s-Block Metal Dibenzoazepinate Complexes: Evidence for Mg–Alkene Encapsulation
Freitag, Benjamin; Elsen, Holger; Pahl, Jürgen; Ballmann, Gerd; Herrera, Alberto; Dorta, Romano; Harder, Sjoerd; Organometallics 36 (2017) 1860–; doi:10.1021/acs.organomet.7b00200

data_4087266
_publ_section_title
;
 s-Block Metal Dibenzoazepinate Complexes: Evidence for Mg--Alkene
 Encapsulation
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1860
_journal_paper_doi               10.1021/acs.organomet.7b00200
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C26 H34 Li N O3'
_chemical_formula_sum            'C26 H34 Li N O3'
_chemical_formula_weight         415.48
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-23
_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            8
_cell_length_a                   15.6271(6)
_cell_length_b                   16.3930(6)
_cell_length_c                   18.2668(6)
_cell_measurement_reflns_used    7890
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.4780
_cell_measurement_theta_min      3.5810
_cell_volume                     4679.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega  -72.00   32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   77.0000 -150.0000 104

  2 omega   95.00  144.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000   30.0000 49

  3 omega   95.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000    0.0000 33

  4 omega   94.00  173.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000 -150.0000 79

  5 omega   95.00  161.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000 -180.0000 66

  6 omega   83.00  154.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000 -180.0000 71

  7 omega  -68.00   25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.0659   57.0000    0.0000 93

  8 omega   89.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  -90.0000 89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0973755000
_diffrn_orient_matrix_UB_12      -0.0137370000
_diffrn_orient_matrix_UB_13      0.0053816000
_diffrn_orient_matrix_UB_21      -0.0002984000
_diffrn_orient_matrix_UB_22      0.0396742000
_diffrn_orient_matrix_UB_23      0.0763944000
_diffrn_orient_matrix_UB_31      -0.0156055000
_diffrn_orient_matrix_UB_32      0.0841091000
_diffrn_orient_matrix_UB_33      -0.0351684000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16693
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.621
_diffrn_reflns_theta_min         3.623
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.997
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.4193
_exptl_crystal_size_mid          0.327
_exptl_crystal_size_min          0.2025
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.5(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         8960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.9640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                8378
_reflns_number_total             8960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00200_si_002.cif
_cod_data_source_block           rodo160818a
_cod_depositor_comments
'Adding full bibliography for 4087263--4087266.cif.'
_cod_database_code               4087266
_chemical_oxdiff_formula         'C H N Li O'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5(2) 0.5(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Others
 Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=1-FVAR(1)
 Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=FVAR(1)
 Sof(H52C)=Sof(H52D)=Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=1-FVAR(2)
 Sof(H52A)=Sof(H52B)=Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C15(H15A,H15B), C21(H21A,H21B), C44(H44A,H44B), C45(H45A,
 H45B), C52(H52A,H52B), C52(H52C,H52D), C17(H17A,H17B), C23(H23A,H23B),
 C22(H22A,H22B), C16(H16A,H16B), C50(H50A,H50B), C50(H50C,H50D), C18(H18A,H18B),
  C20(H20A,H20B), C41(H41A,H41B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C47(H47A,H47B), C47(H47C,H47D), C42(H42A,H42B), C46(H46A,H46B),
 C43(H43A,H43B), C51(H51A,H51B), C48(H48A,H48B), C49(H49A,H49B), C48A(H48C,
 H48D), C51A(H51C,H51D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C11(H11), C28(H28), C13(H13), C5(H5), C12(H12), C30(H30), C7(H7),
 C10(H10), C39(H39), C31(H31), C8(H8), C29(H29), C4(H4), C34(H34), C33(H33),
 C38(H38), C3(H3), C36(H36), C37(H37)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-08-18
_olex2_submission_special_instructions 'No special instructions were received'