Noncovalent immobilization and surface characterization of lanthanide complexes on carbon electrodes
Lionetti, Davide; Day, Victor W.; Blakemore, James; Dalton Trans.  (2017) –; doi:10.1039/C7DT02577G

data_7043990
_publ_section_title
;
 Noncovalent immobilization and surface characterization of lanthanide
 complexes on carbon electrodes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02577G
_journal_year                    2017
_chemical_formula_moiety         'C51 H75 Eu1 N4 O3'
_chemical_formula_sum            'C51 H75 Eu N4 O3'
_chemical_formula_weight         944.11
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-08-16 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   16.2194(7)
_cell_length_b                   16.2194(7)
_cell_length_c                   26.9621(15)
_cell_measurement_reflns_used    9517
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      69.65
_cell_measurement_theta_min      3.15
_cell_volume                     6142.6(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49515
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         70.074
_diffrn_reflns_theta_min         3.146
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.569
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1688 before and 0.0758 after correction. The Ratio of minimum to maximum transmission is 0.7385. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.887
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3877
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+15.2378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1126
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3536
_reflns_number_total             3877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02577g2.cif
_cod_data_source_block           L(tBu)Eu
_cod_original_cell_volume        6142.6(6)
_cod_database_code               7043990
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.549
_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. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(C15A)
Uanis(C16) = Uanis(C16A)
Uanis(C17) = Uanis(C17A)
Uanis(C14) = Uanis(C14A)
3. Same fragment restrains
{C14, C15, C16, C17} sigma for 1-2: 0.02, 1-3: 0.04
as
{C14A, C15A, C16A, C17A}
4. Others
 Sof(C14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C9(H9)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C15A(H15D,H15E,H15F),
 C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F)
;
_olex2_submission_special_instructions 'No special instructions were received'