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_4087264
_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         'C36 H36 Mg N2 O2'
_chemical_formula_sum            'C36 H36 Mg N2 O2'
_chemical_formula_weight         552.98
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_cell_angle_alpha                90.0
_cell_angle_beta                 98.106(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   45.3947(11)
_cell_length_b                   10.3734(2)
_cell_length_c                   15.2106(4)
_cell_measurement_reflns_used    15074
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.3150
_cell_measurement_theta_min      3.9340
_cell_volume                     7091.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -70.00 -26.00   1.00   40.00    --  -11.70 128.00  86.98   44
  2  \w    -44.00  64.00   1.00   40.00    --  -11.70  77.00 -30.00  108
  3  \w    -16.00  85.00   1.00   40.00    --   12.17  57.00 120.00  101
  4  \w    -20.00  88.00   1.00   40.00    --   12.17  77.00-120.00  108
  5  \w    -12.00  86.00   1.00   40.00    --   12.17  38.00  30.00   98
  6  \w    -10.00  62.00   1.00   40.00    --   14.00-111.00 -85.81   72
  7  \w    -18.00  57.00   1.00   40.00    --   14.00-102.00 100.46   75
  8  \w    -20.00  53.00   1.00   40.00    --   12.17 -99.00-150.00   73
  9  \w    -18.00  51.00   1.00   40.00    --   14.00-102.00   2.18   69
;
_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      -0.0116875000
_diffrn_orient_matrix_UB_12      -0.0423904000
_diffrn_orient_matrix_UB_13      0.0216068000
_diffrn_orient_matrix_UB_21      -0.0395879500
_diffrn_orient_matrix_UB_22      0.0361241500
_diffrn_orient_matrix_UB_23      0.0000629000
_diffrn_orient_matrix_UB_31      -0.0235870000
_diffrn_orient_matrix_UB_32      -0.0397264000
_diffrn_orient_matrix_UB_33      -0.0230158000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            65831
_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         28.061
_diffrn_reflns_theta_min         2.972
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.999
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.202
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         8559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0704
_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^)+(0.0600P)^2^+21.8520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7588
_reflns_number_total             8559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00200_si_002.cif
_cod_data_source_block           hasj170214b
_cod_depositor_comments
'Adding full bibliography for 4087263--4087266.cif.'
_cod_database_code               4087264
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Mg O'
_cell_oxdiff_angle_alpha         90.0259(19)
_cell_oxdiff_angle_beta          98.1301(19)
_cell_oxdiff_angle_gamma         89.9830(18)
_cell_oxdiff_length_a            45.4076(10)
_cell_oxdiff_length_b            10.3738(2)
_cell_oxdiff_length_c            15.2067(3)
_cell_oxdiff_measurement_reflns_used 28437
_cell_oxdiff_volume              7091.1(3)
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.02
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C29(H29A,H29B), C33(H33A,H33B), C31(H31A,H31B), C30(H30A,
 H30B), C36(H36A,H36B), C35(H35A,H35B), C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2), C27(H27), C7(H7), C3(H3), C26(H26), C16(H16), C13(H13),
 C5(H5), C10(H10), C25(H25), C24(H24), C11(H11), C12(H12), C4(H4), C22(H22),
 C18(H18), C21(H21), C17(H17), C19(H19)
;
_olex2_date_sample_data_collection 2017-02-14
_olex2_submission_original_sample_id hasj170214b
_olex2_submission_special_instructions 'No special instructions were received'