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_7128231
_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         'C75 H97 F2 Mg2 N4, B C24 F20'
_chemical_formula_sum            'C99 H97 B F22 Mg2 N4'
_chemical_formula_weight         1820.23
_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                90.874(2)
_cell_angle_beta                 90.208(3)
_cell_angle_gamma                92.266(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6804(4)
_cell_length_b                   16.3144(5)
_cell_length_c                   22.7319(7)
_cell_measurement_reflns_used    15494
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.7960
_cell_measurement_theta_min      3.4630
_cell_volume                     4698.4(3)
_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 0.988
_diffrn_measured_fraction_theta_max 0.951
_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    -53.00 -10.00   1.00    3.00    --  -41.15 125.00  30.00   43
  2  \w    -95.00  -8.00   1.00    3.00    --  -41.15 125.00 120.00   87
  3  \w    -95.00 -68.00   1.00    3.00    --  -41.15 125.00  30.00   27
  4  \w   -107.00 -22.00   1.00    3.00    --  -41.15 -38.00 -30.00   85
  5  \w   -114.00 -17.00   1.00    3.00    --  -41.15 -38.00-120.00   97
  6  \w     81.00 113.00   1.00   12.00    --  104.96  45.00-150.00   32
  7  \w    138.00 178.00   1.00   12.00    --  104.96  45.00-150.00   40
  8  \w     79.00 178.00   1.00   12.00    --  104.96  30.00  30.00   99
  9  \w     43.00 133.00   1.00   12.00    --  104.96 -30.00  30.00   90
 10  \w     42.00 121.00   1.00   12.00    --  104.96-125.00  60.00   79
 11  \w     29.00 136.00   1.00   12.00    --  104.96 -77.00  60.00  107
 12  \w     31.00 138.00   1.00   12.00    --  104.96 -77.00-150.00  107
 13  \w     29.00 120.00   1.00   12.00    --  104.96 -30.00-150.00   91
;
_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     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28675
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.922
_diffrn_reflns_theta_min         3.312
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.287
_exptl_crystal_description       block
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1219
_refine_ls_number_reflns         17831
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0620P)^2^+1.3098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15664
_reflns_number_total             17831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01691a2.cif
_cod_data_source_block           hasj180220a
_cod_depositor_comments
'Adding full bibliography for 7128228--7128235.cif.'
_cod_original_cell_volume        4698.4(2)
_cod_database_code               7128231
_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
2. Restrained distances
 C75-C70 \\sim C75A-C70 \\sim C75A-C74A \\sim C75-C74 \\sim C74-C73 \\sim
C74A-C73A \\sim C73A-C72A ~
 C73-C72 \\sim C72A-C71A \\sim C72-C71 \\sim C71A-C70 \\sim C71-C70
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C71A \\sim C71 \\sim C72 \\sim C72A \\sim C73 \\sim C73A \\sim C74 \\sim C74A
\\sim C75A \\sim C75 \\sim C70: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C70, C75A, C75, C74A, C74, C73, C73A, C72, C72A, C71, C71A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C75A)=Sof(H75A)=Sof(C74A)=Sof(H74A)=Sof(C73A)=Sof(H73A)=Sof(C72A)=
 Sof(H72A)=Sof(C71A)=Sof(H71A)=1-FVAR(1)
 Sof(C75)=Sof(H75)=Sof(C74)=Sof(H74)=Sof(C71)=Sof(H71)=Sof(C73)=Sof(H73)=
 Sof(C72)=Sof(H72)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C32(H32), C46(H46), C29(H29), C61(H61), C49(H49), C20(H20), C17(H17), C58(H58)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C25(H25), C3(H3), C26(H26), C4(H4), C5(H5), C37(H37), C65(H65),
 C2(H2), C27(H27), C1(H1), C42(H42), C75A(H75A), C74A(H74A), C73A(H73A),
 C72A(H72A), C71A(H71A), C43(H43), C44(H44), C69(H69), C15(H15), C14(H14),
 C56(H56), C75(H75), C13(H13), C66(H66), C54(H54), C67(H67), C68(H68), C55(H55),
  C74(H74), C71(H71), C73(H73), C72(H72)
6.c Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C30(H30a,H30b,H30c), C6(H6a,H6b,H6c), C48(H48a,H48b,
 H48c), C35(H35a,H35b,H35c), C33(H33a,H33b,H33c), C47(H47a,H47b,H47c), C34(H34a,
 H34b,H34c), C31(H31a,H31b,H31c), C50(H50a,H50b,H50c), C19(H19a,H19b,H19c),
 C62(H62a,H62b,H62c), C39(H39a,H39b,H39c), C59(H59a,H59b,H59c), C21(H21a,H21b,
 H21c), C22(H22a,H22b,H22c), C18(H18a,H18b,H18c), C51(H51a,H51b,H51c), C63(H63a,
 H63b,H63c), C60(H60a,H60b,H60c)
;
_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
;