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_7128228
_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         'C60 H49 B F20 Mg N2'
_chemical_formula_sum            'C60 H49 B F20 Mg N2'
_chemical_formula_weight         1213.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-05
_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                 98.9620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.5682(4)
_cell_length_b                   14.32480(10)
_cell_length_c                   21.1084(2)
_cell_measurement_reflns_used    23790
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.4660
_cell_measurement_theta_min      3.9730
_cell_volume                     12117.00(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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    '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 0.999
_diffrn_measured_fraction_theta_max 0.984
_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    -65.00  34.00   1.00    5.50    --  -40.61  38.00  60.00   99
  2  \w   -113.00 -12.00   1.00    5.50    --  -40.61 -57.00 -90.00  101
  3  \w      1.00  82.00   1.00    5.50    --   40.61 -99.00 120.00   81
  4  \w     24.00 110.00   1.00   22.00    --  107.07 -94.00 -30.00   86
  5  \w     78.00 178.00   1.00   22.00    --  107.07  61.00  30.00  100
  6  \w     35.00 136.00   1.00   22.00    --  107.07 -61.00-120.00  101
  7  \w     19.00 178.00   1.00   22.00    --  107.07   0.00   0.00  159
  8  \w   -113.00 -12.00   1.00    5.50    --  -40.61 -57.00  90.00  101
  9  \w   -113.00 -12.00   1.00    5.50    --  -40.61 -57.00   0.00  101
 10  \w     54.00 178.00   1.00   22.00    --  107.07  15.00-180.00  124
 11  \w     74.00 178.00   1.00   22.00    --  107.07  77.00-150.00  104
 12  \w     74.00 178.00   1.00   22.00    --  107.07  77.00 -30.00  104
 13  \w     24.00 110.00   1.00   22.00    --  107.07 -94.00 150.00   86
;
_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      0.0035669000
_diffrn_orient_matrix_UB_12      0.0722466000
_diffrn_orient_matrix_UB_13      -0.0525338000
_diffrn_orient_matrix_UB_21      0.0211857000
_diffrn_orient_matrix_UB_22      -0.0698889000
_diffrn_orient_matrix_UB_23      -0.0318689000
_diffrn_orient_matrix_UB_31      -0.0318750000
_diffrn_orient_matrix_UB_32      -0.0384150000
_diffrn_orient_matrix_UB_33      -0.0409780000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47636
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.750
_diffrn_reflns_theta_min         3.808
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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 yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             4960
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         12062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0390P)^2^+15.1315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10887
_reflns_number_total             12062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01691a2.cif
_cod_data_source_block           hasj180903d
_cod_depositor_comments
'Adding full bibliography for 7128228--7128235.cif.'
_cod_database_code               7128228
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N Mg B F Cl'
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.777
_reflns_odcompleteness_completeness 99.88
_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.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C19(H19), C22(H22), C31(H31), C34(H34)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28), C29(H29)
2.d Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C12(H12a,H12b,H12c), C20(H20a,H20b,H20c), C21(H21a,H21b,
 H21c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C32(H32a,H32b,H32c), C33(H33a,
 H33b,H33c), C35(H35a,H35b,H35c), C36(H36a,H36b,H36c)
;
_olex2_date_sample_data_collection 2018-09-03
_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 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.663