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_7128232
_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 H47 Mg N2, B C24 F20'
_chemical_formula_sum            'C58 H47 B F20 Mg N2'
_chemical_formula_weight         1187.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-06-03
_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
_cell_angle_beta                 106.9367(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9261(2)
_cell_length_b                   20.4561(2)
_cell_length_c                   17.1852(2)
_cell_measurement_reflns_used    7604
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.6710
_cell_measurement_theta_min      3.9390
_cell_volume                     5355.86(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_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 0.965
_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   -109.00 -18.00   1.00   12.50    --  -41.64 -38.00  90.00   91
  2  \w   -110.00 -65.00   1.00   12.50    --  -41.64 -38.00  30.00   45
  3  \w     23.00  97.00   1.00   12.50    --   41.64-125.00   0.00   74
  4  \w     35.00  80.00   1.00   50.00    --  106.30 -61.00 -30.00   45
  5  \w     24.00  98.00   1.00   50.00    --  106.30 -94.00-150.00   74
  6  \w     90.00 116.00   1.00   50.00    --  106.30 -61.00 -30.00   26
  7  \w    135.00 175.00   1.00   50.00    --  106.30  45.00-120.00   40
  8  \w     33.00  74.00   1.00   50.00    --  106.30 -45.00-150.00   41
  9  \w     87.00 132.00   1.00   50.00    --  106.30 -45.00-150.00   45
 10  \w     27.00  86.00   1.00   50.00    --  106.30 -94.00 150.00   59
 11  \w     81.00 107.00   1.00   50.00    --  106.30  45.00-120.00   26
 12  \w    117.00 164.00   1.00   50.00    --  106.30  30.00 -30.00   47
 13  \w     78.00 104.00   1.00   50.00    --  106.30  30.00 -30.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0374861000
_diffrn_orient_matrix_UB_12      -0.0695765000
_diffrn_orient_matrix_UB_13      0.0009308000
_diffrn_orient_matrix_UB_21      -0.0131922000
_diffrn_orient_matrix_UB_22      -0.0120864000
_diffrn_orient_matrix_UB_23      0.0841550000
_diffrn_orient_matrix_UB_31      -0.0929008000
_diffrn_orient_matrix_UB_32      -0.0263152000
_diffrn_orient_matrix_UB_33      -0.0411508000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20676
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.752
_diffrn_reflns_theta_min         3.331
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.18b (Rigaku Oxford Diffraction, 2018)
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    1.472
_exptl_crystal_description       plank
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         10462
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0521P)^2^+0.9502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8283
_reflns_number_total             10462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01691a2.cif
_cod_data_source_block           hasj190529a
_cod_depositor_comments
'Adding full bibliography for 7128228--7128235.cif.'
_cod_original_cell_volume        5355.89(13)
_cod_database_code               7128232
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C58H47BF20MgN2
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.751
_reflns_odcompleteness_completeness 99.46
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C31-C30 \\sim C31A-C30A \\sim C34A-C30A \\sim C34-C30 \\sim C32A-C31A \\sim
C32-C31 \\sim C33A-C32A ~
 C33-C32 \\sim C33-C34 \\sim C33A-C34A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C30A \\sim C31A \\sim C32A \\sim C33A \\sim C34A \\sim C30 \\sim C31 \\sim C32
\\sim C33 \\sim C34: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
4. Rigid body (RIGU) restrains
 C30A, C31A, C32A, C33A, C34A, C30, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=
 Sof(C34)=Sof(H34)=1-FVAR(1)
 Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=
 Sof(H33A)=Sof(C34A)=Sof(H34A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b)
6.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C30A(H30A),
 C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34)
6.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c),
 C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C25(H25a,H25b,H25c), C26(H26a,H26b,
 H26c), C28(H28a,H28b,H28c), C29(H29a,H29b,H29c)
;
_olex2_date_sample_data_collection 2019-05-29
_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 1.793
_oxdiff_exptl_absorpt_empirical_full_min 0.624