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_4087265
_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         'C56 H40 Mg2 N4, 5(C3 H3)'
_chemical_formula_sum            'C71 H55 Mg2 N4'
_chemical_formula_weight         1012.81
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_cell_angle_alpha                93.888(3)
_cell_angle_beta                 97.013(3)
_cell_angle_gamma                117.926(4)
_cell_formula_units_Z            2
_cell_length_a                   10.6789(5)
_cell_length_b                   11.3975(5)
_cell_length_c                   24.8650(8)
_cell_measurement_reflns_used    11359
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      29.2960
_cell_measurement_theta_min      3.3740
_cell_volume                     2626.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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      99.98(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 0.996
_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    -20.00  88.00   1.00   40.00    --   12.17  77.00 -90.00  108
  2  \w    -20.00  88.00   1.00   40.00    --   12.17  77.00  30.00  108
  3  \w    -20.00  88.00   1.00   40.00    --   12.17  77.00 150.00  108
  4  \w      8.00  74.00   1.00   40.00    --   12.17-135.00 -33.00   66
  5  \w     35.00  81.00   1.00   40.00    --   12.17 178.00 -90.00   46
  6  \w      8.00  74.00   1.00   40.00    --   12.17-135.00 146.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0622672000
_diffrn_orient_matrix_UB_12      0.0081280000
_diffrn_orient_matrix_UB_13      -0.0036957000
_diffrn_orient_matrix_UB_21      -0.0184241000
_diffrn_orient_matrix_UB_22      -0.0318100000
_diffrn_orient_matrix_UB_23      -0.0274571000
_diffrn_orient_matrix_UB_31      -0.0401501000
_diffrn_orient_matrix_UB_32      -0.0631314000
_diffrn_orient_matrix_UB_33      0.0086972000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31043
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.025
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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    1.280
_exptl_crystal_description       plank
_exptl_crystal_F_000             1066
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         10715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0754
_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^)+(0.0179P)^2^+5.1586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8966
_reflns_number_total             10715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00200_si_002.cif
_cod_data_source_block           hasj170215b
_cod_depositor_comments
'Adding full bibliography for 4087263--4087266.cif.'
_cod_database_code               4087265
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H Mg N'
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C35(H35), C36(H36), C21(H21), C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
 C55(H55), C2(H2), C30(H30), C13(H13), C27(H27), C52(H52), C50(H50), C22(H22),
 C10(H10), C16(H16), C31(H31), C26(H26), C12(H12), C44(H44), C53(H53), C49(H49),
  C25(H25), C18(H18), C33(H33), C17(H17), C60(H60), C54(H54), C5(H5), C3(H3),
 C40(H40), C32(H32), C38(H38), C11(H11), C41(H41), C24(H24), C62(H62), C19(H19),
  C39(H39), C4(H4), C57(H57), C58(H58), C61(H61), C46(H46), C47(H47), C45(H45),
 C59(H59), C71(H71), C70(H70), C69(H69), C67(H67), C68(H68), C66(H66), C65(H65),
  C64(H64), C63(H63)
;
_olex2_date_sample_data_collection 2017-02-15
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.243
_oxdiff_exptl_absorpt_empirical_full_min 0.807