Synthesis of Homoleptic, Divalent Lanthanide (Sm, Eu) Complexes via Oxidative Transmetallation
Gompa, Thaige P.; Jiang, Ningxin; Bacsa, John; La Pierre, Henry Storms; Dalton Transactions  (2019) –; doi:10.1039/C9DT04230J

data_7701801
_publ_section_title
;
 Synthesis of Homoleptic, Divalent Lanthanide (Sm, Eu) Complexes via
 Oxidative Transmetallation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04230J
_journal_year                    2019
_chemical_formula_moiety         'C24 H55 N O6 Si2'
_chemical_formula_sum            'C24 H55 N O6 Si2'
_chemical_formula_weight         509.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-30
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2019-09-11 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                79.543(4)
_cell_angle_beta                 79.198(4)
_cell_angle_gamma                64.407(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2019(9)
_cell_length_b                   9.4820(10)
_cell_length_c                   20.813(2)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      32.507
_cell_measurement_theta_min      2.613
_cell_volume                     1598.4(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX2 v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      185(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41132
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.397
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.7035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1166 before and 0.0625 after correction. The Ratio of minimum to maximum transmission is 0.9423. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_description       prism
_exptl_crystal_F_000             564
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         9720
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0460P)^2^+0.4938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7378
_reflns_number_total             9720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04230j2.cif
_cod_data_source_block           tpg-01-161
_cod_database_code               7701801
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1
 0.95 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C8(H8A,H8B,
 H8C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C19(H19A,H19B,H19C), C4(H4A,
 H4B,H4C), C16(H16A,H16B,H16C), C7(H7A,H7B,H7C), C24(H24A,H24B,H24C), C20(H20A,
 H20B,H20C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C6(H6A,H6B,
 H6C), C11(H11A,H11B,H11C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              93649
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id TPG-01-161
_olex2_submission_special_instructions 'No special instructions were received'