Homoleptic Chiral Benzamidinate Complexes of the Heavier Alkaline Earth Metals and the Divalent Lanthanides
He, Meng; Gamer, Michael T.; Roesky, Peter W.; Organometallics 35 (2016) 2638–; doi:10.1021/acs.organomet.6b00373

data_4088734
_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
;
 Homoleptic Chiral Benzamidinate Complexes of the Heavier Alkaline Earth
 Metals and the Divalent Lanthanides
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2638
_journal_paper_doi               10.1021/acs.organomet.6b00373
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C92 H92 Ba2 N8'
_chemical_formula_sum            'C92 H92 Ba2 N8'
_chemical_formula_weight         1584.41
_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             2016-03-30
_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                   13.4080(3)
_cell_length_b                   17.5419(5)
_cell_length_c                   36.4878(12)
_cell_measurement_reflns_used    38685
_cell_measurement_temperature    200
_cell_measurement_theta_max      26.16
_cell_measurement_theta_min      1.29
_cell_volume                     8582.0(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            43060
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.034
_diffrn_reflns_theta_min         1.288
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.8683
_exptl_absorpt_correction_T_min  0.6938
_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    1.226
_exptl_crystal_description       prism
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.469
_exptl_crystal_size_mid          0.336
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 5765 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         16813
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0278P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0496
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                14187
_reflns_number_total             16813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00373_si_002.cif
_cod_data_source_block           3
_cod_database_code               4088734
_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. Rigid body (RIGU) restrains
 C79B, C80B, C81B, C82B, C83B, C84B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C79A, C80A, C81A, C82A, C83A, C84A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: H78A(0.5) H78(0.5) C77A(0.5) H77A(0.5) H77B(0.5) H77C(0.5)
 C79A(0.5) C80A(0.5) H80A(0.5) C81A(0.5) H81A(0.5) C82A(0.5) H82A(0.5)
 C83A(0.5) H83A(0.5) C84A(0.5) H84A(0.5) C77B(0.5) H77D(0.5) H77E(0.5)
 H77F(0.5) C80B(0.5) H80B(0.5) C79B(0.5) C84B(0.5) H84B(0.5) C83B(0.5)
 H83B(0.5) C82B(0.5) H82B(0.5) C81B(0.5) H81B(0.5)
4.a Ternary CH refined with riding coordinates:
 C9(H9), C17(H17), C32(H32), C40(H40), C55(H55), C63(H63), C78(H78A), C78(H78),
  C86(H86)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C49(H49),
  C50(H50), C51(H51), C52(H52), C53(H53), C57(H57), C58(H58), C59(H59),
 C60(H60), C61(H61), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C72(H72),
  C73(H73), C74(H74), C75(H75), C76(H76), C88(H88), C89(H89), C90(H90),
 C91(H91), C92(H92), C80A(H80A), C81A(H81A), C82A(H82A), C83A(H83A), C84A(H84A),
  C80B(H80B), C84B(H84B), C83B(H83B), C82B(H82B), C81B(H81B)
4.c Fitted hexagon refined as free rotating group:
 C79A(C80A,C81A,C82A,C83A,C84A), C80B(C79B,C84B,C83B,C82B,C81B)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C39(H39A,H39B,
 H39C), C54(H54A,H54B,H54C), C62(H62A,H62B,H62C), C85(H85A,H85B,H85C),
 C77A(H77A,H77B,H77C), C77B(H77D,H77E,H77F)
;
_shelx_res_checksum              8435
_shelx_hkl_checksum              88263
_shelx_fab_checksum              93809
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'