Smart lanthanide antennas for sensing water.
Fueyo-González, Francisco; Garcia-Fernandez, Emilio; Martínez, David; Infantes, Lourdes; Orte, Angel; González-Vera, Juan A; Herranz, Rosario; Chemical communications (Cambridge, England) 56 (2020) 5484–5487; doi:10.1039/d0cc01725f

data_7126424
_publ_section_title
;
 Smart lanthanide antennas for sensing water.
;
_journal_issue                   41
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5484
_journal_page_last               5487
_journal_paper_doi               10.1039/d0cc01725f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '3(C F3 O3 S), C32 H48 Eu N2 O14 P2, H2 O'
_chemical_formula_sum            'C35 H50 Eu F9 N2 O24 P2 S3'
_chemical_formula_weight         1363.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2020-01-14
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-29 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.115(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.919(6)
_cell_length_b                   13.486(9)
_cell_length_c                   24.950(6)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.526
_cell_measurement_theta_min      1.597
_cell_volume                     5171(4)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_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    'ShelXS-86 Patterson'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Silicon pixel detector'
_diffrn_detector_type            'Pilatus 6M - Dectris'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  Syncrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82653
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            59598
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        29.730
_diffrn_reflns_theta_max         31.526
_diffrn_reflns_theta_min         1.597
_diffrn_source                   synchrotron
_diffrn_source_type              'BL13-XALOC, Alba Synchrotron'
_exptl_absorpt_coefficient_mu    2.240
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_F_000             2752
_refine_diff_density_max         2.756
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         10354
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0911P)^2^+20.7676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9422
_reflns_number_total             10354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01725f2.cif
_cod_data_source_block           tubo2
_cod_depositor_comments
'Adding full bibliography for 7126421--7126424.cif.'
_cod_database_code               7126424
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N201-H201
 0.84 with sigma of 0.01
 O1-H1A = O1-H1B
 0.84 with sigma of 0.01
 O2-H2A = O2-H2B
 0.84 with sigma of 0.01
 O3-H3A = O3-H3B
 0.84 with sigma of 0.01
 O4-H4A = O4-H4B
 0.84 with sigma of 0.01
 H201-C201 = H201-C210
 1.88 with sigma of 0.02
 H2A-H2B
 1.34 with sigma of 0.02
 H3A-H3B
 1.34 with sigma of 0.02
 Eu1-H3B
 2.9 with sigma of 0.02
 H4A-H4B
 1.34 with sigma of 0.02
 C3A-F31A \\sim C3A-F32A \\sim C3A-F33A \\sim C3B-F31B \\sim C3B-F32B \\sim
C3B-F33B
 with sigma of 0.01
 S3A-C3A \\sim S3B-C3B
 with sigma of 0.01
 P1-O13A \\sim P1-O13B \\sim P1-O14A \\sim P1-O14B
 with sigma of 0.01
 O13A-C12A \\sim O13B-C12B \\sim O14A-C14A \\sim O14B-C14B
 with sigma of 0.01
 C12A-C13A \\sim C12B-C13B \\sim C14A-C15A \\sim C14B-C15B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C14B) \\sim Ueq, Uanis(C15B) \\sim Ueq, Uanis(C15D) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C14A) = Uanis(C14B)
Uanis(C15A) = Uanis(C15B)
Uanis(C15C) = Uanis(C15D)
4. Same fragment restrains
{S3A, O32A, O33A, C3A, F31A, F32A, F33A} sigma for 1-2: 0.02, 1-3: 0.04
as
{S3B, O32B, O33B, C3B, F31B, F32B, F33B}
5. Others
 Sof(S3B)=Sof(O32B)=Sof(O33B)=Sof(C3B)=Sof(F31B)=Sof(F32B)=Sof(F33B)=1-FVAR(1)
 Sof(S3A)=Sof(O32A)=Sof(O33A)=Sof(C3A)=Sof(F31A)=Sof(F32A)=Sof(F33A)=FVAR(1)
 Sof(H21F)=Sof(H21G)=Sof(C15D)=Sof(H15J)=Sof(H15K)=Sof(H15L)=1-FVAR(2)
 Sof(H21H)=Sof(H21I)=Sof(C15C)=Sof(H15G)=Sof(H15H)=Sof(H15I)=FVAR(2)
 Sof(O13B)=Sof(C12B)=Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=1-FVAR(3)
 Sof(O13A)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(C13A)=Sof(H13A)=Sof(H13B)=
 Sof(H13C)=FVAR(3)
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(O14B)=Sof(C14B)=Sof(H14C)=
 Sof(H14D)=1-FVAR(4)
 Sof(O14A)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=FVAR(4)
 Fixed Uiso: H1A(0.08) H1B(0.08) H2A(0.08) H2B(0.08) H3A(0.08) H3B(0.08)
 H4A(0.08) H4B(0.08) H5A(0.08) H5B(0.08) H101(0.08) H201(0.08)
6.a Secondary CH2 refined with riding coordinates:
 C104(H10A,H10B), C105(H10C,H10D), C12A(H12A,H12B), C12B(H12C,H12D), C14A(H14A,
 H14B), C14B(H14C,H14D), C204(H20A,H20B), C205(H20C,H20D), C212(H21A,H21B),
 C214(H21H,H21I), C214(H21F,H21G)
6.b Me refined with riding coordinates:
 C116(H11A,H11B,H11C), C213(H21C,H21D,H21E), C216(H21J,H21K,H21L)
6.c Aromatic/amide H refined with riding coordinates:
 C107(H107), C108(H108), C1AA(H1AA), C208(H208)
6.d Idealised Me refined as rotating group:
 C13A(H13A,H13B,H13C), C13B(H13D,H13E,H13F), C15A(H15A,H15B,H15C), C15B(H15D,
 H15E,H15F), C15C(H15G,H15H,H15I), C15D(H15J,H15K,H15L)
;
_shelx_res_checksum              70308
_olex2_submission_special_instructions 'No special instructions were received'