Understanding the role of ring strain in β-alkyl migration at Mg and Zn centres.
Parr, Joseph M.; Phanopoulos, Andreas; Vickneswaran, Aaranjah; Crimmin, Mark R.; Chemical science 14 (2023) 1590–1597; doi:10.1039/d2sc06288g

data_1568253
_publ_section_title
;
 Understanding the role of ring strain in &#x3b2;-alkyl migration at Mg
 and Zn centres.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              1590
_journal_page_last               1597
_journal_paper_doi               10.1039/d2sc06288g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C34 H50 N2 Zn'
_chemical_formula_sum            'C34 H50 N2 Zn'
_chemical_formula_weight         552.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-07 deposited with the CCDC.	2023-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0449(2)
_cell_length_b                   16.2449(2)
_cell_length_c                   26.5593(3)
_cell_measurement_reflns_used    16785
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      73.6310
_cell_measurement_theta_min      4.3070
_cell_volume                     6491.17(14)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.988
_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    -72.00  34.00   1.00    3.96    --  -42.36  77.00 -60.00  106
  2  \w    -71.00  30.00   1.00    3.96    --  -42.36  57.00-150.00  101
  3  \w    -71.00  30.00   1.00    3.96    --  -42.36  57.00  90.00  101
  4  \w     30.00 132.00   1.00   10.05    --  105.75 -30.00 -90.00  102
  5  \w     93.00 178.00   1.00   10.05    --  105.75  30.00-120.00   85
  6  \w     65.00 122.00   1.00   10.05    --  105.75-125.00-120.00   57
  7  \w     43.00 109.00   1.00   10.05    --  105.75 -95.00 -30.00   66
  8  \w     33.00 132.00   1.00   10.05    --  105.75 -45.00-180.00   99
  9  \w     29.00 134.00   1.00   10.05    --  105.75 -30.00  60.00  105
 10  \w     30.00 127.00   1.00   10.05    --  105.75 -77.00  60.00   97
;
_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      -0.0643802000
_diffrn_orient_matrix_UB_12      -0.0181980000
_diffrn_orient_matrix_UB_13      -0.0437244000
_diffrn_orient_matrix_UB_21      -0.0574655000
_diffrn_orient_matrix_UB_22      0.0743152000
_diffrn_orient_matrix_UB_23      0.0156162000
_diffrn_orient_matrix_UB_31      0.0549848000
_diffrn_orient_matrix_UB_32      0.0560661000
_diffrn_orient_matrix_UB_33      -0.0348160000
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            36227
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.727
_diffrn_reflns_theta_min         3.328
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83859
_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    1.130
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_preparation       'DippZnH + methylene cyclobutane'
_exptl_crystal_recrystallization_method 'Crystallised from pentane'
_exptl_crystal_size_max          0.0811
_exptl_crystal_size_mid          0.0688
_exptl_crystal_size_min          0.0448
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+3.0368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5624
_reflns_number_total             6480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06288g3.cif
_cod_data_source_block           5b
_cod_depositor_comments
'Adding full bibliography for 1568253--1568256.cif.'
_cod_database_code               1568253
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H50 N2 Zn1'
_chemical_oxdiff_usercomment     AV029
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.909
_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:
 C7(H7), C10(H10), C27(H27), C24(H24), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C22(H22), C21(H21), C4(H4), C5(H5), C3(H3), C20(H20)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C26(H26A,H26B,H26C), C9(H9A,H9B,H9C), C8(H8A,H8B,
 H8C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              2295
_olex2_submission_original_sample_id MRC2228
_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 1.124
_oxdiff_exptl_absorpt_empirical_full_min 0.910