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_4087263
_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         '1(C40 H44 Ca N2 O3)'
_chemical_formula_sum            'C40 H44 Ca N2 O3'
_chemical_formula_weight         640.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 118.294(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.2869(5)
_cell_length_b                   15.1455(2)
_cell_length_c                   22.4287(5)
_cell_measurement_reflns_used    11754
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.2960
_cell_measurement_theta_min      4.4970
_cell_volume                     6666.2(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 0.993
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega   15.00  112.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909   57.0000  -60.0000 97

  2 omega   62.00  170.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   15.0000  -60.0000 108

  3 omega  127.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000  150.0000 50

  4 omega   33.00  122.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   90.0000 89

  5 omega   47.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   90.0000 62

  6 omega   34.00  121.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000   30.0000 87

  7 omega  -68.00   28.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000 -120.0000 96
;
_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      0.0582683000
_diffrn_orient_matrix_UB_12      0.0530193000
_diffrn_orient_matrix_UB_13      0.0564025000
_diffrn_orient_matrix_UB_21      -0.0308370000
_diffrn_orient_matrix_UB_22      0.0862924000
_diffrn_orient_matrix_UB_23      -0.0389469000
_diffrn_orient_matrix_UB_31      -0.0425901000
_diffrn_orient_matrix_UB_32      0.0100595000
_diffrn_orient_matrix_UB_33      0.0372057000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24055
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.571
_diffrn_reflns_theta_min         4.506
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.942
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.76065
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       block
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.2571
_exptl_crystal_size_mid          0.1841
_exptl_crystal_size_min          0.1273
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         12947
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+1.4180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11375
_reflns_number_total             12947
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00200_si_002.cif
_cod_data_source_block           hasj160808b
_cod_depositor_comments
'Adding full bibliography for 4087263--4087266.cif.'
_cod_original_cell_volume        6666.3(3)
_cod_database_code               4087263
_chemical_oxdiff_formula         'C H N O Ca Si'
_reflns_odcompleteness_completeness 99.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid body (RIGU) restrains
 C56A, C57A, C58A, C59A, C60A, C55A, N4A, C68A, C67A, C66A, C65A, C64A, C63A,
 C62A, C61A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H79C)=Sof(H79D)=Sof(C80A)=Sof(H80C)=Sof(H80D)=1-FVAR(1)
 Sof(H79A)=Sof(H79B)=Sof(C80)=Sof(H80A)=Sof(H80B)=FVAR(1)
 Sof(H75C)=Sof(H75D)=Sof(C76A)=Sof(H76C)=Sof(H76D)=1-FVAR(2)
 Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=FVAR(2)
 Sof(C58A)=Sof(H58A)=Sof(C61A)=Sof(H61A)=Sof(C60A)=Sof(C57A)=Sof(H57A)=
 Sof(C59A)=Sof(H59A)=Sof(C62A)=Sof(H62A)=Sof(C55A)=Sof(C56A)=Sof(H56A)=Sof(N4A)=
 Sof(C63A)=Sof(C68A)=Sof(C67A)=Sof(H67A)=Sof(C66A)=Sof(H66A)=Sof(C65A)=
 Sof(H65A)=Sof(C64A)=Sof(H64A)=1-FVAR(3)
 Sof(N4)=Sof(C68)=Sof(C55)=Sof(C67)=Sof(H67)=Sof(C56)=Sof(H56)=Sof(C63)=
 Sof(C58)=Sof(H58)=Sof(C64)=Sof(H64)=Sof(C60)=Sof(C66)=Sof(H66)=Sof(C59)=
 Sof(H59)=Sof(C61)=Sof(H61)=Sof(C57)=Sof(H57)=Sof(C62)=Sof(H62)=Sof(C65)=
 Sof(H65)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B), C77(H77A,H77B), C34(H34A,
 H34B), C32(H32A,H32B), C29(H29A,H29B), C37(H37A,H37B), C78(H78A,H78B),
 C38(H38A,H38B), C39(H39A,H39B), C73(H73A,H73B), C79(H79A,H79B), C79(H79C,H79D),
  C30(H30A,H30B), C40(H40A,H40B), C69(H69A,H69B), C72(H72A,H72B), C74(H74A,
 H74B), C31(H31A,H31B), C70(H70A,H70B), C80(H80A,H80B), C75(H75A,H75B),
 C75(H75C,H75D), C71(H71A,H71B), C76(H76A,H76B), C80A(H80C,H80D), C76A(H76C,
 H76D)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C8(H8), C7(H7), C2(H2), C10(H10), C48(H48), C47(H47), C42(H42),
 C16(H16), C12(H12), C5(H5), C53(H53), C27(H27), C43(H43), C3(H3), C11(H11),
 C50(H50), C67(H67), C52(H52), C44(H44), C4(H4), C45(H45), C51(H51), C17(H17),
 C26(H26), C19(H19), C21(H21), C18(H18), C22(H22), C56(H56), C25(H25), C24(H24),
  C58(H58), C64(H64), C66(H66), C59(H59), C61(H61), C57(H57), C62(H62),
 C65(H65), C58A(H58A), C61A(H61A), C57A(H57A), C59A(H59A), C62A(H62A),
 C56A(H56A), C67A(H67A), C66A(H66A), C65A(H65A), C64A(H64A)
;
_shelx_res_checksum              67458
_shelx_hkl_checksum              33081
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-08-08
_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 4.405
_oxdiff_exptl_absorpt_empirical_full_min 0.209