Retro-Diels-Alder decomposition of norbornadiene mediated by a cationic magnesium complex.
Thum, Katharina; Pahl, Jürgen; Eyselein, Jonathan; Elsen, Holger; Langer, Jens; Harder, Sjoerd; Chemical communications (Cambridge, England) 57 (2021) 5278–5281; doi:10.1039/d1cc01691a

data_7128230
_publ_section_title
;
 Retro-Diels-Alder decomposition of norbornadiene mediated by a cationic
 magnesium complex.
;
_journal_issue                   43
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5278
_journal_page_last               5281
_journal_paper_doi               10.1039/d1cc01691a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C34 H46 Mg N2'
_chemical_formula_sum            'C34 H46 Mg N2'
_chemical_formula_weight         507.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-29 deposited with the CCDC.	2021-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                74.655(4)
_cell_angle_beta                 87.535(4)
_cell_angle_gamma                78.126(4)
_cell_formula_units_Z            2
_cell_length_a                   9.2377(4)
_cell_length_b                   12.4708(7)
_cell_length_c                   13.7451(6)
_cell_measurement_reflns_used    5748
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.9320
_cell_measurement_theta_min      3.3100
_cell_volume                     1494.22(13)
_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_temperature      100.0(2)
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.948
_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    -66.00  28.00   1.00    1.00    --  -41.15  38.00   0.00   94
  2  \w    -96.00  -3.00   1.00    1.00    --  -41.15 125.00  60.00   93
  3  \w   -113.00 -17.00   1.00    1.00    --  -41.15 -38.00-180.00   96
  4  \w     56.00 116.00   1.00    1.00    --  104.96 -30.00 -60.00   60
  5  \w     80.00 177.00   1.00    1.00    --  104.96  45.00  90.00   97
  6  \w    121.00 169.00   1.00    1.00    --  104.96 125.00  60.00   48
  7  \w     87.00 178.00   1.00    1.00    --  104.96  30.00 150.00   91
  8  \w     41.00 121.00   1.00    1.00    --  104.96-125.00 -60.00   80
  9  \w     32.00 137.00   1.00    1.00    --  104.96 -77.00  90.00  105
 10  \w     29.00 132.00   1.00    1.00    --  104.96 -30.00 120.00  103
 11  \w     22.00 108.00   1.00    1.00    --  104.96 -94.00   0.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9006
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.926
_diffrn_reflns_theta_min         3.334
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.607
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0691P)^2^+0.6776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5118
_reflns_number_total             5648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01691a2.cif
_cod_data_source_block           hasj180206a
_cod_depositor_comments
'Adding full bibliography for 7128228--7128235.cif.'
_cod_database_code               7128230
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Sof(H5D)=Sof(H5E)=Sof(H5F)=1-FVAR(1)
 Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C17(H12), C32(H27), C20(H15), C29(H24)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H3), C13(H8), C2(H33), C27(H22), C14(H9), C1(H34), C15(H10), C25(H20),
 C26(H21), C4(H31), C3(H32), C5(H30)
3.c Idealised Me refined as rotating group:
 C6(H1A,H1B,H1C), C19(H13A,H13B,H13C), C18(H14A,H14B,H14C), C34(H28A,H28B,
 H28C), C21(H16A,H16B,H16C), C10(H5A,H5B,H5C), C10(H5D,H5E,H5F), C30(H25A,H25B,
 H25C), C22(H17A,H17B,H17C), C33(H29A,H29B,H29C), C31(H26A,H26B,H26C)
;
_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
- Detector area scaling
;