Atom economic access to cationic magnesium complexes
Brouillet, Etienne Volcan; Brown, Scott; Kennedy, Alan; Rae, Annabel; Walton, Heather; Robertson, Stuart Duncan; Dalton Transactions  (2023) –; doi:10.1039/D3DT02669H

data_7713887
_publ_section_title
;
 Atom economic access to cationic magnesium complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02669H
_journal_year                    2023
_chemical_formula_moiety         'C25 H31 Al O'
_chemical_formula_sum            'C25 H31 Al O'
_chemical_formula_weight         374.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-06-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-08-15 deposited with the CCDC.	2023-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   14.26750(10)
_cell_length_b                   13.07620(10)
_cell_length_c                   47.5036(2)
_cell_measurement_reflns_used    224879
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.1020
_cell_measurement_theta_min      2.7700
_cell_volume                     8862.49(10)
_computing_cell_refinement       CrysalisPro
_computing_data_collection       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Synergy-i'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            292014
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         73.126
_diffrn_reflns_theta_min         3.506
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.51a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .12
_exptl_crystal_size_min          .03
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         17727
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0745P)^2^+1.9089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.974
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                17374
_reflns_number_total             17727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02669h2.cif
_cod_data_source_block           al(tolyl)3_auto(1)
_cod_database_code               7713887
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(2)
 0.46(2)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C11(H11A,H11B), C13(H13A,H13B), C16(H16A,H16B),
 C18(H18A,H18B), C21(H21A,H21B), C23(H23A,H23B)
3.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C29(H29), C30(H30), C33(H33), C34(H34), C36(H36),
 C37(H37), C40(H40), C41(H41), C43(H43), C44(H44), C47(H47), C48(H48), C50(H50),
  C51(H51), C54(H54), C55(H55), C57(H57), C58(H58), C61(H61), C62(H62),
 C64(H64), C65(H65), C68(H68), C69(H69), C71(H71), C72(H72), C75(H75), C76(H76),
  C78(H78), C79(H79), C82(H82), C83(H83), C85(H85), C86(H86), C89(H89),
 C90(H90), C92(H92), C93(H93), C96(H96), C97(H97), C99(H99), C100(H100),
 C103(H103), C104(H104), C106(H106), C107(H107)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C31(H31A,H31B,H31C), C38(H38A,H38B,H38C), C45(H45A,H45B,H45C), C52(H52A,
 H52B,H52C), C59(H59A,H59B,H59C), C66(H66A,H66B,H66C), C73(H73A,H73B,H73C),
 C80(H80A,H80B,H80C), C87(H87A,H87B,H87C), C94(H94A,H94B,H94C), C101(H10D,H10E,
 H10F), C108(H10A,H10B,H10C)
;
_shelx_res_checksum              70773
_olex2_submission_special_instructions 'No special instructions were received'