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_7701802
_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         '0.05(C48 H108 N2 O12 Si4 Sm)'
_chemical_formula_sum            'C2.34 H5.27 N0.1 O0.59 Si0.2 Sm0.05'
_chemical_formula_weight         56.98
_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   geom
_audit_creation_date             2018-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-09-05 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.444(6)
_cell_angle_gamma                90
_cell_formula_units_Z            82
_cell_length_a                   21.438(5)
_cell_length_b                   15.090(3)
_cell_length_c                   21.412(4)
_cell_measurement_reflns_used    6683
_cell_measurement_temperature    107(2)
_cell_measurement_theta_max      26.269
_cell_measurement_theta_min      2.300
_cell_volume                     6447(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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_temperature      106.92
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1689
_diffrn_reflns_av_unetI/netI     0.1267
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            85838
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.347
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.035
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1126 before and 0.0834 after correction. The Ratio of minimum to maximum transmission is 0.7776. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.109
_refine_diff_density_max         1.341
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.00049(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         15980
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.0714
_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^)+33.9154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9557
_reflns_number_total             15980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04230j2.cif
_cod_data_source_block           mo_a377_0ma
_cod_original_formula_sum        'C2.34 H5.27 N0.10 O0.59 Si0.20 Sm0.05'
_cod_database_code               7701802
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.853
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Sm1-O1A \\sim Sm1-O1B
 with sigma of 0.002
 Si1-O1A \\sim Si1-O1B
 with sigma of 0.002
 C2A-C1A \\sim C4A-C1A \\sim C3A-C1A
 with sigma of 0.002
 Sm1-O7B \\sim Sm1-O7A
 with sigma of 0.002
 Si3-O7B \\sim Si3-O7A
 with sigma of 0.002
 C26A-C25A \\sim C28A-C25A \\sim C27A-C25A
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C3B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C2B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O1A) = Uanis(O1B)
Uanis(C1A) = Uanis(C1B)
Uanis(C2A) = Uanis(C2B)
Uanis(C3A) = Uanis(C3B)
Uanis(C4A) = Uanis(C4B)
Uanis(O7B) = Uanis(O7A)
Uanis(C26B) = Uanis(C26A)
Uanis(C28B) = Uanis(C28A)
Uanis(C25A) = Uanis(C25B)
Uanis(C27A) = Uanis(C27B)
4. Same fragment restrains
{O1B, C1B, C2B, C3B, C4B} sigma for 1-2: 0.002, 1-3: 0.004
as
{O1A, C1A, C2A, C3A, C4A}
{O7B, C25B, C26B, C27B, C28B} sigma for 1-2: 0.002, 1-3: 0.004
as
{O7A, C25A, C26A, C27A, C28A}
5. Others
 Sof(O1B)=Sof(C1B)=Sof(C2B)=Sof(H2BB)=Sof(H2BC)=Sof(H2BD)=Sof(C3B)=Sof(H3BB)=
 Sof(H3BC)=Sof(H3BD)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=1-FVAR(1)
 Sof(O1A)=Sof(C1A)=Sof(C2A)=Sof(H2AB)=Sof(H2AC)=Sof(H2AD)=Sof(C3A)=Sof(H3AB)=
 Sof(H3AC)=Sof(H3AD)=Sof(C4A)=Sof(H4AB)=Sof(H4AC)=Sof(H4AD)=FVAR(1)
 Sof(O7B)=Sof(C25B)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27B)=
 Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(2)
 Sof(O7A)=Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27A)=
 Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(2)
6.a Idealised Me refined as rotating group:
 C00O(H00A,H00B,H00C), C00R(H00D,H00E,H00F), C00T(H00G,H00H,H00I), C00W(H00J,
 H00K,H00L), C00X(H00M,H00N,H00O), C01A(H01A,H01B,H01C), C01B(H01D,H01E,H01F),
 C01C(H01G,H01H,H01I), C01D(H01J,H01K,H01L), C01E(H01M,H01N,H01O), C01F(H01P,
 H01Q,H01R), C01G(H01S,H01T,H01U), C01H(H01V,H01W,H01X), C01I(H01Y,H,HA),
 C01J(H01Z,HB,HC), C01K(H01,HD,HE), C01L(H0AA,HF,HG), C01M(H1AA,HH,HI),
 C01N(H2AA,HJ,HK), C01O(H3AA,HL,HM), C01P(H4AA,HN,HO), C01Q(H5AA,HP,HQ),
 C01R(H6AA,HR,HS), C010(H7AA,HT,HU), C011(H8AA,HV,HW), C014(H9AA,HX,HY),
 C015(H0BA,HZ,H5BA), C016(H1BA,H6BA,H7BA), C017(H2BA,H8BA,H9BA), C018(H3BA,H0CA,
 H1CA), C2A(H2AB,H2AC,H2AD), C3A(H3AB,H3AC,H3AD), C4A(H4AB,H4AC,H4AD), C2B(H2BB,
 H2BC,H2BD), C3B(H3BB,H3BC,H3BD), C4B(H4BA,H4BB,H4BC), C26A(H26A,H26B,H26C),
 C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C26B(H26D,H26E,H26F), C27B(H27D,
 H27E,H27F), C28B(H28D,H28E,H28F)
;
_olex2_submission_special_instructions 'No special instructions were received'