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

data_4085558
_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         'C40 H51.99 O3 Sr2'
_chemical_formula_sum            'C40 H52 O3 Sr2'
_chemical_formula_weight         756.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-12
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                83.166(2)
_cell_angle_beta                 78.276(3)
_cell_angle_gamma                81.623(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9969(4)
_cell_length_b                   12.5155(3)
_cell_length_c                   12.7690(3)
_cell_measurement_reflns_used    11417
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      66.8090
_cell_measurement_theta_min      3.5090
_cell_volume                     1849.28(9)
_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)'
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_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -22.00   81.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.8405  -99.0000   60.0000 103

  2 omega   16.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.8405   57.0000 -180.0000 99

  3 omega  -18.00   67.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.8405  -38.0000 -150.0000 85

  4 omega   10.00   47.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -105.9572 37

  5 omega   81.00  108.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  106.6984 27

  6 omega   81.00  120.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   17.8783 39

  7 omega   10.00   36.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  106.6984 26

  8 omega  137.00  163.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000    0.0000 -180.0000 26

  9 omega   37.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -60.0000 38

 10 omega  128.00  154.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000    0.0000 26

 11 omega   41.00   66.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000    0.0000 25

 12 omega   32.00   57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  150.0000 25

 13 omega   79.00  148.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000  -60.0000 69

 14 omega   20.00   74.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   90.0000 54

 15 omega   30.00  100.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -180.0000 70

 16 omega   19.00   60.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000    0.0000 41

 17 omega   89.00  115.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  -30.0000 26

 18 omega   76.00  160.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000   90.0000 84

 19 omega   76.00  102.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000    0.0000 -180.0000 26

 20 omega   61.00   87.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   90.0000 26

 21 omega   88.00  129.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -105.9572 41

 22 omega  122.00  164.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000  -60.0000 42

 23 omega   86.00  113.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   41.0000  -31.0000 27

 24 omega  122.00  169.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   41.0000  -31.0000 47

 25 omega   28.00   60.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -30.0000 32

 26 omega   99.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -30.0000 25

 27 omega   71.00  128.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -88.0000  173.5327 57

 28 omega   51.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  150.0000 25

 29 omega   67.00  154.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  -90.0000 87

 30 omega   49.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -150.0000 26

 31 omega   12.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  120.0000 28

 32 omega   43.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  120.0000 34

 33 omega   60.00   94.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   60.0000 34

 34 omega  123.00  149.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000  150.0000 26

 35 omega  135.00  161.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   60.0000  -46.3992 26

 36 omega   64.00  107.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   60.0000 43

 37 omega   28.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -88.0000  173.5327 26

 38 omega -116.00  -11.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8405  -63.0000 -122.2955 105

 39 omega -116.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8405  -57.0000    0.0000 104

 40 omega -121.00   -8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8405  -77.0000  -30.0000 113

 41 omega -121.00   -8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8405  -77.0000 -180.0000 113

 42 omega  -68.00   34.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8405   38.0000 -120.0000 102

 43 omega -121.00   -8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8405  -77.0000  120.0000 113

 44 omega   66.00  168.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000   60.0000 102
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1144726000
_diffrn_orient_matrix_UB_12      0.0285370000
_diffrn_orient_matrix_UB_13      0.0191369000
_diffrn_orient_matrix_UB_21      -0.0648940000
_diffrn_orient_matrix_UB_22      0.0964916000
_diffrn_orient_matrix_UB_23      0.0609302000
_diffrn_orient_matrix_UB_31      -0.0125628000
_diffrn_orient_matrix_UB_32      -0.0740818000
_diffrn_orient_matrix_UB_33      0.1059936000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26180
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         66.832
_diffrn_reflns_theta_min         3.550
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.060
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_T_min  0.615
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6517
_refine_ls_number_restraints     553
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0382P)^2^+0.4632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5585
_reflns_number_total             6517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5010868_si_002.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 4085558--4085559.cif.'
_cod_original_cell_volume        1849.28(10)
_cod_database_code               4085558
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C40 H52 O3 Sr2'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O3-C37B \\sim O3-C37A \\sim O3-C37C
 with sigma of 0.02
 O3-C40B \\sim O3-C40C \\sim O3-C40A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C40A) = Uanis(C40B) = Uanis(C40C)
Uanis(C39C) = Uanis(C39A) = Uanis(C39B)
Uanis(C38C) = Uanis(C38B) = Uanis(C38A)
Uanis(C37A) = Uanis(C37C) = Uanis(C37B)
4. 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
5. Same fragment restrains
{C37B, C38B, C39B, C40B}
{C37C, C38C, C39C, C40C}
as
{C37A, C38A, C39A, C40A}
6. Others
 1*[Sof(C37A)+Sof(H37A)+Sof(H37B)+Sof(C38A)+Sof(H38A)+Sof(H38B)+Sof(C39A)+
 Sof(H39A)+Sof(H39B)+Sof(C40A)+Sof(H40A)+Sof(H40B)]+1*[Sof(C37B)+Sof(H37C)+
 Sof(H37D)+Sof(C38B)+Sof(H38C)+Sof(H38D)+Sof(C39B)+Sof(H39C)+Sof(H39D)+
 Sof(C40B)+Sof(H40C)+Sof(H40D)]+1*[Sof(C37C)+Sof(H37E)+Sof(H37F)+Sof(C38C)+
 Sof(H38E)+Sof(H38F)+Sof(C39C)+Sof(H39E)+Sof(H39F)+Sof(C40C)+Sof(H40E)+
 Sof(H40F)]=1 with esd of 0.001
 Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(C39A)=
 Sof(H39A)=Sof(H39B)=Sof(C40A)=Sof(H40A)=Sof(H40B)=FVAR(1)
 Sof(C37B)=Sof(H37C)=Sof(H37D)=Sof(C38B)=Sof(H38C)=Sof(H38D)=Sof(C39B)=
 Sof(H39C)=Sof(H39D)=Sof(C40B)=Sof(H40C)=Sof(H40D)=FVAR(2)
 Sof(C37C)=Sof(H37E)=Sof(H37F)=Sof(C38C)=Sof(H38E)=Sof(H38F)=Sof(C39C)=
 Sof(H39E)=Sof(H39F)=Sof(C40C)=Sof(H40E)=Sof(H40F)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37A(H37A,H37B),
 C38A(H38A,H38B), C39A(H39A,H39B), C40A(H40A,H40B), C37B(H37C,H37D), C38B(H38C,
 H38D), C39B(H39C,H39D), C40B(H40C,H40D), C37C(H37E,H37F), C38C(H38E,H38F),
 C39C(H39E,H39F), C40C(H40E,H40F)
7.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), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28)
;
_shelx_res_checksum              85674
_shelx_hkl_checksum              44485
_olex2_submission_special_instructions 'No special instructions were received'