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_4088736
_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         'C54 H62 N4 O2 Yb'
_chemical_formula_sum            'C54 H62 N4 O2 Yb'
_chemical_formula_weight         972.11
_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             2016-04-04
_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                   11.6521(2)
_cell_length_b                   19.2686(3)
_cell_length_c                   21.4853(4)
_cell_measurement_reflns_used    67034
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      1.75
_cell_volume                     4823.87(14)
_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    'SHELXT-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 0.995
_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  0.0279
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            69712
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.097
_diffrn_reflns_theta_min         1.896
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  0.9266
_exptl_absorpt_correction_T_min  0.8880
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       prism
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.225
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 3620 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9538
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0182
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0402
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                8597
_reflns_number_total             9538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00373_si_002.cif
_cod_data_source_block           5
_cod_database_code               4088736
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C41A \\sim C46A \\sim C45A \\sim C44A \\sim C43B \\sim C42B: within 1.7A with
sigma of 0.006 and sigma for terminal atoms of 0.012
C41B \\sim C46B \\sim C45B \\sim C44B \\sim C43A \\sim C42A: within 1.7A with
sigma of 0.006 and sigma for terminal atoms of 0.012
C50 \\sim C49B \\sim C48: within 1.7A with sigma of 0.006 and sigma for
terminal atoms of 0.012
C33A \\sim C38A \\sim C37A \\sim C36A \\sim C35A \\sim C34A: within 1.7A with
sigma of 0.006 and sigma for terminal atoms of 0.012
C33B \\sim C38B \\sim C37B \\sim C36B \\sim C35B \\sim C34B: within 1.7A with
sigma of 0.006 and sigma for terminal atoms of 0.012
O2 \\sim C54A \\sim C53A \\sim C52 \\sim C51: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: C33B(0.5) C38B(0.5) H38B(0.5) C37B(0.5) H37B(0.5) C36B(0.5)
 H36B(0.5) C35B(0.5) H35B(0.5) C34B(0.5) H34B(0.5) H32A(0.5) H32(0.5) H40A(0.5)
 H40(0.5) C41B(0.5) C42A(0.5) H42A(0.5) C43A(0.5) H43A(0.5) C44B(0.5) H44B(0.5)
 C45B(0.5) H45B(0.5) C46B(0.5) H46B(0.5) H48C(0.5) H48D(0.5) H48A(0.5)
 H48B(0.5) C49B(0.5) H49A(0.5) H49B(0.5) H50C(0.5) H50D(0.5) H50A(0.5)
 H50B(0.5) C53A(0.5) H53A(0.5) H53B(0.5) C54B(0.5) H54A(0.5) H54B(0.5)
 C53B(0.5) H53C(0.5) H53D(0.5) C49A(0.5) H49C(0.5) H49D(0.5) C54A(0.5)
 H54C(0.5) H54D(0.5) C41A(0.5) C42B(0.5) H42B(0.5) C43B(0.5) H43B(0.5)
 C44A(0.5) H44A(0.5) C45A(0.5) H45A(0.5) C46A(0.5) H46A(0.5) H52A(0.5)
 H52B(0.5) H52C(0.5) H52D(0.5) C33A(0.5) C38A(0.5) H38A(0.5) C37A(0.5)
 H37A(0.5) C36A(0.5) H36A(0.5) C35A(0.5) H35A(0.5) C34A(0.5) H34A(0.5)
4.a Ternary CH refined with riding coordinates:
 C9(H9), C17(H17), C32(H32A), C32(H32), C40(H40A), C40(H40)
4.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C48(H48C,H48D), C48(H48A,H48B), C49B(H49A,H49B), C50(H50C,
 H50D), C50(H50A,H50B), C51(H51A,H51B), C53A(H53A,H53B), C54B(H54A,H54B),
 C53B(H53C,H53D), C49A(H49C,H49D), C54A(H54C,H54D), C52(H52A,H52B), C52(H52C,
 H52D)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C7(H7), C6(H6), C5(H5),
 C4(H4), C3(H3), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C38B(H38B),
 C37B(H37B), C36B(H36B), C35B(H35B), C34B(H34B), C30(H30), C29(H29), C28(H28),
 C27(H27), C26(H26), C42A(H42A), C43A(H43A), C44B(H44B), C45B(H45B), C46B(H46B),
  C42B(H42B), C43B(H43B), C44A(H44A), C45A(H45A), C46A(H46A), C38A(H38A),
 C37A(H37A), C36A(H36A), C35A(H35A), C34A(H34A)
4.d Fitted hexagon refined as free rotating group:
 C33B(C38B,C37B,C36B,C35B,C34B), C41B(C42A,C43A,C44B,C45B,C46B), C41A(C42B,
 C43B,C44A,C45A,C46A), C33A(C38A,C37A,C36A,C35A,C34A)
4.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              93321
_shelx_hkl_checksum              49818
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'