 C19B-C18B = C19A-C18A = C30A-C29A = C30B-C29B = C41B-C42B = C41A-C42A
 1.33 with sigma of 0.02
 C20B-C19B = C20A-C19A = C31B-C30B = C31A-C30A = C42B-C43B = C42A-C43A
 1.42 with sigma of 0.02
 C20B-C16B = C20A-C16A = C31B-C27B = C31A-C27A = C43B-C39B = C43A-C39A
 1.38 with sigma of 0.02
 C18A-C16A
 2.45 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C39B) = Uanis(C39A)
Uanis(C41B) = Uanis(C42A)
Uanis(C16A) = Uanis(C16B)
Uanis(C30A) = Uanis(C29B)
Uanis(C29A) = Uanis(C30B)
Uanis(C27A) = Uanis(C27B)
4. Rigid body (RIGU) restrains
 C39B, S40B, C41B, C42B, C43B, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C39A, S40A, C41A, C42A, C43A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C16B, S17B, C18B, C19B, C20B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C16A, S17A, C18A, C19A, C20A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27B, S28B, C31B, C29A, C30A, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29B, C30B, C27A, S28A, C31A, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C14A, C13B, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C14B, C13A, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C12B, C11A, O11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11, C11B, C12A, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C27B, S28B, C29B, C30B, C31B} sigma for 1-2: 0.02, 1-3: 0.02
as
{C27A, S28A, C29A, C30A, C31A}
{C13, C16A, S17A, C18A, C19A, C20A, C16B, S17B, C18B, C19B, C20B} sigma for
1-2: 0.02, 1-3: 0.02
as
{C13, C16A, S17A, C18A, C19A, C20A, C16B, S17B, C18B, C19B, C20B}
{C39B, S40B, C41B, C42B, C43B} sigma for 1-2: 0.02, 1-3: 0.02
as
{C39A, S40A, C41A, C42A, C43A}
6. Others
 Sof(C16A)=Sof(S17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=
 Sof(H20A)=1-FVAR(1)
 Sof(C16B)=Sof(S17B)=Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=
 Sof(H20B)=FVAR(1)
 Sof(C39B)=Sof(S40B)=Sof(C41B)=Sof(H41B)=Sof(C42B)=Sof(H42B)=Sof(C43B)=
 Sof(H43B)=1-FVAR(2)
 Sof(C39A)=Sof(S40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=
 Sof(H43A)=FVAR(2)
 Sof(C27B)=Sof(S28B)=Sof(C29B)=Sof(H29B)=Sof(C30B)=Sof(H30B)=Sof(C31B)=
 Sof(H31B)=1-FVAR(3)
 Sof(C27A)=Sof(S28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=
 Sof(H31A)=FVAR(3)
 Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(C11A)=Sof(H11C)=Sof(H11D)=1-FVAR(4)
 Sof(C11B)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12F)=Sof(H12G)=FVAR(4)
 Sof(C13B)=Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14C)=Sof(H14D)=1-FVAR(5)
 Sof(C14B)=Sof(H14A)=Sof(H14B)=Sof(C13A)=Sof(H13C)=Sof(H13D)=FVAR(5)
7.a Secondary CH2 refined with riding coordinates:
 C11B(H11A,H11B), C12B(H12A,H12B), C14B(H14A,H14B), C13B(H13A,H13B), C12A(H12F,
 H12G), C13A(H13C,H13D), C14A(H14C,H14D), C11A(H11C,H11D)
7.b Aromatic/amide H refined with riding coordinates:
 C41B(H41B), C42B(H42B), C43B(H43B), C29B(H29B), C30B(H30B), C31B(H31B),
 C29A(H29A), C30A(H30A), C31A(H31A), C18A(H18A), C19A(H19A), C20A(H20A),
 C18B(H18B), C19B(H19B), C20B(H20B), C21(H21), C28(H28), C14(H14), C41A(H41A),
 C42A(H42A), C43A(H43A)
7.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12C,H12D,H12E)
;
_shelx_res_checksum              31094
_olex2_submission_special_instructions 'No special instructions were received'