Synthesis of a Dinuclear Europium (III) Complex through Deprotonation and Oxygen-Atom Transfer of Trimethylamine N-Oxide
Li, Yangjuan; Chen, xiuting; gong, yu; Dalton Transactions  (2019) –; doi:10.1039/C9DT04234B

data_7701805
_publ_section_title
;
 Synthesis of a Dinuclear Europium (III) Complex through Deprotonation and
 Oxygen-Atom Transfer of Trimethylamine N-Oxide
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04234B
_journal_year                    2019
_chemical_formula_moiety         C21H63EuN3OPSi6
_chemical_formula_sum            'C21 H63 Eu N3 O P Si6'
_chemical_formula_weight         241.74
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-31 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.69510(10)
_cell_length_b                   14.69510(10)
_cell_length_c                   11.27440(10)
_cell_measurement_reflns_used    11063
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      74.4970
_cell_measurement_theta_min      3.4350
_cell_volume                     2108.48(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.19a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.19a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.19a (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  63.00   0.50    0.05    --   46.75 -56.00-175.00  176
  2  \w   -172.00 -80.00   0.50    0.05    --  -99.00 -64.00  -2.00  184
  3  \w   -172.00 -76.00   0.50    0.05    --  -99.00 -87.00 -39.00  192
  4  \w   -119.00 -71.00   0.50    0.05    --  -46.75-125.00-150.00   96
  5  \w   -119.00 -71.00   0.50    0.05    --  -46.75-125.00 -30.00   96
  6  \w     31.00 109.00   0.50    0.05    --  103.86 -94.00 120.00  156
  7  \w     31.00 109.00   0.50    0.05    --  103.86 -94.00-150.00  156
  8  \w     31.00 109.00   0.50    0.05    --  103.86 -94.00 -30.00  156
  9  \w     23.00 119.00   0.50    0.05    --   46.75  77.00-150.00  192
 10  \w     31.00 119.00   0.50    0.05    --   46.75  56.00 -33.00  176
 11  \w     32.00 121.00   0.50    0.05    --   46.75  38.00 120.00  178
 12  \w     86.00 111.00   0.50    0.05    --  103.86  15.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0015090000
_diffrn_orient_matrix_UB_12      -0.1040989000
_diffrn_orient_matrix_UB_13      0.0226400000
_diffrn_orient_matrix_UB_21      0.0907819000
_diffrn_orient_matrix_UB_22      0.0558956000
_diffrn_orient_matrix_UB_23      0.0894341000
_diffrn_orient_matrix_UB_31      -0.0801404000
_diffrn_orient_matrix_UB_32      -0.0262373000
_diffrn_orient_matrix_UB_33      0.1007946000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12326
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.526
_diffrn_reflns_theta_max         66.526
_diffrn_reflns_theta_min         5.241
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.753
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.19a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.006
_exptl_crystal_size_mid          0.006
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         2469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+2.9334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2360
_reflns_number_total             2469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04234b2.cif
_cod_data_source_block           exp_225
_cod_original_formula_sum        C21H63EuN3OPSi6
_cod_database_code               7701805
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.927
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C007(H00A,H00B,H00C), C008(H00D,H00E,H00F), C009(H00G,H00H,H00I), C00A(H00J,
 H00K,H00L), C00B(H00M,H00N,H00O), C00C(H00P,H00Q,H00R), C00D(H00S,H00T,H00U)
;
_shelx_res_checksum              18250
_shelx_fab_checksum              49834
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.591
_oxdiff_exptl_absorpt_empirical_full_min 0.787