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_4088878
_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         'C84 H108 Cl2 N8 Nd2, 2(C7 H8)'
_chemical_formula_sum            'C98 H124 Cl2 N8 Nd2'
_chemical_formula_weight         1773.42
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                93.1880(10)
_cell_angle_beta                 106.4590(10)
_cell_angle_gamma                107.3440(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9693(2)
_cell_length_b                   14.7087(2)
_cell_length_c                   15.8593(2)
_cell_measurement_reflns_used    151863
_cell_measurement_temperature    205
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      1.84
_cell_volume                     2314.79(6)
_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      205
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.0166
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            80060
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.104
_diffrn_reflns_theta_min         1.839
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.215
_exptl_absorpt_correction_T_max  0.7352
_exptl_absorpt_correction_T_min  0.6019
_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    1.272
_exptl_crystal_description       prism
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.626
_exptl_crystal_size_mid          0.418
_exptl_crystal_size_min          0.297
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 7918 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         17608
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0181
_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^)+(0.0399P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0467
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.932
_reflns_Friedel_fraction_max     0.921
_reflns_number_gt                16991
_reflns_number_total             17608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00523_si_002.cif
_cod_data_source_block           4
_cod_database_code               4088878
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76: within 1.7A with sigma
of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: C92A(0.5) H92A(0.5) H92B(0.5) H92C(0.5) C92B(0.5) H92D(0.5)
 H92E(0.5) H92F(0.5) C93B(0.5) C94B(0.5) H94B(0.5) C95B(0.5) H95B(0.5)
 C96B(0.5) H96B(0.5) C97B(0.5) H97B(0.5) C98B(0.5) H98B(0.5) C93A(0.5)
 C98A(0.5) H98A(0.5) C97A(0.5) H97A(0.5) C96A(0.5) H96A(0.5) C95A(0.5)
 H95A(0.5) C94A(0.5) H94A(0.5)
4.a Ternary CH refined with riding coordinates:
 C6(H6), C14(H14), C27(H27), C35(H35), C48(H48), C56(H56), C69(H69), C77(H77)
4.b 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), C51(H51), C52(H52), C53(H53),
 C54(H54), C55(H55), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C72(H72),
  C73(H73), C74(H74), C75(H75), C76(H76), C80(H80), C81(H81), C82(H82),
 C83(H83), C84(H84), C94B(H94B), C95B(H95B), C96B(H96B), C97B(H97B), C98B(H98B),
  C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C98A(H98A), C97A(H97A),
 C96A(H96A), C95A(H95A), C94A(H94A)
4.c Fitted hexagon refined as free rotating group:
 C93A(C98A,C97A,C96A,C95A,C94A)
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), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C57(H57A,H57B,H57C), C66(H66A,
 H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C),
 C78(H78A,H78B,H78C), C92A(H92A,H92B,H92C), C92B(H92D,H92E,H92F), C85(H85A,H85B,
 H85C)
;
_shelx_res_checksum              58007
_shelx_hkl_checksum              82222
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'