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_7701800
_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         'C48 H108 Cl Cu2 K N2 O12 Si4'
_chemical_formula_sum            'C48 H108 Cl Cu2 K N2 O12 Si4'
_chemical_formula_weight         1219.35
_chemical_name_systematic        Cu2KClN2O12Si4C48H108
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-29
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.06.07 svn.r3419 for OlexSys, GUI svn.r5353)
;
_audit_update_record
;
2019-09-05 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.541(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.524(8)
_cell_length_b                   19.826(9)
_cell_length_c                   19.692(8)
_cell_measurement_reflns_used    9298
_cell_measurement_temperature    190
_cell_measurement_theta_max      30.415
_cell_measurement_theta_min      2.280
_cell_volume                     7401(5)
_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)'
_diffrn_ambient_temperature      191.07
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.980
_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  0.0802
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            182799
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.354
_diffrn_reflns_theta_min         2.319
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.9988
_exptl_absorpt_correction_T_min  0.7336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1461 before and 0.0802 after correction. The Ratio of minimum to maximum transmission is 0.7345. The \l/2 correction factor is Not present.'
_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    1.094
_exptl_crystal_description       prism
_exptl_crystal_F_000             2624
_exptl_crystal_preparation       N.A.
_exptl_crystal_recrystallization_method N.A.
_exptl_crystal_size_max          0.549
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.258
_refine_diff_density_max         0.607
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.00083(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         21842
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0628P)^2^+12.4695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13735
_reflns_number_total             21842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04230j2.cif
_cod_data_source_block           1
_cod_original_cell_volume        7401(6)
_cod_database_code               7701800
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C21A) = Uanis(C21B)
Uanis(C22A) = Uanis(C22B)
Uanis(C23A) = Uanis(C23B)
Uanis(C24A) = Uanis(C24B)
Uanis(O7A) = Uanis(O7B)
Uanis(C25A) = Uanis(C25B)
Uanis(C27A) = Uanis(C27B)
Uanis(C28A) = Uanis(C28B)
Uanis(C26A) = Uanis(C26B)
Uanis(O9A) = Uanis(O9B)
Uanis(C33A) = Uanis(C33B)
Uanis(C36A) = Uanis(C36B)
Uanis(C34A) = Uanis(C34B)
Uanis(C35A) = Uanis(C35B)
Uanis(O8A) = Uanis(O8B)
Uanis(C29A) = Uanis(C29B)
Uanis(C31A) = Uanis(C31B)
Uanis(C32A) = Uanis(C32B)
Uanis(C30A) = Uanis(C30B)
3. Same fragment restrains
{C21B, C22B, C23B, C24B} sigma for 1-2: 0.002, 1-3: 0.004
as
{C21A, C22A, C23A, C24A}
{O7B, C25B, C26B, C27B, C28B} sigma for 1-2: 0.002, 1-3: 0.004
as
{O7A, C25A, C26A, C27A, C28A}
{O9B, C33B, C34B, C35B, C36B} sigma for 1-2: 0.002, 1-3: 0.004
as
{O9A, C33A, C34A, C35A, C36A}
{O8B, C29B, C31B, C32B} sigma for 1-2: 0.002, 1-3: 0.004
as
{O8A, C29A, C30A, C31A}
4. Others
 Sof(C21B)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23B)=Sof(H23D)=
 Sof(H23E)=Sof(H23F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23A)=Sof(H23A)=
 Sof(H23B)=Sof(H23C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=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)
 Sof(O9B)=Sof(C33B)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35B)=
 Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(3)
 Sof(O9A)=Sof(C33A)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35A)=
 Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(3)
 Sof(O8B)=Sof(C29B)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32B)=
 Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(4)
 Sof(O8A)=Sof(C29A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31A)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(4)
5.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C22A(H22A,H22B,H22C), C23A(H23A,H23B,H23C), C24A(H24A,
 H24B,H24C), C26A(H26A,H26B,H26C), C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C),
 C34A(H34A,H34B,H34C), C35A(H35A,H35B,H35C), C36A(H36A,H36B,H36C), C30A(H30A,
 H30B,H30C), C31A(H31A,H31B,H31C), C32A(H32A,H32B,H32C), C22B(H22D,H22E,H22F),
 C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F), C26B(H26D,H26E,H26F), C27B(H27D,
 H27E,H27F), C28B(H28D,H28E,H28F), C34B(H34D,H34E,H34F), C35B(H35D,H35E,H35F),
 C36B(H36D,H36E,H36F), C31B(H31D,H31E,H31F), C32B(H32D,H32E,H32F), C30B(H30D,
 H30E,H30F)
;
_olex2_exptl_crystal_mounting_method N.A.
_olex2_submission_original_sample_id Cu2KClN2O12Si4C48H108
_olex2_submission_special_instructions 'No special instructions were received'