Enantiopure Amidinate Complexes of the Rare-Earth Elements
Brunner, Tobias S.; Benndorf, Paul; Gamer, Michael T.; Knöfel, Nicolai; Gugau, Katharina; Roesky, Peter W.; Organometallics 35 (2016) 3474–; doi:10.1021/acs.organomet.6b00523

data_4088880
_publ_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_publ_section_title
;
 Enantiopure Amidinate Complexes of the Rare-Earth Elements
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3474
_journal_paper_doi               10.1021/acs.organomet.6b00523
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C50 H70 Cl2 Li N4 O2 Sm'
_chemical_formula_sum            'C50 H70 Cl2 Li N4 O2 Sm'
_chemical_formula_weight         987.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6919(2)
_cell_length_b                   16.0293(2)
_cell_length_c                   21.4446(3)
_cell_measurement_reflns_used    43512
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      1.39
_cell_volume                     5050.22(12)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2009)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, PLATON (A.L.Spek, 2009)'
_computing_molecular_graphics    'Diamond 2/3, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  STOE-IPDS2-200K
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54484
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         1.586
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.308
_exptl_absorpt_correction_T_max  0.8816
_exptl_absorpt_correction_T_min  0.6773
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       prism
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.209
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 3963 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         9926
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0187
_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^)+(0.0255P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0422
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9228
_reflns_number_total             9926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00523_si_002.cif
_cod_data_source_block           6
_cod_database_code               4088880
_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
C47A \\sim C48A \\sim C49A \\sim C50A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C43B \\sim C44B \\sim C45B \\sim C46B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
 Fixed Sof: O2A(0.5) O2B(0.5) C43A(0.5) H43A(0.5) H43B(0.5) C44A(0.5)
 H44A(0.5) H44B(0.5) C45A(0.5) H45A(0.5) H45B(0.5) C46A(0.5) H46A(0.5)
 H46B(0.5) C47A(0.5) H47A(0.5) H47B(0.5) C48A(0.5) H48A(0.5) H48B(0.5)
 C49A(0.5) H49A(0.5) H49B(0.5) C50A(0.5) H50A(0.5) H50B(0.5) C43B(0.5)
 H43C(0.5) H43D(0.5) C44B(0.5) H44C(0.5) H44D(0.5) C45B(0.5) H45C(0.5)
 H45D(0.5) C46B(0.5) H46C(0.5) H46D(0.5) C47B(0.5) H47C(0.5) H47D(0.5)
 C48B(0.5) H48C(0.5) H48D(0.5) C49B(0.5) H49C(0.5) H49D(0.5) C50B(0.5)
 H50C(0.5) H50D(0.5)
4.a Ternary CH refined with riding coordinates:
 C6(H6), C14(H14), C27(H27), C35(H35)
4.b Secondary CH2 refined with riding coordinates:
 C43A(H43A,H43B), C44A(H44A,H44B), C45A(H45A,H45B), C46A(H46A,H46B), C47A(H47A,
 H47B), C48A(H48A,H48B), C49A(H49A,H49B), C50A(H50A,H50B), C43B(H43C,H43D),
 C44B(H44C,H44D), C45B(H45C,H45D), C46B(H46C,H46D), C47B(H47C,H47D), C48B(H48C,
 H48D), C49B(H49C,H49D), C50B(H50C,H50D)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C38(H38),
  C39(H39), C40(H40), C41(H41), C42(H42)
4.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C15(H15A,
 H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C28(H28A,H28B,H28C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              8848
_shelx_hkl_checksum              45697
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'