Stereoselective Insertion of Cyclopropenes into Mg–Mg Bonds
Rekhroukh, Feriel; Zhang, Linxing; Kong, Richard Y.; White, Andrew J. P.; Crimmin, Mark Richard; Chemical Communications  (2022) –; doi:10.1039/D2CC02931F

data_7130302
_publ_section_title
;
 Stereoselective Insertion of Cyclopropenes into Mg--Mg Bonds
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02931F
_journal_year                    2022
_chemical_formula_moiety         'C90 H102 Mg2 N8, (C5 H12)'
_chemical_formula_sum            'C95 H114 Mg2 N8'
_chemical_formula_weight         1416.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-20 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.506(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.0624(13)
_cell_length_b                   15.1465(4)
_cell_length_c                   25.3866(13)
_cell_measurement_reflns_used    3868
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      72.6750
_cell_measurement_theta_min      4.0700
_cell_volume                     8872.0(9)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.946
_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    -67.00  27.00   1.00   22.95    --  -42.23  77.00-180.00   94
  2  \w    -97.00  -2.00   1.00   22.95    --  -42.23 125.00   0.00   95
  3  \w     76.00 172.00   1.00  100.98    --  105.13 125.00 -60.00   96
  4  \w     79.00 172.00   1.00  100.98    --  105.13 125.00-180.00   93
  5  \w     35.00  61.00   1.00  100.98    --  105.13 -61.00   0.00   26
  6  \w     75.00 128.00   1.00  100.98    --  105.13 -61.00   0.00   53
  7  \w     44.00 136.00   1.00  100.98    --  105.13 -77.00-120.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0597415000
_diffrn_orient_matrix_UB_12      -0.0001304000
_diffrn_orient_matrix_UB_13      -0.0062125000
_diffrn_orient_matrix_UB_21      0.0099361000
_diffrn_orient_matrix_UB_22      0.0958087000
_diffrn_orient_matrix_UB_23      0.0238992000
_diffrn_orient_matrix_UB_31      -0.0280483000
_diffrn_orient_matrix_UB_32      0.0341142000
_diffrn_orient_matrix_UB_33      -0.0667877000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15104
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.439
_diffrn_reflns_theta_min         3.491
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       block
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0694P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5234
_reflns_number_total             8461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02931f3.cif
_cod_data_source_block           4c-DMAP2
_cod_database_code               7130302
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C81 H110 Mg2 N4 O2'
_chemical_oxdiff_usercomment     FR_005
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.833
_reflns_odcompleteness_completeness 98.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C39(H39), C15(H15), C11(H11), C18(H18), C23(H23), C14(H14),
 C40(H40), C34(H34), C12(H12), C43(H43), C42(H42), C5(H5), C13(H13), C32(H32),
 C9(H9), C8(H8), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C29(H29a,H29b,H29c), C27(H27a,H27b,H27c), C36(H36a,H36b,
 H36c), C37(H37a,H37b,H37c), C28(H28a,H28b,H28c), C20(H20a,H20b,H20c), C38(H38a,
 H38b,H38c), C45(H45a,H45b,H45c), C44(H44a,H44b,H44c)
;
_shelx_res_checksum              42954
_shelx_hkl_checksum              22605
_shelx_fab_checksum              95388
_platon_squeeze_void_probe_radius 1.20
_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 1.483
_oxdiff_exptl_absorpt_empirical_full_min 0.813