1,3-C-H bond activation on a transient gallium(I)/isocyanate adduct.
Puthiyaveetil, Sruthi S.; Kassymbek, Aishabibi; Dmitrienko, Anton; Pilkington, Melanie; Nikonov, Georgii I.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt03367h

data_7714455
_publ_section_title
;
 1,3-C-H bond activation on a transient gallium(I)/isocyanate adduct.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt03367h
_journal_year                    2023
_chemical_formula_moiety         'C41 H51 Ga N4 O2, 1(C7 H8)'
_chemical_formula_sum            'C47.99 H58.99 Ga N4 O2'
_chemical_formula_weight         793.61
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-08-21 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0810(11)
_cell_length_b                   14.5969(16)
_cell_length_c                   29.227(3)
_cell_measurement_reflns_used    9373
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      28.376
_cell_measurement_theta_min      2.454
_cell_volume                     4300.8(8)
_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      150.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            78002
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.481
_diffrn_reflns_theta_min         1.972
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  0.7421
_exptl_absorpt_correction_T_min  0.6949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1273 before and 0.0820 after correction. The Ratio of minimum to maximum transmission is 0.9364. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_recrystallization_method 'from toluene at -30C in a glovebox'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.096(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         10728
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0362P)^2^+2.3483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                10084
_reflns_number_total             10728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03367h2.cif
_cod_data_source_block           ak186_150k_0m
_cod_database_code               7714455
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.853
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.904(10)
 0.096(10)
2. 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
3. Restrained distances
 C42-C43 \\sim C42A-C43A
 with sigma of 0.02
 C43-C44 \\sim C43A-C44A
 with sigma of 0.02
 C43-C48 \\sim C43A-C48A
 with sigma of 0.02
 C44-C45 \\sim C44A-C45A
 with sigma of 0.02
 C45-C46 \\sim C45A-C46A
 with sigma of 0.02
 C46-C47 \\sim C46A-C47A
 with sigma of 0.02
 C47-C48 \\sim C47A-C48A
 with sigma of 0.02
 C42-C44 \\sim C42A-C44A
 with sigma of 0.04
 C42-C48 \\sim C42A-C48A
 with sigma of 0.04
 C43-C45 \\sim C43A-C45A
 with sigma of 0.04
 C43-C47 \\sim C43A-C47A
 with sigma of 0.04
 C44-C46 \\sim C44A-C46A
 with sigma of 0.04
 C44-C48 \\sim C44A-C48A
 with sigma of 0.04
 C45-C47 \\sim C45A-C47A
 with sigma of 0.04
 C46-C48 \\sim C46A-C48A
 with sigma of 0.04
 C42A-C43A \\sim C42B-C43B
 with sigma of 0.02
 C43A-C44A \\sim C43B-C44B
 with sigma of 0.02
 C43A-C48A \\sim C43B-C48B
 with sigma of 0.02
 C44A-C45A \\sim C44B-C45B
 with sigma of 0.02
 C45A-C46A \\sim C45B-C46B
 with sigma of 0.02
 C46A-C47A \\sim C46B-C47B
 with sigma of 0.02
 C47A-C48A \\sim C47B-C48B
 with sigma of 0.02
 C42A-C44A \\sim C42B-C44B
 with sigma of 0.04
 C42A-C48A \\sim C42B-C48B
 with sigma of 0.04
 C43A-C45A \\sim C43B-C45B
 with sigma of 0.04
 C43A-C47A \\sim C43B-C47B
 with sigma of 0.04
 C44A-C46A \\sim C44B-C46B
 with sigma of 0.04
 C44A-C48A \\sim C44B-C48B
 with sigma of 0.04
 C45A-C47A \\sim C45B-C47B
 with sigma of 0.04
 C46A-C48A \\sim C46B-C48B
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C42) = Uanis(C42A) = Uanis(C43) = Uanis(C43A) = Uanis(C44) = Uanis(C44A)
= Uanis(C45) = Uanis(C45A) = Uanis(C46) = Uanis(C46A) = Uanis(C47) =
Uanis(C47A) = Uanis(C48) = Uanis(C48A)
Uanis(C47B) = Uanis(C42B) = Uanis(C43B) = Uanis(C44B) = Uanis(C48B) =
Uanis(C45B) = Uanis(C46B) = Uanis(C46A) = Uanis(C42A) = Uanis(C43A) =
Uanis(C44A) = Uanis(C48A) = Uanis(C45A) = Uanis(C47A) = Uanis(C46) = Uanis(C42)
= Uanis(C43) = Uanis(C44) = Uanis(C48) = Uanis(C45) = Uanis(C47)
5. Others
 1*[Sof(C42)+Sof(H2A)+Sof(H2B)+Sof(H2C)+Sof(C43)+Sof(C44)+Sof(H4)+Sof(C45)+
 Sof(H5)+Sof(C46)+Sof(H6)+Sof(C47)+Sof(H7)+Sof(C48)+Sof(H8)]+1*[Sof(C42A)+
 Sof(H2AA)+Sof(H2AB)+Sof(H2AC)+Sof(C43A)+Sof(C44A)+Sof(H4A)+Sof(C45A)+Sof(H5A)+
 Sof(C46A)+Sof(H6A)+Sof(C47A)+Sof(H7A)+Sof(C48A)+Sof(H8A)]+1*[Sof(C42B)+
 Sof(H42A)+Sof(H42B)+Sof(H42C)+Sof(C43B)+Sof(C44B)+Sof(H44B)+Sof(C45B)+
 Sof(H45B)+Sof(C46B)+Sof(H46B)+Sof(C47B)+Sof(H47B)+Sof(C48B)+Sof(H48B)]=1 with
 esd of 0.001
 Sof(C42)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C43)=Sof(C44)=Sof(H4)=Sof(C45)=
 Sof(H5)=Sof(C46)=Sof(H6)=Sof(C47)=Sof(H7)=Sof(C48)=Sof(H8)=FVAR(1)
 Sof(C42A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C43A)=Sof(C44A)=Sof(H4A)=
 Sof(C45A)=Sof(H5A)=Sof(C46A)=Sof(H6A)=Sof(C47A)=Sof(H7A)=Sof(C48A)=Sof(H8A)=
 FVAR(2)
 Sof(C42B)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C43B)=Sof(C44B)=Sof(H44B)=
 Sof(C45B)=Sof(H45B)=Sof(C46B)=Sof(H46B)=Sof(C47B)=Sof(H47B)=Sof(C48B)=
 Sof(H48B)=FVAR(3)
6.a Free rotating group:
 C42(C43,C44,C45,C46,C47,C48)
6.b Ternary CH refined with riding coordinates:
 C15(H15), C12(H12), C24(H24), C27(H27)
6.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C41(H41), C21(H21), C31(H31), C35(H35), C39(H39), C38(H38), C34(H34),
 C8(H8B), C10(H10), C20(H20), C22(H22), C40(H40), C3(H3A), C9(H9), C33(H33),
 C32(H32), C44(H4), C45(H5), C46(H6), C47(H7), C48(H8), C44A(H4A), C45A(H5A),
 C46A(H6A), C47A(H7A), C48A(H8A), C44B(H44B), C45B(H45B), C46B(H46B),
 C47B(H47B), C48B(H48B)
6.d Idealised Me refined as rotating group:
 C5(H5B,H5C,H5D), C1(H1A,H1B,H1C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C),
 C16(H16A,H16B,H16C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C25(H25A,H25B,
 H25C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C), C42(H2A,H2B,H2C), C42A(H2AA,
 H2AB,H2AC), C42B(H42A,H42B,H42C)
;
_shelx_res_checksum              71969
_olex2_exptl_crystal_mounting_method
'on a glass microloop covered with Paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'