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_7128233
_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         'C63 H53 B F20 Mg N2'
_chemical_formula_sum            'C63 H53 B F20 Mg N2'
_chemical_formula_weight         1253.19
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-17
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2021-03-29 deposited with the CCDC.	2021-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                97.935(3)
_cell_angle_beta                 98.421(3)
_cell_angle_gamma                115.012(4)
_cell_formula_units_Z            2
_cell_length_a                   12.5647(6)
_cell_length_b                   13.9361(6)
_cell_length_c                   18.4496(4)
_cell_measurement_reflns_used    6674
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.5320
_cell_measurement_theta_min      3.5500
_cell_volume                     2823.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      100.0(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 0.959
_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    -91.00 -55.00   1.00   12.50    --  -41.39 125.00  90.00   36
  2  \w   -112.00 -13.00   1.00   12.50    --  -41.39 -57.00-120.00   99
  3  \w    -63.00  28.00   1.00   12.50    --  -41.39  57.00  30.00   91
  4  \w    -65.00  31.00   1.00   12.50    --  -41.39  38.00-180.00   96
  5  \w     43.00 132.00   1.00   40.00    --  106.30 -61.00 -30.00   89
  6  \w     33.00 131.00   1.00   40.00    --  106.30 -30.00  60.00   98
  7  \w     57.00 129.00   1.00   40.00    --  106.30 -30.00-120.00   72
  8  \w     33.00 117.00   1.00   40.00    --  106.30-125.00-120.00   84
  9  \w     83.00 178.00   1.00   40.00    --  106.30  30.00  90.00   95
 10  \w    104.00 178.00   1.00   40.00    --  106.30  45.00  30.00   74
 11  \w     24.00 102.00   1.00   40.00    --  106.30 -94.00 -60.00   78
 12  \w    122.00 173.00   1.00   40.00    --  106.30 125.00   0.00   51
 13  \w     87.00 117.00   1.00   40.00    --  106.30-125.00  90.00   30
 14  \w     84.00 138.00   1.00   40.00    --  106.30 -77.00  30.00   54
;
_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      -0.0878489000
_diffrn_orient_matrix_UB_12      0.0392374000
_diffrn_orient_matrix_UB_13      0.0275334000
_diffrn_orient_matrix_UB_21      0.1068542000
_diffrn_orient_matrix_UB_22      0.1110837000
_diffrn_orient_matrix_UB_23      0.0393924000
_diffrn_orient_matrix_UB_31      -0.0132636000
_diffrn_orient_matrix_UB_32      0.0421918000
_diffrn_orient_matrix_UB_33      -0.0720310000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18589
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.866
_diffrn_reflns_theta_min         3.590
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         10978
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0511P)^2^+0.2807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8529
_reflns_number_total             10978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01691a2.cif
_cod_data_source_block           hasj190614a
_cod_depositor_comments
'Adding full bibliography for 7128228--7128235.cif.'
_cod_database_code               7128233
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C63 H53 B F20 Mg N2'
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.844
_reflns_odcompleteness_completeness 99.64
_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
 C35-C34 \\sim C36-C35 \\sim C32-C39 \\sim C39-C38A
 with sigma of 0.02
 C37-C36 \\sim C38A-C37
 with sigma of 0.02
 C37-C36A \\sim C38-C37
 with sigma of 0.02
 C36A-C35 \\sim C39-C38
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C37 \\sim C36 \\sim C38 \\sim C36A \\sim C38A: within 4A with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C35, C37, C39, C36, C38, C36A, C38A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H35A)=Sof(H37A)=Sof(H39A)=Sof(C36A)=Sof(H36C)=Sof(C38A)=Sof(H38A)=
 Sof(H38B)=1-FVAR(1)
 Sof(H35)=Sof(H37)=Sof(H39)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C38)=Sof(H38)=
 FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C32(H32), C34(H34), C35(H35),
 C35(H35A), C39(H39), C39(H39A)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C36(H36A,H36B), C38A(H38A,H38B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C37(H37),
 C37(H37A), C38(H38), C36A(H36C)
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 2019-06-14
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.783
_oxdiff_exptl_absorpt_empirical_full_min 0.405