Dibenzylstrontium and -barium: Simple Molecules with Complex Structures
Izod, Keith; Waddell, Paul G.; Organometallics 34 (2015) 2726–; doi:10.1021/om5010868

data_4085559
_publ_section_title
;
 Dibenzylstrontium and -barium: Simple Molecules with Complex Structures
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2726
_journal_paper_doi               10.1021/om5010868
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C29 H37 Ba1.5 O2'
_chemical_formula_sum            'C29 H37 Ba1.5 O2'
_chemical_formula_weight         623.59
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-15
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 123.613(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.5531(8)
_cell_length_b                   8.97743(15)
_cell_length_c                   26.8011(9)
_cell_measurement_reflns_used    30663
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.6880
_cell_measurement_theta_min      3.0260
_cell_volume                     5320.6(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details
;
  1 omega  -20.00   84.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   77.0000 -150.0000 104

  2 omega  -16.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   38.0000  150.0000 91

  3 omega  -69.00  -32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -19.0000   90.0000 37

  4 omega  -27.00   18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -19.0000   90.0000 45

  5 omega  -34.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -38.0000 -180.0000 71

  6 omega  -11.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -93.0000  -52.0000 61

  7 omega  -15.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   38.0000   30.0000 101

  8 omega  -65.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000  -72.0000   55.0844 110

  9 omega   43.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000 -124.0000 -125.5069 26

 10 omega  -35.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289   38.0000  120.0000 102

 11 omega  -38.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289   57.0000  -60.0000 103

 12 omega  -23.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   77.0000    0.0000 112

 13 omega   -4.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000 -180.0000 56

 14 omega   -4.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000 -150.0000 56

 15 omega  -16.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   38.0000  120.0000 96

 16 omega   -4.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000   30.0000 56
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0141345000
_diffrn_orient_matrix_UB_12      0.0302744000
_diffrn_orient_matrix_UB_13      -0.0137158000
_diffrn_orient_matrix_UB_21      -0.0270136000
_diffrn_orient_matrix_UB_22      -0.0108624000
_diffrn_orient_matrix_UB_23      -0.0286240000
_diffrn_orient_matrix_UB_31      -0.0099888000
_diffrn_orient_matrix_UB_32      0.0721944000
_diffrn_orient_matrix_UB_33      0.0014570000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            83669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.372
_diffrn_reflns_theta_min         2.786
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.240
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         6763
_refine_ls_number_restraints     345
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+11.3040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5781
_reflns_number_total             6763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5010868_si_002.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 4085558--4085559.cif.'
_cod_original_cell_volume        5320.6(3)
_cod_original_formula_sum        'C29 H37 Ba1.50 O2'
_cod_database_code               4085559
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C29 H37 O2 Ba2'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C27A) = Uanis(C23A)
Uanis(C28A) = Uanis(C28B)
Uanis(C23A) = Uanis(C24A)
Uanis(C24A) = Uanis(C28A)
Uanis(C29) = Uanis(C29A)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H22C)=Sof(H22D)=Sof(H25C)=Sof(H25D)=Sof(H26C)=Sof(H26D)=Sof(C23B)=
 Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C27B)=Sof(H27C)=
 Sof(H27D)=Sof(C28B)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=1-FVAR(1)
 Sof(H22A)=Sof(H22B)=Sof(H25A)=Sof(H25B)=Sof(H26A)=Sof(H26B)=Sof(C29)=
 Sof(H29A)=Sof(H29B)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=
 Sof(H24B)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C22(H22C,H22D), C25(H25A,H25B), C25(H25C,H25D), C26(H26A,
 H26B), C26(H26C,H26D), C29(H29A,H29B), C23A(H23A,H23B), C24A(H24A,H24B),
 C27A(H27A,H27B), C28A(H28A,H28B), C23B(H23C,H23D), C24B(H24C,H24D), C27B(H27C,
 H27D), C28B(H28C,H28D), C29A(H29C,H29D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21)
;
_shelx_res_checksum              98653
_shelx_hkl_checksum              7304
_olex2_submission_special_instructions 'No special instructions were received'