Facile C–H Bond Activation on a Transient Gallium Imide
Kassymbek, Aishabibi; Spasyuk, Denis M.; Dmitrienko, Anton; Pilkington, Melanie; Nikonov, Georgii I.; Chemical Communications  (2022) –; doi:10.1039/D2CC01857H

data_7130128
_publ_section_title
;
 Facile C--H Bond Activation on a Transient Gallium Imide
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01857H
_journal_year                    2022
_chemical_formula_moiety         'C37 H55 Ga N4 Si'
_chemical_formula_sum            'C37 H55 Ga N4 Si'
_chemical_formula_weight         653.66
_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
_audit_creation_date             2022-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-21 deposited with the CCDC.	2022-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                109.708(3)
_cell_angle_beta                 93.827(3)
_cell_angle_gamma                97.512(3)
_cell_formula_units_Z            4
_cell_length_a                   9.8888(6)
_cell_length_b                   20.6827(13)
_cell_length_c                   21.1123(12)
_cell_measurement_reflns_used    9633
_cell_measurement_temperature    152.11
_cell_measurement_theta_max      30.70
_cell_measurement_theta_min      2.19
_cell_volume                     4001.7(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_temperature      152.11
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            119007
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.060
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1199 before and 0.0685 after correction. The Ratio of minimum to maximum transmission is 0.8949. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       prism
_exptl_crystal_F_000             1400
_exptl_crystal_recrystallization_method 'from toluene at -30C'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         19841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0226P)^2^+3.6776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16693
_reflns_number_total             19841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01857h2.cif
_cod_data_source_block           ak_azpy_152k_0m
_cod_database_code               7130128
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.808
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12A(H12A), C15A(H15A), C24A(H24A), C27A(H27A), C12(H12), C15(H15), C24(H24),
 C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 N4A(H4A), C3A(H3A), C8A(H8A), C9A(H9A), C10A(H10A), C20A(H20A), C21A(H21A),
 C22A(H22A), C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A), C3(H3), C8(H8),
 C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32), C33(H33), C34(H34),
 C35(H35)
2.c Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C5A(H5AA,H5AB,H5AC), C13A(H13A,H13B,H13C), C14A(H14A,
 H14B,H14C), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C25A(H25A,H25B,H25C),
 C26A(H26A,H26B,H26C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C35A(H35A,
 H35B,H35C), C36A(H36A,H36B,H36C), C37A(H37A,H37B,H37C), C3AA(H3AA,H3AB,H3AC),
 C5(H5A,H5B,H5C), C13(H13D,H13E,H13F), C14(H14D,H14E,H14F), C16(H16D,H16E,H16F),
  C17(H17D,H17E,H17F), C25(H25D,H25E,H25F), C26(H26D,H26E,H26F), C29(H29D,H29E,
 H29F), C30(H30A,H30B,H30C), C36(H36D,H36E,H36F), C37(H37D,H37E,H37F), C38(H38A,
 H38B,H38C)
;
_shelx_res_checksum              44243
_shelx_hkl_checksum              462
_shelx_fab_checksum              39035
_olex2_exptl_crystal_mounting_method
'on a glass microloop covered with perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'